U.S. patent application number 11/484019 was filed with the patent office on 2007-05-10 for point-of-use mixing method with first derivative homogeneity monitoring.
Invention is credited to Gary R. Anderson, Matt Fowler.
Application Number | 20070106425 11/484019 |
Document ID | / |
Family ID | 37517091 |
Filed Date | 2007-05-10 |
United States Patent
Application |
20070106425 |
Kind Code |
A1 |
Anderson; Gary R. ; et
al. |
May 10, 2007 |
Point-of-use mixing method with first derivative homogeneity
monitoring
Abstract
There is disclosed a system and method of formulating a batch
comprising at least two chemicals. An embodiment is disclosed
wherein a feedforward algorithm can be used to control the target
blend. Subsequently a feedback closed loop control loop algorithm
is provided for a multivariant blend. Use of this approach allows
for a continuously autoreplenished and controlled blend. Also
disclosed is the ability to control via feedforward and feedback
algorithms a fast responding control mode that allows for the
elimination of a container. This approach will allow for "one pass"
blending with control. The controller implements an automated fault
detection and correction system, thereby identifying necessary
maintenance prior to failure. If failure does occur the signature
recognition allows rapid analysis and correction thus maximizing
tool availability.
Inventors: |
Anderson; Gary R.; (Austin,
TX) ; Fowler; Matt; (Austin, TX) |
Correspondence
Address: |
MEYERTONS, HOOD, KIVLIN, KOWERT & GOETZEL, P.C.
700 LAVACA, SUITE 800
AUSTIN
TX
78701
US
|
Family ID: |
37517091 |
Appl. No.: |
11/484019 |
Filed: |
July 10, 2006 |
Related U.S. Patent Documents
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
|
|
11177930 |
Jul 8, 2005 |
|
|
|
11484019 |
Jul 10, 2006 |
|
|
|
Current U.S.
Class: |
700/265 ;
700/285; 702/23 |
Current CPC
Class: |
G05D 11/139 20130101;
G05D 11/133 20130101; B01F 13/1055 20130101; H01L 21/67253
20130101; B01F 15/00207 20130101 |
Class at
Publication: |
700/265 ;
700/285; 702/023 |
International
Class: |
G05B 21/00 20060101
G05B021/00 |
Claims
1. A method of producing a composition, the composition comprising
two or more chemicals, the method comprising: obtaining a total
flow rate for the composition; determining the flow rate for each
chemical, wherein the sum of the flow rates for each chemical
equals the total flow rate, and wherein the flow rate of each
chemical is determined based on a predetermined composition
formulation; initiating flow of each chemical into a mixing area,
wherein each chemical is flowed at the determined flow rate, and
wherein the chemicals are combined in the mixing area to produce
the composition; transferring the composition into an analyzer,
wherein the analyzer is configured to measure the quantity of one
or more chemicals of the composition; determining the homogeneity
of the composition as the composition is flowed through the
analyzer, wherein the homogeneity is determined as a function of an
average deviation of the quantity of one or more chemicals of the
composition with respect to an average quantity of the chemicals of
the composition over a predetermined time period; designating the
composition as properly mixed if one or more chemicals of the
composition is within a predetermined concentration range and if
the homogeneity of the composition is at least at a predetermined
homogeneity value.
2. The method of claim 1, wherein determining the average deviation
comprises: collecting a predetermined number of quantity
measurements for one or more chemicals in the composition over a
predetermined time period; determining the average quantity of one
or more chemicals in the composition for the plurality of
concentration measurements taken over the predetermined time
period; determining, for each measured quantity of one or more
chemicals of the composition, the standard deviation of the
measured quantity with respect to the average quantity; determining
one or more average standard deviation values of one or more of the
chemicals; determining the homogeneity of the composition, wherein
the homogeneity of the composition is a function of one or more
average standard deviations.
3. The method of claim 2, wherein the composition comprises two or
more chemicals, wherein the homogeneity of the composition is a
function of the average standard deviation of two or more
chemicals.
4. The method of claim 1, further comprising transferring the
properly mixed composition to a semiconductor fabrication tool.
5. The method of claim 1, wherein the composition is produced as a
continuously flowing composition.
6. The method of claim 1, wherein the composition comprises an
aqueous solution of one or more chemicals.
7. The method of claim 1, wherein at least one of the chemical is
an inorganic base.
8. The method of claim 1, wherein at least one of the chemicals is
a mineral acid.
9. The method of claim 1, wherein at least one of the chemicals is
hydrogen peroxide.
10. The method of claim 1, wherein at least one analyzer is a
spectral absorption analytical device.
11. The method of claim 1, wherein at least one analyzer is a
conductance measurement device.
12. The method of claim 1, wherein at least one analyzer is a Raman
spectrophotometer.
13. The method of claim 1, wherein the composition, after passing
through the analyzer is passed to a waste drain if one or more of
the chemicals are not within a predetermined quantity range.
14. The method of claim 1, further comprising determining error
correction values if one or more chemicals are not within a
predetermined quantity range.
15. The method of claim 14, wherein determining the flow rate for
each chemical comprises using one or more error correction values
to determine the flow rate, wherein the one or more error
correction values are obtained from previous use of the system.
16. The method of claim 1, further comprising adjusting the flow
rate of one or more chemicals based on the measured quantity of one
or more of the chemicals.
17. The method of claim 1, further comprising adjusting the flow
rate of each of the chemicals if one or more chemicals of the
composition are not within a predetermined quantity range.
18. The method of claim 1, wherein prior to initiating flow of each
chemical into the mixing area, the method further comprises:
sending a zero point control signal from a controller to at least
one chemical dispensing device, wherein the zero point control
signal causes the chemical dispensing device to move to a zero flow
state configuration; detecting if a fluid is flowing through one or
more of the chemical dispensing devices after the chemical
dispensing device receives the zero point control signal, wherein
if fluid flow is detected through one or more of the chemical
dispensing devices, one or more of the chemical dispensing devices
are adjusted until flow of fluid through the one or more chemical
dispensing devices is inhibited.
19. A method of producing a composition, the composition comprising
two or more chemicals, the method comprising: obtaining a total
flow rate for the composition; determining the flow rate for each
chemical, wherein the sum of the flow rates for each chemical
equals the total flow rate, and wherein the flow rate of each
chemical is determined based on a predetermined composition
formulation; initiating flow of each chemical into a mixing area,
wherein each chemical is flowed at the determined flow rate, and
wherein the chemicals are combined in the mixing area to produce
the composition; transferring the composition into an analyzer,
wherein the analyzer is configured to measure the quantity of one
or more chemicals of the composition; determining the homogeneity
of the composition as the composition is flowed through the
analyzer, wherein the homogeneity is determined as a function of an
average change in the quantity of one or more chemicals of the
composition over a predetermined time period; designating the
composition as properly mixed if one or more chemicals of the
composition is within a predetermined concentration range and if
the homogeneity of the composition is at least at a predetermined
homogeneity value.
20. The method of claim 19, wherein determining an average change
in quantity comprises: taking a plurality of quantity measurements
of the composition over a predetermined time period; determining
the change in quantity with respect to time for each quantity
measurement; determining one or more average change in quantity
with respect to time of one or more of the chemicals; determining
the homogeneity of the composition, wherein the homogeneity of the
composition is a function of one or more average changes.
21. The method of claim 20, wherein the composition comprises two
or more chemicals, wherein the homogeneity of the composition is a
function of the average changes of two or more chemicals.
22. The method of claim 19, further comprising transferring the
properly mixed composition to a semiconductor fabrication tool.
23. The method of claim 19, wherein the composition is produced as
a continuously flowing composition.
24. The method of claim 19, wherein the composition comprises an
aqueous solution of one or more chemicals.
25. The method of claim 19, wherein at least one of the chemical is
an inorganic base.
26. The method of claim 19, wherein at least one of the chemicals
is a mineral acid.
27. The method of claim 19, wherein at least one of the chemicals
is hydrogen peroxide.
28. The method of claim 19, wherein at least one analyzer is a
spectral absorption analytical device.
29. The method of claim 19, wherein at least one analyzer is a
conductance measurement device.
30. The method of claim 19, wherein at least one analyzer is a
Raman spectrophotometer.
31. The method of claim 19, wherein the composition, after passing
through the analyzer is passed to a waste drain if one or more of
the chemicals are not within a predetermined quantity range.
32. The method of claim 19, further comprising determining error
correction values if one or more chemicals are not within a
predetermined quantity range.
33. The method of claim 32, wherein determining the flow rate for
each chemical comprises using one or more error correction values
to determine the flow rate, wherein the one or more error
correction values are obtained from previous use of the system.
34. The method of claim 19, further comprising adjusting the flow
rate of one or more chemicals based on the measured quantity of one
or more of the chemicals.
35. The method of claim 19, further comprising adjusting the flow
rate of each of the chemicals if one or more chemicals of the
composition are not within a predetermined quantity range.
36. The method of claim 19, wherein prior to initiating flow of
each chemical into the mixing area, the method further comprises:
sending a zero point control signal from a controller to at least
one chemical dispensing device, wherein the zero point control
signal causes the chemical dispensing device to move to a zero flow
state configuration; detecting if a fluid is flowing through one or
more of the chemical dispensing devices after the chemical
dispensing device receives the zero point control signal, wherein
if fluid flow is detected through one or more of the chemical
dispensing devices, one or more of the chemical dispensing devices
are adjusted until flow of fluid through the one or more chemical
dispensing devices is inhibited.
37. A method of formulating a composition comprising two or more
chemicals, comprising: dispensing at least two chemicals into a
container until the container is filled to a predetermine volume;
determining the homogeneity of the composition while the container
is being filled and/or after the container is filled to the
predetermined volume, wherein the homogeneity is determined as a
function of an average deviation of the quantity of one or more
chemicals of the composition with respect to an average quantity of
the chemicals of the composition over a predetermined time period;
determining the quantity of one or more of the chemicals in the
container after the homogeneity of the mixture is at least at a
predetermined homogeneity value.
38. The method of claim 37, wherein determining the average
deviation comprises: collecting a predetermined number of quantity
measurements for one or more chemicals in the composition over a
predetermined time period; determining the average quantity of one
or more chemicals in the composition for the plurality of quantity
measurements taken over the predetermined time period; determining,
for each measured quantity of one or more chemicals of the
composition, the standard deviation of the measured quantity with
respect to the average quantity; determining one or more average
standard deviation values of one or more of the chemicals;
determining the homogeneity of the composition, wherein the
homogeneity of the composition is a function of one or more average
standard deviations.
39. The method of claim 38, wherein the composition comprises two
or more chemicals, wherein the homogeneity of the composition is a
function of the average standard deviation of two or more
chemicals.
40. The method of claim 37, wherein dispensing the at least two
chemicals into the container until the container is filled to a
predetermine volume comprises: admitting at least two chemicals to
a container until the container is partially filled to a fraction
of the full container volume; determining the homogeneity of the
mixture in the partially filled container; determining the quantity
of each chemical needed to fill the container to the predetermined
volume, wherein the quantity of each chemical is calculated as a
function of the determined quantity of one or more of the chemicals
in the mixture; dispensing the determined quantity of the chemicals
to the container.
41. The method of claim 40, wherein determining the amount of each
chemical needed to fill the container comprises: calculating a
correction factor for at least one of the chemicals, wherein the
correction factor is the ratio of a target quantity to the
determined quantity for at least one of the chemicals in the
partially filled container; calculating the theoretical amount of
each of the chemicals needed to fill the container to a second
fraction of the full container volume by determining the difference
between the desired quantity of chemical in the container when
filled to the second fraction of the full container volume and the
determined quantity of the chemical in the partially filled
container; and calculating the actual amount of each of the
chemicals needed to fill the container to a predetermined volume by
multiplying one or more of the calculated theoretical amounts by
the correction factor.
42. The method of claim 40, wherein determining the amount of each
chemical needed to fill the container comprises: calculating a
correction factor for at least one of the chemicals, wherein the
correction factor is the ratio of a target quantity to the
determined quantity for at least one of the chemicals when
dispensed into a container, wherein the correction factor is
determined prior to formulating the composition; calculating the
theoretical amount of each of the chemicals needed to fill the
container to a second fraction of the full container volume by
determining the difference between the desired quantity of chemical
in the container when filled to the second fraction of the full
container volume and the determined quantity of the chemical in the
partially filled container, and calculating the actual amount of
each of the chemicals needed to fill the container to a
predetermined volume by multiplying one or more of the calculated
theoretical amounts by the correction factor.
43. The method of claim 40, further comprising repeatedly
performing the following until the predetermined volume of the
composition is obtained: determining the amount of each chemical
needed to fill the container to one or more additional fractions of
the full container volume, wherein the amount of each chemical
added for each additional fraction is calculated as a function of
the determined quantity of one or more of the chemicals in the
partially filled container; dispensing the determined amount of the
chemicals into the container.
44. The method of claim 37, wherein if at least a portion of the
composition is removed from the container, the method further
comprises: determining the quantity of one or more of the chemicals
in the remaining composition; determining the volume of chemicals
needed to at least partially refill the container; determining the
amount of each chemical needed to produce the determined volume,
wherein the amount of each chemical is calculated as a function of
the determined quantity of one or more of the chemicals in the
remaining composition; and dispensing the determined amount of the
chemicals into the container.
45. The method of claim 37, wherein determining the quantity of one
or more of the chemicals in the container comprises determining a
weight percentage of one or more of the chemicals.
46. The method of claim 37, wherein one chemical of the composition
is water.
47. The method of claim 37, wherein one chemical of the composition
is an inorganic base.
48. The method of claim 37, wherein one chemical of the composition
is ammonium hydroxide.
49. The method of claim 37, wherein one chemical of the composition
is a mineral acid.
50. The method of claim 37, wherein one chemical of the composition
is hydrogen peroxide.
51. The method of claim 37, wherein the composition comprises a
mixture of ammonium hydroxide, hydrogen peroxide, and water.
52. The method of claim 37, wherein the composition comprises a
mixture of hydrogen chloride, hydrogen peroxide, and water.
53. The method of claim 37, wherein the composition comprises a
mixture of sulfuric acid, hydrogen peroxide, and water.
54. The method of claim 37, wherein the composition comprises a
mixture of ammonium hydroxide, hydrogen fluoride, and water.
55. The method of claim 37, wherein determining a quantity of one
or more of the chemicals in the container comprises determining one
or more spectroscopic properties of the composition.
56. The method of claim 55, wherein at least one of the
spectroscopic properties is Raman spectroscopy.
57. The method of claim 37, wherein determining a quantity of one
or more of the chemicals in the container comprises determining a
conductance of the composition.
58. The method of claim 37, wherein one or more chemicals are
supplied to the container from a bulk chemical storage, the method
further comprising blending one or more of the chemicals with water
prior to dispensing the chemical into the container.
59. The method of claim 37, wherein prior to dispensing at least
two chemicals into the container, the method further comprises:
sending a zero point control signal from a controller to at least
one chemical dispensing device, wherein the zero point control
signal causes the chemical dispensing device to move to a zero flow
state configuration; detecting if a fluid is flowing through one or
more of the chemical dispensing devices after the chemical
dispensing device receives the zero point control signal, wherein
if fluid flow is detected through one or more of the chemical
dispensing devices, one or more of the chemical dispensing devices
are adjusted until flow of fluid through the one or more chemical
dispensing devices is inhibited.
60. The method of claim 37, further comprising transferring the
composition to a semiconductor fabrication tool.
61. A method of formulating a composition comprising two or more
chemicals, comprising: dispensing at least two chemicals into a
container until the container is filled to a predetermine volume;
determining the homogeneity of the composition while the container
is being filled and/or after the container is filled to the
predetermined volume, wherein the homogeneity is determined as a
function of an average change in the quantity of one or more
chemicals of the composition over a predetermined time period;
determining the quantity of one or more of the chemicals in the
container after the homogeneity of the mixture is at least at a
predetermined homogeneity value.
62. The method of claim 61, wherein determining an average change
in quantity comprises: taking a plurality of quantity measurements
of the composition over a predetermined time period; determining
the change in quantity with respect to time for each quantity
measurement; determining one or more average change in quantity
with respect to time of one or more of the chemicals; determining
the homogeneity of the composition, wherein the homogeneity of the
composition is a function of one or more average changes.
63. The method of claim 62, wherein the composition comprises two
or more chemicals, wherein the homogeneity of the composition is a
function of the average change of two or more chemicals.
64. The method of claim 61, wherein dispensing the at least two
chemicals into the container until the container is filled to a
predetermine volume comprises: admitting at least two chemicals to
a container until the container is partially filled to a fraction
of the full container volume; determining the homogeneity of the
mixture in the partially filled container; determining the quantity
of each chemical needed to fill the container to the predetermined
volume, wherein the quantity of each chemical is calculated as a
function of the determined quantity of one or more of the chemicals
in the mixture; dispensing the determined quantity of the chemicals
to the container.
65. The method of claim 64, wherein determining the amount of each
chemical needed to fill the container comprises: calculating a
correction factor for at least one of the chemicals, wherein the
correction factor is the ratio of a target quantity to the
determined quantity for at least one of the chemicals in the
partially filled container; calculating the theoretical amount of
each of the chemicals needed to fill the container to a second
fraction of the full container volume by determining the difference
between the desired quantity of chemical in the container when
filled to the second fraction of the full container volume and the
determined quantity of the chemical in the partially filled
container; and calculating the actual amount of each of the
chemicals needed to fill the container to a predetermined volume by
multiplying one or more of the calculated theoretical amounts by
the correction factor.
66. The method of claim 64, wherein determining the amount of each
chemical needed to fill the container comprises: calculating a
correction factor for at least one of the chemicals, wherein the
correction factor is the ratio of a target quantity to the
determined quantity for at least one of the chemicals when
dispensed into a container, wherein the correction factor is
determined prior to formulating the composition; calculating the
theoretical amount of each of the chemicals needed to fill the
container to a second fraction of the full container volume by
determining the difference between the desired quantity of chemical
in the container when filled to the second fraction of the full
container volume and the determined quantity of the chemical in the
partially filled container; and calculating the actual amount of
each of the chemicals needed to fill the container to a
predetermined volume by multiplying one or more of the calculated
theoretical amounts by the correction factor.
67. The method of claim 64, further comprising repeatedly
performing the following until the predetermined volume of the
composition is obtained: determining the amount of each chemical
needed to fill the container to one or more additional fractions of
the full container volume, wherein the amount of each chemical
added for each additional fraction is calculated as a function of
the determined quantity of one or more of the chemicals in the
partially filled container; dispensing the determined amount of the
chemicals into the container.
68. The method of claim 61, wherein if at least a portion of the
composition is removed from the container, the method further
comprises: determining the quantity of one or more of the chemicals
in the remaining composition; determining the volume of chemicals
needed to at least partially refill the container; determining the
amount of each chemical needed to produce the determined volume,
wherein the amount of each chemical is calculated as a function of
the determined quantity of one or more of the chemicals in the
remaining composition; and dispensing the determined amount of the
chemicals into the container.
69. The method of claim 61, wherein determining the quantity of one
or more of the chemicals in the container comprises determining a
weight percentage of one or more of the chemicals.
70. The method of claim 61, wherein one chemical of the composition
is water.
71. The method of claim 61, wherein one chemical of the composition
is an inorganic base.
72. The method of claim 61, wherein one chemical of the composition
is ammonium hydroxide.
73. The method of claim 61, wherein one chemical of the composition
is a mineral acid.
74. The method of claim 61, wherein one chemical of the composition
is hydrogen peroxide.
75. The method of claim 61, wherein the composition comprises a
mixture of ammonium hydroxide, hydrogen peroxide, and water.
76. The method of claim 61, wherein the composition comprises a
mixture of hydrogen chloride, hydrogen peroxide, and water.
77. The method of claim 61, wherein the composition comprises a
mixture of sulfuric acid, hydrogen peroxide, and water.
78. The method of claim 61, wherein the composition comprises a
mixture of ammonium hydroxide, hydrogen fluoride, and water.
79. The method of claim 61, wherein determining a quantity of one
or more of the chemicals in the container comprises determining one
or more spectroscopic properties of the composition.
80. The method of claim 79, wherein at least one of the
spectroscopic properties is Raman spectroscopy.
81. The method of claim 61, wherein determining a quantity of one
or more of the chemicals in the container comprises determining a
conductance of the composition.
82. The method of claim 61, wherein one or more chemicals are
supplied to the container from a bulk chemical storage, the method
further comprising blending one or more of the chemicals with water
prior to dispensing the chemical into the container.
83. The method of claim 61, wherein prior to dispensing at least
two chemicals into the container, the method further comprises:
sending a zero point control signal from a controller to at least
one chemical dispensing device, wherein the zero point control
signal causes the chemical dispensing device to move to a zero flow
state configuration; detecting if a fluid is flowing through one or
more of the chemical dispensing devices after the chemical
dispensing device receives the zero point control signal, wherein
if fluid flow is detected through one or more of the chemical
dispensing devices, one or more of the chemical dispensing devices
are adjusted until flow of fluid through the one or more chemical
dispensing devices is inhibited.
84. The method of claim 61, further comprising transferring the
composition to a semiconductor fabrication tool.
Description
PRIORITY CLAIM
[0001] This application is a continuation-in-part of U.S. patent
application Ser. No. 11/177,930 entitled "Chemical Mixing
Apparatus, System and Method", filed Jul. 8, 2005, which is
incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates in general to an apparatus,
system and method for mixing chemicals. More particularly the
present invention general relates to such an apparatus, system and
method for mixing chemicals in a precise manner in accordance with
a given formulation.
[0004] 2. Description of the Relevant Art
[0005] This section describes the background of the disclosed
embodiment of the present invention. There is no intention, either
express or implied, that the background art discussed in this
section legally constitutes prior art.
[0006] Currently, many manufacturing processes require the use of
blended chemical compositions to treat parts during different steps
of the process. Historically, these blended compositions have
depended upon the input chemical control devices to achieve the
desired mixture, then the mixture is tested in line for acceptable
use. In some cases, an external analytical instrument or laboratory
is used to confirm the blended mixture. In some other cases, an
in-line test on the product is used.
[0007] While these methods may be successful for some applications
to assure quality of process, they each may employ unwanted and
undesirable delays. If the test fails, draining and refilling the
chemistry subsequent to the test results may be required. This may
result in unacceptable delays, additional costs and additional
cycle time to the manufacturing process in certain
applications.
[0008] It is therefore desirable to have improved methods of
preparing compositions for use in manufacturing processes in an
efficient and highly accurate manner. Such process should be able
to consistently and accurately produce compositions having a
predetermined formulation.
SUMMARY
[0009] An apparatus, systems and methods for mixing chemicals are
disclosed herein. The apparatus, systems and methods disclosed
herein may be applicable to both batch processing of chemical
compositions and point of use or single pass compositions. The
apparatus, systems and methods disclosed herein may be used for
mixing of solids, liquids, gases and combinations thereof.
[0010] In one embodiment, a method of producing a composition, the
composition including two or more chemicals, includes: obtaining a
total flow rate for the composition; determining the flow rate for
each chemical, wherein the sum of the flow rates for each chemical
equals the total flow rate, and wherein the flow rate of each
chemical is determined based on a predetermined composition
formulation; initiating flow of each chemical into a mixing area,
wherein each chemical is flowed at the determined flow rate, and
wherein the chemicals are combined in the mixing area to produce
the composition; transferring the composition into an analyzer,
wherein the analyzer is configured to measure the quantity of one
or more chemicals of the composition; determining the homogeneity
of the composition as the composition is flowed through the
analyzer; and designating the composition as properly mixed if one
or more chemicals of the composition is within a predetermined
concentration range and the homogeneity of the composition is
greater than or equal to a predetermined homogeneity value.
[0011] In another embodiment, a method of formulating a batch,
includes: admitting at least two chemicals to a given size
container to a fraction of the full container volume for a desired
batch; determining the homogeneity of the mixture in the partially
filled container; determining the quantities of each chemical in
the container after the homogeneity of the mixture is greater than
or equal to a predetermined homogeneity value; determining the
quantity of each component needed to fill the container to a
predetermined level; dispending the determined quantities of the
chemicals into the container. The quantity of each component needed
to fill the container to the predetermined level may be calculated
as a function of the determined quantity of one or more chemicals
in the mixture. The above-described methods may also be embodied on
a computer readable medium and in a controller of a chemical mixing
system.
[0012] Homogeneity of a composition or mixture may be determined as
a function of an average variation of the quantity of one or more
components over a predetermined period of time. In one embodiment,
the homogeneity of the composition may be determined from the
average deviation of the quantity of one or more chemicals of the
composition with respect to an average quantity of the chemicals of
the composition over a predetermined time period. Determining the
average deviation includes: collecting a collecting a predetermined
number of quantity measurements for one or more chemicals in the
composition over a predetermined time period; determining the
average quantity of one or more chemicals in the composition for
the plurality of concentration measurements taken over the
predetermined time period; determining, for each measured quantity
of one or more chemicals of the composition, the standard deviation
of the measured quantity with respect to the average quantity;
determining one or more average standard deviation values of one or
more of the chemicals; determining the homogeneity of the
composition, wherein the homogeneity of the composition is a
function of one or more average standard deviations. The
homogeneity of the composition may be determined as a function of
the average standard deviation of a single chemical or of two or
more chemicals.
[0013] In another embodiment, the homogeneity of a composition may
be determined from an average change in concentration of one or
more chemicals of the composition over a predetermined period of
time. Determining the average change in concentration includes:
taking a plurality of quantity measurements of the composition over
a predetermined time period; determining the change in quantity
with respect to time for each quantity measurement; determining one
or more average change in quantity with respect to time of one or
more of the chemicals; determining the homogeneity of the
composition, wherein the homogeneity of the composition is a
function of one or more average changes. In another embodiment, the
homogeneity of a composition may be determined from an average
deviation of one or more chemicals of the composition with respect
to a model concentration of the one or more components of the
composition over a predetermined period of time.
[0014] In another embodiment, a method of forming a composition
includes starting a blending apparatus, wherein the blending
apparatus includes: a container; two or more chemical dispensing
devices, each chemical dispensing device having an input and an
output, each input coupled to a chemical supply and each output
coupled to the container; and a controller coupled to the chemical
dispensing devices. A zero point control signal is then sent from
the controller to at least one of the chemical dispensing devices,
wherein the zero point control signal causes the chemical
dispensing device to move to a zero flow state configuration. After
the chemical dispensing devices receive the zero point control
signal, one or more of the chemical dispensing devise are monitored
for fluid flowing through the chemical dispensing device, wherein
if fluid flow is detected through one or more of the chemical
dispensing devices, one or more of the chemical dispensing devices
are adjusted until flow of fluid through the one or more chemical
dispensing devices is inhibited. Once proper adjustment of one or
more chemical dispensing devices has been achieved, a dispense
control signal is sent to one or more of the chemical dispensing
devices, wherein the dispense control signal causes the chemical
dispensing device to dispense one or more chemicals into the
container. A similar method may be used for a point of use system,
in which the container described above is replaced by a mixer.
[0015] The above-described methods may be used for a variety of
compositions. In some embodiments the composition may be an aqueous
solution of one or more chemicals. Examples of chemicals that may
be used in a composition include inorganic bases, mineral acids,
and peroxides (e.g., hydrogen peroxide).
[0016] A variety of analyzers may be used to determine the quantity
of one or more of the chemicals in a mixture or composition. In
some embodiments, an analyzer may be a spectral absorption
analytical device (e.g., a Raman spectrophotometer). In other
embodiments, an analyzer may be a conductance measurement device.
The term "analyzer" as used herein refers to a single analytical
device or a plurality of analytical devices.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Other objects, features and advantages of the invention will
appear on reading the following description, given as a
non-limiting example, and made with reference to the appended
drawings in which:
[0018] FIG. 1 is a schematic view of a chemical mixing system;
[0019] FIG. 2 is a schematic cross-sectional view of a container
being filled using a fractional fill method;
[0020] FIG. 3 is a flow chart of a fractional fill mixing
method;
[0021] FIGS. 4 and 5 are flow charts of another fractional fill
mixing method;
[0022] FIG. 6 depicts a flow chart of a homogeneity determination
method;
[0023] FIG. 7 depicts a schematic view of an embodiment of a
plurality of chemical dispensing devices;
[0024] FIG. 8 depicts a flow chart of a zero point control
method;
[0025] FIG. 9 is a schematic view of a point of use chemical mixing
system;
[0026] FIG. 10 is a flow chart of a general control method for
mixing chemicals;
[0027] FIG. 11 is a flow chart for a general control method of
mixing chemicals for both batch and continuous applications;
and
[0028] FIG. 12 is a flow chart for automatic fault detection and
control for the chemical mixing system.
[0029] While the invention is susceptible to various modifications
and alternative forms, specific embodiments thereof are shown by
way of example in the drawings and will herein be described in
detail. It should be understood, however, that the drawing and
detailed description thereto are not intended to limit the
invention to the particular form disclosed, but on the contrary,
the intention is to cover all modifications, equivalents and
alternatives falling within the spirit and scope of the present
invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0030] According to certain embodiments, there is provided a system
and method of formulating a composition comprising at least two
chemicals. Chemicals that may be used include, but are not limited
to acids (e.g., inorganic acids, mineral acids, and organic acids),
bases (e.g., inorganic bases and organic bases), and carrier fluids
(e.g., water, alcohols, etc.). Chemicals that may be mixed include
solids, liquids, gases and combinations thereof. Generally, the
chemicals are dispensed into a container to partially fill it. The
quantities of the chemicals in the container are determined, and a
ratio of a target quantity to the determined current quantity for
at least one chemical is calculated. As used herein the "quantity"
of a chemical refers to any of the following measurements of the
chemical: weight, volume, weight percent, volume percent and
concentration. The next quantity of that chemical to be admitted to
the admixture is calculated by multiplying the target quantity by
the calculated ratio to determine a corrected quantity. The
corrected quantity of the chemical is dispensed to the admixture,
and a quantity of another chemical is admitted to the admixture to
adjust the proportion of chemicals to the target formulation. These
steps may be repeated until a desired quantity of a predetermined
composition is produced. Systems and methods for blending chemicals
in this manner are described in U.S. Published Patent Application
2006/0009875 published Jan. 12, 2006 and U.S. patent application
Ser. No. 11/177,930, both of which are incorporated herein by
reference.
[0031] According to certain embodiments, there is provided a
fractional fill mixing apparatus, system and method for mixing
chemicals to form a composition. In one embodiment, the fractional
fill apparatus, system and method includes a container for holding
chemicals, an in-line analytical instrument for measuring the
quantity of one or more chemicals disposed within the container,
and one or more chemical dispensing devices for dispensing
chemicals into the container. A controller is operatively coupled
to one or more of the chemical dispensing devices and the
analytical instrument. The controller further employs a fractional
fill algorithm for dispensing at least two chemicals to the
container to a fraction of the full volume for a desired batch.
[0032] According to certain embodiments of the invention, a
controller executes the fractional fill mixing algorithm to cause
an initial fraction of the total volume of the container to be
filled in the filling sequence. This fractional volume is
recirculated to assure a homogeneous mixture, and the in-line
analytical instrument determines the constituent parts of the
mixture and communicates the information regarding the current
mixture to the controller. The controller executing a fractional
fill mixing algorithm, adjusts the chemical dispensing devices in a
manner that corrects errors between the actual values and the
desired values of the chemicals in the composition in subsequent
fractions or portions of the total volume of the composition. The
resulting composition is the desired mixture and no additional
testing is required for many applications.
[0033] Referring now to the drawings and, more particularly, to
FIG. 1, there is shown a fractional fill mixing apparatus or system
10, which is used to combine two or more chemicals in a tank or
container 12. It should be understood, that while the system
depicted is configured for mixing of liquids, modifications can be
made to such system to allow mixing of solids and gases as well as,
or in combination with liquids. An analyzer or analytical
instrument 14 is configured to measure the quantities of each
chemical in container 12. While only one analyzer is depicted, it
should be understood that a plurality of analytical devices may be
used to perform different types of analytical tests. Chemical
dispensing devices, shown generally at 16, controllably dispense
two or more chemicals into container 12. Chemical dispensing
devices 16 dispense chemicals received from a plurality of chemical
supply inlets, such as first chemical supply inlet 18, second
chemical supply inlet 20, and third chemical supply inlet 22. Each
chemical supply inlet 18, 20, and 22, is coupled to a plurality of
chemical supply sources (e.g., containers containing bulk
chemicals). A manifold 24 receives the plurality of chemicals from
chemical dispensing devices 16. The chemicals then flow from
manifold 24 to container 12.
[0034] As shown in FIG. 2, in use, according to a fractional fill
mixing algorithm, container 12 initially may contain a residual
volume of one or more of the chemicals to be mixed, as indicated by
volLowLev 200. The low volume of container 12 is indicated
generally at 210. According to an embodiment, container 12 is then
fractionally filled through two or more fractional or partial
filling sequences, the volume of each are indicated at 202, 204,
206, and 208, respectively. As indicated in FIG. 2, for example, a
fractional filling sequence generally may include four fractional
filling sequences volFrac1, volFrac2, volFrac3, and volFrac4. It
should be noted that container 12 may have additional volume
capacity above high-volume point 212 (not shown). Thus, high-volume
point 212 indicates the volume that will be achieved when the
fractional fill sequence is complete but not necessarily indicates
the maximum capacity of container 12.
[0035] As shown in FIG. 3, the fractional fill mixing method begins
in block 27. The fractional fill mixing method dispenses at least
two chemicals to container 12 to a fraction of a predetermined
volume of a desired composition to be produced (28). The mixture
may be blended using a mixing device. Blending of the chemicals in
the container is continued until the mixture is determined to be
substantially homogeneous (30). If the mixture is not homogeneous,
blending of the chemicals may be continued until the mixture is
substantially homogeneous. A quantity of each chemical in the
container is then determined (32). The quantities of each chemical
measured in container 12 may be in weight, volume, percent by
weight, percent by volume, or as a concentration. The method then
calculates the ratio of the determined current quantity for at
least one of the chemicals to the target quantity for the desired
composition (34). The method then calculates the next quantity of
at least one chemical needed by multiplying the target quantity of
the chemical by the calculated ratio (34) to determine a corrected
quantity (36). The method then directs one or more of the chemical
dispensing devices 16 to dispense the corrected quantity of one or
more of the chemicals to the admixture in container 12 (38). The
process as shown in blocks 30, 32, 34, 36, and 38 may be repeated
until the container is filled (42) to the desired volume of the
composition. When container 12 is filled to the desired volume of
the composition, the process terminates (44).
[0036] Considering now the method as just described in greater
detail, and with reference to FIG. 2, the method includes
determining a desired fractional filling sequence to be performed.
Specifically, the number of fractional fills, and the quantity of
each fractional fill, is determined by a user. For example, FIG. 2
shows a container 12 that will contain the intermediate admixtures
and, ultimately, the final desired volume of the composition to be
created from the method. FIG. 2 shows a plurality of volume levels
representing successive fractional fill sequences. In the present
example, four fractional filling sequences are to be performed,
however it should be understood that more or less than four
fractional filing sequences may be used. In an embodiment, the
first fractional filling sequence fills container 12 to
approximately 50% of its volume as shown by area 202. This volume
is indicated as volFrac 1. The partial fill volume is equal to 50%
in this example including the residual volume as indicated by
volLowLev 200. The residual volume is the volume of a residual
chemical or composition already present in the container 12 before
the fractional fill method is commenced. There may or may not be a
residual volume, as it depends on the user requirements. The
residual volume of the chemical or composition in container 12
normally includes one or more chemicals that will form part of the
current batch. The second fractional fill fills the container an
additional 25% of volume as indicated by the area 204 where the
volume for this fractional fill is represented by volFrac 2. The
third and fourth fractional volumes, volFrac 3 and volFrac 4
indicated by 206 and 208, respectively, each fill the container an
additional 12.5% until the container is approximately full as
indicated by arrow 212.
[0037] The fractional volumes and percentages just recited are for
example purposes only and could be modified as desired to achieve
various filling sequences as will become apparent to those skilled
in the art. More or less fractional filling sequences may be used
to achieve a desired volume of a predetermined composition. For
example, instead of four fractional filling sequences, three
fractional filling sequences could be used where each fractional
volume sequence could include 33% or one-third of the approximate
container volume.
[0038] The total volume of the composition in container 12,
according to the exemplary fractional filing sequence is
represented by the variable totalVol which equals
(VolLowLev+volFrac 1+volFrac 2+volFrac 3+volFrac 4). totalVol may
also be represented by (chem1TotalVol+chem2TotalVol+diwAddedVol).
chem1TotalVol represents the total volume of the first chemical in
the composition. chem2TotalVol represents the total volume of the
second chemical in the composition. DiwAddedVol represents the
volume of the third chemical, typically deionized water, in the
composition. It should be noted that diwAddedVol represents the
third chemical and normally is deionized water but may be any other
chemical that is desired to be part of the batch. For the sake of
clarity for subsequent examples, the residual volume of the
admixture in container 12 is assumed to be the same chemical as
diwAddedVol, the third chemical of the exemplary batch, so that
when diwAddedVol and VolLowLev are combined, the total volume of
the third chemical results.
[0039] The fractional fill mixing method then begins by filling the
container to the first fractional fill percentage in the sequence.
In our example, this is 50% as represented by VolFrac1 202, as best
shown in FIG. 2. The actual volume of the first chemical to meet
the requirements for the current fractional fill sequence is then
calculated. This volume is represented by chem1FracVol.
chem1FracVol is equal to chem1TotalVolpourUp1Frac where pourUp1Frac
is a fractional fill percentage of the first fill sequence, in the
present example, 50%. chem2FracVol is calculated using a similar
formula.
[0040] Calculation of the total volume of the first chemical must
then be calculated as represented by chem1TotalVol. chem1TotalVol
is defined as chem1Ratiox where x is an intermediate variable. x is
defined as TotalVol/(chem1Ratio+chem2Ratio+diwRatio). chem1Ratio
and chem2Ratio are defined as the ratio of the volume to be filled
for the first and second chemicals, respectively. diwRatio is a
ratio of the volume to be filled for the third chemicals.
[0041] The volume of the third chemical added to VolLowLev to
obtain totalVol is defined as diwAddedVol which equals
(diwRatiox)-VolLowLev.
[0042] The fractional fill mixing method next includes calculating
the target quantity of one chemical based on the target volumetric
blending ratio and the supply concentration of the chemical. The
target quantity of one chemical is referred to as concChem1, which
is defined as
(chem1RatiobulkChem1)/(chem1Ratio+chem2Ratio+diwRatio). Where
chem1Ratio and chem2Ratio and diwRatio represent the ratios of the
volume to be filled for the first, second, and third chemical,
respectively, for the current fractional fill sequence. BulkChem1
represents the supply concentration of the first chemical. The
target quantity of the other chemicals are calculated using similar
formulas where the numerator of the above equation is replaced with
the ratio and concentration of the bulk chemical supply from the
respective chemical being calculated. Now that chem1FracVol has
been calculated, chem2FracVol and diwFracVol are also calculated as
just described.
[0043] At this point in the method for fractional fill mixing
according to one embodiment of the invention, the first fraction is
poured by controller 26 sending a signal to chemical supply control
device 16 to dispense the volume of chemical represented by
chem1FracVol, then to dispense the volume of chemical represented
by chem2FracVol, and finally to dispense the volume of chemical as
represented by diwFracVol. Depending on what type of chemical
supply control device 16 is employed, the controller 26 may drive
the supply control device 16 to dispense the required amount of
chemicals using suitable equipment, such as pumps or gravity feed
dispensing devices for flow controllers or others. For pumps, for
example, the number of strokes of the pump may be conventionally
calculated by the controller 12 and for gravity fed dispensing
devices, the dispensing time may be conventionally calculated by
the controller 12.
[0044] Each chemical is dispensed by chemical control devices 126,
128, and 130 into container 12. In some embodiments, a manifold 24
is used to collect chemicals from each of the chemical control
devices and deliver the chemicals to container 12. In container 12,
blending of the chemicals may occur. Blending may be accomplished
by the process of admitting the chemicals into the container or
using various mechanical means to blend the chemicals together.
After the chemicals have been added to container 12, a portion of
the admixture may be sent to an analyzer to determine the
quantities of one or more of the chemicals in the container. In
some embodiment, determining the quantities includes determining: a
concentration of one or more of the chemicals; a weight percent of
one or more of the chemicals; or a volume percent of one or more of
the chemicals.
[0045] In order to more accurately determine if the quantities of
one or more chemicals that are measured in container 12 are the
true quantities of one or more of the chemicals, a homogeneity
analysis of the composition may be performed. In one embodiment,
the homogeneity of an admixture disposed in container 12 may be
determined as a function of an average variation of the quantity of
one or more chemicals of the admixture over a predetermined time.
When the homogeneity of the admixture reaches a predetermined
minimum value, the admixture may be considered to be homogeneous.
Once the admixture is considered to be homogenous, the quantity of
one or more of the chemicals may be determined and used for the
subsequent calculations.
[0046] Now that the first fractional fill has been admitted to
container 12, subsequent fractional fill sequences must be
calculated and admitted to container 12. To perform the remaining
fractional fill sequences, an ideal chemical fraction, such as
idealChem1Frac, may be calculated. An ideal chemical fraction may
be calculated for each chemical to be admitted to container 12. By
way of example, idealChem1Frac is defined as
(chem1TotalVolpourUp2Frac) where chem1TotalVol represents the total
volume of the first chemical to meet the requirements for the
current fractional fill sequence and pourUp2Frac is the subsequent
fractional fill percentage in the sequence. For example, since this
is the second correction fill sequence, pourUp2Frac in this example
would now be equal to 25%. Other ideal chemical fractions may also
be calculated for each chemical by using a similar formula where
chem1TotalVol is replaced with the total volume of the other
chemical being evaluated.
[0047] Next, the actual volume of each chemical to meet the
requirements for the current fractional fill sequence must be
calculated. By way of example, the actual volume of the first
chemical to meet the requirements for the current fractional fill
sequence is represented by chem1FracVol which is defined as
(idealChem1FracconcChem1)/chem1Val where chem1Val is the measured
quantity or concentration of the first chemical in the batch. A
similar formula may be used to calculate the actual volumes of the
other chemicals to be added to the admixture during this fractal
fill sequence where the theoretical quantity/concentration of the
other chemicals, ideal chemical fractions, and measured
quantities/concentrations may be replaced in the appropriate
portions of the above formula.
[0048] The method further includes calculating the difference
between the ideal and actual volume of the first chemical,
chem1FracDelta. This is calculated by subtracting chem1FracVol from
idealChem1Frac. The same formula is used for the second chemical to
calculate chem2FracDelta using its actual volume to meet the
requirements of the current fractional fill sequence and ideal
chemical fraction.
[0049] The actual volume of the third chemical to meet the
requirements for the current fractional fill sequence may use a
different formula. diwFracVol is equal to
(diwAddedVolpourUp2Frac)+chem1FracDelta+chem2FracDelta where
diwAddedVol is the volume of the third chemical at its VolLowLev to
obtain total volume for the third chemical. This, as discussed
above, assumes that VolLowLev, which represents the residual volume
in the container, is the same chemical as the third chemical.
chem1FracDelta is defined as the difference between the ideal and
actual volume of the first chemical and chem2FracDelta is defined
as the difference between the ideal and actual volume of the second
chemical. Thus, diwFracVol serves to volumetrically fill the
remaining volume for the current fractional fill sequence.
[0050] As previously stated, diwAddedVol represents the volume of
the third chemical added to VolLowLev to obtain total volume.
diwAddedVol is defined as diwRatiox-VolLowLev where x is defined as
(TotalVol/(chem1Ratio+chem2Ratio+diwRatio)). If it is determined
that diwFracVol is negative, diwFracVol is then reduced by
multiplying the first chemical volume to be admitted to the
admixture for the current fractional fill sequence by
((totalVol-VolLowLev)pourUp2Frac)/(chem1FracVol+chem2FracVol). The
volume of the second chemical is also reduced by multiplying it by
the same formula.
[0051] It should be noted that the target quantity of one chemical
represented in percent by weight may be modified as a function of
specific gravity of each chemical in the batch. For example,
concChem1, by example, may be modified as a function of specific
gravity by employing the following replacement formula
(chem1RatiobulkChem1sGravChem1)/((chem1RatiosGravChem1)+(chem2RatiosGravC-
hem2))+(diwRatiosGravChem3) where concChem1 is the target
concentration of the first chemical, chem1Ratio is a ratio of the
volume to be filled for the first chemical. chem2Ratio is a ratio
of the volume to be filled for the second chemical. diwRatio is the
ratio of the volume to be filled for the third chemical. BulkChem1
is the supply concentration of the first chemical. sGravChem1,
sGravChem2, sGravChem3 represent the specific gravity for the
first, second, and third chemicals, respectively.
[0052] It should be noted that the above method may be used with
concentrated bulk chemicals normally having the concentration
measured in percent by weight. Therefore, in the foregoing
examples, the formulas listed hereinabove in conjunction with the
method for performing fractional fill mixing may use percent by
weight concentration as the measure for quantity of the
contemplated chemical in the admixture or from the chemical supply.
Alternatively, in other contemplated examples of embodiments of the
invention not disclosed herein, percent by volume concentration or
other concentration measurement values may be used in some
circumstances depending on the type of analytical instrument 14 in
use.
[0053] Subsequent fractional fill sequences are then calculated and
added to the admixture in container 12 using the same formulas and
methods stated hereinabove for the foregoing examples.
[0054] An alternate control scheme is based on a concentration
correction algorithm. The controller dosing algorithm may be based
on the objective function:
m.sub.ix.sub.n,i+m.sub.i+1x.sub.n,i=x.sub.n*(m.sub.i+m.sub.i+1)
[0055] where m represents the mass; i represents the iteration
index, i.e., an index value representing the fraction being filled;
n represents a component index value; and x is the liquid mass
fraction. Any variable having the * symbol as a superscript
represents a target or desired value. Note that the a symbol
without a component index refers to a value of all components, or
the overall value of that symbol. For example, m.sub.i+1 connotes
the total mass of the fill sequence iteration i+1, whereas
m.sub.n,i+1 implies only the mass component n in fill sequence
iteration i+1. Generalized iteration indices are expressed relative
to the present. For example, V.sub.i indicates the volume in the
system at the end of the last fill iteration--i.e., the present
volume; V.sub.i+1 represents the volume in the next fill sequence
iteration.
[0056] Assuming that the density of the current tank contents and
the density of the mixture about to be dispensed are not vastly
different, the ratio m.sub.i:m.sub.i+1 will be approximately equal
to the ratio of V.sub.i:V.sub.i+1 where V is the volume of the
liquid. Thus, after algebraic manipulation the dosing algorithm is:
x.sub.n,i+1=x.sub.n*+(V.sub.i/V.sub.i+1)(x.sub.n*-x.sub.n,i)
[0057] Using this relationship, the volume of any component needed
to fill the container during a selected iteration of the fill
sequence can be derived as follows. Since: x n , i + 1 = x n * + (
V i / V i + 1 ) .times. ( x n * - x n , i ) = m n , i + 1 / m i + 1
##EQU1## and .times. .times. where ##EQU1.2## m i + 1 = V i + 1
.function. ( n .times. x n , i + 1 .times. d n ) ##EQU1.3## m n , i
+ 1 = x n , s .times. d n .times. V n , i + 1 ##EQU1.4## The volume
of the component may be determined from: V n , i + 1 = x n , i + 1
.times. V i + 1 .function. ( n .times. x n , i + 1 .times. d n ) /
( x n , s .times. d n ) ##EQU2## where x.sub.n,s is the
concentration of the supply source of component n and d.sub.n is
the density of component n.
[0058] The error in at the end of any correction is used to
modulate the "effective concentration" of the supply source of the
components. After each filing sequence, the following error
adaptation is performed to determine a corrected supply source
concentration.
x.sub.n,s(corrected)(x.sub.n/x.sub.n*)*x.sub.n,s(current) The
corrected supply source concentration may be used for subsequent
calculations.
[0059] In one embodiment, the fractional fill mixing apparatus,
system, and method may be used for chemical blending or mixing
concentrated chemicals for use in the manufacture of semiconductor
wafers. Chemicals that may be used to prepare compositions for use
in the manufacture of semiconductor wafers includes, but are not
limited to an oxidizing agent (e.g., H.sub.2O.sub.2), a base (e.g.,
NH.sub.4OH) or an acid (e.g., HCl, H.sub.2SO.sub.4, HF, HNO.sub.3,
H.sub.3COOH). Additionally, compositions for use in the manufacture
of semiconductor wafers include, but is not limited to water or IPA
or another primary chemical constituent. The composition may be
useful for echtant, selectivity, accelerants, suppressants, and
dilute chemicals of interest as examples. Processes that employ
these requirements include as examples cleans, etches, slurries,
polymer removal and electroplating. Some examples of compositions
are provided in Table 1. The column labeled "Label" refers to
common industry nomenclature for the composition. The column "Alt
Label" refers to an alternate designation for the listed
composition. The listing "TEMP" refers to temperature of
composition. Analytical technologies such as those supplied by
spectral absorption or conductance technologies may be employed in
making realtime insitu measurements of these specific compositions.
TABLE-US-00001 TABLE 1 Label Alt. Label Chem 1 Chem 2 Chem 3 SC1
APM NH.sub.4OH H.sub.2O.sub.2 H.sub.2O HF HF TEMP -- SC2 HPM HCl
H.sub.2O.sub.2 H.sub.2O SPM H.sub.2SO.sub.4 H.sub.2O.sub.2 H.sub.2O
BHF NH.sub.4OH HF H.sub.2O
[0060] With reference to FIGS. 4 and 5, there is shown another
embodiment of the present invention which includes a fractional
fill method incorporating self diagnostics. The method of this
embodiment begins at 46 as best shown in FIG. 4. Stored
user-defined parameter values are gathered by the controller 12 for
subsequent use within the fractional fill method (48). These
user-defined parameter values may include the number of fractional
fill sequences to be performed, and the relative fill volume
percentages. The user-defined parameter values may also include
information such as concentration information regarding the bulk
chemicals to be added to the admixture.
[0061] The method calculates the proper volumes of chemicals to be
added to the admixture for the first fractional fill sequence (50).
Those chemicals are then added to the admixture. Feedback from an
analytical instrument, such as analytical instrument 14, provides
the quantity, expressed in a percent by weight, or percent by
volume concentration or other, of each of the chemicals in the
admixture stored in the container 12 for the first fractional fill
sequence (52). A decision is then made whether the method is within
the first fractional fill sequence or the second fractional fill
sequence (54). If this is true, self-diagnostics are then performed
(56).
[0062] As best seen in FIG. 5, self-diagnostics begin at 58. The
method of the example then evaluates whether or not the first
fractional fill sequence was complete (60). If it was complete, the
determination is made whether or not the first fractional sequence
delta values are already stored (62). The first fractional fill
sequence delta values represent the difference between the
theoretical volumes of the chemicals that should be dispensed into
the admixture compared to a revised volume for a chemical that may
be admitted to the admixture due to a variance detected by the
analytical instrument 14.
[0063] If those fractional filled delta values are not already
stored, the controller 26 stores those fractional delta values
(64). The method as executed by controller 26 then determines
whether the second fractional fill sequence is complete (66). If
not, the self-diagnostics method is terminated (74) and the method
then returns to the method as shown in FIG. 4 at 76. If the second
fractional fill sequence has been completed, then the second
fractional fill delta values are captured and the differences
between the first fractional fill delta values and the second
fractional filled delta values are then calculated (68).
[0064] According to this embodiment, if any of the second
fractional fill delta values are greater than or equal to the first
fractional fill delta values (70), then the filling sequence is
stopped and an error message is displayed (72). This result occurs
when the fractional fill method is unable to correct any deviation
in chemical concentration or quantity between the first fractional
fill sequence and the second fractional fill sequence. In other
words, if a deviation or delta is discovered in any of the
chemicals for the first fractional fill and then a corrective
partial fill of chemicals is added in the second fractional fill
sequence, it is assumed that quantity of chemicals will be more
accurate than the first fractional fill. If it is discovered that
the deviation or delta of any of the chemicals did not decrease
between the first fractional fill sequence and the second
fractional fill sequence, the fractional fill method is then deemed
to be unable to complete the creation of the desired batch.
[0065] Referring back to decision box 70 on FIG. 5, if any of the
second fractional fill delta values are not greater than or equal
to the first fractional fill delta values then the self-diagnostics
method terminates (74) and returns to the fractional fill method as
shown on FIG. 4 at 76.
[0066] Referring now to FIG. 4, the method evaluates whether the
blended constituents are on target (78). In other words, the
analytical instrument 14 analyzes the quantity, percent by weight,
percent by volume, concentration or other property of the chemicals
depending on the example in the admixture. If they are not on
target, an error correction is then calculated for the subsequent
fractional fill sequence as described previously (80). The error
correction is then in the calculation of the amount of each
chemical used for the subsequent fractional fill (82). If the
blended constituents are on target, the volumes for each chemical
are then calculated for the subsequent fractional fill sequence
without having any error correction applied (82).
[0067] The method of the present embodiment, as shown in FIG. 4,
then determines if the fourth fraction is complete (84). It should
be understood that if the stored user-defined parameter values call
for less or more than four fractional fill sequences, the method
evaluates whether all of the desired fractional fill sequences have
been completed.
[0068] If the fourth or final fractional fill has been completed,
then the method of the present embodiment terminates (86) where
closed loop control of the admixture in container 12 may begin. The
closed loop control approach may be feedforward or feedback. The
blending may occur via liquid flow controllers, metering pump,
critical orifice or gravimetric such as preweigh or a continuous
drip method as examples. It should be understood that prior to
determining the quantity of chemicals in the mixture at any of the
steps in the above-described method, the homogeneity of the
composition may be determined and such measurements may be delayed
until the composition is determined to be homogeneous.
[0069] In another embodiment, collected analytical data may be used
to control the amount of each chemical added in a feedback loop.
For each chemical of the composition, a target quantity is
predetermined by the user. As the composition is prepared, the
analyzer determines the actual quantity of each chemical of the
composition. The error (E) is represented as the difference between
the target quantity (R) and the measured quantity (B). If the error
is larger than a predetermined set point, the controller takes
appropriate action to modify the metering of the chemicals. In an
embodiment, the controller determines how much to vary the quantity
of each chemical to bring the batch composition within the targeted
range. The change in quantity, can be determined based on the
following equation: quant=gain*error The allowable error range and
the gain parameter are preset for each chemical. This methodology
may be used during a fractional filling method or during a
continuous or point-of use blending method.
[0070] Reliability and accuracy of a blend may be improved by
determining if a composition is homogeneously blended prior to
performing calculations based on measured quantities of one or more
chemicals. Generally data related to the quantity of one or more
chemicals is collected from the analyzer over a period of time. The
variation of the quantity of one or more of the chemicals over the
period of time is measured. Through a variety of statistical
techniques the collected data is analyzed to determine if the
composition is homogeneous. In some embodiments, a numerical value,
known herein as the "homogeneity of the composition" is determined.
The homogeneity number is compared to a predetermined minimum
value. If the homogeneity number is equal to or greater than the
predetermined minimum, the composition is considered to be
homogeneously blended.
[0071] FIG. 6 shows a flow chart showing a general method of
determining the homogeneity of a composition. The method generally
begins at (300) where the user-defined parameters are inputted.
User parameters may include information related to the desired
degree of homogeneity, the chemicals to be analyzed, the time
between measurements, and the number of measurements to be taken
before determining the homogeneity. In alternate embodiments, some
or all of the parameters may be predetermined and pre-programmed
into a controller. Based on the desired degree of homogeneity, a
homogeneity number may be determined (302). This user based
homogeneity number is used to determine if the homogeneity of a
composition matches the user-defined (or pre-defined)
specifications.
[0072] In one embodiment, the homogeneity of a solution may be
determined using a statistical analysis of the quantities of one or
more chemicals as they vary over a period of time. The period of
time and the number of measurements taken over the period of time
may be predetermined by the manufacturer or selected by the user.
In some embodiments, at least 10, at least 20, at least 30, at
least 50 or at least 100 measurements may be taken for the
homogeneity analysis. Measurements may be taken at intervals
ranging from 0.1 seconds to 10 seconds apart. In some embodiments,
measurements may be taken at 1-second intervals. As shown at (304)
the quantity of one or more chemicals is measured at least X-1
times, where X represents the number of measurements based on the
parameters for a homogeneity analysis. After the last measurement
is taken (306), i.e., the measurement corresponding to the Xth
measurement, the homogeneity of the composition is calculated using
the X measurements (308). The resulting measured homogeneity is
compared to the user based homogeneity number (310). If the
measured homogeneity number is greater than or equal to the
user-based homogeneity number, the composition is considered to be
homogeneous (312). If the number is less than the user based
homogeneity number, blending of the composition is continued and a
new homogeneity number is calculated after the next measurement is
taken. The new homogeneity number is based on the last X number of
measurements taken.
[0073] The homogeneity of a composition may be determined based on
one chemical of the composition, or on multiple chemicals of the
composition. In one embodiment, the homogeneity number for each of
the chemicals may be determined and compared to a user homogeneity
number. If the calculated homogeneity number for each chemical is
equal to or greater than the user homogeneity number entered for
each chemical, then the composition may be accepted as
homogeneously mixed. In some embodiments, a user homogeneity number
may be entered for each chemical. Alternatively, a single user
homogeneity number may be entered. To determine if a composition is
homogeneous, each of the chemicals will have to have a homogeneity
number that is equal to or greater than the single user homogeneity
number.
[0074] In one embodiment, the average variation of the quantity of
one or more chemicals is related to the average deviation of the
quantity of one or more chemicals with respect to an average
quantity of the chemicals in the composition. Such an average may
be calculated using a Mahalanobis Distance technique. Generally, an
average deviation may be determined by collecting a predetermined
number of quantity measurements for one or more chemicals in the
composition at predetermined time intervals. An average quantity of
each of the measured chemicals may be determined from the
measurements. For each measured quantity of the chemicals, the
standard deviation of the measured quantity with respect to the
average quantity for the chemical is determined. The resulting
plurality of standard deviations may be averaged to give an average
standard deviation of one or more of the chemicals. The homogeneity
of the composition may then be calculated from the average standard
deviation.
[0075] In some embodiments, the homogeneity of a composition may be
determined based on the measured quantity of a single chemical. The
average quantity (.mu.) of a single chemical is determined from:
.mu. = i = 1 N .times. x i / N ##EQU3## where N is the number of
measurements and where x.sub.i represents the ith quantity
measurement. For each measurement, x.sub.i, the deviation
(.sigma..sub.i) of the measurement from the average quantity (.mu.)
is determined and an average deviation (.sigma..sub.R) is
calculated. The formula representing the average deviation is,
therefore: .sigma. R = 1 N * i = 1 N .times. ( x i - .mu. ) 2
##EQU4##
[0076] The homogeneity number may then be determined based on a
user-defined or manufacturer defined tolerance. The tolerance
represents the allowed statistical variation in the quantity of the
chemical of the composition. In an embodiment, the tolerance is
given as a percent value. The higher the percentage the lower the
allowed statistical variation. Generally, for a normal
distribution, the probability, P, of a data point falling within a
specified number of standard deviations n, of the mean is given in
Table 2 below. TABLE-US-00002 TABLE 2 P n.sub.P 90% 1.64485 95%
1.95996 99% 2.5783
The tolerance of the homogeneity measurement may be entered as a
percentage by a user or may be predefined by the manufacturer. The
tolerance of the homogeneity of the composition may be related to
the n.sub.P value in Table 2 above. Using the obtained tolerance,
the measured homogeneity of a chemical in the composition may be
calculated using the formula: .xi..sub.P=1-n.sub.P*.sigma..sub.R
where .xi..sub.P is the homogeneity number at a tolerance of P,
where n.sub.P is as defined in Table 2, and where .sigma..sub.R is
as calculated above. The measured homogeneity number of the
chemical may be compared to a measured homogeneity number entered
by the user or predefined by the manufacturer. If the measured
homogeneity number is equal to or greater than the user homogeneity
number, the composition may be accepted as homogenously mixed.
[0077] Similar equations may be used for determining the
homogeneity of multiple chemicals. In one embodiment, a composition
homogeneity number may be determined as a function of the average
standard deviation of two or more chemicals in the composition. As
described above, .sigma..sub.R, for each chemical may be
determined. Using the average standard deviation of each chemical,
an average standard deviation of the composition may be determined
using the formula: .sigma. COM = i = 1 m .times. .sigma. R , m 2
##EQU5##
[0078] where .sigma..sub.COM is the average standard deviation of
the composition, m represents the number of chemicals being
analyzed, and .sigma..sub.R,m represents the average standard
deviation of chemical "m." The composition homogeneity number may
be determined using the formula:
.xi..sub.P=1-n.sub.P*.sigma..sub.COM
[0079] The measured composition homogeneity number may be compared
to a measured homogeneity number entered by the user or predefined
by the manufacturer. If the measured homogeneity number is equal to
or greater than the user homogeneity number, the composition may be
accepted as homogenously mixed.
[0080] The use of standard deviations to determine the homogeneity
of a composition relies, in part on the variation of the quantity
of one or more chemicals with respect to an average measured
quantity of one or more of the chemicals. In an alternate
embodiment, the homogeneity of a composition may be determined by
measuring the variation of the quantity of one or more chemicals
over time.
[0081] In some embodiments, the homogeneity of a composition may be
determined based on the change in the measured quantity of a single
chemical over a period of time. In an embodiment, measurements of
at least one chemical are made at predetermined time intervals. For
each measurement, x.sub.i, the change (.delta..sub.i) of the
measurement of the quantity at the beginning of the time and at the
end of the time period is determined and divided by the time
interval, the general formula being:
.delta..sub.i=(x.sub.i-1-x.sub.i)/(t.sub.i-1-t.sub.i)
[0082] An average measured change in the quantity of a chemical
(.delta..sub.R) may then be calculated using the following
equation: .delta. R = 1 / N * i = 1 N .times. .delta. i ##EQU6##
where N is the number of measurements and where .delta..sub.i
represents the ith quantity measurement.
[0083] The homogeneity number may then be determined based on a
user-defined or manufacturer defined tolerance, as described above.
Using the obtained tolerance, the measured homogeneity of a
chemical in the composition may be compared to a measured
homogeneity number entered by the user or predefined by the
manufacturer. If the measured homogeneity number is equal to or
greater than the user homogeneity number, the composition may be
accepted as homogenously mixed.
[0084] Similar equations may be used for determining the
homogeneity of multiple chemicals. In one embodiment, a composition
homogeneity number may be determined as a function of the change in
the measured quantity of two or more chemicals in a composition
over a period of time. As described above, .delta..sub.R, for each
chemical may be determined and calculated. Using the average
measured change in the quantity of each chemical, an average
measured change in the quantity of the measured chemicals of a
composition may be determined using the formula: .delta. COM = i =
1 m .times. .delta. R , m 2 ##EQU7##
[0085] where .delta..sub.COM is the average measured change in
quantity of the measured chemicals of the composition, m represents
the number of chemicals being analyzed, and .delta..sub.R,m
represents the average measured change in quantity of chemical "m."
The measured composition homogeneity number may be compared to a
measured homogeneity number entered by the user or predefined by
the manufacturer. If the measured homogeneity number is equal to or
greater than the user homogeneity number, the composition may be
accepted as homogenously mixed.
[0086] By analyzing the rate of change in a set of measurements
(e.g., as described above), it is possible to determine whether or
not a system has sufficiently converged to equilibrium such that
one may obtain accurate measurements about its state. Furthermore,
by evaluating higher order derivatives of the dataset, one may also
estimate the final value of a changing system by extrapolating
where the first derivative will become near-zero; or the point at
which the system is no longer changing appreciably, and thus would
be sufficiently equilibrated. In this manner, the quantity of one
or more of the chemicals of a composition, when the composition is
homogeneously mixed, may be determined prior to the composition
reaching homogeneity.
[0087] Any unbiased indicator of the derivative of a measurement
signal may be used to detect trending. These could be constants
obtained from linear or curvilinear regression, or any method that
produces an unbiased indicator. Analysis of the change in quantity
for previous mixing of the composition may allow the derivation of
a model of the manner in which the quantity of one or more of the
chemicals changes during mixing. Comparison of the quantity
measurements obtained during subsequent mixing of the chemicals to
the model allows an assessment of the progress of the mixing in the
subsequent composition. In one embodiment, the comparison of actual
measurements to the model may allow a user to determine if
homogeneity has been reached by assessing where the measurement
fall within the model. For example, if the measurements are similar
to measurements in a non-homogeneous region of the model, it may be
assumed that the composition is not homogeneously mixed.
[0088] Considering now the fractional fill mixing apparatus of the
disclosed embodiment in greater detail with reference to FIG. 1, a
process pump 88 may be used to re-circulate the chemicals in
container 12 to achieve homogeneity of the mixture. In some
embodiments, process pump 88 may be an air operated process pump.
Process pump 88 may be air operated to minimize the risk of any
explosions or fires since flammable compounds and chemicals may be
flowing through pump 88. Process pump 88 is coupled in fluid
communication with container 12 via a conduit 90. A maintenance
drain 92 may be coupled to conduit 90 to allow draining operations
from the conduit 90.
[0089] A filter 96 is disposed in-line with pump 88 within the
recirculation line of the fractal fill mixing apparatus 10, and a
conduit 98 connects pump 88 to filter 96. A three-way valve 102
(e.g., an air operated valve) is positioned in conduit 98 between
pump 88 and filter 96 to permit additional fluid (e.g., de-ionized
water) to enter conduit 98 for the purpose of flushing out the
fractional fill mixing apparatus 10. A second three-way valve 100
is also positioned in conduit 98 to permit draining between
batches. Gas may also be introduced into conduit 98 through valve
104. In some embodiments, pressurized gas (e.g., nitrogen, air,
argon, or helium) may be introduced into the fractional fill mixing
apparatus 10 through valve 104. Three-way valve 106 is connected in
fluid communication down stream of the filter 96 to selectively
permit chemicals stored in container 12 to be delivered via a
conduit 124 to a process tool and/or container (not shown) for
utilization of the batch or to be recirculated back to the manifold
via conduit 120. A conduit 108 connects the filter 96 in fluid
communication with the valve 106, and an analytical pump 112. In
some embodiments, pump 112 may be activated to draw at least a
portion of the fluid flowing through conduit 108 into analyzer 14.
A conduit 114 is connected in fluid communication between the
conduit 108 and the pump 112 to allow fluid to be drawn from
conduit 108 to pump 112.
[0090] The analyzer or analytical instrument 14 is connected in
fluid communication with the output of the pump 112 via a conduit
116. The analyzer 14 may be a high precision chemical concentration
monitor. An example of such a device is the SC-1 monitor
manufactured by HORIBA and marketed as model no. CS-131. Other
monitors include, but are not limited to, HORIBA model No. CM-210
for DHF compositions, HORIBA model No. CS-137 for BHF compositions,
HORIBA model No. CS-150 for SPM compositions, and HORIBA model No.
CS-152 for SC2 compositions. The analytical instrument or analyzer
14 is connected in fluid communications with a by-pass
re-circulation conduit 120 via a conduit 118, so that the mixture
is re-circulated through both the analyzer 14 and the by-pass
conduit 120 until the delivery valve 106 is actuated to deliver the
batch to a process tool and/or container via the conduit 124. In
the embodiment depicted, the mixture is re-circulated to container
12 via manifold 24.
[0091] Manifold 24 is connected in fluid communication to the
chemical supply control device generally indicated at 16 via three
conduits 132, 134 and 136. Chemical supply control device 16
includes three independent chemical control devices 126, 128 and
130. Each control device is capable of accurately dispensing
chemicals from a bulk supply (not shown) into the manifold 24.
Chemical control devices 126, 128 and 130 are each independently
fed from chemical supply tubes 18, 20, and 22, respectively.
Manifold 24 is connected in fluid communication with container 12
via conduit 122.
[0092] Chemical control devices 126, 128, 130 may be any number of
control devices known in the art, including, but not limited to,
pumps, gravity feed systems, flow controllers, etc. Examples of
metering pumps that could be used include pumps that are driven by
dry reed contact closures and are characterized by CC (volume) per
stroke such as contact closure cycle. Further details regarding
chemical control devices may be found in U.S. patent application
Ser. No. 11/177,930.
[0093] FIG. 7 depicts a detailed view of an embodiment of chemical
control devices 126, 128 and 130. In this embodiment, the
ingredient control devices include two liquid flow controllers (126
and 128) for ingredients 1 and 2. Ingredient 3, in this embodiment,
is deionized water, but could also be any other ingredient suitable
for formulating the desired composition. Ingredient 3 is dispensed
gravimetrically from tank 130. Tank 130 is kept filled with at
least some water. In some embodiments, pre-blending of one or more
chemicals may be desired before dispensing the chemicals into
container 12. For example, it is known that HF is more difficult to
blend homogenously with water than other chemicals. By pre-blending
HF with water prior to dispensing into container 12, the
homogeneity of the composition may be reached in less time than if
no pre-blending was performed. In other embodiments, the bulk
chemical supply may be a concentrated source of a chemical.
Pre-blending of a chemical may allow the concentration of the
chemical entering the container to be lowered, allowing more
accurate measurements of the dispensing of the chemical.
[0094] In one embodiment, pre-blending of the composition may be
accomplished by adding an additional dispense line 135 to the
ingredient control devices. In the depicted embodiment, water from
chemical dispense device 130 may be added via conduit 135 to
conduit 133. Conduit 133 is used to dispense one of the chemical
used to form the mixture. The combination of chemical from chemical
control device 128 and water from chemical control device 130 may
be passed to a mixer 137, where pre-blending of the chemical and
water may be accomplished. The pre-blended chemical may be passed
to manifold 24 and forwarded to container 12 for further blending.
It should be understood that pre-blending may be accomplished
between any number of chemicals is not intended to be restricted to
blending of chemicals with solvent. Additionally, it should be
understood that mixer 137 is not required. Pre-blending may occur
by simply having the dispense conduits of two or more chemicals
converge upstream of manifold 24.
[0095] The accuracy of the dispensing of the chemicals for the
mixture relies, in part, in accurate zero point control of the
chemical control devices. Zero point control refers to placing the
controller in a state in which no flow of chemical is detected from
the control device. During use, a controller may be given a zero
point control signal. In response to a zero point control signal,
the chemical control device may alter its configuration to halt or
inhibit flow of the chemical through the control device. In some
embodiments, a chemical control device may not properly close,
allowing some chemical flow through the device, even though the
zero point control signal was received. In such a situation, the
actual amount of chemical flowing through the chemical control
device may be greater than the amount of chemical that is assumed
to be flowing through the control device.
[0096] FIG. 8 depicts a flow chart of a method of zero point flow
control for a chemical control device. The method begins at (350),
when a zero point control signal is sent to one or more chemical
control devices. Each of the chemical control devices, upon receipt
of the zero point control signal, will adjust the internal
configuration to stop or inhibit flow of the chemical. In some
embodiments, the adjustment may include altering the position of a
valve to stop or inhibit the flow of fluid. In other embodiments,
one or more pumps associated with the chemical control device may
be stopped. After the chemical control device has received the
control signal, the flow of chemicals from the one or more chemical
control devices is monitored (352). If the chemical control devices
have accurately reset into a zero state, the monitored flow of
chemical through the chemical control device should be
substantially zero. Under such situations, the device may be
certified as being properly reset to a zero state and the mixing
process begun (354).
[0097] If a detectable amount of chemical is flowing through one or
more of the chemical control devices, the controller may send a
warning indication to a user that the controllers are not
functioning properly. In response, the chemical control device may
be adjusted such that flow of the chemical through the chemical
control device may be inhibited (356). One or more reset signals
may also be sent to one or more of the chemical control devices.
The reset signals may cause one or more of the chemical control
devices to reset into a default position. The default position may
be a position which inhibits flow of the chemical. Alternatively,
the indication of improper functioning of one or more chemical
control devices to the user, may prompt the user to perform
maintenance on one or more of the chemical control devices. Such
maintenance may include manually adjusting the position of one or
more valves such that the zero state of the chemical control device
inhibits the flow of fluid through the device. After maintenance
and adjustment of the chemical control device has been performed,
the zero state of the chemical control device may be retested to
ensure proper functioning. If the retesting of the device shows
proper operation of the device, the device may be certified as
being properly reset to a zero state and the mixing process begun
(354).
[0098] In operation and with reference to FIG. 1, the controller 26
receives a series of composition parameters that describe the
desired quantities of each chemical to be blended together in
container 12. Controller 26 then performs a first fractional fill
sequence as previously described. Controller 26 sends commands to
the chemical supply control device 16 to dispense the proper amount
of chemicals for the first fractional fill. When this occurs,
chemical control devices 126, 128 and 130 begin accurately
dispensing chemicals from their respective bulk chemical supplies
(not shown) via conduits 18, 20 and 22, respectively. Each chemical
is then dispensed into manifold 24 through conduits 132, 134, and
136. The chemicals are partially mixed in manifold 24 and then
supplied to container 12 through conduit 122. After the first
fractional fill sequence is complete, the analyzer 14 is enabled to
measure the quantity of each of the chemical constituents in the
mixture formed in container 12.
[0099] To accomplish this, pump 88 is activated to re-circulate the
mixture from the container 12, which causes the mixture stored in
container 12 to flow through the conduits 90 and 98 through the
filter 96 and through the conduit 108. During this operation, the
maintenance drain valve 92 and chemical delivery valve 106 are
closed. Three-way valves 100, 102 and 104 are set in a position to
allow free flow of fluid through conduit 98, while inhibiting flow
of other fluids into conduit 98. The mixture from container 12 then
continues to flow through the by-pass conduit 120 through the
manifold 24 and back into the container 12. In this regard, the
mixture stored in container 12 is circulated through the various
conduits to mix the mixture to create a more homogeneous mixture
before the analytical instrument 14 measures its concentration. The
analytical pump 112 is then enabled to pump some of the admixture
from the conduit 108 through the conduit 114, through the pump 112,
and through the analytical instrument 14 where the quantity of
chemicals in the mixture may be measured. The mixture then exits
the analytical instrument 14 via the conduit 118 to join the
mixture flowing through conduit 120.
[0100] For subsequent fractional fill sequences, the same general
method as just described is performed again. In the present
example, before subsequent fractional fill sequences are performed,
the process pump 88 and analytical pump 112 are both disabled,
although for other applications they may not be disabled.
Subsequent to the completion of all the fractional fill sequences
or at other times, the bath temperature controller 170 may be
enabled to control the heater 150 to heat the mixture in container
12 to a predetermined temperature. This may be required for some
mixtures for subsequent use in a manufacturing process or other
process or purpose.
[0101] After all of the fractional fill sequences are complete, it
may be desired for some applications to transfer the mixture stored
in the container 12 to a process tool and/or container for
subsequent use. That may be accomplished by first ensuring that the
maintenance drain 92 is closed. Three-way valves 100, 102 and 104
are set in a position to allow free flow of fluid through conduit
98, while inhibiting flow of other fluids into conduit 98. For
dispensing of the composition, the valve 106 is now positioned to
allow flow of the composition out of the mixing system and inhibits
recirculation of the composition through conduit 120: Process pump
88 is then enabled to pump the composition from container 12
through the conduit 90, the pump 88, the conduit 98, the filter 96
and through conduit 108. Because valve 106 is now open, the
composition then flows through valve 106 and through the conduit
124 where it is delivered to the process tool, container, or other
destination.
[0102] A reclaim drain three-way valve 140 is disposed between
conduits, 138 and 142, so that when reclaimed drain valve 140 is
open, recycled composition may be reclaimed into container 12
through conduits 138, 142, and through valve 140. It should be
noted that in all other operations of the fractional fill mixing
system 10, reclaim drain valve 140 is normally closed. A Flush
Drain cycle may be used which includes: opening drain valve 100 and
opening a fluid flush valve 102 and running the process pump 88.
This will result in simultaneously draining the container and
flushing the entire system including the manifold 24 and analyzer
14 with a cleaning fluid (e.g., water). This state remains for a
designated parameter time. Turning off flush valve 102 completes
the Flush Drain cycle. Nitrogen or some other inert gas (e.g.,
helium, argon, etc.) is introduced to force the container and
associated plumbing to be drained of the cleaning fluid. The drain
process continues until the container reaches a pre-determined low
level of fluid. A system error may be indicated if a predetermined
maximum drain time is exceeded. Drain valve 100 and gas valve 104
are closed after the process is completed. This would complete a
Flush Drain Cycle and the apparatus would be ready for one or more
fill cycles. Several fill cycles may be used to fill container 12.
The intent of separating the fill cycles is to achieve a full
container with the desired blended chemistry as soon as possible.
The fractions are variable that can be adjusted to optimize the
time to blend ready.
[0103] In operation, controller 26 communicates to the bath
temperature controller 170 through a serial communications line 160
(e.g., under the RS485 protocol). Likewise, controller 26 may also
communicate to the chemical supply control device 16 and its
individual chemical control devices 126, 128 and 130 through
communication line 188 (e.g., a digital serial line or through an
analog signal source). Further details regarding the controller and
electronic interfaces may be found in U.S. Published Patent
Application 2006/0009875 published Jan. 12, 2006 and U.S. patent
application Ser. No. 11/177,930.
[0104] FIG. 9 depicts a schematic diagram of a system for point of
use chemical mixing of chemicals. Referring now to the drawings
and, more particularly, to FIG. 9, there is shown a point of use
mixing apparatus or system 11, which is used to mix two or more
chemicals in a mixing area 13. An analyzer or analytical instrument
14 is configured to measure the quantities of each chemical flowing
from the mixing area. A chemical supply control device shown
generally at 16, controllably dispenses two or more chemicals into
the mixing area 13. The chemical supply control device 16 dispenses
chemicals through a plurality of chemical supply inlets, as has
been previously discussed. Each chemical supply inlet is connected
in fluid communication with a plurality of chemical supplies (not
shown). A manifold 24 receives the plurality of chemicals from
chemical supply control devices. The chemicals then flow from
manifold 24 to the mixing area 13. The chemicals are blended and
passed from the mixing area for analysis and eventual dispensing.
It should be understood that a manifold differs from a container or
tank. A manifold is configured to receive chemicals from one or
more chemical sources and transmit the chemicals to an attached
conduit. Chemicals have little or no residence time in the manifold
and are rapidly transferred to the conduit.
[0105] Considering now the point of use chemical mixing system of
the disclosed embodiment in greater detail with reference to FIG.
9, a process pump 88 may be used to re-circulate the chemicals
through the system to achieve homogeneity of the mixture. In some
embodiments process pump 88 may be an air operated process pump.
Process pump 88 may be air operated to minimize the risk of any
explosions or fires since flammable compounds and chemicals may be
flowing through pump 88. Process pump 88 is coupled in fluid
communication with mixer 13 via a conduit 90. A maintenance drain
92 may be coupled to conduit 90 to allow draining operations from
the conduit 90.
[0106] A filter 96 is disposed in-line with pump 88 within the
recirculation line of the point of use mixing apparatus 11, and a
conduit 98 connects pump 88 to filter 96. A three-way valve 102
(e.g., an air operated valve) is positioned in conduit 98 between
pump 88 and filter 96 to permit additional fluid (e.g., de-ionized
water) to enter conduit 98 for the purpose of flushing out the
point of use mixing apparatus 10. A second three-way valve 100 is
also positioned in conduit 98 to permit draining of the
composition. Gas may also be introduced into conduit 98 through
valve 104. In some embodiments, pressurized gas (e.g., nitrogen,
air, argon, or helium) may be introduced into the fractional fill
mixing apparatus 10 through valve 104.
[0107] Three-way valve 106 is connected in fluid communication
downstream of the filter 96 to selectively permit the composition
to be delivered via a conduit 124 to a process tool and/or
container for utilization of the composition or to be recirculated
back to manifold 24 via conduit 120. Recirculation to manifold 24
allows mixing of the composition with additional chemicals being
introduced into the system. By recirculation the composition to the
manifold, enhanced mixing may be achieved due to the mixing forces
created by entry of the composition into the manifold. A conduit
108 connects the filter 96 in fluid communication with the valve
106, and an analytical pump 112. In some embodiments, pump 112 may
be activated to draw at least a portion of the fluid flowing
through conduit 108 into analyzer 14. A conduit 114 is connected in
fluid communication between the conduit 108 and the pump 112 to
allow fluid to be drawn from conduit 108 to pump 112.
[0108] The analyzer or analytical instrument 14 is connected in
fluid communication with the output of the pump 112 via a conduit
116. The analyzer 14 may be a high precision chemical concentration
monitor. An example of such a device is the SC-1 monitor
manufactured by HORIBA and marketed as model no. CS-131. Other
monitors include, but are not limited to, HORIBA model No. CM-210
for DHF compositions, HORIBA model No. CS-137 for BHF compositions,
HORIBA model No. CS-150 for SPM compositions, and HORIBA model No.
CS-152 for SC2 compositions. The analytical instrument or analyzer
14 is connected in fluid communications with a by-pass
re-circulation conduit 120 via a conduit 118, so that the mixture
is re-circulated through both the analyzer 14 and the by-pass
conduit 120 until the delivery valve 106 is actuated to deliver the
batch to a process tool and/or container via the conduit 124. In
the embodiment depicted, the mixture is re-circulated to mixer 13
via manifold 24.
[0109] Manifold 24 is connected in fluid communication to the
chemical supply control device generally indicated at 16 via three
conduits 132, 134 and 136. Chemical supply control device 16
includes three independent chemical control devices 126, 128 and
130. Each control device is capable of accurately dispensing
chemicals from a bulk supply (not shown) into the manifold 24.
Chemical control devices 126, 128 and 130 are each independently
fed from chemical supply tubes 18, 20, and 22, respectively.
Manifold 24 is connected in fluid communication with container 12
via conduit 122. A pre-blending chemical dispensing system, as
described with respect to FIG. 7, may also be used in a
point-of-use blending system.
[0110] Chemical control devices 126, 128, 130 may be any number of
control devices known in the art, including, but not limited to,
pumps, gravity feed systems, flow controllers, etc. Examples of
metering pumps that could be used include pumps that are driven by
dry reed contact closures and are characterized by CC (volume) per
stroke such as contact closure cycle. Further details regarding
chemical control devices may be found in U.S. patent application
Ser. No. 11/177,930.
[0111] Referring now to FIG. 10, a single control algorithm may be
applied by user selectable methods for either batch or point of use
processing. Since the control action is the same, the method
employed is situational and user dependent. The control algorithm
provides the user with gain and dead band control so that the user
can optimize the control action appropriate to the users'
situation. The algorithm also contains a variable, which holds the
error correction value for each chemical control device to be used
for each blend sequence. This variable is updated, as required,
based on the analytical feedback delta to desired blend, either in
the continuous mode, or the periodic testing mode. A standard SISO
control is applied to each chemical and a user-defined delay is
applied between actions to allow time for the analytical to provide
feedback and see the effect of each action upon the multi-variant
chemicals. As the fluid level in the container becomes vanishing
small the control and blending shrink to a small volume for mixing
the desired blend. This allows a faster response time to provide
process flexibility and tool versatility because blends can be
provided at the point of use with the decision to make blend
changes while the composition is in use.
[0112] Turning to FIG. 10, the process begins at 700. User defined
parameters are initially collected by the controller (701). These
parameters include the chemical ratios for each chemical of the
composition. Alternatively, parameters for commonly used
compositions may be preset into the controller, in which case the
user selects which of the preset compositions are to be made. Also
input initially is information collected by one or more analytical
instruments (702) during previous chemical blends. Data collected
by analytical instruments during previous chemical blends may be
used to modify the control parameters for subsequent runs.
[0113] After the parameters have been obtained, the controller
determines the appropriate dispensing quantity for each chemical of
the composition to produce the desired composition. For batch
processing the controller determines the amount of each chemical
that is to be dispensed into a container, as discussed previously.
For point of use processing, the flow rate of each chemical is
calculated. The flow rate of each chemical may be calculated using
a feed-forward algorithm based on the total flow rate desired, the
supply composition and the target composition. Analytical
measurements received during previous use of the mixing system may
be used to provide error correction values.
[0114] In a feed forward algorithm, for a point of use mixing
process, the total flow of the process stream is typically a
user-selected parameter. The total flow of the process stream is
the sum of the flow of each chemical being added to the mixing
area, as represented by the equation:
TotalFlow=chem1Flow+chem2Flow+diwFlow It should be noted that while
the above equation is directed to a composition that includes two
chemicals and deionized water, the same general equation would
apply for more or less than three chemicals.
[0115] The mixing method next includes calculating the target
quantity of one chemical based on the user supplied blending ratio
and the supply concentration of the chemical (703). The target
quantity of one chemical is referred to as chem1Targ, which is
defined as (chem1RatiobulkChem1)/(chem1Ratio+chem2Ratio+diwRatio).
Where chem1Ratio and chem2Ratio and diwRatio represent the ratios
of the volume to be filled for the first, second, and third
chemical, respectively, for the current sequence. These values are
either preset into the controller or are defined by the user at
start-up of the process. BulkChem1 represents the supply
concentration of the first chemical. The target quantity of the
other chemicals are calculated using similar formulas where the
numerator of the above equation is replaced with the ratio and
concentration of the bulk chemical supply from the respective
chemical being calculated. chem2Targ and diwTarg are also
calculated as just described.
[0116] After determining the target quantity of each chemical, the
flow rate of each chemical is determined using the following
equations: Chem1Flow=(chem1Targ/bulkChem1)*totalFlow
Chem2Flow=(chem2Targ/bulkChem2)*totalFlow The above equations
assume that the specific gravity of each chemical and the final
composition is 1. If the specific gravity is not equal to one, the
following equations are used:
Chem1Flow=(chem1Targ*totalFlow*sGravPosite)/(bulkChem1*sGravChem1)
Chem2Flow=(chem2Targ*totalFlow*sGravPosite)/(bulkChem1*sGravChem2)
where sGravPosite is the specific gravity of the blended
composition stream. SgravChem1 and sGravChem2 are the specific
gravity of chemical 1 and chemical 2, respectively. The total flow
of the third chemical, in this case deionized water, is determined
from the following equation.
DiwFlow=totalFlow-chem1Flow-chem2Flow
[0117] The flow rate may also be modified based on one or more
correction values that have been stored based on previous use of
the mixing system. The stored error correction values (704) may be
used to modify the flow rates according to the following equations:
Chem1FlowCorrected=Chem1Flow*ErrorCorr1 Where ErrorCorr1 an error
correction value determined from the analytical results of the
process. This value would be 1 if no error correction is needed.
The value can be calculated from the equation:
ErrorCorr1=Chem1Targ/Chem1Measured Where Chem1Measured is the
amount of chemical 1 measured in the produced composition. A
similar correction value can be determined and used for chemical
2.
[0118] In one embodiment, flow of each chemical of the composition
is controlled by metering pumps. The metering pumps may be operated
using voltage control to control the flow rate at which the
chemical is supplied. The following equations may be used to
determine a voltage applied to the metering pump to achieve the
calculated flow rate. chem1Dac=(chem1Flow/chem1RangeFS)*DAC_SIG_FS
chem2Dac=(chem2Flow/chem2RangeFS)*DAC_SIG_FS
diwDac=(diwFlow/diwRangeFS)*DAC_SIG_FS where chem1RangeFS,
chem2RangeFS and diwRangeFS represent the maximum flow rate of the
pump coupled to the respective chemical supply sources and
DAC_SIG_FS represents the voltage applied to achieve the maximum
flow rate.
[0119] After determining the process parameters, the chemical
supply control devices are operated to begin producing a
composition stream. The composition stream passes into an analyzer
where the quantity of each chemical is determined. The composition
is then checked for homogeneity (706). If the composition is not
homogeneous, then the composition is placed into a recirculation
mode (705). The composition is then recirculated until the
composition is homogeneously blended.
[0120] After the composition has reached homogeneity, the analyzer
determines the quantity of one or more chemicals of the
composition. The analyzer provides analytical feedback (707) to the
controller regarding the quantity of the chemicals in the
composition. The controller also analyzes the collected data to
determine if the chemicals are within a target range (711). In one
embodiment, if the chemicals are not within the target range an
error correction value, calculated as described above, is
determined and stored. The error correction value may be used to
alter the flow rate of each of the chemicals to bring the blended
composition to the target formulation.
[0121] In another embodiment, the collected analytical data may be
used to control the pumping parameters in a feedback loop. For each
chemical of the composition, a target concentration is
predetermined by the user. As the composition is prepared, the
analyzer determines the actual concentration of each chemical of
the composition. The error (E) is represented as the difference
between the target concentration (R) and the measured concentration
(B). If the error is larger than a predetermined set point, the
controller takes appropriate action to modify the metering of the
chemicals. In an embodiment, metering of the chemicals may be
controlled by modifying the voltage applied to one or more metering
pumps. The change in voltage, can be determined based on the
following equation:
.DELTA.M=(100/PB)*(((.DELTA.t/T.sub.R)*E.sub.N)+.DELTA.E) where
.DELTA.M is the change (increase or decrease) in the DAC voltage
(scaled by chemRange/10 v); PB is the Proportional Band (classical
definition); T.sub.R is the reset time (seconds); .DELTA.t is the
scan time (seconds); E.sub.N is the current error; and .DELTA.E is
the change in error since the last scan. The parameters PB and
T.sub.R are preset for each chemical.
[0122] The cycle is then looped through until the chemicals are
within a target range (711). Upon completion of the process, the
cycle is terminated (710) and the chemicals dispensed.
[0123] In some embodiments, a recycle loop may be used to recycle
the process stream back to the mixing area if the process stream
does not meet the predetermined composition formulation.
Alternatively, the composition may be directed to a drain where the
composition is disposed of or reused in another process, if the
composition formulation is out of a predetermined range. One
advantage of using a combination of a feed forward and feedback
control system is that the amount of composition that is produced
is minimized. This is due in part to the quick response time of the
system. Additionally, the storage or error correction values helps
the system create a composition that is close to the desired
formulation when the process is initiated. By minimizing the amount
of non-usable composition, a recirculation system may not be
required. By eliminating recirculation of the composition, the
system may be more responsive to user needs to modify the
composition formulation during use of the system.
[0124] In an embodiment, a controller may be configured to control
both point of use and batch processing methods. The system may
include a combination of mixing areas and batch storage containers
to allow multiple uses of the system. A general control method is
presented in FIG. 11. Initiation of the process begins (800) and
data regarding the specific parameters of the process are collected
from the controller memory and the user. Information that is
collected includes information regarding the type of device used to
dispense each of the chemicals of the composition (802). Examples
of dispensing methods include, but are not limited to liquid flow
controllers, metering pumps, gravimetric dispensers, critical
orifice dispensing and continuous flow.
[0125] After gathering the information regarding the system and
user parameters, the type of process is chosen (801). The process
choices, in some embodiments include bulk chemical dispense (803),
point of use small container (804) and point of use--single pass
(805). The bulk chemical dispense may be represented by a
non-resident large volume container. A point of use small container
may be a container that is resident on a process tool.
[0126] If either of the container options (803 or 804) are chosen,
a fractional fill controlling scheme may be used (806). In some
embodiments, a replenishment cycle is followed in which the
container is replenished as the composition is used. This
replenishment cycle is followed while chemistry is recirculated
(807) and determination is made as to whether the container is full
(808) and continues under the initial fill (817) until the
fractional filling is complete.
[0127] Once the container is filled, confirmation of the blended
target (809) is achieved and confirmed. If the target is not
achieved, the blend may be discarded into a drain (816). In the
case of a tank or container approach, recirculation may continue
(807) until the feedback closed loop control scheme (815) achieves
the desired target concentration.
[0128] In addition to blending to target (809) an additional
requirement may be the homogeneity of the blend (810). If this is
confirmed (810) then the blend may be released to process (811). If
the mixture does not meet the homogeneity requirements, a point of
use single pass blend is sent to a drain, or a tank/container batch
would be recirculated until homogeneity is achieved.
[0129] Process indicators (812) include, but are not limited to,
endpoint detection, metrology or parametric values determined
during the fabrication process. This feedback may be used to
provide stored data for feed forward control (814) as well as for
adjustment of feedback closed loop control (813).
[0130] In an embodiment, a controller includes an automatic
detection and correction of fault system. A flow chart of an
automatic detection and correction of fault system is shown in FIG.
12. Prior to any blend all inputs 902 are analyzed to ensure that
the normal "state" exists for any chemical or subassembly 901. The
state or functioning of many components are analyzed prior to
initializing the process. Examples of components of the blending
system that are analyzed include: pressure of various fluid
dispensing systems; temperature of the system at various positions;
proper functioning of the analytical equipment; flow signals; and
proper I/O received from components.
[0131] These conditions are then analyzed for signature failures
903 that either prevent blending 904 or allow an automatic
correction strategy to be implemented 907. If the error is not
correctable 905 or the error cannot be eliminated 908, a flag is
provided to require maintenance 906. In any case an internal data
log is generated to allow fast response for maintenance repair and
the tool and fab automation are informed 910. After the initial
blend cycle, subsequent blending also receives information via
feedback from process which can come from the tool or APC
(Automated Process Control) or from the various sensors present in
the blending module 911.
[0132] All analyses disclosed herein are not limited to any one
analytical approach. Absorption Spectroscopy which includes these
classifications UV/VIS, NIR, MidIR, RAMAN as well as analytical
instruments that provide output such as conductivity, refractive
index, ultrasonic form a subset of the analytical approaches that
could be used to analyze compositions.
[0133] In this patent, certain U.S. patents, U.S. patent
applications, and other materials (e.g., articles) have been
incorporated by reference. The text of such U.S. patents, U.S.
patent applications, and other materials is, however, only
incorporated by reference to the extent that no conflict exists
between such text and the other statements and drawings set forth
herein. In the event of such conflict, then any such conflicting
text in such incorporated by reference U.S. patents, U.S. patent
applications, and other materials is specifically not incorporated
by reference in this patent.
[0134] Further modifications and alternative embodiments of various
aspects of the invention may be apparent to those skilled in the
art in view of this description. Accordingly, this description is
to be construed as illustrative only and is for the purpose of
teaching those skilled in the art the general manner of carrying
out the invention. It is to be understood that the forms of the
invention shown and described herein are to be taken as the
presently preferred embodiments. Elements and materials may be
substituted for those illustrated and described herein, parts and
processes may be reversed, and certain features of the invention
may be utilized independently, all as would be apparent to one
skilled in the art after having the benefit of this description to
the invention. Changes may be made in the elements described herein
without departing from the spirit and scope of the invention as
described in the following claims. In addition, it is to be
understood that features described herein independently may, in
certain embodiments, be combined.
* * * * *