U.S. patent application number 12/153266 was filed with the patent office on 2008-09-18 for precoat film forming method, idling method of film forming device, loading table structure, film forming device and film forming method.
Invention is credited to Toshio Hasegawa, Satoshi Wakabayashi.
Application Number | 20080226822 12/153266 |
Document ID | / |
Family ID | 26572381 |
Filed Date | 2008-09-18 |
United States Patent
Application |
20080226822 |
Kind Code |
A1 |
Wakabayashi; Satoshi ; et
al. |
September 18, 2008 |
Precoat film forming method, idling method of film forming device,
loading table structure, film forming device and film forming
method
Abstract
The precoat film forming method has the deposition step of
feeding processing gas into the film forming device having the
loading table structure 18 internally which has the loading table
16 for loading the article W to be processed and depositing the
precoat film 22 composed of a TiN film on the surface of the
loading table and the stabilization step of exposing and
stabilizing the precoat film in NH.sub.3 (ammonia) containing gas
by keeping the loading table at a temperature higher than the
temperature at the deposition step. By doing this, the precoat film
is stabilized, thereby even during a period of idling, there is no
need to lower the temperature of the loading table and the
throughput can be improved. Further, the film forming method for
depositing a predetermined film on the surface of the article W to
be processed using high-melting point metallic compound gas and
reducing gas in the processing container 4 which can be evacuated
feeds oxidizing gas into the processing container during or
immediately after the film forming process. By doing this, the
sheet resistance can be greatly prevented from a change with
time.
Inventors: |
Wakabayashi; Satoshi;
(Nirasaki-Shi, JP) ; Hasegawa; Toshio;
(Yamanashi-Ken, JP) |
Correspondence
Address: |
Smith, Grambrell & Russell, LLP;Beveridge, DeGrandi, Weilacher
Young Intellectual Property Group, 1850 M Street, N.W. (Suite 800)
Washington
DC
20036
US
|
Family ID: |
26572381 |
Appl. No.: |
12/153266 |
Filed: |
May 15, 2008 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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11009714 |
Dec 13, 2004 |
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12153266 |
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10400660 |
Mar 28, 2003 |
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11009714 |
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09711900 |
Nov 15, 2000 |
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10400660 |
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Current U.S.
Class: |
427/255.391 |
Current CPC
Class: |
C23C 16/4404 20130101;
C23C 16/34 20130101; C23C 16/56 20130101; C23C 16/4411 20130101;
C23C 16/4581 20130101 |
Class at
Publication: |
427/255.391 |
International
Class: |
C23C 16/08 20060101
C23C016/08 |
Foreign Application Data
Date |
Code |
Application Number |
Nov 17, 1999 |
JP |
1999-327059 |
Jan 13, 2000 |
JP |
2000-4993 |
Claims
1-16. (canceled)
17. A film forming method comprising: a film forming process of
depositing a predetermined film by a thermal CVD on a surface of an
object to be processed using high-melting point metallic compound
gas, and reducing gas in a processing container which can be
evacuated, wherein oxidizing gas is fed into said processing
container during said film forming process.
18. A film forming method according to claim 17, wherein a flow
rate of the oxidizing gas is within a range of 7 to 67% with
respect to a flow rate of the high-melting point metallic compound
gas.
19. A film forming method according to claim 17, wherein the
oxidizing gas is O.sub.2 or H.sub.2O.
20. A film forming method according to claim 17, wherein the
high-melting point metallic compound gas is a TiCl.sub.4 gas, and
the reducing gas is a NH.sub.3 gas.
21. A film forming method comprising, a film forming process of
depositing a predetermined film by a thermal CVD on a surface of an
object to be processed using high-melting point metallic compound
gas and reducing gas in a processing container which can be
evacuated, wherein oxidizing gas is fed into said processing
container immediately after said film forming process under a
condition in which the object to be processed remains in said
processing container.
22. A film forming method according to claim 21, wherein a process
temperature at said film forming process and a process temperature
at a step of feeding the oxidizing gas are the same.
23. A film forming method according to claim 22, wherein a process
time period for the step of feeding the oxidizing gas is within a
range of 5 to 30 seconds.
24. A film forming method according to claim 21, wherein a flow
rate of the oxidizing gas is within a range of 7 to 67% with
respect to a flow rate of the high-melting point metallic compound
gas.
25. A film forming method according to claim 21, wherein the
oxidizing gas is O.sub.2 or H.sub.2O.
26. A film forming method according to claim 21, wherein the
high-melting point metallic compound gas is a TiCl.sub.4 gas, and
the reducing gas is a NH.sub.3 gas.
Description
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a precoat film forming
method, an idling method of a film forming device, a loading table
structure and a film forming device, and a film forming method for
depositing a film of a semiconductor wafer and others.
[0003] 2. Description of the Related Art
[0004] Generally, in manufacture of semiconductor integrated
circuits, film forming and pattern etching are carried out
repeatedly for a silicon substrate such as a semiconductor wafer or
others and many desired elements are formed.
[0005] Meanwhile, for a lower layer of a wiring layer for enabling
wiring between the elements and electric contact of the elements,
for the purpose of suppressing interdiffusion between Si of the
substrate and the wiring material or for the purpose of preventing
peeling from the primary coat, a barrier metal is used. For the
barrier metal, a material having not only a low electric resistance
but also an outstanding corrosion resistance must be used. As a
barrier metal material for satisfying such as request, a TiN film
is especially apt to be used frequently.
[0006] To form a barrier metal of a TiN film, generally a very thin
Ti film is formed by plasma CVD and nitride-treated and then a TiN
film is formed by heat CVD using TiCl.sub.4 and NH.sub.3 gas.
[0007] The process temperature at the time of forming the Ti film
must be controlled particularly strictly so as to highly keep the
film characteristics in the same way as with forming of a general
thin film.
[0008] On the surface of a loading table for loading a
semiconductor wafer, a precoat film composed of a TiN film is
generally formed beforehand for the purpose of holding the thermal
intra-surface uniformity of the wafer and preventing metal
contamination caused by the metallic element included in the
loading table. The precoat film is removed every cleaning inside
the film forming device, so, when it is cleaned, a precoat film is
thinly deposited on the surface of the loading table as a
pretreatment prior to actual forming of a film on the wafer.
[0009] Meanwhile, the precoat film is formed, for example, in a
high temperature zone such as about 680.degree. C. and as mentioned
above, when it formed once, it is used continuously over a long
period of time until the inside of the film forming device is
cleaned next. In this case, when a so-called idling period which is
not used for the film forming process occurs, the temperature is
lowered to a temperature at which the quality of the precoat film
is not changed, for example, about 300 to 500.degree. C. and the
precoat stands by.
[0010] The temperature changing operation and temperature
stabilization operation of the loading table require a lot of time,
so that it is desirable to keep the loading table temperature at
the process temperature of TiN film forming from the viewpoint of
improving the throughput. However, if the loading table is exposed
at a high temperature, for example, about 680.degree. C., the
precoat film is degenerated due to a very small quantity of outer
gas in the processing container and a very small quantity of leak
gas, and the emissivity and transmission factor are changed. After
all, although the temperature is controlled in the same way, heat
is easily radiated from the loading table due to changing of the
emissivity and transmission factor. Thereby, the supply electric
energy is increased and the wafer temperature is apt to become
higher than expected.
[0011] FIG. 5 is a graph showing the condition at this time and it
shows changes of the film quality (specific resistance) when a
precoat film is deposited on the loading table in the film forming
device and a TiN film is immediately formed at a process
temperature of about 680.degree. C. and thereafter, when the
loading table is conditioned at about 680.degree. C. for 17 hours
and then a film is formed. The drawing shows that the specific
resistance of the TiN film after conditioning for 17 hours is
reduced about 50 .mu..OMEGA.cm compared with that before
conditioning. This means that as converted to a wafer temperature,
the temperature after conditioning for 17 hours is higher by about
20.degree. C.
[0012] In view of such a matter, conventionally, during a period of
idling of the film forming device as mentioned above, the
temperature of the loading table is lowered to about 300 to
500.degree. C. and further inert gas such as N.sub.2 gas is fed,
thereby the degeneration of the precoat film causing instability of
the wafer temperature is prevented.
[0013] As a result, the temperature changing operation and
temperature stabilization operation of the loading table require a
lot of time and even if it is intended to restart the film forming
process, a quick process cannot be performed and a large decrease
of the throughput is caused.
[0014] The present invention has been developed to solve the
aforementioned problems effectively by taking notice of them. An
object of the present invention is to provide a precoat film
forming method, a loading structure, and a film forming device for
not requiring to lower the temperature of a loading table even
during a period of idling by stabilizing a precoat film, thereby
improving the throughput.
[0015] Another object of the present invention is to provide an
idling method of a film forming device for feeding predetermined
gas during a period of idling without stabilizing a precoat film,
thereby not requiring decreasing of the temperature of a loading
table even during a period of idling, thereby improving the
throughput.
[0016] On the other hand, there is the following problem imposed
also regarding the film forming method for a semiconductor
wafer.
[0017] Namely, when a film is to be deposited on the surface of a
semiconductor wafer, in order to keep the electric characteristics
of the deposited film uniform, it is necessary to deposit a film in
the same condition always or everyday and maintain the
reproducibility highly. In a semiconductor wafer processing device
represented by a film forming device, even if the same process
conditions are set, the operation condition of the processing
device itself may be varied delicately with various factors, so
that periodically or non-periodically, for example, a film is
deposited on a test semiconductor wafer every morning and the sheet
resistance is measured, and the operation condition of the
processing device at that time is checked.
[0018] Further, also to maintain the electric characteristics of
the semiconductor integrated circuit itself as designed, it is
desirable that a deposited film maintains the sheet resistance
which is a desired value.
[0019] Meanwhile, although it is desirable that the sheet
resistance of a deposited film is always constant ideally,
actually, it is found that according to the process temperature at
film forming time and the conditioning time from film forming to
measurement of the sheet resistance, the sheet resistance itself is
changed greatly and the change with time is large. The cause is
seemed to be that the deposited film is oxidized by H.sub.2O or
O.sub.2 in the atmosphere.
[0020] As a result, even if the sheet resistance of a deposited
film of a test wafer is measured and checked every morning in order
to ascertain the operation condition of the film forming device,
when the time from film forming to measurement is varied with a
day, for example, even when the film forming device itself is
operated under the same condition, the sheet resistance is greatly
shifted and as a result, a problem arises that the film forming
device is adjusted unnecessarily or a reverse case occurs.
[0021] When the sheet resistance itself of a deposited film is
varied with time like this as mentioned above, a problem arises
that it is difficult to manufacture a semiconductor integrated
circuit as designed.
[0022] This respect will be explained hereunder by referring to
FIGS. 6 and 7. FIG. 6 is a graph showing the relationship between
the process temperature at the time of forming a TiN film and the
oxygen (O) concentration in the film after conditioning for three
days in the atmosphere after film forming. FIG. 7 is a graph
showing the process temperature at the time of forming a TiN film
and the change rate of the sheet resistance after conditioning for
three days in the atmosphere after film forming. The graph in FIG.
6 shows that when the process temperature is about 530.degree. C.,
the oxygen concentration after three days is considerably high such
as 4 atms %, while when the process temperature is about
700.degree. C., the oxygen concentration after three days is
considerably low such as 1.5 atms %.
[0023] FIG. 7 shows the ratio of the sheet resistance immediately
after film forming to the sheet resistance three days after the
film is conditioned for three days in the atmosphere, and when the
process temperature is about 530.degree. C., the sheet resistance
after three days is increased to about two times (100%), and when
the process temperature is about 700.degree. C., the sheet
resistance after three days is decreased to about 1.1 times (10%),
and in either case, the change rate is higher than 5% which is a
target, and it is desired to suppress this change rate smaller
early.
[0024] The present invention has been developed to solve the
aforementioned problems effectively by taking notice of them. An
object of the present invention is to provide a film forming method
for suppressing the change with time of the sheet resistance
greatly.
SUMMERY OF THE INVENTION
[0025] The inventors have accomplished the present invention, as a
result of finding that the reason why the change of substance of
precoat TiN film occur is that there is unstable site in a level of
size of molecule and the site react to other atom gradually for a
long time, after their long devotion to research.
[0026] The invention relating to Claim 1 is characterized in that a
film forming device having a loading table for loading an object to
be processed inside has a deposition step of feeding processing gas
inside the film forming device and depositing a precoat TiN film on
the surface of the loading table and a stabilization step of
reducing and stabilizing the precoat film on the loading table by
keeping it at a temperature higher than the temperature at the
deposition step.
[0027] The precoat TiN film can be stabilized by exposing and
annealing in reducing gas like this. By doing this, during a period
of idling the film forming device, there is no need to lower the
temperature of the loading table, and hence the time required for
raising the temperature at start time of film forming on an object
to be processed is not needed, and the throughput can be improved
in correspondence to it.
[0028] The invention relating to Claim 2 is characterized in that
the reducing reaction at the stabilization step is carried out by
exposing the precoat film in NH.sub.3 (ammonia) containing gas.
[0029] The invention relating to Claim 3 is characterized in that
the temperature of the loading table at the stabilization step is
almost the same as the process temperature when the film forming
process is performed for the aforementioned object to be processed
in the film forming device.
[0030] By doing this, after stabilization of the precoat film, the
operation can be moved to the film forming process of the object to
be processed immediately without changing the temperature of the
loading table, so that the throughput can be improved more.
[0031] The invention relating to Claim 4 is characterized in that
in the film forming device, a Ti film or a Ti containing film is
deposited on the object to be processed.
[0032] The invention relating to Claim 5 is characterized in that a
film forming device having a loading table for loading an object to
be processed inside has a deposition step of feeding processing gas
inside the film forming device and depositing a precoat TiN film on
the surface of the loading table and a stabilization step of
oxidizing and stabilizing the precoat film on the loading table by
keeping it at a temperature higher than the temperature at the
deposition step.
[0033] The precoat TiN film can be stabilized by exposing and
annealing in oxidizing gas like this. By doing this, during a
period of idling the film forming device, there is no need to lower
the temperature of the loading table, and hence the time required
for raising the temperature at start time of film forming on an
object to be processed is not needed, and the throughput can be
improved in correspondence to it.
[0034] The invention relating to Claim 6 is characterized in that
the oxidizing reaction at the stabilization step is carried out by
exposing the precoat film in O.sub.2 (oxygen) containing gas or
H.sub.2O (moisture) containing gas.
[0035] The invention relating to Claim 7 is characterized in that
the temperature of the loading table at the stabilization step is
almost the same as the process temperature when the film forming
process is performed for the aforementioned object to be processed
in the film forming device.
[0036] By doing this, after stabilization of the precoat film, the
film forming process of the object to be processed can be performed
immediately without changing the temperature of the loading table,
so that the throughput can be improved more.
[0037] The invention relating to Claim 8 is characterized in that
in the film forming device, a Ti film or a Ti containing film is
deposited on the object to be processed.
[0038] The invention relating to Claim 9 is characterized in that
in an idling method of a film forming device having a loading
stable with a precoat TiN film formed on the surface in a
processing container which can be evacuated so as to form a Ti film
or a TiN film on an object to be processed, NH.sub.3containing gas
is fed into the processing container.
[0039] By doing this, there is no need to stabilize the precoat TiN
film and only by feeding NH.sub.3 containing gas for the idling
period, for example, even when the loading table is kept at the
film forming process temperature, the precoat film can be prevented
from degeneration. Therefore, the time required for raising the
temperature at start time of film forming on an object to be
processed is not needed, and the throughput can be improved in
correspondence to it.
[0040] The invention relating to Claim 10 is characterized in that
the temperature of the loading table is kept at almost the same
temperature as the temperature at the time of the film forming
process which is performed in the processing container.
[0041] The invention relating to Claim 11 is characterized in that
in a film forming device for performing the film forming process
for depositing a Ti film or a Ti containing film on an object to be
processed, a loading table installed in order to load the object to
be processed and a precoat TiN film which is formed on the surface
of the loading table and subjected to the stabilization process are
installed.
[0042] The invention relating to Claim 12 is characterized in that
a film forming device for forming a Ti film or a Ti containing film
on an object to be processed, includes: a processing container
which can be evacuated, gas feed means for feeding necessary
processing gas into the processing container, a loading table
structure having a loading table for loading the object to be
processed, and a precoat Ti film which is formed on a surface of
the loading table and subjected to a stabilization process; and
heating means for heating the object to be processed.
[0043] The invention relating to Claim 13 is characterized in that
a film forming method for performing the film forming process of
depositing a predetermined film on the surface of an object to be
processed using high-melting point metallic compound gas and
reducing gas in a processing container which can be evacuated feeds
oxidizing gas into the processing container during or immediately
after the film forming process.
[0044] By feeding oxidizing gas into the processing container
during or immediately after the film forming process lie this,
oxygen is positively taken into the deposited film or oxygen is
positively taken into the surface of the deposited film, thereby
the deposited film is stabilized on a chemical composition basis
and as a result, the change of the sheet resistance with time can
be suppressed.
[0045] The invention relating to Claim 14 is characterized in that
the aforementioned high-melting point metallic compound gas is
TiCl.sub.4 gas and the aforementioned reducing gas is NH.sub.3
gas.
[0046] The invention relating to Claim 15 is characterized in that
the aforementioned oxidizing gas is O.sub.2 gas.
[0047] The invention relating to Claim 16 is characterized in that
the aforementioned oxidizing gas is H.sub.2O gas.
BRIEF DESCRIPTION OF THE DRAWINGS
[0048] FIG. 1 is a schematic view showing a film forming device to
which the loading table structure and film forming method of the
present invention are applied.
[0049] FIGS. 2A, 2B, and 2C are drawings showing the steps of
forming a precoat film on a loading table using NH.sub.3 gas. FIGS.
2A, 2B, and 2C show the condition before a precoat film is formed,
the condition that a precoat film is formed, and the stabilization
step respectively.
[0050] FIG. 3 is a drawing showing the step of stabilizing a
precoat film on a loading table using O.sub.2 gas.
[0051] FIG. 4 is a graph showing changes of the specific resistance
of a TiN film versus the stabilization annealing time.
[0052] FIG. 5 is a drawing showing changes of the film quality
(specific resistance) when a precoat film is deposited in a film
forming device and a TiN film is formed immediately and thereafter,
when a loading table is conditioned for 17 hours and then a film is
formed.
[0053] FIG. 6 is a graph showing the relationship between the
process temperature at the time of forming a TiN film and the
oxygen (O) concentration in the film after conditioning in the
atmosphere for 3 days after film forming.
[0054] FIG. 7 is a graph showing the process temperature at the
time of forming a TiN film and the change rate of the sheet
resistance after conditioning in the atmosphere for 3 days after
film forming.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0055] The embodiments of the present invention will be explained
hereunder with reference to FIGS. 1 to 4.
[0056] Firstly, the embodiments of a precoat film forming method,
an idling method of a film forming device, a loading table
structure, and a film forming device will be explained with
reference to FIGS. 1 to 4.
[0057] FIG. 1 is a schematic view showing a film forming device
having the loading table structure of the present invention, and
FIGS. 2A to 2C are a step drawing showing the steps of forming and
stabilizing a precoat film on a loading table using NH.sub.3 gas,
and FIG. 3 is a step drawing showing the step of stabilizing a
precoat film on a loading table using O.sub.2 gas.
[0058] In this embodiment, a case that a TiN film is formed by a
film forming device will be explained as an example.
[0059] As shown in the drawing, a film forming device 2 has a
processing container 4 formed in a cylindrical shape using, for
example, stainless steel. In a bottom 6 of the processing container
4, an exhaust vent 8 for exhausting the atmosphere in the container
is formed, and an exhaust system 12 with an evacuation pump 10
installed is connected to the exhaust vent 8, and the processing
container 4 can be internally evacuated uniformly from the
peripheral part of the bottom.
[0060] In the processing container 4, a loading table structure 18
has a support 14 and a circular loading table 16 supported on it is
installed On the circular loading table 16, for example, a
semiconductor wafer W is loaded as an article to be processed.
Concretely, the loading table 16 has a lower table 16A made of
ceramics such as, for example, AlN which is directly supported by
the support 14 and an upper table 16B made of AlN which is joined
to the top thereof. Between the junction surfaces thereof, a
resistance heater 20 is held as a heating means. The lower table
16A and the upper table 16B are joined on the junction surfaces by,
for example, bonding. On the surface of the loading table 16, that
is, on the side of the lower table 16A and the side and top of the
upper table 16B, a stabilized precoat film 22 composed of a TiN
film which is a characteristic of the present invention is formed
overall. The thickness of the precoat film 22 is, for example,
about 1 .mu.m and the film forming and stabilization process will
be described later.
[0061] On the other hand, on the ceiling part of the processing
container 4, a ceiling part 26 where a shower head 24 is
integratedly installed as a gas feed means for feeding necessary
processing gas is air-tightly attached against the side wall of the
container. The shower head 24 is installed opposite to the loading
table 16 so as to cover almost overall the top thereof and a
processing space S is formed between the shower head 24 and the
loading table 16. The shower head 24 introduces various gases into
the processing space S in showers. In an injection surface 28 at
the bottom of the shower head 24, many injection holes 30 for
injecting gas are formed. Inside the shower head 24, a diffusion
plate 34 having many diffusion holes 32 is installed and gas can be
diffused.
[0062] On the upper part of the shower head 24, a gas introduction
port 36 for introducing gas into the head is installed. To the gas
introduction port 36, a feed path 38 for letting gas flow is
connected. To the feed path 38, a plurality of branch pipes 40 are
connected. To each branch pipe 40, as film forming gas, for
example, a TiCl.sub.4 gas source 42 for collecting TiCl.sub.4 gas
and an NH.sub.3 gas source 44 for collecting NH.sub.3 gas and as
inert gas, for example, an N.sub.2 gas source 46 for collecting
N.sub.2 gas and an O.sub.2 gas source 48 for collecting O.sub.2 gas
are connected. Each gas flow rate is controlled by a flow rate
controller installed to each branch pipe, for example, a mass flow
controller 50. Here, a case that each gas at film forming time is
fed in one feed path 38 in a mixed state is indicated. However, the
present invention is not limited to it and a so called post mix gas
transfer configuration that a part of gases or all gases are fed
individually in different paths and mixed in the shower head 24 or
the processing space S may be used. By doing this, reaction
products of TiCl.sub.4 and O.sub.2 can be prevented from adhering
inside the feed path.
[0063] On the side wall of the processing container 4 and the side
wall of the shower head 24, in order to control the temperature of
each side wall, a temperature control jacket 52 for selectively
feeding, for example, a cooled or heated thermal medium as required
is installed respectively. On the side wall of the container, a
gate valve 54 which can be opened or closed air-tightly during
transfer of a wafer is installed. Although not shown in the
drawing, needless to say, a wafer lifter pin for lifting or
lowering a wafer during transfer of the wafer is installed. On the
side wall of the processing container 4, a load lock chamber 74
which can be evacuated is installed so as to be interconnected via
the gate valve 54. In the load lock chamber 74, a multi-joint arm
76 for transferring the wafer W is installed so as to freely
rotate, extend and retract. Also into the load lock chamber 74,
N.sub.2 gas can be fed as required. In place of the load lock
chamber 74, a transfer chamber may be installed, though it is no
particular object. To the load lock chamber 74, a cassette chamber
not shown in the drawing is connected.
[0064] Next, the forming method for a precoat film of the present
invention which is executed using a device structured as mentioned
above will be explained by referring to FIGS. 2A, 2B, 2C, and
3.
[0065] Firstly, the loading table 16 in the processing container 4
is set in the state that no semiconductor wafer W is loaded, and
the processing container 4 is closed. The processing container 4 is
in the state that for example, the cleaning process is performed at
the prestep and unnecessary films are all removed, thereby no
precoat film is adhered to the surface of the loading table 16 as
shown in FIG. 2A, and the material of the loading table 16 is
exposed.
[0066] When the processing container 4 is enclosed, TiCl.sub.4 gas
and NH.sub.3 gas as film forming gas and N.sub.2 gas as carrier gas
are introduced into the processing container 4 from the shower head
24 respectively at a predetermined flow rate. The processing
container 4 is evacuated by the evacuation pump 10 and kept at a
predetermined pressure.
[0067] The loading table 16 at this time is heated and kept at a
predetermined temperature by the resistance heater 20 buried in the
loading table 16. By this thermal CVD operation, on the surface of
the loading table 16, as shown in FIG. 2B, a TiN film is deposited
and a thin precoat film 22 is formed.
[0068] The process conditions at this time are that when the
dimension of the loading table 16 is the 8-inch wafer size, the
flow rate of TiCl.sub.4 gas is about 30 to 50 sccm, and the flow
rate of NH.sub.3 gas is about 400 sccm, and the flow rate of
N.sub.2 gas is about 500 sccm, and the process pressure is about 40
Pa (.apprxeq.300 mTorr), and the process temperature is about
680.degree. C. The process temperature is not limited to it and any
temperature higher than the temperature at which a TiN film can be
formed by the thermal CVD, for example, 400.degree. C. or more may
be acceptable.
[0069] When the deposition step is finished by forming the precoat
film 22 with a thickness of, for example, about 1 .mu.m like this,
the operation is moved to the stabilization step for stabilizing
the precoat film 22 next. At the stabilization step, in order to
stabilize the surface of the TiN precoat film 22 in the imperfect
reaction state by annealing as shown in FIG. 2C, the temperature of
the loading table 16 is raised to a temperature higher by, for
example, about 50.degree. C. than the process temperature at the
time of forming a TiN film, that is, up to about 730.degree. C. The
rise temperture is not limited to 50.degree. C., and any
temperature higher than the TiN film forming temperature is
acceptable, and when the temperature is higher, the stabilization
process can be performed more quickly.
[0070] As annealing gas at this time, NH.sub.3 gas is used, and as
dilution gas, N.sub.2 gas is used. The process conditions at this
time are that the flow rate of NH.sub.3 gas is about 1000 sccm, and
the flow rate of N.sub.2 gas is about 500 sccm, and the process
pressure is about 40 Pa (.apprxeq.300 mTorr) to 1333 Pa
(.apprxeq.10 Torr). When the stabilization process is performed for
a predetermined time, for example, about 2 minutes, unstable atoms
(site) of the surface of the precoat film 22 are reacted with
NH.sub.3 gas and changed to TiN perfectly and enters the stable
state. By doing this, the precoat film stabilization process is
finished.
[0071] Hereafter, it is desirable to load a semiconductor wafer in
the processing container 4 and perform the normal film forming
process, for example, continuously form a TiN film by the thermal
CVD, for example, using TiCl.sub.4 gas and NH.sub.3 gas, for
example, at a process temperature of 680.degree. C. When
semiconductor wafers W to be processed are used up, the precoat
film 22 is chemically stable as mentioned above, so that there is
no need to lower the temperature of the loading table 16 as
conventionally and it is desirable to perform idling in the state
that the temperature is kept at the process temperature, that is,
about 680.degree. C. here until a semiconductor wafer to be
processed next occurs. Therefore, when a semiconductor wafer to be
processed next occurs, since the temperature of the loading table
16 is kept at the process temperature during a period of idling,
the film forming process can be started immediately. Therefore, the
time required for raising the loading table 16 up to the process
temperature can be omitted and the throughput can be improved in
correspondence with it.
[0072] The forming process of the precoat film 22 and stabilization
process thereof as mentioned above are generally performed whenever
the processing container 4 is internally cleaned as mentioned
above.
[0073] Here, although NH.sub.3 containing gas is used at the
stabilization step, O.sub.2 containing gas or H.sub.2O containing
gas may be used in place of it. FIG. 3 is a drawing showing the
condition when the stabilization process is performed using O.sub.2
gas and N.sub.2 gas as O.sub.2 containing gas. The deposition
process is performed as explained in FIG. 2B. At the stabilization
step shown in FIG. 3, O.sub.2 gas is fed in place of NH.sub.3 gas
previously shown in FIG. 2C. In place of N.sub.2 gas as carrier
gas, another inert gas, for example, He, Ne, or Ar may be fed.
[0074] The process conditions at this time are that the flow rate
of O.sub.2 gas is about 200 sccm, and the flow rate of N.sub.2 gas
is about 100 sccm, and the process temperature is about 680.degree.
C., and the process pressure is about 133 Pa (.apprxeq.1 Torr).
[0075] In this case, oxygen is rich in activity, so that the
process temperature at the stabilization step can be set to
680.degree. C. which is the same as the film forming temperature of
the precoat film 22 of a TiN film, accordingly there is no need to
change the temperature of the loading table 16 for stabilization of
the precoat film, and the film forming process can be performed for
a semiconductor wafer immediately after the stabilization process
of the precoat film, and the throughput can be improved more in
correspondence with it.
[0076] By the stabilization process, unstable atoms and molecules
(site) of the surface of the precoat film 22 are reacted with
O.sub.2 gas and changed perfectly to TiO or TiON and enters the
stable state. For stabilization, although depending on the O.sub.2
gas concentration, when the precoat film 22 is 1 .mu.m in
thickness, it is desirable to perform the annealing process at
least for about 2 minutes.
[0077] The process temperature of the stabilization process using
O.sub.2 gas, since O.sub.2 gas is rich in reactivity as mentioned
above, may be lower than the film forming temperature of the TiN
precoat film 22 and for example, the TiN precoat film 22 can be
stabilized, for example, at about 400.degree. C.
[0078] Actually under the aforementioned process conditions, the
stabilization process is performed for a TiN precoat film using
O.sub.2 gas and N.sub.2 gas and evaluated, so that the evaluation
results will be explained by referring to FIG. 4.
[0079] FIG. 4 is a graph showing changes of the specific resistance
of a TiN film versus the stabilization annealing process. Here, for
annealing the precoat film, the stabilization annealing processing
time is variously changed to 0, 2, 4, 6, and 8 minutes, and a TiN
film is actually deposited on a wafer using a loading table with
precoat which is annealed like this, and the specific resistance of
the TiN film on the wafer is measured. As clearly shown in the
graph, when the O.sub.2annealing process is not performed, the
specific resistance is 450 .mu..OMEGA.cm, while when the O.sub.2
annealing process is performed for 2 minutes or more, the specific
resistance is stabilized at almost 400 .mu..OMEGA.cm. Therefore, it
is found that when the O.sub.2 annealing process is performed for 2
minutes or more, the TiN precoat film 22 is chemically
stabilized.
[0080] In the aforementioned respective embodiments, the
stabilization process of chemically stabilizing the TiN precoat 22
beforehand is performed, thereby the precoat film 22 is prevented
from degeneration during idling of the film forming device.
However, the present invention is not limited to it and even if the
stabilization process is not performed as mentioned above, during
idling of the film forming device, by feeding NH.sub.3 containing
gas (pure NH.sub.3 gas is included) continuously in the processing
container 4, the same operation effect as the aforementioned can be
produced.
[0081] Namely, in this case, the stabilization process of the
precoat film as shown in FIG. 2C or 3 is not performed, and during
idling of the device, NH.sub.3 gas and N.sub.2 gas are fed
continuously into the processing container 4, and by doing this,
the TiN precoat film 22 is prevented from degeneration. The gas
flow rate at this time, for example, is about 500 sccm for NH.sub.3
gas and about 500 sccm for N.sub.2 gas. According to this, the
unstable part of the surface of the precoat film 22 is occupied by
NH.sub.3gas, so that the precoat film 22 is not reacted with other
gases. Even in this case, during idling of the device, if the
temperature of the loading table 16 is kept at the same temperature
as the process temperature when a TiN film is formed on a wafer,
for example, 680.degree. C., when it is necessary to form a TiN
film on a wafer, the film forming process can be immediately
performed without changing the temperature of the loading table 16,
so that the throughput can be improved.
[0082] In the aforementioned respective embodiments, the film
forming device is explained using a device for forming a TiN film
on the surface of a semiconductor wafer by the thermal CVD as an
example. However, the present invention is not limited to it and
the present invention can be applied to all film forming devices
for forming a Ti film or a film containing Ti such as TiN. For
example, also to a plasma CVD film forming device for forming a Ti
film by the plasma CVD using, for example, TiCl.sub.4 gas and
H.sub.3 gas, the present invention can be applied.
[0083] As a heating means, also to a device using not only a
resistance heater but also a lamp heater, the present invention can
be applied. Further, an article to be processed is not limited to a
semiconductor wafer and the present invention can be applied also
to a glass substrate and an LCD substrate.
[0084] As explained above, according to the precoat film forming
method, film forming device idling method, loading table structure,
and film forming device of the present invention, the following
outstanding operation effects can be produced.
[0085] According to the inventions relating to Claims 1 and 2, a
precoat film composed of a TiN film can be stabilized by exposing
and annealing in NH.sub.3 containing gas. By doing this, there is
no need to lower the temperature of the loading table during a
period of idling of the film forming device, thereby the time
required for raising the temperature at start time of film forming
for an article to be processed is not required, so that the
throughput can be improved in correspondence with it.
[0086] According to the inventions relating to Claims 5 and 6, a
precoat film composed of a TiN film can be stabilized by exposing
and annealing in O.sub.2 containing gas or H.sub.2O containing gas.
By doing this, there is no need to lower the temperature of the
loading table during a period of idling of the film forming device,
thereby the time required for raising the temperature at start time
of film forming for an article to be processed is not required, so
that the throughput can be improved in correspondence with it.
[0087] According to the inventions relating to Claims 3 and 7, when
the stabilization process is to be performed using O.sub.2
containing gas, H.sub.2O containing gas or NH.sub.3 containing gas,
the temperature is set to almost the same temperature as the
process temperature when the film forming process is performed for
an article to be processed, thereby a precoat film is stabilized,
and then the film forming process for the article to be processed
can be performed immediately without raising the temperature of the
loading table, so that the throughput can be improved more.
[0088] According to the inventions relating to Claims 9 and 10,
there is no need to stabilize a precoat film composed of a TiN
film, and when NH.sub.3 containing gas is just fed during a period
of idling, for example, even if the loading table is kept at the
film forming process temperature, the precoat film can be prevented
from degeneration. Therefore, the time required for raising the
temperature at start time of film forming for an article to be
processed is not required, so that the throughput can be improved
in correspondence with it.
[0089] According to the inventions relating to Claims 11 and 12,
since the precoat film of the loading table is stabilized, there is
no need to lower the temperature of the loading table during a
period of idling of the film forming device, thereby the time
required for raising the temperature at start time of film forming
for an article to be processed is not required, so that the
throughput can be improved in correspondence with it.
[0090] Next, the embodiment of the film forming method relating to
the present invention will be explained.
[0091] Firstly, the load lock chamber 74 is evacuated almost to the
same pressure as that of the processing container 4 which is set in
the vacuum state beforehand and then the gate valve 54 is opened so
as to interconnect the chambers 74 and 4. Then, the multi-joint arm
76 is driven, and an unprocessed semiconductor wafer W in the load
lock chamber 74 is loaded and transferred into the processing
container 4, and it is loaded on the loading table 16.
[0092] When the wafer W is loaded like this, the film forming
process is started. Here, a TiN film is formed by the thermal CVD
using, for example, TiCl.sub.4 gas and NH.sub.3 gas, for example,
at a process temperature of 680.degree. C.
[0093] In this case, N.sub.2 gas may be used as carrier gas. During
the film forming process, as oxidizing gas, for example, O.sub.2
gas and H.sub.2O gas (water vapor) are fed into the processing
container 4 at the same time at a predetermined flow rate
respectively within an unexcessive range, and a deposited film is
formed by partial oxidation. Here, as oxidizing gas, O.sub.2 gas is
used.
[0094] The process conditions at this time, in a case of 8-inch
wafer size, for example, the process pressure is about 40 Pa
(.apprxeq.300 mTorr), and the process temperature is about
680.degree. C., and the flow rate of TiCl.sub.4 gas is about 30
sccm, and the flow rate of NH.sub.3gas is about 400 sccm, and the
flow rate of N.sub.2gas is about 50 sccm, and the flow rate of
O.sub.2gas is about 5 sccm.
[0095] By partial oxidization by O.sub.2 gas in this way, a TiN
film containing TiON molecules is formed in a thickness of about 20
nm (the film forming time is about 50 seconds).
[0096] The sheet resistance of the TiN film containing TiON
molecules is measured immediately after film forming and 3 days
after film forming respectively. The increase rate (change rate) of
the sheet resistance is only about several % and can be suppressed
within 5% which is a target and a satisfactory result can be
obtained.
[0097] Next, the feed amount of O.sub.2 gas is changed variously,
and the same film forming process is performed, and the sheet
resistance is measured. It is desirable to set the feed rate of
O.sub.2 gas within the range from about 7 to 67% (2 to 20 sccm) of
the flow rate of TiCl.sub.4 gas which is raw material gas, more
preferably, within the range from about 17 to 33% (5 to 10
sccm).
[0098] In the aforementioned embodiment, during forming of a TiN
film, O.sub.2 gas is introduced into the processing container 4
together with raw material gas. However, the present invention is
not limited to it and after forming of a TiN film, as a postprocess
under existence of a wafer, oxidizing gas may be fed into the
processing container 4 for a predetermined time. Namely, in this
case, O.sub.2 gas which is oxidizing gas is not fed during forming
of a TiN film and firstly, a TiN film is deposited by the thermal
CVD using the conventional ordinary film forming method. When a TiN
film with a predetermined thickness is formed, the wafer is left in
the current state without being unloaded, and TiCl.sub.4 gas and
NH.sub.3 gas are stopped feeding, and at the same time, as
oxidizing gas, for example, O.sub.2 gas is fed into the processing
container 4 for a predetermined time, and the surface of the TiN
film is oxidized, and a TiON film is formed partially.
[0099] The process conditions in this case, as mentioned above, are
the same as those when O.sub.2 gas is fed during forming of a TiN
film, and it is desirable to keep the process pressure and process
temperature at 40 Pa and 680.degree. C. respectively and set the
flow rate of O.sub.2 gas within the range from 2 to 20 sccm,
preferably within the range from 5 to 10 sccm. The time of the
postprocess may be, for example, within the range from 5 to 30
seconds and when the postprocess is performed for an excessively
long period of time, the TiN film is undesirably oxidized
excessively.
[0100] Even when O.sub.2gas is fed in the postprocess after forming
of the TiN firm like this, the sheet resistance of the TiN film can
be greatly prevented from a change with time and the change of the
sheet resistance can be suppressed to less than 5%.
[0101] In the aforementioned respective embodiments, a case that
O.sub.2 gas is used as oxidizing gas is explained as an example.
The present invention is not limited to it and another oxidizing
gas, for example, H.sub.2O gas (water vapor) may be used.
[0102] Here, a case that a TiN film is deposited as a film
containing a high-melting point metal is explained as an example.
However, the present invention is not limited to it and needless to
say, for example, even when a WN (tungsten nitride) film is to be
deposited, the method of the present invention can be applied to
it.
[0103] Furthermore, here, an example that a semiconductor wafer is
used as an article to be processed is explained. However, the
present invention is not limited to it and the method of the
present invention can be also applied to an LCD substrate, a glass
substrate, and others.
[0104] As explained above, according to the film forming method
relating to Claim 13, when a nitride film containing a high-melting
point metal is to be deposited, a part of it is oxidized and
stabilized by feeding oxidizing gas during or after the film
forming process, thereby the sheet resistance of the deposited film
can be greatly prevented from a change with time.
* * * * *