U.S. patent number 3,603,284 [Application Number 05/000,344] was granted by the patent office on 1971-09-07 for vapor deposition apparatus.
This patent grant is currently assigned to International Business Machines Corporation. Invention is credited to Richard R. Garnache.
United States Patent |
3,603,284 |
Garnache |
September 7, 1971 |
VAPOR DEPOSITION APPARATUS
Abstract
A vapor deposition reactor having a gaseous phase inlet and exit
system including inlet means, located at one end of a reaction
chamber, including a porous gas distribution baffle which forms a
plenum and which uniformly delivers gaseous materials to
substantially all of the horizontal cross-sectional area of the
reaction chamber and further including an exit means, located at
the other end of the chamber, comprising a porous pressure baffle
for uniformly allowing the removal of gaseous materials from the
chamber to prevent recirculation of reaction byproducts.
Inventors: |
Garnache; Richard R. (South
Burlington, VT) |
Assignee: |
International Business Machines
Corporation (Armonk, NY)
|
Family
ID: |
21691104 |
Appl.
No.: |
05/000,344 |
Filed: |
January 2, 1970 |
Current U.S.
Class: |
118/725;
118/730 |
Current CPC
Class: |
C30B
25/08 (20130101); C23C 16/4588 (20130101); C30B
25/14 (20130101) |
Current International
Class: |
C30B
25/08 (20060101); C23C 16/458 (20060101); C30B
25/14 (20060101); C23c 011/00 () |
Field of
Search: |
;118/48-49.5
;117/16-17.2R,17.2P,16R,16A ;148/174,175 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Kaplan; Morris
Claims
What is claimed is:
1. Apparatus for performing vapor transport processes on substrate
surfaces utilizing gaseous phase materials, comprising:
a reaction chamber having a longitudinal axis;
a substrate holder for maintaining substrate surfaces substantially
parallel to said longitudinal axis;
heating means for uniformly heating substrate surfaces to the
reaction temperature;
gaseous phase inlet means located at one end of said chamber
comprising: a gas distribution baffle, forming a plenum, said
baffle extending substantially throughout the cross-sectional area
of said chamber, said baffle capable of providing sufficient gas
resistance to develop substantially uniform back pressure across
said baffle, and said baffle also capable of delivering
substantially uniform mass flow into said chamber with a planar
velocity front, said velocity front moving parallel to said chamber
axis and said substrate surfaces; and
a gaseous phase exit pressure baffle located at the other end of
said chamber and extending over substantially all of the
cross-sectional area of said chamber, said exit baffle capable of
providing substantially uniform gas resistance for maintaining a
uniform mass flow rate per unit area across said other end of said
chamber to prevent recirculation of the gaseous phase materials and
reaction byproducts in said chamber.
2. Apparatus as defined in claim 1 wherein said gas distribution
baffle and said exit pressure baffle are perforated steel
plates.
3. Apparatus as defined in claim 1 wherein said gas distribution
baffle is a sintered steel plate and said exit pressure baffle is a
perforated steel plate.
4. Apparatus as described in claim 1 wherein the gas resistance of
said exit pressure baffle is about one-twentieth that of said gas
distribution baffle.
5. Apparatus as defined in claim 1 wherein said substrate holder is
a graphite susceptor.
6. Apparatus as defined in claim 1 wherein said substrate holder is
substantially in the form of a hollow right circular cylinder.
7. Apparatus as defined in claim 6 wherein said heating means is an
RF coil for inductively coupling energy to said substrate
holder.
8. Apparatus as described in claim 7 wherein said substrate holder
is rotated in said chamber to insure uniform heating of said
substrate surfaces.
9. Apparatus as claimed in claim 1 wherein there is provided a heat
shield mounted between said gaseous phase inlet means and said
substrate holder to protect said gas distribution baffle from
energy radiated by said substrate holder.
10. In a vapor transport reactor including a reaction chamber
having a longitudinal axis, a substrate holder for holding
substrates having reaction surfaces, heating means for heating
means for heating substrates to a reaction temperature, gaseous
phase inlet means and gaseous phase exit means, the improvement
comprising:
gaseous phase inlet means located at one end of the reaction
chamber comprising: a gas distribution baffle forming a plenum,
said baffle extending substantially throughout the cross-sectional
area of the chamber, said baffle capable of providing sufficient
gas resistance to gaseous phase material to develop substantially
uniform back pressure across said baffle, and said baffle also
capable of delivering substantially uniform mass flow into the
chamber, said flow having a substantially planar velocity front
moving parallel to the longitudinal axis of the chamber and the
substrate surfaces; and
gaseous phase exit means comprising: an exit pressure baffle
located at the other end of the chamber and extending over
substantially all of the cross-sectional area of the chamber, said
exit pressure baffle capable of providing substantially uniform gas
resistance to gaseous phase material in the chamber to maintain a
uniform mass flow rate per unit area across the chamber to prevent
recirculation of gaseous phase materials and reaction byproducts.
Description
This invention relates to vapor transport chemical vapor deposition
processes, and more particularly, to an improved apparatus for
carrying out these processes.
BACKGROUND
As is well known in the art, vapor transport chemical vapor
deposition reactions have many applications in the area of
semiconductor and other solid state device manufacturing. In
essence, any heat induced gaseous reaction producing desirable
byproducts might be utilized.
Many different processes and reactions have been used in what is
generally termed vapor growth; for example, various pyrolytic and
disproportionation reactions have been employed, in addition to the
well-known epitaxial semiconductor deposition process, for the
deposition of oxides, nitrides, and metals. One of the most
frequently used of these already developed processes is one
involving the hydrogen reduction of silicon tetrachloride at an
elevated temperature.
One object of many chemical vapor deposition systems is to produce
a uniform product. If uniform products cannot be produced, great
expense is entailed either by redesigning device specifications to
fit the variations of the product produced or by the rejection of a
large percentage of the products.
The problems which have been faced previously in chemical vapor
deposition processes include: contamination of the reaction
chamber; lack of uniformity of deposit thickness on all substrates
in a single reaction vessel, as well as individual substrates; the
presence of spikes on the surface of the substrates; and long
cycles involved in the batch operations currently employed.
PRIOR ART
The various different forms of apparatus disclosed in the prior art
are of significance only to illustrate the unsolved problems
heretofore involved in producing acceptable products. Early in the
development of the vapor deposition art, when most manufacturers
were merely experimenting with chemical vapor deposition, two
common forms of apparatus known as "closed" or "open" tubes were
used. The small capacity of the tubes and the time consumed
preparing for the deposition process made economical manufacturing
difficult. Subsequently, a reaction chamber known as a "barrel
reactor" received wide application in the field. An example of such
a reactor is disclosed in U.S. Pat. No. 3,424,629,to Ernst et al.,
issued Jan. 28, 1969,and assigned to the assignee of the instant
invention.
The barrel reactor consists of a barrellike chamber which contains
a cylindrical susceptor upon which a number of substrates may be
mounted circumferentially. Gaseous reactants admitted at the bottom
of the reactor by a halo-shaped inlet system are passed over the
substrate surfaces, usually heated by an externally located RF
coil. Exhaust gases are removed from the reactor through a port
located in the top of the reactor.
However, the barrel reactor did not solve all of the problems found
in the prior art. The primary advantage of the barrel reactor was
to increase batch sizes over the open tube method. Deposits
produced in barrel reactors still had many drawbacks. For example,
dust particle counts as high as 100,000 particles per ft..sub.3
could easily cause contamination of substrates. Film thickness
variations on the order of .+-. 0.5 microns on a single wafer are
also common. Other problems such as the presence of epitaxial
spikes are often found.
It is therefore an object of this invention to improve the quality
of vapor deposition products and the operating characteristics of
barrel reactors in general by decreasing the duty cycle required to
perform each batch operation.
Another object is to reduce the contamination level in deposited
films by reducing the dust count inside the reactor.
A further object of this invention is to provide more uniform
chemical vapor deposition deposits.
A still further object of this invention is to substantially reduce
or eliminate the number of spikes formed in deposited films.
SUMMARY OF THE INVENTION
Briefly considered, the reactor of the present invention is
constructed to realize the aforementioned objects, goals and
advantages and comprises a barrel reactor having a gaseous phase
inlet system including a gas distribution baffle extending
substantially across the entire horizontal cross-sectional area of
the reaction chamber which provides uniform distribution of
reactants entering the chamber and a planar velocity front
substantially throughout the chamber. An exit pressure baffle also
extending substantially across the entire horizontal
cross-sectional area of the chamber is utilized to maintain a
constant mass flow from the chamber and to prevent recirculation of
the gaseous products leaving the chamber.
The foregoing and other objects, features and advantages of the
invention will be apparent from the following more particular
description of preferred embodiments of the invention as
illustrated in the accompanying drawing.
The FIGURE shows a partial sectional view of a preferred embodiment
of the present invention.
DETAILED DESCRIPTION
The reaction that is illustratively employed to demonstrate the
preferred embodiment is the reduction of silicon tetrachloride by
hydrogen, described by the equation:
SiC1.sub.4 + 2H.sub.2 Heat Si + 4HCL.
In actuality the reaction is more complex and depends upon the
reactant concentrations, temperature, pressure, and reactor
geometry, all of which may result in various side reactions. Since
the reaction is reversible, etching and mass transport processing
may also occur.
Although the method and apparatus of the present invention will be
described in the specific context of the above reaction, it will be
apparent to those skilled in the art that other vapor transport
reactions may be similarly utilized. Thus, the apparatus of the
present invention is not. Tied to a single reaction or process
since the only limiting criteria for advantageous application of
the instant apparatus is that a reducible vapor source, or a heat
induced chemical reaction byproduct be available. For example, the
following types of reaction are possible: disproportionation,
decomposition, condensation and gas cracking. Additionally, since a
number of such reactions are reversible, the removal of films, or
material, from substrate surfaces, as well as the deposition of
material, is possible. Thus, reference to vapor deposition
processes in describing the instant invention may also be
considered to include any heat induced chemical vapor deposition or
etching process.
Referring to the FIGURE, there is shown a partial sectional view of
a vapor deposition reactor, generally designated 10, comprising an
opaque quartz cylinder 12, which is capped at both ends by hollow
plates 14 and 16 made of stainless steel, through which cooling
water may be circulated, by means not shown, defining a reaction
chamber 18. The reaction chamber may, for example, be 9 inches in
diameter and 18 inches high. Tie rods 20, with the aid of O-rings
22 and 24, enable chamber 18 to remain airtight during the vapor
deposition process. The lower plate 16 and O-ring 24, are attached
to a hydraulic cylinder (not shown) which opens and closes the
reactor. Situated within the reaction chamber 18, and mounted on a
fused-quartz rod 26 is a substrate holder, graphite susceptor 28,
having mounted around its circumference, and substantially parallel
to the chamber's longitudinal axis, as defined by rod 26, a
plurality of substrates 30 upon which deposition is desired. The
susceptor may be cut from commercially available high purity
graphite and is substantially in the form of a hollow right
cylinder having a wall thickness of about three-eighths inch. The
substrate holder is preferably tapered about 3.degree. from bottom
to top and is counterbored in order to provide recesses to support
substrates. The susceptor may be mounted on rod 26 by a star
plate.
Supported by the top plate 14 and extending across the horizontal
cross section of the chamber, there is provided a gaseous phase
inlet means including a gas distribution baffle 38 forming, with
plate 14, a first plenum 36. Gaseous phase materials, reactant
gases SiC1.sub.4 and H.sub.2, generally designated by arrow 32, are
introduced through tube 34 into the plenum 36. Plenum 36 and gas
distribution baffle 38 together provide a means for evenly
delivering the reactant gases 32 over substantially all of the
horizontal cross-sectional area at the top of the reaction chamber
18. Gas distribution baffle 38 may be constructed from a perforated
plate or a sintered material having a gas resistance sufficient to
develop substantially uniform back pressure to maintain even gas
distribution over the entire surface area of the baffle, and
thereby deliver a uniform mass flow into substantially the entire
horizontal cross-sectional area of the chamber 18. Baffle 38 may be
one-eighth inch thick sintered stainless steel filter plate having
an average pore size of 10 microns. Additionally, gas distribution
baffle 38 may be a perforated metal plate providing that the proper
number and size holes may be provided to achieve the desired
pressure drop and gas distribution in the reaction chamber 18.
Also shown is a heat shield 40 which may be mounted on the reaction
chamber side of gas distribution baffle 38. The purpose of heat
shield 40 is to reflect energy radiated from the heat shield 40 is
to reflect energy radiated from the heated susceptor 28 which may
prove harmful to baffle 38, depending upon the material of which
the baffle is constructed. Heat shield 40 is merely a thin
stainless steel, or molybdenum plate, about 0.040 inch thick,
having a number of 0.081-inch diameter holes 41 drilled on
0.25-inch centers. The plate is constructed such that it will not
substantially disturb the gas flow through the chamber but will
effectively prevent baffle 38 from overheating and perhaps
out-gassing or decomposing. It should be understood that the
addition of heat shield 40 is merely optional as it is used, or not
used, depending upon the temperature at the top of the reaction
chamber and the material of which gas distribution baffle 38 is
made.
The gaseous materials, after passing through heat shield 40, enter
chamber 18 having a planar velocity front--i.e., the gas velocity
at all points on a horizontal cross-sectional area of the chamber
is constant. Because susceptor 28 is a thin walled cylinder and
substrates 30 are substantially flush with the outer surface of the
susceptor, little resistance is met by the gas as it passes over
susceptor 28. Thus, a substantially planar velocity front is
maintained throughout the length of chamber 18.
After passing over the susceptor 28, reactant gases leave the
bottom of the chamber 18 through the following means. Mounted in
the bottom of the reaction chamber, and extending across
substantially the entire horizontal cross-sectional area of the
chamber is a gaseous phase exit pressure baffle 42 which like gas
distribution baffle 38 may be made of a sintered or porous
material. Although it is desirable to provide the same pressure
drop across exit pressure baffle 42 as that provided by gas
distribution baffle 38, it is preferable that the porosity of
baffle 42 be greater than baffle 38. The reason for this is
twofold; first, because various deposits may tend to form in the
pores of exit pressure baffle 42 thereby gradually increasing its
resistance to gas flow, and second, because it is important only to
maintain the planar velocity front until the gaseous materials have
passed the susceptor, it is only necessary to maintain a pressure
drop across exit pressure baffle 42. Therefore, the gas resistance
presented by baffle 42 is substantially less than that of gas
distribution baffle 38, on the order of one-twentieth. This may be
achieved by utilizing a perforated plate, or sintered material,
that is more porous, or less dense, than utilized at the inlet of
the chamber. Pressure baffle 42 is mounted on bottom plate 16 and
maintained by rings 44 and 46. Exhaust gases are passed from a
second plenum 48 through exhaust tubes 50 and delivered to the
atmosphere or a reclamation process.
In order to raise and maintain the temperature of the substrate
surfaces to the proper reaction temperature, a heating means is
required. An RF source is preferred, Although a resistance heater
may also be used. An RF generator, not shown, is used to
inductively heat susceptor 28 to the required temperatures. The
generator is coupled to a water-cooled helical coil 52 which is
permanently positioned outside quartz cylinder 12. It will be noted
that this arrangement of a cylindrical load coupled to the helical
RF coil 52 provides excellent heating efficiency Since all points
on the circumference of the susceptor 28 are the same distance away
from the RF coil, temperature uniformity can be readily established
in the horizontal direction (within a row of substrates 30 on
susceptor 28). To achieve temperature uniformity in a vertical
direction, the coil spacings are adjusted. The susceptor 28 is
rotated at a rate of approximately 3 r.p.m. by motor 54 to maintain
temperature uniformity of .+-. 5.degree. C. at a temperature of
1130.degree. C. (which is the preferred temperature selected for
the aforedescribed reaction) over the entire circumferential
surface area of susceptor 28. For a more complete description of
the structural details of the graphite susceptor 28, reference is
made to the aforementioned patent.
EXAMPLE
In order to show an example of the operation and results achieved
by the instant invention, the following description of the
reactor's operation and performance is provided.
The basic operating procedure of the instant invention is best
described in terms of the specific example of its operation as
already referred to above--i.e., the hydrogen reduction of silicon
tetrachloride.
Substrates 30, highly polished semiconductor wafers, are loaded
onto graphite susceptor 28 while bottom plate 16 is in the
previously referred to lowered position. During this time, it may
be desirable to allow a nominal flow of inert gas, such as argon,
to enter inlet tube 34 in order to maintain chamber 18 in a
relatively clean condition. Bottom plate 16 is then raised in order
to close reactor 10 for the deposition process. Chamber 18 is then
purged for about one minute by an inert gas, preferably argon,
which is maintained at any desirable flow rate which will insure
adequate purging. Due to the high cost of argon, it is acceptable
to utilize a purge rate of about one-tenth that of the reactant
gases to be referred to later. The rate used in the preferred
embodiment should be sufficient to produce a streaming velocity in
excess of the diffusion velocity for impurities in the purging
gas.
As the purge gas passes into plenum 36, it is uniformly distributed
across the surface of gas distribution baffle 38 providing a back
pressure of about 2-4 p.s.i. and a substantially planar velocity
front within chamber 18. Due to the relatively wide chamber cross
section, as compared with its length, the formation of a boundary
layer, caused by frictional contact between gas flowing through the
reaction chamber and the internal surfaces of quartz cylinder 12,
is for all practical purposes, insignificant.
Because the purged gas enters chamber 18 with a planar velocity
front and because of the low gas resistance presented by susceptor
28, reaction chamber 18 is effectively purged in a very short
period of time.
After the chamber has been purged, the inert purge gas is replaced
by hydrogen at a flow rate of about 150 liters per minute for a
period of about 2 minutes to displace the purge gas and establish a
total hydrogen ambient for the vapor deposition reaction. This rate
will produce a streaming velocity in excess of the diffusion
velocity for impurities in the hydrogen gas. The RF heating coils
are energized while additional hydrogen is passed through the
chamber for about 7 minutes while the substrates are raised to the
reaction temperature of 1130 .+-. 5.degree. C., Just prior to
admission the reactant gas flow is vented to purge the feed system
and establish equilibrium flow before it is injected into the
reactor. For a 7-inch long susceptor the SiC1.sub.4 is admitted to
the reaction chamber in a hydrogen carrier at a rate of about 150
liters per minute in a SiC1.sub.4 /H.sub.2 ratio of about 0.01 for
6-14 minutes depending upon the film thickness desired. In general,
higher streaming velocities are required for longer susceptors.
The gas distribution baffle 38 and exit gas pressure baffle 42 act
on the reactant gases in the same manner as described above with
reference to the purge gas. Additionally, due to the fact that the
reactant gas concentration is substantially equal throughout the
cross-sectional area of the chamber, because of the relatively
short length of susceptor 28, uniquely uniform deposition of
reaction byproducts are obtained.
After the desired deposition time has elapsed hydrogen alone is
passed through the chamber for about 15 seconds to remove all
traces of SiC1.sub.4 .
The RF power is then turned off and the substrates are cooled in
hydrogen for about 6 minutes. Finally, the hydrogen is purged from
the chamber with argon which further cools the substrates for about
2 minutes. The reactor is opened and the coated substrates are
removed from the susceptor.
A summary of the improvements achieved by the novel inlet and exit
system of the subject invention, as compared with the prior art
barrel reactor is given below.
The dust particle count of particles(greater than one-half micron)
in the chamber, as determined by a commercial dust counter, is
about 100 particles/ft..sup.3. This is a 1,000 to 1 reduction from
the count of 100,000 particles/ft..sup.3 as found in a reactor not
equipped with the novel inlet and exit system.
The uniformity of deposit, as determined by the infrared
interference technique, for a 6-micron film, previously .+-. 0.5
microns on a single substrate, was reduced to .+-. 0.1 microns for
all substrates within the chamber.
The presence of spikes found on substrates was reduced from about
80 to 100 per substrate to about one or two per substrate.
The duty cycle for the entire deposition operation was reduced by a
factor of from two to three times that required by prior art
reactors due primarily to the efficient purging action of the
planar gas velocity front.
In summary, what has been disclosed is a novel structure for a
vapor deposition reactor which significantly improves the quality
of vapor deposition products. A structure which enables shortened
duty cycles due to more efficient purging of the reaction chamber
both before and after deposition. Such a reactor includes a gas
distribution baffle which delivers gases to the reaction chamber
uniformly throughout its horizontal cross section and a pressure
baffle which assures uniform removal of the gases from each portion
of the horizontal cross-sectional area of the chamber at a uniform
rate.
While the invention has been particularly shown and described with
reference to a preferred embodiment thereof, it will be understood
by those skilled in the art that the foregoing and other changes in
form and details may be made therein without departing from the
spirit and scope of the invention.
* * * * *