CN117660920A - MPCVD device and method for improving uniformity of diamond film - Google Patents
MPCVD device and method for improving uniformity of diamond film Download PDFInfo
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- CN117660920A CN117660920A CN202311669257.1A CN202311669257A CN117660920A CN 117660920 A CN117660920 A CN 117660920A CN 202311669257 A CN202311669257 A CN 202311669257A CN 117660920 A CN117660920 A CN 117660920A
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- 239000010432 diamond Substances 0.000 title claims abstract description 102
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 102
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 15
- 239000010453 quartz Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 12
- 238000010899 nucleation Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
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- 238000003698 laser cutting Methods 0.000 claims description 3
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- 230000003746 surface roughness Effects 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides an MPCVD device and a method for improving the uniformity of a diamond film, wherein the MPCVD device for improving the uniformity of the diamond film comprises a reaction chamber, a sample table and a microwave assembly, wherein the center of the top of the reaction chamber is provided with an air inlet, and the side surface of the bottom of the reaction chamber is uniformly provided with a plurality of air outlets; the sample table is arranged in the reaction chamber and is connected with the center of the bottom of the reaction chamber; the microwave component is arranged at one side of the reaction chamber and is connected and communicated with the reaction chamber. The MPCVD method for improving the uniformity of the diamond film provided by the invention is produced by using the MPCVD device for improving the uniformity of the diamond film. According to the MPCVD device for improving the uniformity of the diamond film, at least four air outlets are uniformly formed in the bottom, so that the air flow mode is changed, the distribution uniformity of an air flow field in a cavity is improved, the surface temperature of a substrate and the distribution uniformity of active groups in the cavity are improved, and the quality and uniformity of the diamond film are further improved.
Description
Technical Field
The invention belongs to the technical field of diamond material growth, and particularly relates to an MPCVD device and method for improving uniformity of a diamond film.
Background
Diamond, which is the most hard material on earth, is becoming an irreplaceable material in applications such as precision machining, infrared window and heat dissipating substrate due to its excellent thermal, optical and chemical stability. In precision mechanical applications, diamond film cutters significantly improve cutting efficiency and greatly extend the useful life of the cutting tool; the excellent heat conductivity of the diamond can timely emit heat in the running process of a circuit, so that the running power of a precise instrument is greatly improved, and various electronic devices are prevented from being damaged due to heat aggregation; in addition, the diamond film has great application potential in the fields of high-power CO2 lasers, quantum detectors and the like. However, natural diamond often contains impurities, resulting in reduced quality of diamond, and is scarce in quantity and expensive, and far from meeting the needs of people, so that the preparation of high quality diamond by artificial synthesis has been a pursued goal.
The MPCVD method is accepted as the best method for preparing high-quality diamond by virtue of the advantages of high growth quality, stable and controllable deposition parameters, large-area preparation, easy film formation and the like. The technical principle is that high-intensity microwaves generated by a microwave generator excite carbon-containing gas above a sample stage in a decomposition reactor to form active carbon-containing groups and atomic hydrogen, and plasma is formed, so that a diamond film is deposited on the sample stage. In the prior art, factors influencing the quality of diamond film mainly include microwave power, deposition gas pressure, substrate temperature, carbon source concentration, gas flow rate, and sample stage geometry. The flow mode of the gas can influence the gas flow field of the reaction chamber under high power density, and the change of the gas flow field can also influence the growth quality and uniformity of the diamond film.
The current MPCVD device has great difference in the arrangement of the positions of the reaction gas inlet and outlet holes, but the design initially mainly aims at the positions and the intensity of an electric field and plasma, and the uniformity of a diamond film is not further optimized by the gas flow field distribution problem caused by the gas outlet holes.
Disclosure of Invention
The embodiment of the invention provides an MPCVD device and method for improving the uniformity of a diamond film, and aims to provide a device and method for improving the distribution of a gas flow field of a reaction chamber and further improving the growth quality and uniformity of the diamond film.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides an MPCVD apparatus for improving uniformity of a diamond film, comprising:
the reaction chamber is provided with an air inlet in the center of the top, a plurality of air outlets are uniformly formed in the side surface of the bottom, and the number of the air outlets is at least four;
the sample table is connected with the center of the bottom of the reaction chamber in the reaction chamber, and is suitable for placing a substrate; and
the microwave assembly is arranged at one side of the reaction chamber, is connected and communicated with the reaction chamber and is used for transmitting microwaves into the reaction chamber.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, the reaction chamber includes:
a side wall;
the lower flange is arranged on the lower side of the side wall and connected with the side wall, and at least four air outlets are uniformly formed in the side surface of the lower flange;
the bottom plate is arranged at the lower side of the lower flange and is connected with the lower flange; and
the top plate is arranged on the upper side of the side wall and connected with the side wall, and the air inlet is formed in the center of the top plate.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, the reaction chamber further includes a quartz wall, and the quartz wall is enclosed inside the side wall, and an upper end of the quartz wall is connected with the top plate, and a lower end of the quartz wall is connected with the lower flange.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, sealing rings are sandwiched between the quartz wall and the top plate, between the quartz wall and the lower flange, and between the lower flange and the bottom plate.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, the sample stage is disposed at an upper center of the base plate and is connected to the base plate.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, a groove is formed on an upper side of the sample stage, and the groove is adapted to be placed with a substrate; the diameter of the groove is 1-2 mm larger than that of the substrate.
With reference to the first aspect, in a possible implementation manner of the MPCVD apparatus for improving uniformity of a diamond film provided by the present invention, the microwave assembly includes:
the microwave source is arranged on one side of the side wall and used for generating microwaves; and
one end of the waveguide tube is connected and communicated with the microwave source, and the other end of the waveguide tube is connected with the side wall and communicated with the inside of the side wall.
In a second aspect, an embodiment of the present invention further provides an MPCVD method for improving uniformity of a diamond film, using the MPCVD apparatus for improving uniformity of a diamond film, including the steps of:
s01, ultrasonically cleaning the silicon substrate in acetone for 5-10 minutes, ultrasonically cleaning the silicon substrate in alcohol for 5-10 minutes, removing pollutants such as organic matters, impurities and the like, finally boiling and cleaning the silicon substrate in hot alcohol for 5 minutes, and air-drying the silicon substrate for later use.
S02, adopting a polymer auxiliary seeding process, and seeding diamond seed crystals on the surface of the cleaned silicon wafer.
S03, placing the sown silicon wafer substrate in the center of the sample stage, and ensuring that the sample is positioned in the center of the chamber.
S04, after the air pressure of the cavity reaches the back vacuum degree, starting microwaves; after starting, adjusting microwave power and chamber pressure to enable the temperature of the substrate to reach an expected value; then, the hydrogen flow rate and the methane flow rate were set as growth values, and growth of the diamond film was performed.
S05, after the diamond growth is finished, diamond powder with the particle size of 10 mu m and 3 mu m is sequentially used for grinding the diamond layer, and the surface roughness of the diamond layer is reduced by polishing, so that the surface of the diamond layer is flattened; then, removing the edge polycrystal by a laser cutting method.
In combination with the second aspect, in a possible implementation manner of the MPCVD method for improving uniformity of a diamond film provided by the present invention, the polymer assisted seeding process is to soak the substrate with the polydimethyldiallyl ammonium chloride polymer, and then soak the substrate after the polymer treatment in the negatively charged diamond nano-suspension.
With reference to the second aspect, in a possible implementation manner of the MPCVD method for improving uniformity of a diamond film provided by the present invention, the process parameters in step S04 are: the microwave power is 3-4 kW, the deposition temperature is 750800 ℃, the deposition atmosphere is the mixed gas of methane and hydrogen, and the methane proportion is controlled within the range of 1.5-3%.
The MPCVD device for improving the uniformity of the diamond film has the beneficial effects that: compared with the prior art, the MPCVD device for improving the uniformity of the diamond film provided by the invention has the advantages that the bottom is uniformly provided with at least four air outlets, compared with the original air outlet, the air flow mode is changed, the distribution uniformity of the air flow field in the cavity is improved, and therefore, the surface temperature of the substrate and the distribution uniformity of active groups in the cavity are improved, and the quality and uniformity of the diamond film are further improved.
The MPCVD method for improving the uniformity of the diamond film has the beneficial effects that: compared with the prior art, the MPCVD method for improving the uniformity of the diamond film provided by the invention has the advantages that on one hand, the device is used for production, and the quality and uniformity of the diamond film are improved; on the other hand, a polymer auxiliary seeding process is adopted in the diamond growth process, and a layer of uniform diamond seed crystal is obtained on the surface of the silicon substrate, so that a compact and continuous diamond nucleation layer can be rapidly formed in the diamond growth process, and the quality and uniformity of the diamond film are further improved.
Drawings
FIG. 1 is a schematic diagram of a front view of an MPCVD apparatus for improving uniformity of a diamond film according to an embodiment of the present invention;
reference numerals illustrate:
1. a bottom plate; 2. a reaction chamber; 3. a sample stage; 4. a microwave source;
5. a waveguide; 6. a side wall; 7. a top plate; 8. a lower flange; 9. quartz walls;
10. an air inlet; 11. and an air outlet.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present application unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
In the description of the present application, it should be understood that, where azimuth terms such as "front, rear, upper, lower, left, right", "transverse, vertical, horizontal", and "top, bottom", etc., indicate azimuth or positional relationships generally based on those shown in the drawings, only for convenience of description and simplification of the description, these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present application; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways and the spatially relative descriptions used herein are construed accordingly.
In addition, the terms "first", "second", etc. are used to define the components, and are merely for convenience of distinguishing the corresponding components, and unless otherwise stated, the terms have no special meaning, and thus should not be construed as limiting the scope of the present application.
Referring to fig. 1 together, an MPCVD apparatus for improving uniformity of diamond film according to the present invention will now be described. The MPCVD device for improving the uniformity of the diamond film comprises a reaction chamber 2, a sample table 3 and a microwave assembly, wherein an air inlet 10 is arranged in the center of the top of the reaction chamber 2, a plurality of air outlets 11 are uniformly formed in the side surface of the bottom of the reaction chamber, and the number of the plurality of air outlets 11 is at least four; the sample table 3 is arranged in the reaction chamber 2, is connected with the center of the bottom of the reaction chamber 2, and is suitable for placing a substrate on the sample table 3; the microwave component is arranged at one side of the reaction chamber 2, is connected and communicated with the reaction chamber 2, and is used for emitting microwaves into the reaction chamber 2.
Specifically, the reaction chamber 2 has a square structure, and an air outlet 11 is formed in the middle of the bottoms of the four side walls of the reaction chamber 2.
The MPCVD device for improving the uniformity of the diamond film has the beneficial effects that: compared with the prior art, the MPCVD device for improving the uniformity of the diamond film provided by the invention has the advantages that the bottom is uniformly provided with the at least four air outlets 11, compared with the original air outlet 11, the air flow mode is changed, and the distribution uniformity of the air flow field in the cavity is improved, so that the surface temperature of the substrate and the distribution uniformity of active groups in the cavity are improved, and the quality and uniformity of the diamond film are further improved.
As shown in fig. 1, in a specific implementation manner of an MPCVD apparatus for improving uniformity of a diamond film provided by the embodiment of the invention, a reaction chamber 2 includes a side wall 6, a lower flange 8, a bottom plate 1 and a top plate 7, wherein a cross section of the side wall 6 in a vertical direction is square, the lower flange 8 is arranged at a lower side of the side wall 6 and is connected with the side wall 6, and at least four air outlets 11 are uniformly formed on a side surface of the lower flange 8; the bottom plate 1 is arranged at the lower side of the lower flange 8 and is connected with the lower flange 8; the top plate 7 is arranged on the upper side of the side wall 6 and connected with the side wall 6, and the center of the top plate 7 is provided with an air inlet 10.
The side wall 6 is a metal plate and is fixed with the lower flange 8 and the top plate 7 through screws; the air outlets 11 are arranged around the lower flange 8.
As shown in fig. 1, in a specific implementation manner of the MPCVD apparatus for improving uniformity of diamond film provided by the embodiment of the invention, the reaction chamber 2 further includes a quartz wall 9, the quartz wall 9 is enclosed inside the side wall 6, the upper end is connected with the top plate 7, and the lower end is connected with the lower flange 8.
Further, sealing rings are interposed between the quartz wall 9 and the top plate 7, between the quartz wall 9 and the lower flange 8, and between the lower flange 8 and the bottom plate 1, to form a sealed chamber.
As shown in fig. 1, in a specific embodiment of the MPCVD apparatus for improving uniformity of diamond film provided in the embodiment of the present invention, a sample stage 3 is provided at the center of the upper side of a base plate 1 and is connected to the base plate 1.
As shown in fig. 1, in a specific implementation manner of an MPCVD apparatus for improving uniformity of a diamond film provided by the embodiment of the invention, a groove is formed on an upper side of a sample stage 3, and a substrate is suitable for being placed in the groove; the diameter of the groove is 1-2 mm larger than the diameter of the substrate; on one hand, the substrate is ensured not to deviate in the diamond growth process, and on the other hand, the substrate can not be taken out due to edge polycrystal is prevented.
As shown in fig. 1, in a specific implementation manner of the MPCVD apparatus for improving uniformity of diamond film provided in the embodiment of the present invention, a microwave assembly includes a microwave source 4 and a waveguide 5, where the microwave source 4 is disposed on one side of a side wall 6, and is used for generating microwaves; one end of the waveguide 5 is connected and communicated with the microwave source 4, and the other end is connected with the side wall 6 and communicated with the inside of the side wall 6.
Microwaves generated by the microwave source 4 are introduced into the cavity through the waveguide 5 to form a suspended plasma sphere on the sample stage 3.
Based on the same inventive concept, the embodiments of the present application also provide an MPCVD method for improving uniformity of a diamond film, using the MPCVD apparatus for improving uniformity of a diamond film described above, and comprising the steps of:
s01, ultrasonically cleaning the silicon substrate in acetone for 5-10 minutes, ultrasonically cleaning the silicon substrate in alcohol for 5-10 minutes, removing pollutants such as organic matters, impurities and the like, finally boiling and cleaning the silicon substrate in hot alcohol for 5 minutes, and air-drying the silicon substrate for later use.
S02, adopting a polymer auxiliary seeding process, and seeding diamond seed crystals on the surface of the cleaned silicon wafer: firstly, soaking in polydimethyl diallyl ammonium chloride polymer for 2 hours, flushing with deionized water, putting into diamond nano-suspension, soaking for 1 hour, flushing with deionized water, and drying with nitrogen.
S03, placing the sown silicon wafer substrate in the center of the sample stage 3, and ensuring that the sample is in the center of the chamber.
S04, after the air pressure of the chamber reaches 3.0x10 < -2 > mbar, starting microwaves; after starting, the microwave power is adjusted to 3.5kW, the chamber pressure is 160mbar, the deposition temperature is 750800 ℃, the deposition atmosphere is a mixed gas of methane and hydrogen, the methane concentration is 2%, the growth time is 72h, and the growth of the diamond film is carried out.
S05, after the diamond growth is finished, diamond powder with the particle size of 10 mu m and 3 mu m is sequentially used for grinding the diamond layer, and the surface roughness of the diamond layer is reduced by polishing, so that the surface of the diamond layer is flattened; then, removing the edge polycrystal by a laser cutting method.
The MPCVD method for improving the uniformity of the diamond film has the beneficial effects that: compared with the prior art, the MPCVD method for improving the uniformity of the diamond film provided by the invention has the advantages that on one hand, the device is used for production, and the quality and uniformity of the diamond film are improved; on the other hand, a polymer auxiliary seeding process is adopted in the diamond growth process, and a layer of uniform diamond seed crystal is obtained on the surface of the silicon substrate, so that a compact and continuous diamond nucleation layer can be rapidly formed in the diamond growth process, and the quality and uniformity of the diamond film are further improved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. An MPCVD apparatus for improving uniformity of a diamond film, comprising:
the reaction chamber (2) is provided with an air inlet (10) at the center of the top, a plurality of air outlets (11) are uniformly formed in the side surface of the bottom, and the number of the air outlets (11) is at least four;
a sample stage (3) connected with the center of the bottom of the reaction chamber (2) in the reaction chamber (2), wherein the sample stage (3) is suitable for placing a substrate; and
the microwave assembly is arranged at one side of the reaction chamber (2), is connected and communicated with the reaction chamber (2) and is used for transmitting microwaves into the reaction chamber (2).
2. MPCVD apparatus for improving uniformity of diamond films according to claim 1, characterized in that said reaction chamber (2) comprises:
a side wall (6);
the lower flange (8) is arranged at the lower side of the side wall (6) and is connected with the side wall (6), and at least four air outlets (11) are uniformly formed in the side surface of the lower flange (8);
the bottom plate (1) is arranged at the lower side of the lower flange (8) and is connected with the lower flange (8); and
the top plate (7) is arranged on the upper side of the side wall (6) and connected with the side wall (6), and the air inlet (10) is formed in the center of the top plate (7).
3. MPCVD apparatus for improving uniformity of diamond films according to claim 2, characterized in that the reaction chamber (2) further comprises quartz walls (9), said quartz walls (9) being enclosed inside the side walls (6), the upper end being connected to the top plate (7) and the lower end being connected to the lower flange (8).
4. An MPCVD apparatus for improving uniformity of diamond film according to claim 3, wherein sealing rings are interposed between said quartz wall (9) and said top plate (7), between said quartz wall (9) and said lower flange (8), and between said lower flange (8) and said bottom plate (1).
5. MPCVD apparatus for improving uniformity of diamond film according to claim 2, wherein said sample stage (3) is provided at the center of the upper side of said base plate (1) and is connected to said base plate (1).
6. MPCVD apparatus for improving uniformity of diamond film according to claim 5, wherein a recess is provided on the upper side of the sample stage (3), said recess being adapted for placing a substrate therein; the diameter of the groove is 1-2 mm larger than that of the substrate.
7. The MPCVD apparatus for improving uniformity of a diamond film according to claim 2, wherein the microwave assembly comprises:
a microwave source (4) arranged at one side of the side wall (6) and used for generating microwaves; and
and one end of the waveguide tube (5) is connected and communicated with the microwave source (4), and the other end of the waveguide tube is connected with the side wall (6) and communicated with the inside of the side wall (6).
8. An MPCVD method for improving uniformity of a diamond film, wherein the MPCVD apparatus for improving uniformity of a diamond film according to any one of claims 1 to 7 is used and comprises the steps of:
s01, ultrasonically cleaning a silicon substrate in acetone for 5-10 minutes, ultrasonically cleaning the silicon substrate in alcohol for 5-10 minutes, removing pollutants, finally boiling and cleaning the silicon substrate in hot alcohol for 5 minutes, and air-drying the silicon substrate for later use;
s02, adopting a polymer auxiliary seeding process, and seeding diamond seed crystals on the surface of the cleaned silicon wafer;
s03, placing the sown silicon wafer substrate in the center of a sample table, and ensuring that a sample is positioned in the center of a cavity;
s04, after the air pressure of the cavity reaches the back vacuum degree, starting microwaves; after starting, adjusting microwave power and chamber pressure to enable the temperature of the substrate to reach an expected value; then, setting the hydrogen flow and the methane flow as growth values, and carrying out the growth of the diamond film;
s05, after the diamond growth is finished, diamond powder with the particle size of 10 mu m and 3 mu m is sequentially used for grinding the diamond layer, and the surface roughness of the diamond layer is reduced by polishing, so that the surface of the diamond layer is flattened; then, removing the edge polycrystal by a laser cutting method.
9. The MPCVD method of claim 8, wherein the polymer assisted seeding process comprises immersing the substrate in a polydimethyldiallylammonium chloride polymer and immersing the polymer-treated substrate in a negatively charged diamond nanosuspension.
10. The MPCVD method for improving uniformity of a diamond film according to claim 8, wherein the process parameters in step S04 are: the microwave power is 3-4 kW, the deposition temperature is 750800 ℃, the deposition atmosphere is the mixed gas of methane and hydrogen, and the methane proportion is controlled within the range of 1.5-3%.
Priority Applications (1)
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CN202311669257.1A CN117660920A (en) | 2023-12-06 | 2023-12-06 | MPCVD device and method for improving uniformity of diamond film |
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CN202311669257.1A CN117660920A (en) | 2023-12-06 | 2023-12-06 | MPCVD device and method for improving uniformity of diamond film |
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