CN114231953A - Method for preparing nano diamond film by microwave plasma chemical vapor deposition method - Google Patents
Method for preparing nano diamond film by microwave plasma chemical vapor deposition method Download PDFInfo
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- CN114231953A CN114231953A CN202111403601.3A CN202111403601A CN114231953A CN 114231953 A CN114231953 A CN 114231953A CN 202111403601 A CN202111403601 A CN 202111403601A CN 114231953 A CN114231953 A CN 114231953A
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 37
- 239000002113 nanodiamond Substances 0.000 title claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 61
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000010410 layer Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 12
- 239000010432 diamond Substances 0.000 claims abstract description 12
- 238000011282 treatment Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 6
- 239000012790 adhesive layer Substances 0.000 claims abstract description 4
- 238000011221 initial treatment Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 44
- 238000000151 deposition Methods 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007517 polishing process Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000006911 nucleation Effects 0.000 abstract description 7
- 238000010899 nucleation Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0236—Pretreatment of the material to be coated by cleaning or etching by etching with a reactive gas
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
- C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
Abstract
The invention discloses a method for preparing a nano-diamond film by utilizing a microwave plasma chemical vapor deposition method, which relates to the technical field of diamond films and comprises the following steps: step S1: preparing a process substrate and diamond; microwave plasma chemical vapor deposition equipment, a magnetron sputtering instrument and a spin coater; acetone solution, ethanol solution, hydrofluoric acid and deionized water; step S2: performing primary treatment; step S3: treating again, namely placing the ground substrate into an acetone solution, an ethanol solution, hydrofluoric acid and deionized water for cleaning in sequence; drying the substrate after cleaning; step S4: preparing an adhesion layer; step S5: starting to prepare a membrane; step S6: subsequent treatment; step S7: and (4) manufacturing and analyzing. The method has the advantages of simple steps, less impurities, capability of improving the adhesive force between the structures by arranging the adhesive layer, and high nucleation density of the prepared film.
Description
Technical Field
The invention relates to the technical field of diamond films, in particular to a method for preparing a nano diamond film by utilizing a microwave plasma chemical vapor deposition method.
Background
The nano diamond film has the characteristics of wear resistance, high insulation, uniform film layer, high density and corrosion resistance.
The microwave plasma chemical vapor deposition method ionizes reaction gas molecules to generate plasma, and then a film is formed after deposition on a substrate.
The existing film-making method has the disadvantages of complex film-making operation and high difficulty, the adhesion force between the prepared film and a substrate is poor, the prepared film is difficult to meet the high process requirement, and the film may contain more impurities after film-forming, so that the quality of the film is poor
Disclosure of Invention
The invention aims to provide a method for preparing a nano-diamond film by using a microwave plasma chemical vapor deposition method, which has the advantages of simple steps, less impurities, capability of improving the adhesive force between structures by arranging an adhesive layer, high nucleation density of the prepared film and capability of solving the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the method for preparing the nano-diamond film by utilizing the microwave plasma chemical vapor deposition method comprises the following steps of:
step S1: the preparation process comprises the following steps: a substrate and diamond; preparing equipment: microwave plasma chemical vapor deposition equipment, a magnetron sputtering instrument and a spin coater; preparing a working liquid: acetone solution, ethanol solution, hydrofluoric acid and deionized water;
step S2: performing primary treatment, namely polishing the surface of the substrate by adopting a mirror polishing process; mechanically grinding the substrate using the diamond powder having a particle size of 60-100 nm;
step S3: treating again, namely placing the ground substrate into the acetone solution, the ethanol solution, the hydrofluoric acid and the deionized water for cleaning in sequence; drying the substrate after cleaning;
step S4: preparing an adhesion layer, namely placing the substrate in the magnetron sputtering instrument and mounting the substrate on a rotating frame; sputtering an adhesion layer made of metal nickel on the surface of the substrate by using the magnetron sputtering instrument; after the treatment is finished, placing the substrate in the microwave plasma chemical vapor deposition equipment for film preparation;
step S5: starting the microwave plasma chemical vapor deposition equipment to form a film; and vacuum preparation is carried out; preparing gas; high methane concentration deposition; deposition at low methane concentration;
step S6: performing subsequent treatment, namely continuously operating the microwave plasma chemical vapor deposition equipment for 10min to prepare a nano diamond film;
step S7: and (3) manufacturing and analyzing, namely detecting the components and the quality of the manufactured nano-diamond film, and summarizing, counting and analyzing data.
Optionally, the substrate in step S1 is a silicon wafer.
Optionally, in the process of preparing the adhesion layer in step S4, the rotating frame continuously rotates at an adjustable speed.
Optionally, after the transition layer is formed on the surface of the substrate in the step S4, the substrate is placed in the diamond micro powder, the acetone solution and the deionized water to be sequentially subjected to ultrasonic cleaning, and after cleaning, drying is performed.
Optionally, the vacuum preparation in step S5 is to pump the microwave plasma chemical vapor deposition apparatus to vacuum by using a vacuum pump.
Optionally, the gas preparation in step S5 is to introduce a mixed gas of methane and hydrogen as a reaction gas into the microwave plasma chemical vapor deposition apparatus.
Optionally, in the step S5, the deposition with high methane concentration is performed at a flow rate of 3-5 sccm when the flow rate of the introduced hydrogen is unchanged.
Optionally, in the step S5, the deposition with low methane concentration is performed under the condition that the flow rate of the introduced hydrogen gas is unchanged, the flow rate of the introduced methane gas is 1-2 sccm, and the deposition time is 185 min.
Compared with the prior art, the invention has the following beneficial effects:
the substrate is polished, so that the subsequent film forming efficiency and the subsequent film forming quality are improved; by grinding the substrate, the nucleation density of the nano-diamond film can be increased.
Secondly, the impurities on the surface of the substrate are removed through the treatment of an acetone solution; residual liquid in the cleaning process of the acetone solution can be removed through the treatment of the ethanol solution; the silicon oxide layer on the surface of the substrate can be taken out by treatment with hydrofluoric acid.
Through the preparation of the adhesion layer, the adhesion of the film to the substrate can be improved, and the overall stability and the service life of the film are better.
Fourthly, the microwave plasma chemical vapor deposition equipment is started, the equipment is vacuumized, and mixed gas is introduced at different concentrations, so that the nucleation rate and the quality of the formed film are higher.
Drawings
FIG. 1 is a process flow diagram of the structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: the method for preparing the nano-diamond film by utilizing the microwave plasma chemical vapor deposition method comprises the following steps of:
step S1: the preparation process comprises the following steps: a substrate and diamond; preparing equipment: microwave plasma chemical vapor deposition equipment, a magnetron sputtering instrument and a spin coater; preparing a working liquid: acetone solution, ethanol solution, hydrofluoric acid and deionized water.
Step S2: performing primary treatment, namely polishing the surface of the substrate by adopting a mirror polishing process; the substrate is mechanically ground by using diamond powder with the grain diameter of 60-100nm, and the subsequent film forming efficiency and film forming quality are improved by polishing the substrate; by grinding the substrate, the nucleation density of the nano-diamond film can be increased.
Step S3: treating again, namely placing the ground substrate into an acetone solution, an ethanol solution, hydrofluoric acid and deionized water for cleaning in sequence; drying the substrate after cleaning, and removing impurities on the surface of the substrate through treatment of an acetone solution; residual liquid in the cleaning process of the acetone solution can be removed through the treatment of the ethanol solution; the silicon oxide layer on the surface of the substrate can be taken out through hydrofluoric acid treatment; the cleaning by the deionized water cleaning enables the solution on the surface of the substrate to be comprehensively processed, and the substrate is clean after being cleaned.
Step S4: preparing an adhesion layer, namely placing the substrate in a magnetron sputtering instrument and mounting the substrate on a rotating frame; sputtering an adhesion layer made of metallic nickel on the surface of the substrate by a magnetron sputtering instrument; after the treatment is finished, the substrate is placed in microwave plasma chemical vapor deposition equipment to wait for film making, the film is directly made on the substrate due to the fact that the existing mode is mostly used for making the film, but the adhesive force of the substrate is difficult to meet the higher requirement in the industry, the mode can improve the adhesive force of the film to the substrate through the arrangement of the adhesive layer, and the stability and the service life of the whole film are better.
Step S5: starting a microwave plasma chemical vapor deposition device; and vacuum preparation is carried out; preparing gas; high methane concentration deposition; and (3) depositing under low methane concentration, starting equipment, adjusting the equipment environment, introducing mixed gas, and introducing different concentrations, so that the nucleation rate and the quality of the formed film are higher.
Step S6: and (3) performing subsequent treatment, namely continuously operating the microwave plasma chemical vapor deposition equipment for 10min to prepare the nano-diamond film, slowly cooling the substrate and the film to room temperature, avoiding the film damage caused by sudden cooling, achieving the heat preservation effect and being beneficial to prolonging the service life of the film.
Step S7: the manufactured nano-diamond film is subjected to component and quality detection, data gathering statistics and analysis, the film is inspected, the quality problem of the film can be found timely, a user can make adjustment timely, the data are gathered and analyzed, and subsequent users can conveniently conduct centralized analysis on the data.
Further, the substrate in step S1 is a silicon wafer.
In order to make the adhesion layer more even, further, the in-process of step S4 adhesion layer preparation, the swivel mount carries out continuous rotation, and pivoted speed is adjustable, through making the swivel mount rotate for in sputtering work, can carry out even sputtering to the substrate on it, make the adhesion layer of its surface formation comparatively smooth and comparatively level, and the simple operation, do not need the manual a plurality of faces to the substrate of user to adjust.
In order to ensure the quality of the transition layer, further, after the transition layer is formed on the surface of the substrate in the step S4, the substrate is placed in the micro powder of the diamond, acetone solution and deionized water are sequentially subjected to ultrasonic cleaning, and after cleaning is completed, drying is carried out, so that impurities on the transition layer can be cleaned, the adhesion layer can be deeply cleaned, secondary conditions are carried out on the substrate, and the cleanness of the substrate and the adhesion layer is ensured.
In order to ensure the quality of the film, the vacuum preparation in step S5 is to pump the microwave plasma chemical vapor deposition apparatus to vacuum by a vacuum pump, so as to reduce the error of the film-making operation by pumping to vacuum, and the vacuum pumping can be performed according to the design specification, so as to ensure the film-forming quality of the film.
Further, the gas preparation in step S5 is to introduce the mixed gas of methane and hydrogen as the reaction gas into the microwave plasma chemical vapor deposition apparatus, so that the mixed gas of methane and hydrogen can meet the requirement of chemical vapor deposition, which is a necessary condition for preparing the thin film.
In order to improve the film forming quality of the nano-diamond film, further, the high methane concentration deposition in the step S5 is to increase the nucleation rate of the subsequent nano-diamond film through the high methane concentration deposition step, wherein the introduction flow rate of methane is 3-5 sccm under the condition that the introduction flow rate of hydrogen is unchanged.
Further, in the step S5, the low methane concentration deposition is performed by performing the low methane concentration deposition step on the substrate, wherein the flow rate of the introduced methane is 1 to 2sccm, the deposition time is 185min, and the flow rate of the introduced hydrogen is not changed.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The method for preparing the nano-diamond film by utilizing the microwave plasma chemical vapor deposition method is characterized by comprising the following steps of: the method comprises the following steps:
step S1: the preparation process comprises the following steps: a substrate and diamond; preparing equipment: microwave plasma chemical vapor deposition equipment, a magnetron sputtering instrument and a spin coater; preparing a working liquid: acetone solution, ethanol solution, hydrofluoric acid and deionized water;
step S2: performing primary treatment, namely polishing the surface of the substrate by adopting a mirror polishing process; mechanically grinding the substrate using the diamond powder having a particle size of 60-100 nm;
step S3: treating again, namely placing the ground substrate into the acetone solution, the ethanol solution, the hydrofluoric acid and the deionized water for cleaning in sequence; drying the substrate after cleaning;
step S4: preparing an adhesion layer, namely placing the substrate in the magnetron sputtering instrument and mounting the substrate on a rotating frame; sputtering an adhesion layer made of metal nickel on the surface of the substrate by using the magnetron sputtering instrument; after the treatment is finished, placing the substrate in the microwave plasma chemical vapor deposition equipment for film preparation;
step S5: starting the microwave plasma chemical vapor deposition equipment to form a film; and vacuum preparation is carried out; preparing gas; high methane concentration deposition; deposition at low methane concentration;
step S6: performing subsequent treatment, namely continuously operating the microwave plasma chemical vapor deposition equipment for 10min to prepare a nano diamond film;
step S7: and (3) manufacturing and analyzing, namely detecting the components and the quality of the manufactured nano-diamond film, and summarizing, counting and analyzing data.
2. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: the substrate in step S1 is a silicon wafer.
3. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: in the preparation process of the adhesive layer in the step S4, the rotating frame continuously rotates at an adjustable speed.
4. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: and S4, after a transition layer is formed on the surface of the substrate, placing the substrate in the micro powder of the diamond, and then carrying out ultrasonic cleaning on the acetone solution and the deionized water in sequence, and drying after cleaning.
5. The method for preparing a nanodiamond film using a microwave plasma chemical vapor deposition method according to any one of claims 1-4, wherein: the vacuum preparation in step S5 is to pump the microwave plasma chemical vapor deposition apparatus to vacuum by using a vacuum pump.
6. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: the gas preparation in the step S5 is to introduce a mixed gas of methane and hydrogen as a reaction gas into the microwave plasma chemical vapor deposition apparatus.
7. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: the high methane concentration deposition in the step S5 is carried out under the condition that the flow of the introduced hydrogen is unchanged, and the flow of the introduced methane is 3-5 sccm.
8. The method for preparing a nano-diamond film using a microwave plasma chemical vapor deposition method according to claim 1, wherein: the low-methane-concentration deposition in the step S5 is carried out under the condition that the flow of the introduced hydrogen is unchanged, the flow of the introduced methane is 1-2 sccm, and the deposition time is 185 min.
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| US5188862A (en) * | 1989-09-26 | 1993-02-23 | Idemitsu Petrochemical Company Limited | Microwave plasma generating apparatus and process for the preparation of diamond thin film utilizing same |
| CN102965666A (en) * | 2012-11-27 | 2013-03-13 | 郑州大学 | Flexible substrate nanometer diamond film and preparation method thereof |
| CN109811303A (en) * | 2019-01-23 | 2019-05-28 | 上海大学 | Nano-diamond film preparation method based on DLC film middle layer |
| CN111005004A (en) * | 2019-12-13 | 2020-04-14 | 昆明理工大学 | Method for preparing nano-diamond film by using methanol-argon |
| US20210140038A1 (en) * | 2018-03-29 | 2021-05-13 | Ningb0 Institute Of Materials Technology & Engineering, Chinese Academy Of Sciences | Self-supporting ultra-fine nanocrystalline diamond thick film |
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|---|---|---|---|---|
| US5188862A (en) * | 1989-09-26 | 1993-02-23 | Idemitsu Petrochemical Company Limited | Microwave plasma generating apparatus and process for the preparation of diamond thin film utilizing same |
| CN102965666A (en) * | 2012-11-27 | 2013-03-13 | 郑州大学 | Flexible substrate nanometer diamond film and preparation method thereof |
| US20210140038A1 (en) * | 2018-03-29 | 2021-05-13 | Ningb0 Institute Of Materials Technology & Engineering, Chinese Academy Of Sciences | Self-supporting ultra-fine nanocrystalline diamond thick film |
| CN109811303A (en) * | 2019-01-23 | 2019-05-28 | 上海大学 | Nano-diamond film preparation method based on DLC film middle layer |
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