CN111118471A - Preparation method of high-quality polycrystalline diamond film - Google Patents

Preparation method of high-quality polycrystalline diamond film Download PDF

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CN111118471A
CN111118471A CN202010040561.XA CN202010040561A CN111118471A CN 111118471 A CN111118471 A CN 111118471A CN 202010040561 A CN202010040561 A CN 202010040561A CN 111118471 A CN111118471 A CN 111118471A
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diamond film
diamond
polycrystalline diamond
film
growth
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李红东
万琳丰
王旌丞
成绍恒
王启亮
刘钧松
高楠
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Jilin University
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Jilin University
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C16/44—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
    • C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C16/44—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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C16/56—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
    • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64—Flat crystals, e.g. plates, strips or discs

Abstract

The invention discloses a preparation method of a high-quality polycrystalline diamond film, and belongs to the technical field of polycrystalline diamond film growth. The main steps include the growth of low-quality self-supporting chemical vapor deposition diamond film, high-temperature annealing, ultrasonic cleaning, secondary growth in MPCVD equipment, etc. The invention firstly obtains the self-supporting diamond film through the high-speed growth process, and then continues to grow to obtain the high-quality film after high-temperature annealing. The method can greatly improve the preparation efficiency of the self-supporting diamond film and is beneficial to promoting the expansion of the application of the diamond.

Description

Preparation method of high-quality polycrystalline diamond film
Technical Field
The invention belongs to the technical field of polycrystalline diamond film growth, and particularly relates to a preparation method of a high-quality polycrystalline diamond film.
Background
Diamond is a very important wide bandgap (Eg-5.5 eV) semiconductor material, and has many excellent properties, such as: the diamond has the advantages of extremely high breakdown electric field, power quality factor and electron and hole mobility, can realize n-type and p-type conductivity through doping, highest room temperature thermal conductivity, extremely low thermal expansion coefficient, anti-irradiation property, very strong chemical stability and the like, and the excellent properties enable the diamond to be applied to solar blind deep ultraviolet detectors, monitoring and detection of high-energy particles such as X rays, nuclear radiation and the like, high-power electronic devices, microwave power devices and the like. As an important third-generation semiconductor material, the diamond can be widely applied to the fields of aerospace, national defense and military industry and the like such as optics, microelectronics, nuclear energy and the like, and has an irreplaceable important position of other materials.
Among diamond film materials, the micron-sized diamond film is the earliest and is the most widely applied polycrystalline diamond film material at present. Large area polycrystalline diamond is more readily available and the cost of deposition is relatively low compared to single crystal diamond. High-quality polycrystalline diamond films are currently used in a plurality of fields such as cutting tools, heat sinks, optical windows and the like. The common method for preparing high-quality polycrystalline diamond film is Microwave Plasma Chemical Vapor Deposition (MPCVD), which utilizes microwave to excite deposition gas to generate glow discharge in a reaction chamber, ionizes molecules of the reaction gas to generate plasma, and deposits on a substrate to obtain the diamond film. In the whole preparation process, the electron density in the plasma is high, the atomic hydrogen concentration is high, the maximum kinetic energy of ions is low, and stable plasma can be obtained under higher pressure, so that the preparation method has obvious advantages in the aspect of depositing large-area diamond films. Meanwhile, the MPCVD method has the advantages of low deposition temperature, concentrated discharge area without diffusion, no gas pollution and electrode pollution, stable work, easy and accurate control, high deposition speed, being beneficial to nucleation and the like, thereby being the best method for preparing the high-quality diamond film. Silicon and molybdenum are the most widely used substrate materials for making polycrystalline diamond free-standing films. As belonging to the heteroepitaxy process, the concentration of the carbon source is generally lower in the process of preparing the high-quality diamond polycrystalline film so as to maintain the growth rate of the film at a lower level and ensure the crystal quality of the film. Generally speaking, increasing the methane content in the growth atmosphere and introducing a proper amount of nitrogen can effectively increase the deposition rate of the diamond film, but the high deposition rate often causes the quality of the diamond film to be reduced, and generally shows that obvious grain boundaries exist among diamond grains. A large amount of non-diamond such as amorphous carbon, graphite and the like at the grain boundary can greatly reduce the performances such as the heat conductivity, the wear resistance and the like of the diamond film. In this case, the growth rate of high quality polycrystalline diamond film is typically below 5 microns per hour, and the deposition time often takes several days to obtain a self-supporting diamond film. This makes the film preparation less efficient, which affects its practical application. Therefore, there is a need to develop a new method for efficiently obtaining high quality self-supporting diamond polycrystalline film.
Disclosure of Invention
The invention aims to overcome the defects in the background art and provide a novel method for preparing a high-quality polycrystalline diamond film. Firstly, preparing a low-quality self-supporting diamond polycrystalline film at a high speed under the condition of high methane concentration and other parameters, then removing non-diamond phases in the film grain boundary by using a high-temperature oxidation method, and finally depositing under the condition of low-speed growth to finally obtain the self-supporting high-quality diamond polycrystalline film.
The method utilizes a high-speed growth process to obtain the low-quality diamond polycrystalline film, and utilizes a high-temperature oxidation method to eliminate non-diamond phases among grains, and the retained diamond grains can be used as an epitaxial growth substrate for further growth. Therefore, when the diamond is further prepared by using low-speed growth parameters, the process is homoepitaxial growth, the nucleation and growth speed is relatively high, and the high quality is easy to maintain. The crystal grains remained after the high-temperature treatment still preserve the basic structure of the low-quality self-supporting diamond film, and the crystal grains are connected in the further growth process to obtain the high-quality diamond polycrystalline film with compact structure. Compared with the traditional method, the method can obtain the high-quality self-supporting film in a shorter time, and greatly improve the preparation efficiency.
The technical scheme of the invention is as follows:
a preparation method of a high-quality polycrystalline diamond film comprises the following steps:
1) using a monocrystalline silicon wafer or a molybdenum wafer as a substrate, grinding by using diamond powder, and then using a microwave plasma CVD device to carry out film deposition, wherein the growth parameters are set as follows: the power is 2000-2500W, the pressure is 10-15 Kpa, the substrate temperature is 800-1000 ℃, and the atmosphere is H2:CH4:N2200-500: 5-10: 0.5-2, wherein the gas flow unit is sccm, and the growth time is 10 hours, so as to obtain a self-supporting Chemical Vapor Deposition (CVD) diamond film;
2) placing the obtained self-supporting Chemical Vapor Deposition (CVD) diamond film in a high-temperature annealing furnace, and carrying out high-temperature treatment for 15 min;
3) ultrasonically cleaning the sample treated in the step 2) for 2-3 times by using alcohol, and removing residues among the cylindrical diamonds on the surface (100);
4) placing the treated self-supporting polycrystalline diamond into a cavity of an MPCVD equipment, and setting growth parameters as follows: the power is 2000-2500W, the pressure is 10-15 kPa, the temperature is 800-900 ℃, and the atmosphere H2:CH4And (5-10) the gas flow unit sccm, and the growth time is 5h, so as to obtain the high-quality polycrystalline diamond film.
In the step 1), the diamond powder grinding treatment is specifically to grind for 10 minutes by using diamond powder with the average particle size of less than 1 micron to grind uniform scratches on the surface of the substrate.
In step 2), the treatment temperature is preferably 800 ℃ and the treatment atmosphere is air.
The method adopts the mode of growth → high-temperature oxidation → growth for the first time to obtain the high-quality polycrystalline diamond film material. The invention firstly obtains the self-supporting diamond film through the high-speed growth process, and then continues to grow to obtain the high-quality film after high-temperature annealing. The method can greatly improve the preparation efficiency of the self-supporting diamond film and is beneficial to promoting the expansion of the application of the diamond.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) front view of a low-quality self-supporting polycrystalline diamond film prepared in step 1) of example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) cross-sectional photograph of the low-quality self-supporting polycrystalline diamond film prepared in step 1) of example 1.
FIG. 3 is a Scanning Electron Microscope (SEM) cross-sectional photograph of the textured free-standing polycrystalline diamond film after step 2) high temperature annealing of example 1.
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a high-quality free-standing polycrystalline diamond film obtained by secondary growth by the MPCVD method in step 3) of example 1.
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of a low-quality self-supporting polycrystalline diamond film prepared in step 1) of example 2.
FIG. 6 is a cross-sectional Scanning Electron Microscope (SEM) photograph of the textured free-standing polycrystalline diamond film after high temperature annealing at step 2) of example 2.
FIG. 7 is a Scanning Electron Microscope (SEM) photograph of a high-quality free-standing polycrystalline diamond film obtained by secondary growth by the MPCVD method in step 3) of example 2.
Detailed Description
The present application is described in further detail below with reference to the accompanying drawings and examples, which are intended to facilitate the understanding of the present application and are not intended to limit the same in any way.
Example 1
1) Preparing a low-quality self-supporting polycrystalline diamond film: using molybdenum as a substrate, grinding diamond powder with the average particle size of less than 1 micron for 10 minutes before growth to grind uniform scratches on the surface of the substrate, cleaning the ground surface by using absolute alcohol, and drying the ground surface. Using microwave plasmaBulk CVD apparatus, film deposition, growth parameters: gas pressure of 15kPa, power of 2000W, temperature of 800 ℃ and gas flow proportion H2∶CH4∶N2Deposition time 10h at 500: 10: 1(sccm) to obtain a textured free-standing CVD polycrystalline diamond film (100). Sample morphology is shown in FIG. 1 and FIG. 2. It can be seen that the sample is due to N2Has a high (100) orientation, a grain size of about 40 microns, a film thickness of about 140 microns, and a growth rate of about 14 microns/hour. It can be seen that there is a clear demarcation between grains and a large number of non-diamond structures. This shows that under the parameters, the growth speed of the diamond film is fast, but the non-diamond phase in the film is more and the quality is lower,
2) putting the diamond film obtained in the step 1) into a tube furnace, and annealing for 15 minutes at 800 ℃ in an air atmosphere. The morphology of the diamond film obtained after the treatment is shown in figure 3. It can be seen that the diamond grains remain after the high temperature treatment, but there are many gaps between the grains, because the oxidation resistance of diamond is stronger than that of non-diamond phases such as amorphous carbon, graphite, etc., and therefore non-diamond components are removed at the grain boundaries after the high temperature treatment.
3) Taking the polycrystalline diamond film obtained in the step 2) as a substrate, and carrying out secondary growth by an MPCVD method. The growth parameters were as follows: power 2kW, pressure 10kPa, substrate temperature 800 ℃ and atmosphere H2:CH4Growth time was about 5h at 500: 5. As shown in FIG. 4, the obtained high quality self-supporting Chemical Vapor Deposition (CVD) diamond film has complete and compact surface grains, no obvious non-diamond phase among grains, and different grain sizes, because the original grains continue to grow in the secondary growth process and the grains are filled with small grains.
Example 2
1) Preparing a low-quality self-supporting polycrystalline diamond film: using molybdenum as a substrate, grinding diamond powder with the average particle size of less than 1 micron for 10 minutes before growth to grind uniform scratches on the surface of the substrate, cleaning the ground surface by using absolute alcohol, and drying the ground surface. Using microwave plasma CVD device to deposit film and grow ginsengNumber: gas pressure 10kPa, power 2500W, temperature 900 deg.C, gas flow ratio H2∶CH4∶N2Deposition time 10h at 500: 20: 1(sccm) yielded a (100) textured free-standing CVD polycrystalline diamond film. The sample morphology is shown in FIG. 5. It can be seen that the crystal grains on the surface of the sample show (100) orientation, the size of the crystal grains is about 30 microns, obvious boundaries exist among the crystal grains, the shapes of the boundaries are irregular, and the crystal grains are of non-diamond structures in the crystal boundaries.
2) Putting the diamond film obtained in the step 1) into a tube furnace, and annealing for 15 minutes at 800 ℃ in an air atmosphere. The morphology of the diamond film obtained after the treatment is shown in figure 6. It can be seen that the diamond grains remain after the high temperature treatment, but there are many voids between the grains.
3) Taking the polycrystalline diamond film obtained in the step 2) as a substrate, and carrying out secondary growth by an MPCVD method. The growth parameters are as follows, power is 2kW, pressure is 10kPa, substrate temperature is 900 ℃, and atmosphere H2:CH4The growth time is about 5h at 500: 10. As shown in FIG. 7, the obtained high-quality self-supporting Chemical Vapor Deposition (CVD) diamond film has the advantages of different grain sizes on the surface of the film, complete crystal form, compact grains and no obvious non-diamond phase at the grain boundary.

Claims (3)

1. A preparation method of a high-quality polycrystalline diamond film comprises the following steps:
1) using a monocrystalline silicon wafer or a molybdenum wafer as a substrate, grinding by using diamond powder, and then using a microwave plasma CVD device to carry out film deposition, wherein the growth parameters are set as follows: the power is 2000-2500W, the pressure is 10-15 Kpa, the substrate temperature is 800-1000 ℃, and the atmosphere is H2:CH4:N2200-500: 5-10: 0.5-2, wherein the unit of gas flow is sccm, and the growth time is 10 hours, so as to obtain a self-supporting chemical vapor deposition diamond film;
2) placing the obtained self-supporting chemical vapor deposition diamond film in a high-temperature annealing furnace, and carrying out high-temperature treatment for 15 min;
3) ultrasonically cleaning the sample treated in the step 2) for 2-3 times by using alcohol, and removing residues among the cylindrical diamonds on the surface (100);
4) placing the treated self-supporting polycrystalline diamond into a cavity of an MPCVD equipment, and setting growth parameters as follows: the power is 2000-2500W, the pressure is 10-15 kPa, the temperature is 800-900 ℃, and the atmosphere H2:CH4And (5-10) the gas flow unit sccm, and the growth time is 5h, so as to obtain the high-quality polycrystalline diamond film.
2. The method for preparing a high-quality polycrystalline diamond film according to claim 1, wherein in the step 1), the diamond powder grinding treatment is to grind uniform scratches on the surface of the substrate by using diamond powder with an average particle size of less than 1 μm for 10 minutes.
3. The method for producing a high-quality polycrystalline diamond film according to claim 1, wherein in the step 2), the treatment temperature is 800 ℃ and the treatment atmosphere is air.
CN202010040561.XA 2020-01-15 2020-01-15 Preparation method of high-quality polycrystalline diamond film Pending CN111118471A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112760612A (en) * 2020-12-28 2021-05-07 吉林工程技术师范学院 Preparation method of self-supporting nano-needle porous diamond
CN112941487A (en) * 2021-02-08 2021-06-11 河北普莱斯曼金刚石科技有限公司 Polycrystalline diamond thick film for microwave energy transmission window and preparation method thereof
CN113005517A (en) * 2021-02-25 2021-06-22 廊坊西波尔钻石技术有限公司 Treatment method for reducing internal stress of single crystal diamond
CN114197042A (en) * 2021-11-19 2022-03-18 西安电子科技大学芜湖研究院 Preparation method of polycrystalline diamond film and radiation detector
CN114318531A (en) * 2022-01-06 2022-04-12 济南金刚石科技有限公司 Stripping method applied to MPCVD large-size diamond polycrystal

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103482623A (en) * 2013-09-05 2014-01-01 大连理工大学 Method for preparing nano diamonds by using direct-current arc process
CN109911894A (en) * 2019-03-31 2019-06-21 河北地质大学 The method of MPCVD method growth polycrystalline diamond flag

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103482623A (en) * 2013-09-05 2014-01-01 大连理工大学 Method for preparing nano diamonds by using direct-current arc process
CN109911894A (en) * 2019-03-31 2019-06-21 河北地质大学 The method of MPCVD method growth polycrystalline diamond flag

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112760612A (en) * 2020-12-28 2021-05-07 吉林工程技术师范学院 Preparation method of self-supporting nano-needle porous diamond
CN112760612B (en) * 2020-12-28 2022-07-01 吉林工程技术师范学院 Preparation method of self-supporting nano-needle porous diamond
CN112941487A (en) * 2021-02-08 2021-06-11 河北普莱斯曼金刚石科技有限公司 Polycrystalline diamond thick film for microwave energy transmission window and preparation method thereof
CN112941487B (en) * 2021-02-08 2023-08-04 河北普莱斯曼金刚石科技有限公司 Polycrystalline diamond thick film for microwave energy transmission window and preparation method thereof
CN113005517A (en) * 2021-02-25 2021-06-22 廊坊西波尔钻石技术有限公司 Treatment method for reducing internal stress of single crystal diamond
CN114197042A (en) * 2021-11-19 2022-03-18 西安电子科技大学芜湖研究院 Preparation method of polycrystalline diamond film and radiation detector
CN114318531A (en) * 2022-01-06 2022-04-12 济南金刚石科技有限公司 Stripping method applied to MPCVD large-size diamond polycrystal

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Application publication date: 20200508