CN107937980B - Method for growing single crystal diamond by using human hair as carbon source by using double-substrate-table MPCVD (multi-phase plasma CVD) device - Google Patents

Method for growing single crystal diamond by using human hair as carbon source by using double-substrate-table MPCVD (multi-phase plasma CVD) device Download PDF

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CN107937980B
CN107937980B CN201711250553.2A CN201711250553A CN107937980B CN 107937980 B CN107937980 B CN 107937980B CN 201711250553 A CN201711250553 A CN 201711250553A CN 107937980 B CN107937980 B CN 107937980B
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crystal diamond
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hair
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CN107937980A (en
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马志斌
耿传文
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Wuhan Institute of Technology
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    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • 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
    • C23C16/276—Diamond only using plasma jets
    • 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
    • C23C16/279—Diamond only control of diamond crystallography
    • 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
    • C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • 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

Abstract

The invention discloses a method for growing single crystal diamond by using human hair as a carbon source by using a double-substrate-table MPCVD reaction device, which comprises the following steps: firstly, providing human hair, a single crystal diamond substrate and a double-substrate-table MPCVD reaction device; secondly, placing the single crystal diamond substrate at the groove of the lower substrate table, binding human hair into a hair bundle, and placing the hair bundle in the central hole of the upper substrate table through a conveying device; introducing hydrogen into the reaction device to generate microwave plasma, adjusting the technological parameters of the device, enabling the hair bundle to extend out of the central hole of the upper substrate table at a certain speed and enter the plasma to be etched, and simultaneously growing single crystal diamond; fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source; the method adopts a microwave plasma chemical vapor deposition method to synthesize the single crystal diamond, takes hair as a carbon source, and grows the single crystal diamond while etching human hair in a cavity of a double-substrate MPCVD reaction device.

Description

Method for growing single crystal diamond by using human hair as carbon source by using double-substrate-table MPCVD (multi-phase plasma CVD) device
Technical Field
The invention relates to the technical field of diamond preparation, in particular to a method for growing single crystal diamond by using human hair as a carbon source by using a double-substrate-table MPCVD reaction device.
Background
Diamond is the hardest material known in the world at present, and has a series of physicochemical properties such as high hardness, high melting point, good sound propagation speed, heat conduction, high elastic mold and good biocompatibility, and is receiving attention. At present, the growth of the single crystal diamond mainly takes the introduction of methane and hydrogen as main gases, and can selectively introduce gases such as nitrogen, oxygen and the like. The hair contains keratin as main component 97%, which is composed of amino acids with carbon content over 60% and containing small amount of nitrogen and oxygen. The current technology of converting hair into carbon source gas mainly adopts the technology of generating plasma by arc discharge, and the generated plasma has the problems of difficulty in density adjustment, low power, low efficiency of absorbing energy by electrons and the like.
Based on the above phenomena and problems, there is a need for a method that can combine the gasification of hair and the deposition of diamond in one reaction chamber, and can effectively grow single crystal diamond by using human hair as a carbon source without introducing new impurities during the gasification of hair.
Disclosure of Invention
Based on the defects of the prior art, the technical problem to be solved by the invention is to provide a double-substrate-table MPCVD reaction device, which can integrate the hair gasification and the diamond deposition in one reaction chamber, and can effectively grow the single crystal diamond by taking human hair as a carbon source without introducing new impurities in the hair gasification process.
In order to solve the technical problems, the invention provides a method for growing single crystal diamond by using human hair as a carbon source by using a double-substrate-table MPCVD reaction device, which comprises the following steps:
firstly, preparing a double-substrate-table MPCVD reaction device, a single-crystal diamond substrate and clean and dry human hair;
secondly, tying hair into hair bundles, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a reaction cavity of the double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of a deposition device, extending hairs into the plasma through a conveying device and etching the hairs, and growing single-crystal diamond by using the generated carbon source gas;
and fourthly, cutting off the single crystal substrate by utilizing laser to obtain the single crystal diamond prepared by taking human hair as a carbon source.
Preferably, the method for growing the single crystal diamond by using the double substrate stage MPCVD reaction device to use human hair as a carbon source further comprises a part or all of the following technical features:
as an improvement of the technical scheme, in the double-substrate-table MPCVD reaction device in the first step, the center of the upper substrate table is provided with a through hole with the diameter of 2-3 mm, and the lower substrate table is provided with a groove for placing the single crystal diamond.
As an improvement of the technical proposal, in the double-substrate-table MPCVD reaction device in the first step, the single crystal diamond substrate can be natural diamond, and can also be CVD diamond or HPHT diamond as a substrate.
As an improvement of the technical proposal, in the double-substrate-table MPCVD reaction device in the first step, the cleanliness of the hair is more than SCP4 level.
As an improvement of the technical scheme, the diameter of the hair bundle in the second step is 1.0-2.5 mm.
As an improvement of the technical scheme, in the third step, the temperature of the lower substrate table is 750-1050 ℃, and the temperature of the upper substrate table is 150-200 ℃.
As an improvement of the technical scheme, in the third step, the hair is enabled to extend into the plasma at the speed of 0.06-0.30 m/h through the conveying device and is etched.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the invention utilizes microwave plasma chemical vapor deposition method to introduce hydrogen to etch the human hair on the substrate table, generates high-concentration carbon source gas with a very small amount of oxygen source gas and nitrogen source gas, and utilizes the generated gas to grow the single crystal diamond on the substrate table. The method can integrate the hair gasification and the diamond deposition in one reaction cavity, and can effectively grow the single crystal diamond by taking human hair as a carbon source without introducing new impurities in the hair gasification process.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1 is a schematic structural view of a double-substrate-stage MPCVD reaction apparatus of the present invention.
In the figure: 1. a conveying device; 2. a reaction chamber; 3. an upper substrate stage; 4. a lower substrate stage; 5. plasma is generated.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
Example 1:
firstly, ultrasonically cleaning human hair and a monocrystalline diamond substrate by using acetone and alcohol, and then drying the cleaned hair;
secondly, tying hair into hair bundles with the diameter of 1.0mm, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of a plasma chemical vapor deposition device, controlling the temperature of a lower substrate table to be 750 ℃ and the temperature of an upper substrate table to be 150 ℃, enabling hairs to extend into the plasma at a certain speed and be etched by a conveying device, and simultaneously carrying out growth of single-crystal diamond, wherein the speed is 0.06 m/h;
fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source;
and characterizing the diamond after the deposition by using Raman spectroscopy to obtain 1332cm-1The full width at half maximum of the characteristic peak.
Example 2:
firstly, ultrasonically cleaning human hair and a monocrystalline diamond substrate by using acetone and alcohol, and then drying the cleaned hair;
secondly, tying hair into hair bundles with the diameter of 1.5mm, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of a plasma chemical vapor deposition device, controlling the temperature of a lower substrate table to be 810 ℃ and the temperature of an upper substrate table to be 155 ℃, enabling hairs to extend into the plasma at a certain speed through a conveying device and etching the hairs at the speed of 0.10m/h, and simultaneously growing single-crystal diamonds;
fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source;
and characterizing the diamond after the deposition by using Raman spectroscopy to obtain 1332cm-1The full width at half maximum of the characteristic peak.
Example 3:
firstly, ultrasonically cleaning human hair and a monocrystalline diamond substrate by using acetone and alcohol, and then drying the cleaned hair;
secondly, tying hair into hair bundles with the diameter of 2.0mm, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of a plasma chemical vapor deposition device, controlling the temperature of a lower substrate table to be 880 ℃ and the temperature of an upper substrate table to be 163 ℃, enabling hairs to extend into the plasma at a certain speed and be etched by a conveying device, and simultaneously carrying out growth of single-crystal diamond, wherein the speed is 0.20 m/h;
fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source;
and characterizing the diamond after the deposition by using Raman spectroscopy to obtain 1332cm-1The full width at half maximum of the characteristic peak.
Example 4:
firstly, ultrasonically cleaning human hair and a monocrystalline diamond substrate by using acetone and alcohol, and then drying the cleaned hair;
secondly, tying hair into hair bundles with the diameter of 2.5mm, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of the plasma chemical vapor deposition device, controlling the temperature of a lower substrate table to be 970 ℃ and the temperature of an upper substrate table to be 187 ℃, enabling hairs to extend into the plasma at a certain speed through a conveying device and be etched, controlling the speed to be 0.25m/h, and simultaneously growing single-crystal diamond;
fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source;
and characterizing the diamond after the deposition by using Raman spectroscopy to obtain 1332cm-1The full width at half maximum of the characteristic peak.
Example 5:
firstly, ultrasonically cleaning human hair and a monocrystalline diamond substrate by using acetone and alcohol, and then drying the cleaned hair;
secondly, tying hair into hair bundles with the diameter of 2.5mm, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of the plasma chemical vapor deposition device, wherein the temperature of a lower substrate table is 1045 ℃, the temperature of an upper substrate table is 200 ℃, and hairs are stretched into the plasma at a certain speed and are etched by a conveying device, and the speed is 0.30 m/h;
fourthly, cutting off the monocrystalline substrate by using laser to obtain monocrystalline diamond prepared by taking human hair as a carbon source;
and characterizing the diamond after the deposition by using Raman spectroscopy to obtain 1332cm-1The full width at half maximum of the characteristic peak.
The quality of the single crystal diamond deposited using the home-made high purity carbon source is good, as shown in table 1, which is the average of five test results (examples 1-5).
TABLE 1 comparison of the quality of single crystal diamonds
Figure RE-BDA0001491625520000081
Table 1 can show that the present invention provides a reaction apparatus using a dual substrate stage MPCVD, in which the hair gasification and diamond deposition are integrated in one reaction chamber, and no new impurities are introduced during the hair gasification, so that the single crystal diamond can be effectively grown from human hair as a carbon source, and the quality of the grown single crystal diamond is equivalent to that of the single crystal diamond grown from methane as a carbon source.
The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.

Claims (7)

1. A method for growing single crystal diamond by using human hair as a carbon source by using a double-substrate-table MPCVD reaction device is characterized by comprising the following steps:
firstly, preparing a double-substrate-table MPCVD reaction device, a single-crystal diamond substrate and clean and dry human hair;
secondly, tying hair into hair bundles, placing the hair bundles into a central circular hole of an upper substrate table through a conveying device, and placing a monocrystalline diamond substrate into a groove of a lower substrate table;
introducing hydrogen into a reaction cavity of the double-substrate-table MPCVD reaction device, exciting gas discharge by using microwaves to generate plasma, adjusting the process parameters of a deposition device, extending hairs into the plasma through a conveying device and etching the hairs, and growing single-crystal diamond by using the generated carbon source gas;
and fourthly, cutting off the single crystal substrate by utilizing laser to obtain the single crystal diamond prepared by taking human hair as a carbon source.
2. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: in the double-substrate-table MPCVD reaction device in the first step, the center of the upper substrate table is provided with a through hole with the diameter of 2-3 mm, and the lower substrate table is provided with a groove for placing the single crystal diamond.
3. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: in the double substrate stage MPCVD reaction apparatus described in the first step, the single crystal diamond substrate may be natural diamond, or may be CVD diamond or HPHT diamond as a substrate.
4. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: in the double-substrate-table MPCVD reaction device in the first step, the cleanliness of the hair is above SCP4 level.
5. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: in the second step, the diameter of the hair bundle is 1.0-2.5 mm.
6. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: in the third step, the temperature of the lower substrate table is 750-1050 ℃, and the temperature of the upper substrate table is 150-200 ℃.
7. The method for growing single crystal diamond according to claim 1 by using human hair as a carbon source using a double substrate stage MPCVD reaction apparatus, wherein: and in the third step, the hair is enabled to extend into the plasma at the speed of 0.06-0.30 m/h through the conveying device and is etched.
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CN111705360A (en) * 2020-06-29 2020-09-25 安徽鑫泰钻石有限公司 Method for producing purified single crystal diamond
CN114059159A (en) * 2021-11-18 2022-02-18 北京大学东莞光电研究院 Diamond growth method
CN115198359A (en) * 2022-07-21 2022-10-18 生命珍宝有限公司 Method for cultivating hair carbon source into diamond by MPCVD device
CN115125614A (en) * 2022-07-21 2022-09-30 生命珍宝有限公司 Technology for recycling carbon source gasified by hairs in process of growing diamond by MPCVD method

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