CN111235637A - Method for removing amorphous carbon on surface of CVD diamond - Google Patents

Method for removing amorphous carbon on surface of CVD diamond Download PDF

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Publication number
CN111235637A
CN111235637A CN202010108245.1A CN202010108245A CN111235637A CN 111235637 A CN111235637 A CN 111235637A CN 202010108245 A CN202010108245 A CN 202010108245A CN 111235637 A CN111235637 A CN 111235637A
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amorphous carbon
diamond
potassium dichromate
cvd diamond
cvd
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Inventor
舒国阳
代兵
朱嘉琦
刘康
曹文鑫
赵继文
李一村
韩杰才
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Harbin Institute of Technology
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Harbin 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
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a method for removing amorphous carbon on the surface of a CVD diamond, belonging to the technical field of crystal growth. The invention aims to solve the problems that the existing method for removing amorphous carbon on the surface of a CVD diamond has low cost and low efficiency, can damage or even crack a treated material and a test piece, and cannot remove the amorphous carbon on the surface of the diamond with special structure and appearance. The method comprises the following steps: firstly, ultraviolet light irradiation; secondly, preparing a solution; and thirdly, heating treatment. The method is used for removing the amorphous carbon on the surface of the CVD diamond.

Description

Method for removing amorphous carbon on surface of CVD diamond
Technical Field
The invention belongs to the technical field of crystal growth.
Background
In recent years, large-size diamond materials are becoming basic, critical and even unique material solutions in high-tech fields such as precision machining, high-frequency communication, aerospace, advanced technology and the like due to extremely high hardness, highest thermal conductivity, extremely wide electromagnetic transmission frequency range and excellent anti-irradiation capability and corrosion resistance. The traditional artificial diamond adopts a high temperature High Pressure (HPHT) method, and the diamond prepared by the method has more impurities, higher defect density, relatively poorer quality and smaller size, and is far different from the requirements of related applications, so that the HPHT diamond has the defects of narrower application range, low profit and low competitiveness in the downstream of the industry.
Compared with the HPHT method, the microwave plasma-assisted chemical vapor deposition (MPCVD) method is one of the best methods for preparing large-size diamond which is generally accepted at present, the diamond prepared by the method has the advantages of low impurity concentration, wide transmission waveband, low defect density, large size, controllable growth rate and the like, and various crystalline diamond films with large areas can be prepared, so that the method is considered to be the most promising method for producing artificial diamond in large scale in the future.
After the method is used for epitaxially growing the diamond, the concentration of hydrogen plasma on certain surfaces of a diamond sample is too low in the growth process, so that amorphous carbon sp is generated2The phase can not be effectively removed by etching, so that a large amount of amorphous carbon is remained on the surface, the grown diamond is black, the original excellent optical performance of the diamond is completely lost, and the original excellent characteristics of extremely high mechanical strength, excellent dielectric performance and the like of the diamond material are also lost.
The traditional amorphous carbon removing method is mechanical polishing, a large amount of time and grinding materials are consumed, the cost is greatly wasted, the efficiency is low, certain mechanical damage and even breakage can be caused to a treated material and a test piece, and the existing industrial production requirements cannot be met completely. Furthermore, for diamond articles of particular structure and morphology, this method is completely unsuitable and it is desirable to find a new way to effectively remove the amorphous carbon layer from the outer surface of diamond articles prepared by CVD.
Disclosure of Invention
The invention provides a method for removing amorphous carbon on the surface of a CVD diamond, aiming at solving the problems that the existing method for removing the amorphous carbon on the surface of the CVD diamond has low cost and low efficiency, can damage or even crack a processed material and a test piece, and cannot remove the amorphous carbon on the surface of the diamond with special structure and appearance.
A method for removing amorphous carbon on the surface of CVD diamond is carried out according to the following steps:
firstly, ultraviolet light irradiation:
placing the diamond sample with the surface attached with the amorphous carbon under an ultraviolet lamp, and irradiating the amorphous carbon layer on the surface of the diamond sample for 1-100 min under the conditions that the wavelength is 100-400 nm and the power is 50-1000W, so as to obtain the diamond sample after ultraviolet treatment;
secondly, preparing a solution:
adding potassium dichromate powder into deionized water, stirring, adding 70-98% concentrated sulfuric acid by mass percent at the adding speed of 0.01-10 mL/s, and continuously stirring until the potassium dichromate is dissolved to obtain a red-black potassium dichromate solution;
the volume ratio of the mass of the potassium dichromate powder to the deionized water is 1g (1-1000) mL; the volume ratio of the potassium dichromate powder to concentrated sulfuric acid with the mass percent of 70-98% is 1g (1-1000) mL;
thirdly, heating treatment:
and placing the diamond sample subjected to ultraviolet treatment in a red-black potassium dichromate solution, sealing, then preserving the heat for 1-60 min at the constant temperature of 50-100 ℃ to obtain a diamond sample subjected to heat treatment, and finally cleaning the diamond sample subjected to heat treatment by using clean water to finish the method for removing the amorphous carbon on the surface of the CVD diamond.
The invention has the beneficial effects that: 1. the method adopts the method of sequentially and cooperatively treating the ultraviolet light and the hot solution, can effectively and completely remove the amorphous carbon attached to the surface of the diamond grown by the CVD method, and ensures that the obtained diamond recovers the excellent optical transmittance, hardness and wear resistance.
2. The method can finish the removal in a short time, can quickly remove the amorphous carbon attached to the surface of the diamond grown by the CVD method within 2min, and greatly saves the time cost.
3. The method can remove the amorphous carbon in ultraviolet and solution, can treat diamond products with various special shapes, and solves the problem that the traditional methods such as mechanical polishing and the like can not treat the amorphous carbon attached to the non-planar diamond products.
4. The invention can not cause mechanical damage to the processed material in the processing process.
The method is used for removing the amorphous carbon on the surface of the CVD diamond.
Drawings
FIG. 1 is a diagram of a sample diamond with amorphous carbon attached to the surface thereof in a first step of the example;
FIG. 2 is a diagram of a diamond sample with amorphous carbon removed from the surface obtained in step three of the example;
FIG. 3 is a Raman spectrum; 1 is a diamond sample with amorphous carbon attached to the surface in the first step of the example, and 2 is a diamond sample with amorphous carbon removed from the surface obtained in the third step of the example.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the method for removing the amorphous carbon on the surface of the CVD diamond according to the embodiment is carried out according to the following steps:
firstly, ultraviolet light irradiation:
placing the diamond sample with the surface attached with the amorphous carbon under an ultraviolet lamp, and irradiating the amorphous carbon layer on the surface of the diamond sample for 1-100 min under the conditions that the wavelength is 100-400 nm and the power is 50-1000W, so as to obtain the diamond sample after ultraviolet treatment;
secondly, preparing a solution:
adding potassium dichromate powder into deionized water, stirring, adding 70-98% concentrated sulfuric acid by mass percent at the adding speed of 0.01-10 mL/s, and continuously stirring until the potassium dichromate is dissolved to obtain a red-black potassium dichromate solution;
the volume ratio of the mass of the potassium dichromate powder to the deionized water is 1g (1-1000) mL; the volume ratio of the potassium dichromate powder to concentrated sulfuric acid with the mass percent of 70-98% is 1g (1-1000) mL;
thirdly, heating treatment:
and placing the diamond sample subjected to ultraviolet treatment in a red-black potassium dichromate solution, sealing, then preserving the heat for 1-60 min at the constant temperature of 50-100 ℃ to obtain a diamond sample subjected to heat treatment, and finally cleaning the diamond sample subjected to heat treatment by using clean water to finish the method for removing the amorphous carbon on the surface of the CVD diamond.
The beneficial effects of the embodiment are as follows: 1. the method of sequentially and cooperatively processing the ultraviolet light and the hot solution is adopted in the embodiment, amorphous carbon attached to the surface of the diamond grown by the CVD method can be effectively and completely removed, and the obtained diamond recovers excellent optical transmittance, hardness and wear resistance.
2. The method can finish the removal in a short time, can quickly remove the amorphous carbon attached to the surface of the diamond grown by the CVD method in 2min, and greatly saves the time cost.
3. Because the embodiment removes the amorphous carbon in the ultraviolet and solution, diamond products with various special shapes can be treated, and the problem that the amorphous carbon attached to the non-planar diamond products cannot be treated by the traditional methods such as mechanical polishing and the like is solved.
4. The embodiment does not cause mechanical damage to the material to be processed in the processing process.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the amorphous carbon layer on the surface of the diamond sample is irradiated for 1-100 min under the conditions of a single wave band with the wavelength of 300nm and the power of 50-1000W. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: in the first step, the amorphous carbon layer on the surface of the diamond sample is irradiated for 1-100 min under the conditions that the wave bands with the wavelengths of 250nm, 300nm and 320nm and the power are 50-1000W. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the first step, the amorphous carbon layer on the surface of the diamond sample is irradiated for 60-100 min under the conditions that the wavelength is within 100-400 nm and the power is 50-1000W at one or more wave bands. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the purity of the potassium dichromate powder in the step two is 90-99.99%. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the volume ratio of the mass of the potassium dichromate powder to the deionized water in the second step is 1g (1-10) mL. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the volume ratio of the potassium dichromate powder in the second step to concentrated sulfuric acid with the mass percent of 70-98% is 1g (1-10) mL. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and in the second step, concentrated sulfuric acid with the mass percent of 70-98% is added at the adding speed of 0.1-10 mL/s and is continuously stirred until the potassium dichromate is dissolved. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and in the third step, the temperature is kept for 15-60 min under the condition that the constant temperature is 50-100 ℃. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and in the third step, the temperature is kept for 1-15 min under the condition that the constant temperature is 50-100 ℃. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a method for removing amorphous carbon on the surface of CVD diamond is carried out according to the following steps:
firstly, ultraviolet light irradiation:
placing the diamond sample with the surface attached with the amorphous carbon under an ultraviolet lamp, and irradiating the amorphous carbon layer on the surface of the diamond sample for 60min under the conditions that the wavelengths are 250nm, 300nm and 320nm and the power is 1000W to obtain the diamond sample after ultraviolet treatment;
secondly, preparing a solution:
adding 10g of potassium dichromate powder into 100mL of deionized water, stirring, adding 100mL of 98% concentrated sulfuric acid at the adding speed of 0.1mL/s, and continuously stirring until the potassium dichromate is dissolved to obtain a red-black potassium dichromate solution;
thirdly, heating treatment:
and placing the diamond sample subjected to ultraviolet treatment in a red-black potassium dichromate solution, sealing, then preserving the temperature for 15min at the constant temperature of 100 ℃ to obtain a diamond sample subjected to heat treatment, and finally washing the diamond sample subjected to heat treatment with clean water to obtain the diamond sample with the amorphous carbon on the surface removed.
The thickness of the amorphous carbon layer in the diamond sample with the amorphous carbon attached to the surface in the first step is about 5 microns.
FIG. 1 is a diagram of a sample diamond with amorphous carbon attached to the surface thereof in a first step of the example; FIG. 2 is a diagram of a diamond sample with amorphous carbon removed from the surface obtained in step three of the example; as can be seen, the surface-attached amorphous carbon has been removed, restoring the transparency and luster of the diamond, and the dark areas at the edges and corners are other crystal planes different from the large surface, and have weaker light reflection.
FIG. 3 is a Raman spectrum; 1 is a diamond sample with amorphous carbon attached to the surface in the first step of the embodiment, and 2 is a diamond sample with amorphous carbon removed from the surface obtained in the third step of the embodiment; as can be seen, the Raman spectrum results after the treatment according to the first embodiment showed a characteristic peak (1332 cm) of diamond-1) Has an increased relative intensity, a narrow full width at half maximum, and represents a G peak (1580 cm) of the amorphous carbon phase-1) Disappearance, evidencing removal of amorphous carbon.

Claims (10)

1. A method for removing amorphous carbon on the surface of CVD diamond is characterized by comprising the following steps:
firstly, ultraviolet light irradiation:
placing the diamond sample with the surface attached with the amorphous carbon under an ultraviolet lamp, and irradiating the amorphous carbon layer on the surface of the diamond sample for 1-100 min under the conditions that the wavelength is 100-400 nm and the power is 50-1000W, so as to obtain the diamond sample after ultraviolet treatment;
secondly, preparing a solution:
adding potassium dichromate powder into deionized water, stirring, adding 70-98% concentrated sulfuric acid by mass percent at the adding speed of 0.01-10 mL/s, and continuously stirring until the potassium dichromate is dissolved to obtain a red-black potassium dichromate solution;
the volume ratio of the mass of the potassium dichromate powder to the deionized water is 1g (1-1000) mL; the volume ratio of the potassium dichromate powder to concentrated sulfuric acid with the mass percent of 70-98% is 1g (1-1000) mL;
thirdly, heating treatment:
and placing the diamond sample subjected to ultraviolet treatment in a red-black potassium dichromate solution, sealing, then preserving the heat for 1-60 min at the constant temperature of 50-100 ℃ to obtain a diamond sample subjected to heat treatment, and finally cleaning the diamond sample subjected to heat treatment by using clean water to finish the method for removing the amorphous carbon on the surface of the CVD diamond.
2. A CVD diamond surface amorphous carbon removing method according to claim 1, wherein in the first step, the amorphous carbon layer on the diamond sample surface is irradiated for 1min to 100min under the condition that the wavelength is 300nm and the power is 50W to 1000W.
3. A CVD diamond surface amorphous carbon removing method according to claim 1, wherein in the first step, the amorphous carbon layer on the diamond sample surface is irradiated for 1min to 100min under the condition that the wavelength is 250nm, 300nm and 320nm, the plurality of wave bands and the power are 50W to 1000W.
4. A CVD diamond surface amorphous carbon removing method according to claim 1, wherein in the first step, the amorphous carbon layer on the diamond sample surface is irradiated for 60min to 100min under the condition that the wavelength is within a single wave band or a plurality of wave bands within a range of 100nm to 400nm and the power is 50W to 1000W.
5. A CVD diamond surface amorphous carbon removal method according to claim 1, wherein the purity of the potassium dichromate powder in the second step is 90% -99.99%.
6. A CVD diamond surface amorphous carbon removal method according to claim 1, characterized in that the volume ratio of the mass of the potassium dichromate powder to the deionized water in the second step is 1g (1-10) mL.
7. A CVD diamond surface amorphous carbon removing method according to claim 1, characterized in that the volume ratio of the potassium dichromate powder in the second step to concentrated sulfuric acid with the mass percent of 70% -98% is 1g (1-10) mL.
8. A CVD diamond surface amorphous carbon removing method according to claim 1, characterized in that in the second step, concentrated sulfuric acid with a mass percentage of 70% -98% is added at an adding speed of 0.1-10 mL/s and is continuously stirred until potassium dichromate is dissolved.
9. A CVD diamond surface amorphous carbon removing method according to claim 1, characterized in that in the third step, the temperature is kept at 50-100 ℃ for 15-60 min.
10. A CVD diamond surface amorphous carbon removing method according to claim 1, characterized in that in the third step, the temperature is kept for 1min to 15min at a constant temperature of 50 ℃ to 100 ℃.
CN202010108245.1A 2020-02-21 2020-02-21 Method for removing amorphous carbon on surface of CVD diamond Pending CN111235637A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0648893A (en) * 1992-07-30 1994-02-22 Matsushita Electric Ind Co Ltd Method for surface-treating diamond
CN1400162A (en) * 2001-07-31 2003-03-05 中国科学院兰州化学物理研究所 Method for purifying synthetic diamond semi-finished product containing non-diamond carbon
CN101618868A (en) * 2008-07-03 2010-01-06 中国科学院成都有机化学有限公司 Method for removing amorphous carbon in carbon nanotubes
CN102888584A (en) * 2012-09-17 2013-01-23 上海大学 Method for depositing CdTe thin film based on diamond thin film
CN107128908A (en) * 2017-04-17 2017-09-05 安徽卡尔森新材料科技有限公司 The potent pre-treating method of diamond super fine

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0648893A (en) * 1992-07-30 1994-02-22 Matsushita Electric Ind Co Ltd Method for surface-treating diamond
CN1400162A (en) * 2001-07-31 2003-03-05 中国科学院兰州化学物理研究所 Method for purifying synthetic diamond semi-finished product containing non-diamond carbon
CN101618868A (en) * 2008-07-03 2010-01-06 中国科学院成都有机化学有限公司 Method for removing amorphous carbon in carbon nanotubes
CN102888584A (en) * 2012-09-17 2013-01-23 上海大学 Method for depositing CdTe thin film based on diamond thin film
CN107128908A (en) * 2017-04-17 2017-09-05 安徽卡尔森新材料科技有限公司 The potent pre-treating method of diamond super fine

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