CN114890416A - Method for preparing nano amorphous diamond - Google Patents
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- CN114890416A CN114890416A CN202210672791.7A CN202210672791A CN114890416A CN 114890416 A CN114890416 A CN 114890416A CN 202210672791 A CN202210672791 A CN 202210672791A CN 114890416 A CN114890416 A CN 114890416A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 115
- 239000010432 diamond Substances 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 23
- 230000005540 biological transmission Effects 0.000 claims abstract description 21
- 238000005520 cutting process Methods 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002159 nanocrystal Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 238000010884 ion-beam technique Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 230000007613 environmental effect Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000011282 treatment Methods 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 230000000284 resting effect Effects 0.000 description 6
- 230000009466 transformation Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing nano amorphous diamond, belonging to the technical field of preparation of diamond materials, comprising the following steps: cutting the crystal diamond to obtain a diamond sheet suitable for observing by a transmission electron microscope, putting the diamond sheet on a power-on heating chip, and applying pulse power-on, lithium embedding and heating to the nano crystal diamond sheet. Compared with the traditional method of converting crystals into amorphous diamond by high pressure, the method has the advantages of complex process, high requirement on processing equipment and high cost. The method of the invention utilizes pulse, electrification and heating, has simple operation, low cost and high efficiency, and can efficiently prepare the amorphous diamond.
Description
Technical Field
The invention relates to the technical field of preparation of diamond materials, in particular to a method for preparing nano amorphous diamond.
Background
Diamond is a material with integrated chemical, physical and mechanical properties. The high hardness and wear resistance of diamond makes it widely used in the form of abrasives, cutters, and the like. The high-performance electrochemical material has excellent electrochemical performance, ultra-wide band gap, ultra-high breakdown field strength and high electron and hole mobility, and is called as an ultimate semiconductor; optically, photons with energy less than the band gap energy can be transmitted from infrared to ultraviolet; thermally, the thermal conductivity is superior to that of copper, and the copper-based composite material has application potential in multiple fields.
According to literature reports, the band gap of the amorphous diamond is reduced, and the conductivity is enhanced; and isotropic properties, make up for some short plates of diamond crystals, and can develop new applications of amorphous diamond. At present, the method for preparing the amorphous diamond is limited, and research is less, so that the method for preparing the amorphous diamond is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a method for preparing nano amorphous diamond, which converts the crystalline diamond into the amorphous diamond, and has low cost and high efficiency.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a method for preparing nano amorphous diamond, which comprises the following steps: cutting the crystal diamond to obtain a diamond sheet suitable for observing by a transmission electron microscope, putting the diamond sheet on an electrifying heating chip, and applying pulse electrifying, lithium embedding and heating to the nano crystal diamond sheet.
Further, the crystalline diamond was cut into a micrometer-sized diamond piece by a focused ion beam-scanning electron microscope, the diamond piece having a length of 6 μm, a width of 4 μm, a thickness of 100 and 200nm, and preferably a thickness of 150 nm. The thickness is typically selected to be between 100 and 200nm,<the 100nm sample is too thin and has poor mechanical property, so that the sample is easy to damage;>the 200nm sample is too thick to facilitate lithium intercalation and high resolution image observation. The transformation from the crystal to the amorphous is observed through a transmission electron microscope, in the transmission electron microscope, the thinner the sample is, the clearer the high resolution is, and the transformation from the crystal to the amorphous diamond of the diamond nanosheet can be well observed in the transmission electron microscope at 150 nm. Heating with 1-10mbar H gas introduced into transmission electron microscope 2 Or CO 2 . Hydrogen is the smallest element, the simple substance diamond does not conduct electricity at normal temperature and normal pressure, and hydrogen atoms with small sizes can enter crystal lattices of the diamond more easily, so that the conductivity of the diamond is enhanced; CO 2 2 The diamond material can also react with diamond under the irradiation of electron beams, so that a plurality of defects are caused, and the conductivity of the diamond material is improved.
Further, the electrifying process is to contact the nano-crystal diamond sheet with metal lithium to form a passage. Lithium is the smallest metal, the atomic radius is 1.52 angstroms, the bond length of diamond is 1.55 angstroms, and gaps are enlarged where there are defects in the diamond grains, such as grain boundaries and distortion. Under the drive of voltage, lithium ions can migrate to the diamond end, and the lithium ions are more easily inserted into diamond grain boundaries, so that the performance of the crystal diamond is improved.
Further, the heating temperature is 200-1600 ℃. The diamond is divided into a cubic structure and a hexagonal structure, the structure is stable, the diamond is heated, and energy is provided for C-C bonds, so that lithium ions and hydrogen atoms can enter diamond lattices more easily, the melting point of the diamond is 3500 ℃, and the heating temperature can be higher than 3500 ℃ in principle. However, at higher heating temperatures above 1600 ℃, the diamond surface layer will have an amorphous carbon layer and a graphite layer, so the heating temperature should be less than 1600 ℃.
Further, the pulse voltage was 20V and the frequency was 50Hz, and the application was repeated 200s at a time until the nano-crystalline diamond became nano-amorphous diamond. The pulse voltage is not easy to be too high or too low, the sample is burnt out when the pulse voltage is too high, amorphous transformation cannot occur when the pulse voltage is too low, and 20V is the optimum voltage for the amorphous transformation.
The invention discloses the following technical effects:
the traditional method of high pressure is used for converting crystals into amorphous diamond, the process is complicated, the requirement on processing equipment is high, and the cost is high. The method of the invention utilizes pulse, electrification and heating, has simple operation, low cost and high efficiency, and can efficiently prepare the amorphous diamond.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic view of an experimental apparatus used in the preparation method of the present invention;
FIG. 2 is a high resolution photograph of the original diamond wafer of example 1;
FIG. 3 is a schematic diagram of the experimental apparatus in example 1;
FIG. 4 is a high resolution photograph of example 1, wherein the diamond is completely transformed into amorphous;
FIG. 5 is a high resolution photograph of example 2, in which the diamond portion was transformed to amorphous;
FIG. 6 is a photograph of the diamond converted to amorphous high resolution of example 6;
FIG. 7 is a high-resolution photograph of graphitized diamond after high-temperature reaction of comparative example 4;
FIG. 8 is a photograph showing the high resolution of the diamond of comparative example 5 after it has been gasified.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. It is intended that the specification and examples be considered as exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The experimental device used in the preparation method of the invention is shown in figure 1.
Example 1
Cutting diamond with thickness of 100nm and width of 6 μm on a heating chip with focused ion beam (Fib), contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar H 2 Heating at 500 deg.C, repeatedly applying pulse voltage of 20V for 200s each time, then resting for 20s, and repeatedly treating for 3 times to convert diamond into amorphous state.
The original diamond sample of this example is shown in figure 2 at high resolution, indicating that the original diamond is a very good single crystal. FIG. 3 is a schematic diagram of an experimental apparatus, which is a heating chip electrode, a diamond sheet and lithium metal. Fig. 4 is a high resolution photograph of a diamond completely converted to amorphous.
Example 2
Cutting diamond with thickness of 150nm and width of 6 μm by focused ion beam (Fib), placing on a heating chip, contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 10mbar H 2 The heating temperature was 200 ℃, the pulse voltage was repeatedly applied at 16V for 200s each time, and then left for 30s, and after 4 times of repeated treatments, the diamond portion was transformed into an amorphous state (fig. 5).
Example 3
Cutting diamond with thickness of 100nm and width of 6 μm by focused ion beam (Fib), placing on heating chip electrode, contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar CO 2 Heating at 300 deg.C, repeatedly applying pulse voltage of 20V for 200s each time, then resting for 20s, and repeatedly treating for 2 times to convert diamond into amorphous state.
Example 4
Cutting diamond sheet with 6 μm length, 4 μm width and 200nm thickness with focused ion beam (Fib), placing on a heating chip, contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 10mbar CO 2 Heating at 700 deg.C, repeatedly applying pulse voltage of 20V for 200s each time, then resting for 20s, and repeatedly treating for 2 times to convert diamond into amorphous state.
Example 5
Cutting a diamond sheet with a length of 6 μm, a width of 4 μm and a thickness of 200nm with focused ion beam (Fib), placing on a heating chip, contacting with metal lithium to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar H 2 Heating at 1000 deg.C, repeatedly applying pulse voltage of 20V for 200s each time, then resting for 20s, and repeatedly treating for 2 times to convert diamond into amorphous state.
Example 6
Cutting diamond with thickness of 100nm and width of 6 μm on a heating chip with focused ion beam (Fib), contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar CO 2 The heating temperature is 1600 ℃, the pulse voltage is repeatedly applied for 20V, the duration time is 200s each time, then the rest is carried out for 20s, and after the repeated treatment is carried out for 2 times, the diamond is converted into an amorphous state (figure 6).
Example 7
Cutting diamond with thickness of 200nm and width of 6 μm on a heating chip with focused ion beam (Fib), contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 5mbar H 2 Heating at 1200 deg.C, repeatedly applying pulse voltage of 50V for 200s each time, then resting for 20s, and repeatedly treating for 2 times to convert diamond into amorphous state.
Comparative example 1
Cutting diamond with thickness of 100nm and width of 6 μm by focused ion beam (Fib), placing on a heating chip, contacting with gold needle to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar H 2 The heating temperature is 1200 ℃, the pulse voltage is repeatedly applied for 50V, the duration time is 200s each time, then the rest is carried out for 20s, and after 2 times of repeated treatment, the diamond is not changed.
Comparative example 2
Cutting diamond with thickness of 100nm and width of 6 μm on a heating chip with focused ion beam (Fib), contacting with lithium metal to form a passage, electrifying, placing on the heating chip electrode, transferring to an Environmental Transmission Electron Microscope (ETEM) with a sample rod, introducing 1mbar H 2 The heating temperature is 1200 ℃, the pulse voltage is repeatedly applied for 50V, the duration time is 200s each time, then the rest is carried out for 20s, and after 2 times of repeated treatment, the diamond is not changed.
Comparative example 3
Cutting block crystal diamond with focused ion beam (Fib) into diamond sheet with 6 μm length, 4 μm width and 100nm thickness, placing on heating chip electrode, contacting with metal lithium to form passage, electrifying, placing on copper net, transferring to Environment Transmission Electron Microscope (ETEM) with sample rod, and introducing 1mbar H 2 Heating at 200 deg.C, repeatedly applying pulse voltage of 20V for 200s each time, then resting for 20s, and repeatedly treating for 2 times to obtain diamond filmThere is a variation.
Comparative example 4
Cutting block crystal diamond with focused ion beam (Fib) into diamond sheet with 6 μm length, 4 μm width and 100nm thickness, placing on heating chip electrode, contacting with metal lithium to form passage, electrifying, placing on copper net, transferring to Environment Transmission Electron Microscope (ETEM) with sample rod, and introducing 1mbar H 2 The heating temperature was 1800 ℃, the pulse voltage was repeatedly applied for 20V for 200s each time, followed by rest for 20s, and after 2 times of repeated treatments, the diamond was partially gasified but without amorphization transformation (fig. 7).
Comparative example 5
Cutting block crystal diamond with focused ion beam (Fib) into diamond sheet with 6 μm length, 4 μm width and 100nm thickness, placing on heating chip electrode, contacting with metal lithium to form passage, electrifying, placing on copper net, transferring to Environment Transmission Electron Microscope (ETEM) with sample rod, and introducing 1mbar H 2 The heating temperature was 3600 deg.C, the pulse voltage was repeatedly applied for 20V, each time for 200s, and then the treatment was repeated for 20s, and after 2 times of repeated treatment, the diamond was almost completely gasified (FIG. 8).
Comparative example 6
Cutting block crystal diamond with focused ion beam (Fib) into diamond sheet with 6 μm length, 4 μm width and 100nm thickness, placing on heating chip electrode, contacting with metal lithium to form passage, electrifying, placing on copper net, transferring to Environment Transmission Electron Microscope (ETEM) with sample rod, and introducing 1mbar H 2 The heating temperature is 200 ℃, the pulse voltage of 100V is repeatedly applied, the duration time of each time is 200s, then the rest is carried out for 20s, after the repeated treatment is carried out for 2 times, the contact position of the diamond and the metal lithium is melted, the lithium cannot enter the diamond, and the diamond is not changed.
Comparative example 7
Cutting block crystal diamond with focused ion beam (Fib) into diamond sheet with 6 μm length, 4 μm width and 100nm thickness, placing on heating chip electrode, contacting with metal lithium to form passage, electrifying, placing on copper net, transferring to Environment Transmission Electron Microscope (ETEM) with sample rod, and introducing 1mbar H 2 The heating temperature is 1800 DEG CThe pulse voltage 1V is repeatedly applied for 200s each time, then the rest is carried out for 20s, and after 2 times of repeated treatment, the diamond is not changed.
Comparative example 8
The traditional method for preparing the amorphous diamond still selects a high-temperature high-pressure synthesis method, but the carbon source is not ordinary graphite but fullerene C60, and by means of a novel large-cavity press, C60 molecules in the cavity of the large-cavity press are continuously polymerized, collapsed and finally converted into the transparent amorphous diamond under the ultrahigh pressure of about 25-30GPa and the high temperature of 900-1300 ℃. In detail (Nature, 2021, 599-.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (6)
1. A method for preparing nano amorphous diamond is characterized by comprising the following steps: cutting the crystal diamond to obtain a diamond sheet suitable for observing by a transmission electron microscope, putting the diamond sheet on an electrifying heating chip, and applying pulse electrifying, lithium embedding and heating to the nano crystal diamond sheet.
2. The method for preparing nano amorphous diamond according to claim 1, wherein the crystalline diamond is cut into a micro crystalline diamond sheet having a length of 6 μm, a width of 4 μm, and a thickness of 100 and 200 nm.
3. The method for preparing nano amorphous diamond according to claim 1, wherein the energizing process is to contact the diamond sheet with metallic lithium to form a via.
4. The method for preparing nano amorphous diamond according to claim 1, wherein the heating temperature is 200-1600 ℃.
5. The method for preparing nano amorphous diamond according to claim 1, wherein gas is introduced during heating at 1-10mbar H 2 Or CO 2 。
6. The method for preparing nano amorphous diamond according to claim 1, wherein the pulse voltage is 0 to 50V, the frequency is 50Hz, 200s each time, and then the application is repeated after 20s of rest until the nano crystalline diamond is transformed into the nano amorphous diamond.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070042667A1 (en) * | 2002-03-08 | 2007-02-22 | Chien-Min Sung | Diamond-like carbon energy conversion devices and methods thereof |
| CN101327927A (en) * | 2008-07-11 | 2008-12-24 | 武汉大学 | Method for synthesizing diamond with carbon nanofiber |
| JP2018024541A (en) * | 2016-08-09 | 2018-02-15 | 三菱電機株式会社 | Production method of diamond substrate and production method of semiconductor device |
| CN109825876A (en) * | 2019-02-14 | 2019-05-31 | 北京沃尔德金刚石工具股份有限公司 | The preparation facilities and preparation method of diamond |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070042667A1 (en) * | 2002-03-08 | 2007-02-22 | Chien-Min Sung | Diamond-like carbon energy conversion devices and methods thereof |
| CN101327927A (en) * | 2008-07-11 | 2008-12-24 | 武汉大学 | Method for synthesizing diamond with carbon nanofiber |
| JP2018024541A (en) * | 2016-08-09 | 2018-02-15 | 三菱電機株式会社 | Production method of diamond substrate and production method of semiconductor device |
| CN109825876A (en) * | 2019-02-14 | 2019-05-31 | 北京沃尔德金刚石工具股份有限公司 | The preparation facilities and preparation method of diamond |
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