CN109012496A - A kind of method that shock wave method prepares diamond thin - Google Patents
A kind of method that shock wave method prepares diamond thin Download PDFInfo
- Publication number
- CN109012496A CN109012496A CN201811194667.4A CN201811194667A CN109012496A CN 109012496 A CN109012496 A CN 109012496A CN 201811194667 A CN201811194667 A CN 201811194667A CN 109012496 A CN109012496 A CN 109012496A
- Authority
- CN
- China
- Prior art keywords
- bilayer graphene
- diamond
- preparation
- intercalation compound
- diamond thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- 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
- C01B32/26—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/061—Graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The present invention provides a kind of method that shock wave method prepares diamond thin.Second order graphite intercalation compound is obtained using lodine chloride as intercalator, high-temperature process obtains bilayer graphene material；Bilayer graphene powder is uniformly mixed with pure copper powder and is pressed into be put into shock recovery device after block and carries out impact pressurization, recycles the mixing press body through overbump, copper is removed with nitric acid, obtains diamond thin.The bilayer graphene that the method for the invention uses hardens into the most thin film with diamond hardness after being impacted, in the short time, can be used for protective materials.Higher diamond conversion ratio can be reached within the scope of lower surge by carbon source of bilayer graphene.
Description
Technical field
The present invention relates to diamond preparation field more particularly to it is a kind of using bilayer graphene as raw material shock wave method preparation
Diamond thin.
Background technique
Diamond is a kind of particulate material being made of simple substance carbon, for the highest object of hardness found in the world at present
Matter and graphene, fullerene, carbon nanotube allotrope.Diamond can be used to grind jewel, glass, hard alloy
Equal superhard materials are the cutting tools in craftwork and industry.
Graphene is a kind of two-dimensional material with numerous excellent properties, it has the honeycomb knot of single layer of carbon atom composition
Structure, thickness is only hundred a ten thousandths of human hair's diameter, and intensity surpasses hundred times of steel.Graphene still maintains graphite
The hexagon of carbon atom is distributed in synusia, is still distributed with the carbon atom of diamond there are certain correspondence in structure, is also just deposited
In the condition of direct phase transformation.
There are many kinds of the synthetic methods of diamond, but usually all use the graphite of well-crystallized for synthesis carbon source, this be by
In the crystal structure of graphite and diamond there are obvious corresponding relationship, under high temperature and pressure, carbon atom generates slight shifting to graphite
It is dynamic, diamond can be converted into.But impact synthesis process in, it is necessary to could be obtained under high surge compared with
High diamond conversion ratio.It is used in Chinese invention patent " expansion graphite method of explosion synthesis of diamond " (CN93115929.6)
Expanded graphite that a kind of C axis interlamellar spacing of special " porous " graphite material is widened is seen as impacting diamond synthesis
Carbon source reaches higher diamond conversion ratio within the scope of lower surge.By the initial density for controlling expanded graphite
Synthesis temperature is controlled, compared with kish, higher synthesis temperature can be reached at low pressures.When due to Impulsive load
Between it is extremely short, the general high voltage duration be no more than more than ten microseconds, using kish carry out impact synthesis when, it is necessary to high
Higher diamond conversion ratio could be obtained under surge.The yield of diamond in order to further increase reduces equipment requirement
And reduce energy consumption, it is still necessary to further decrease surge and improve conversion ratio.
Summary of the invention
A kind of method that shock wave method prepares diamond thin, more particularly to one kind are proposed using bilayer graphene as raw material
Shock wave method prepare diamond thin, higher diamond conversion ratio is reached within the scope of lower surge.The double-deck stone
Black alkene has been not belonging to the scope of graphite, but can be considered as and reach the expansion stone that C axis interlamellar spacing is enlarged to " limit " degree
Ink.Using bilayer graphene impact synthesis of artificial diamond, not only met direct phase change conditions, but can reach at low pressures compared with
High synthesis temperature, therefore the nucleation rate of diamond can be improved.
The present invention adopts the following technical scheme:
A kind of method that shock wave method prepares diamond thin, includes the following steps:
(1) second order graphite intercalation compound is obtained using lodine chloride as intercalator, it is high to second order graphite intercalation compound
Temperature processing, lodine chloride decompose generation gas stripping graphite flake layer and obtain bilayer graphene material；
(2) bilayer graphene powder is uniformly mixed with pure copper powder, is put into shock recovery after mixture is pressed into block
Impact pressurization is carried out in device, recycles the mixing press body through overbump, is removed copper with nitric acid, is obtained diamond thin.
The graphite raw material of second order graphite intercalation compound in step (1) is having a size of 10-150 mesh.
High-temperature process temperature in step (1) is 800-1200 DEG C.
As transmission medium, the mass ratio of bilayer graphene powder and pure copper powder is 0.1-1 for pure copper powder in step (2).
Impact moulding pressure in step (2) is 10~150GPa, and the duration is less than 10 μ s.
Nitric acid in step (2) is the aqueous solution of nitric acid that concentration is 20%.
The present invention has the advantage that
(1) to harden into diamond after being impacted, in the short time the same for bilayer graphene in the method for the invention, becomes
Most thin film with diamond hardness, can be applied to protective materials.
(2) what is formed using graphite and expanded graphite as the ballistic method of carbon source is diamond particles, need nucleation process with
And the displacement field match of multilayer.The bilayer graphene that the method for the invention uses only needs position movement slightly can shape under impact
At diamond thin, higher diamond conversion ratio can be reached within the scope of lower surge.
Detailed description of the invention
Fig. 1 is the process flow chart of the method for the present invention.
Fig. 2 is the transmission electron microscope picture that embodiment of the present invention method 1 prepares bilayer graphene.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 60g lodine chloride is uniformly mixed with 1g expanded graphite, is packed into protection gas Ar gas, is enclosed in vial, sets
In 160 DEG C of oil bath environment, 48h is heated, second order graphite intercalation compound is prepared.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into quartz boat and be heated to 800
DEG C, maintain 5min.End of reaction, takes out sample, and cleaning sample obtains bilayer graphene powder aggregates.
(3) 1g bilayer graphene powder is uniformly mixed with 200 mesh pure copper powder of 5g, is put into after being pressed into block
Impact pressurization is carried out in shock recovery device, impact moulding pressure is 20GPa, and the duration is less than 10 μ s.
(4) the mixing press body through overbump is recycled, the aqueous solution of nitric acid that concentration is 20% is put into and removes copper, obtain Buddha's warrior attendant
Stone film.
Fig. 1 is the process flow chart of the present embodiment.
Fig. 2 is the transmission electron microscope picture that the present embodiment prepares bilayer graphene.
Embodiment 2
(1) 60g lodine chloride is uniformly mixed with 1g expanded graphite, is packed into protection gas Ar gas, is enclosed in vial, sets
In 160 DEG C of oil bath environment, 48h is heated, second order graphite intercalation compound is prepared.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into quartz boat and be heated to 800
DEG C, maintain 5min.End of reaction, takes out sample, and cleaning sample obtains bilayer graphene powder aggregates.
(3) 1g bilayer graphene powder is uniformly mixed with 200 mesh pure copper powder of 2g, is put into after being pressed into block
Impact pressurization is carried out in shock recovery device, impact moulding pressure is 20GPa, and the duration is less than 10 μ s.
(4) the mixing press body through overbump is recycled, the aqueous solution of nitric acid that concentration is 20% is put into and removes copper, obtain Buddha's warrior attendant
Stone film.
Embodiment 3
(1) 60g lodine chloride is uniformly mixed with 1g expanded graphite, is packed into protection gas Ar gas, is enclosed in vial, sets
In 160 DEG C of oil bath environment, 48h is heated, second order graphite intercalation compound is prepared.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into quartz boat and be heated to 800
DEG C, maintain 5min.End of reaction, takes out sample, and cleaning sample obtains bilayer graphene powder aggregates.
(3) 1g bilayer graphene powder is uniformly mixed with 200 mesh pure copper powder of 5g, is put into after being pressed into block
Impact pressurization is carried out in shock recovery device, impact moulding pressure is 40GPa, and the duration is less than 10 μ s.
(4) the mixing press body through overbump is recycled, the aqueous solution of nitric acid that concentration is 20% is put into and removes copper, obtain Buddha's warrior attendant
Stone film.
Embodiment 4
(1) 60g lodine chloride is uniformly mixed with 1g expanded graphite, is packed into protection gas Ar gas, is enclosed in vial, sets
In 160 DEG C of oil bath environment, 48h is heated, second order graphite intercalation compound is prepared.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into quartz boat and be heated to 1000
DEG C, maintain 5min.End of reaction, takes out sample, and cleaning sample obtains bilayer graphene powder aggregates.
(3) 1g bilayer graphene powder is uniformly mixed with 200 mesh pure copper powder of 5g, is put into after being pressed into block
Impact pressurization is carried out in shock recovery device, impact moulding pressure is 20GPa, and the duration is less than 10 μ s.
(4) the mixing press body through overbump is recycled, the aqueous solution of nitric acid that concentration is 20% is put into and removes copper, obtain Buddha's warrior attendant
Stone film.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (6)
1. a kind of method that shock wave method prepares diamond thin, includes the following steps:
(1) second order graphite intercalation compound is obtained using lodine chloride as intercalator, at second order graphite intercalation compound high temperature
Reason, lodine chloride decompose generation gas stripping graphite flake layer and obtain bilayer graphene material；
(2) bilayer graphene powder is uniformly mixed with pure copper powder, mixture is pressed into after block and is put into shock recovery device
In carry out impact pressurization, recycle the mixing press body through overbump, remove copper with nitric acid, obtain diamond thin.
2. preparation method according to claim 1, which is characterized in that second order graphite intercalation compound in step (1)
Graphite raw material is having a size of 10-150 mesh.
3. preparation method according to claim 1, which is characterized in that the high-temperature process temperature in step (1) is 800-
1200℃。
4. preparation method according to claim 1, which is characterized in that pure copper powder is double-deck as transmission medium in step (2)
Graphene powder and the mass ratio of pure copper powder are 0.1-1.
5. preparation method according to claim 1, which is characterized in that in step (2) impact moulding pressure be 10~
150GPa, the duration is less than 10 μ s.
6. preparation method according to claim 1, which is characterized in that the slightly acid in step (2) is the nitre that concentration is 20%
Aqueous acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811194667.4A CN109012496B (en) | 2018-09-29 | 2018-09-29 | Method for preparing diamond film by shock wave method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811194667.4A CN109012496B (en) | 2018-09-29 | 2018-09-29 | Method for preparing diamond film by shock wave method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109012496A true CN109012496A (en) | 2018-12-18 |
| CN109012496B CN109012496B (en) | 2021-06-04 |
Family
ID=64612855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811194667.4A Active CN109012496B (en) | 2018-09-29 | 2018-09-29 | Method for preparing diamond film by shock wave method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109012496B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104846A (en) * | 2021-04-08 | 2021-07-13 | 山东大学 | Graphene irreversible pressure-induced sp based on transition metal catalysis3Method for hybrid enhancement |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103328A (en) * | 1993-11-27 | 1995-06-07 | 大连理工大学 | Expansion graphite method for explosion synthesis of diamond |
| US20110006837A1 (en) * | 2009-06-02 | 2011-01-13 | Feng Wang | Graphene Device, Method of Investigating Graphene, and Method of Operating Graphene Device |
| CN103482610A (en) * | 2012-06-14 | 2014-01-01 | 海洋王照明科技股份有限公司 | Graphene preparation method |
| CN105776201A (en) * | 2016-04-07 | 2016-07-20 | 东南大学 | Method for low-temperature and low-pressure nano-diamond synthesis by using oxidized graphene powder |
| CN108314025A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of preparation method of bilayer graphene intercalation compound |
-
2018
- 2018-09-29 CN CN201811194667.4A patent/CN109012496B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103328A (en) * | 1993-11-27 | 1995-06-07 | 大连理工大学 | Expansion graphite method for explosion synthesis of diamond |
| US20110006837A1 (en) * | 2009-06-02 | 2011-01-13 | Feng Wang | Graphene Device, Method of Investigating Graphene, and Method of Operating Graphene Device |
| CN103482610A (en) * | 2012-06-14 | 2014-01-01 | 海洋王照明科技股份有限公司 | Graphene preparation method |
| CN105776201A (en) * | 2016-04-07 | 2016-07-20 | 东南大学 | Method for low-temperature and low-pressure nano-diamond synthesis by using oxidized graphene powder |
| CN108314025A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of preparation method of bilayer graphene intercalation compound |
Non-Patent Citations (1)
| Title |
|---|
| YANG GAO ET AL.: "Ultrahard carbon film from epitaxial two-layer graphene", 《NATURE NANOTECHNOLOGY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104846A (en) * | 2021-04-08 | 2021-07-13 | 山东大学 | Graphene irreversible pressure-induced sp based on transition metal catalysis3Method for hybrid enhancement |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109012496B (en) | 2021-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3816085A (en) | Diamond-nondiamond carbon polycrystalline composites | |
| Davis | Material Review: Alumina (Al 2 O 3). | |
| US6835365B1 (en) | Crystal growth | |
| WO2017139078A1 (en) | Chemical-free production of graphene-reinforced inorganic matrix composites | |
| KR830002648A (en) | Method for preparing cubic boron nitride from hexagonal boron nitride milled without catalyst | |
| JPWO2007029588A1 (en) | High performance composite material and manufacturing method thereof | |
| JP2021073158A (en) | Friable ceramic-bonded diamond composite particle, and method of producing the same | |
| CN104209062A (en) | Ultrahigh hard nano twin diamond block material and preparation method thereof | |
| Fang et al. | A novel technique for the synthesis of nanodiamond powder | |
| CN108840681B (en) | Nano boron carbide and preparation method thereof | |
| CN105013400A (en) | Use of nonmetal catalyst in synthetic diamond | |
| CN109012496A (en) | A kind of method that shock wave method prepares diamond thin | |
| EA200300269A1 (en) | ABRASIVE MATERIAL OF DIAMOND PARTICLES AND METHOD OF ITS MANUFACTURE | |
| CN113233877A (en) | Sodium removal method for calcining alpha alumina | |
| CN1281487C (en) | Method fro directly synthesizing diamond by sintering nanometer carbon tube under low-pressure | |
| Yang et al. | The influence of Li-based catalysts/additives on cBN crystal morphologies synthesized under HPHT | |
| Lu et al. | A CVD method for preparing CNTs-grafted carbon fiber fabrics under quasi-vacuum at low temperature | |
| Tatsii et al. | Structure and properties of Dalan detonation diamonds | |
| Yan et al. | Microstructural features and thermal stability of alumina-bonded nano-polycrystalline diamond synthesized by detonation sintering | |
| Voropaev et al. | Face-centered cubic carbon synthesis under cavitation compression | |
| RU2131763C1 (en) | Method of manufacturing artificial diamonds | |
| CN108187587B (en) | Pure-phase large-scale polycrystalline diamond and synthesis method and application thereof | |
| GB2058840A (en) | Production of polycrystalline cubic boron nitride | |
| WO2015038031A1 (en) | Method for producing crystalline diamond particles | |
| EP0111558A1 (en) | Process for producing diamond particles having a selected morphology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220620 Address after: 230000 Room 203, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee after: Hefei Jiuzhou Longteng scientific and technological achievement transformation Co.,Ltd. Address before: 224000 No.2, hope Avenue South Road, Yancheng City, Jiangsu Province Patentee before: YANCHENG TEACHERS University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221014 Address after: 421000 Liantang Village, Tanzishan Town, Hengnan County, Hengyang City, Hunan Province Patentee after: Hunan Chuan Wei new materials Science and Technology Ltd. Address before: 230000 Room 203, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee before: Hefei Jiuzhou Longteng scientific and technological achievement transformation Co.,Ltd. |
|
| TR01 | Transfer of patent right |