CN105013400A - Use of nonmetal catalyst in synthetic diamond - Google Patents
Use of nonmetal catalyst in synthetic diamond Download PDFInfo
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- CN105013400A CN105013400A CN201510353058.9A CN201510353058A CN105013400A CN 105013400 A CN105013400 A CN 105013400A CN 201510353058 A CN201510353058 A CN 201510353058A CN 105013400 A CN105013400 A CN 105013400A
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Abstract
The invention discloses a use of a nonmetal catalyst in synthetic diamond. Graphite as a carbon source and inorganic non-metallic elements such as Se and/or Te are synthesized into diamond. Under the conditions of a high temperature and high pressure, the non-metallic catalyst Se and Te crystals are in a melt state. The diamond grows in a liquid isotropic environment and has complete crystal structures and uniform particle size distribution. Under special synthesis environmental conditions, mean compressive strength of the diamond is greatly improved than that of the common industrial synthetic diamond. The diamond crystal contains a trace amount of catalyst elements Se and Te which are semiconductor materials and polyelectron systems, realizes diamond semiconductor characteristics by doping and is a novel high temperature-resistant semiconductor material.
Description
Technical field
The present invention relates to the application of nonmetal catalyst in artificially synthesizing diamond field, be specially selenium and/or the application of tellurium in artificially synthesizing diamond.
Background technology
Diamond has the physics and chemistry character of many excellences, it is a kind of limiting functional materials, be widely used in the industrial circles such as oil, machinery, stone material, electronics, chemical industry, traffic, equally also play key player in fields such as national defence, medical treatment, science and technology, decorations.In artificially synthesizing diamond, normal using graphite as carbon source, but be converted into diamond lattic structure carbon by graphite-structure carbon, need abnormal high temperature and pressure (typical temperature > 2000 DEG C, pressure > 12GPa), cost is high, is unfavorable for industrial production.Under high temperature, condition of high voltage, utilize at present catalyst catalytic reaction (i.e. Static Catalyst method) to be the main method of artificially synthesizing diamond.Wherein catalyst comprises the transition metal such as Fe, Ni, Ru, Ta, Co, Cr, Mn, and Fe, Mn, Ni, Ti base alloy system etc.
Present stage, artificially synthesizing diamond obtains immense success, but also there are some problems, there is many deficiencies in such as product in the physical property such as productive rate, crystalline form, inclusion enclave, color and luster, intensity, and be exaggerated, the market demand in comparatively strict, the harsh field that cannot meet the demands along with scientific and technological progress and to the further raising of diamond property demand.Secondly, in diamond synthesizing, catalyst used mostly is metal and alloy thereof, lacks the deep cognition to carbon phase transition process under catalysis and kinetics mechanism, further the extraordinary adamantine development and application of restriction diversity catalyst synthesis.
Summary of the invention
The object of this invention is to provide the application of a kind of nonmetal catalyst in artificially synthesizing diamond.
In order to realize above object, the technical solution adopted in the present invention is:
The application of nonmetal catalyst in artificially synthesizing diamond take graphite as carbon source, and nonmetal catalyst adopts selenium (Se) and/or tellurium (Te).
Described graphite adopts high purity graphite powder or graphite rod.Preferred Se and/or the Te crystal powder of nonmetal catalyst, purity > 99.9%, granularity is 20 ~ 700 orders.The mass ratio of graphite and nonmetal catalyst is 1:(1 ~ 10).Graphite and nonmetal catalyst combination (packaging technology) has laminar contact, powder mixes, catalyst fills out three kinds, the heart.
Diamond synthesis reaction in, device therefor be any one six contain eight (6/8) two-stage supercharging large volume high pressure apparatus.Transmission medium adopts through the magnesia of high temperature sintering process or pyrophillite.Heating material adopts any one in the refractory metal such as graphite or Ta, Mo, Ti.Load shaping front and back, need pretreatment reaction mixture or hydrogen reducing process under a high vacuum.Synthesized in the diamond Thermodynamically stable district of pretreated reactant mixture at carbon, process conditions are: pressure 7 ~ 10GPa, temperature 1500 ~ 1900 DEG C, temperature retention time 10 ~ 120 minutes again.
The application of nonmetal catalyst in artificially synthesizing diamond, comprises the following steps:
1) take graphite as carbon source, the graphite and the catalyst that pressure are caused into chip insert assembled formation in metal molybdenum cup, obtain assembled block;
2) by step 1) gained assembled block first reduction treatment 1 ~ 2h under an atmosphere of hydrogen, then after vacuum drying 1 ~ 2h carries out pretreatment, synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic is placed in after mixed acid carries out heating 24 ~ 48h, and cleaning, to obtain final product.
Step 3) in, described mixed acid is the mixture of any two kinds in nitric acid, sulfuric acid, hydrochloric acid, hydrofluoric acid.The mass concentration of described nitric acid, sulfuric acid, hydrochloric acid or hydrofluoric acid is 10% ~ 30%.
Beneficial effect of the present invention:
The present invention utilizes inorganic non-metallic element S e and/or Te diamond synthesis, and at high temperature under high pressure, catalyst Se, Te crystal becomes molten condition, so diamond grows under liquid phase isotropism environment, crystal formation is complete, even particle size distribution.Special synthetic environment condition makes adamantine mean compressive strength significantly promote than general industry diamond synthesis.The micro-catalyst element S e, the Te that contain in diamond crystal, they are semi-conducting material is also polyelectron system, can realize diamond semiconductor characteristic by doping, becomes a kind of novel fire resistant semi-conducting material.
Accompanying drawing explanation
Fig. 1 is the diamond electromicroscopic photograph before the acid treatment of embodiment 1;
Fig. 2 is the diamond electromicroscopic photograph before the acid treatment of embodiment 4;
Fig. 3 is the diamond electromicroscopic photograph after the acid treatment of embodiment 5.
Detailed description of the invention
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block with half sintered magnesia for transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and Se crystal powder as nonmetal catalyst, the purity > 99.9% of Se crystal powder, granularity is 80 orders, the mass ratio of high purity graphite powder and Se crystal powder is 1:1, adopt laminar contact packaging technology, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9.6GPa, synthesis in 60 minutes is incubated under temperature 1850 DEG C of conditions.Fig. 1 is the diamond electromicroscopic photograph before the acid treatment of this embodiment.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 1h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 10% nitric acid and mass concentration be the mixture of the sulfuric acid of 20%) carry out heating 24h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 2
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block with half sintered magnesia for transmission medium, graphite furnace is calandria, high purity graphite powder is carbon source and Se crystal powder is nonmetal catalyst, the purity > 99.9% of Se crystal powder, granularity is 200 orders, the mass ratio of graphite and Se crystal powder is 1:2, adopt powder Hybrid assembling, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9.6GPa, synthesis in 60 minutes is incubated under temperature 1900 DEG C of conditions.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 2h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 20% nitric acid and mass concentration be the mixture of the sulfuric acid of 10%) carry out heating 48h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 3
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block take pyrophillite as transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and Se crystal powder as nonmetal catalyst, the purity > 99.9% of Se crystal powder, granularity is 300 orders, the mass ratio of high purity graphite powder and Se crystal powder is 1:3, adopt powder Hybrid assembling, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9GPa, synthesis in 120 minutes is incubated under temperature 1900 DEG C of conditions.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 1h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 2h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 30% nitric acid and mass concentration be the mixture of the sulfuric acid of 30%) carry out heating 30h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 4
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block take pyrophillite as transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and Te crystal powder as nonmetal catalyst, the purity > 99.9% of Te crystal powder, granularity is 80 orders, the mass ratio of high purity graphite powder and Te crystal powder is 1:1, adopt laminar contact packaging technology, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9.6GPa, synthesis in 30 minutes is incubated under temperature 1800 DEG C of conditions.Fig. 2 is the diamond electromicroscopic photograph before the acid treatment of this embodiment.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 20% nitric acid and mass concentration be the mixture of the sulfuric acid of 30%) carry out heating 40h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 5
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block take pyrophillite as transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and and Te crystal powder as nonmetal catalyst, the purity > 99.9% of Te crystal powder, granularity is 200 orders, the mass ratio of graphite rod and Te crystal powder is 1:2, adopt powder Hybrid assembling, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9.6GPa, synthesis in 60 minutes is incubated under temperature 1900 DEG C of conditions.Fig. 3 is the diamond electromicroscopic photograph after the acid treatment of this embodiment.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 30% nitric acid and mass concentration be the mixture of the sulfuric acid of 10%) carry out heating 40h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 6
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block take pyrophillite as transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and Te crystal powder as nonmetal catalyst, the purity > 99.9% of Te crystal powder, granularity is 700 orders, the mass ratio of high purity graphite powder and Te crystal powder is 1:3, adopt powder Hybrid assembling, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9GPa, synthesis in 120 minutes is incubated under temperature 1900 DEG C of conditions.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 20% hydrochloric acid and mass concentration be the mixture of the hydrofluoric acid of 30%) carry out heating 40h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 7
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block with semi-sintering magnesia for transmission medium, graphite furnace is calandria, with high purity graphite rod as carbon source and Te crystal powder as nonmetal catalyst, the purity > 99.9% of Te crystal powder, granularity is 300 orders, and the mass ratio of graphite rod and Te crystal powder is 1:8, graphite rod center is hollowed out, adopts catalyst to fill out heart technique.After carrying out reduction and application of vacuum, Synthetic block being put into six increases large volume high pressure apparatus containing eight (6/8) secondarys, is incubated synthesis in 60 minutes under diamond Thermodynamically stable district pressure 9GPa, temperature 1850 DEG C of conditions.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 10% hydrochloric acid and mass concentration be the mixture of the hydrofluoric acid of 20%) carry out heating 36h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Embodiment 8
The application of nonmetal catalyst in artificially synthesizing diamond in the present embodiment, comprise the following steps: Synthetic block pyrophillite is transmission medium, graphite furnace is calandria, with high purity graphite powder as carbon source and Se and Te crystalline mixed powders as nonmetal catalyst, the purity > 99.9% respectively of Se and Te crystal powder, granularity is 600 orders, the mass ratio of high purity graphite powder and catalyst mixture powder is 1:1, adopt laminar contact packaging technology, after carrying out reduction and application of vacuum, Synthetic block is put into six and increase large volume high pressure apparatus containing eight (6/8) secondarys, at diamond Thermodynamically stable district pressure 9.6GPa, synthesis in 60 minutes is incubated under temperature 1800 DEG C of conditions.
The application of nonmetal catalyst in artificially synthesizing diamond of the present embodiment, comprises the following steps:
1) with high purity graphite powder for carbon source, pressure is caused into the graphite of chip and catalyst inserts assembled formation in metal molybdenum cup, obtains assembled block;
2) by step 1) the first reduction treatment 2h under an atmosphere of hydrogen of gained assembled block, then vacuum drying 1h carries out pretreatment, removing stuck foreign matter gas and volatile atoms, then synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic be placed in mixed acid (mass concentration be 30% hydrochloric acid and mass concentration be the mixture of the hydrofluoric acid of 10%) carry out heating 40h, the residues such as removing metal, catalyst, graphite, cleaning, obtains high-purity diamond micropowder.
Claims (10)
1. the application of nonmetal catalyst in artificially synthesizing diamond, is characterized in that: take graphite as carbon source, and nonmetal catalyst adopts Se and/or Te.
2. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: the mass ratio of graphite and nonmetal catalyst is 1:(1 ~ 10).
3. the application of nonmetal catalyst according to claim 2 in artificially synthesizing diamond, is characterized in that: described graphite is high purity graphite powder or graphite rod.
4. the application of nonmetal catalyst according to claim 2 in artificially synthesizing diamond, is characterized in that: described nonmetal catalyst adopts Se and/or Te crystal powder, and purity > 99.9%, granularity is 20 ~ 700 orders.
5. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: graphite is laminar contact with the combination of nonmetal catalyst, powder mixes or catalyst fills out the heart.
6. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: in artificially synthesizing diamond, transmission medium is magnesia through high temperature sintering process or pyrophillite.
7. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: in artificially synthesizing diamond, heating material can adopt any one in graphite, Ta, Mo, Ti.
8. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: the process conditions of artificially synthesizing diamond are: pressure 7 ~ 10GPa, temperature 1500 ~ 1900 DEG C, temperature retention time 10 ~ 120 minutes.
9. the application of nonmetal catalyst according to claim 1 in artificially synthesizing diamond, is characterized in that: comprise the following steps:
1) take graphite as carbon source, the graphite and the catalyst that pressure are caused into chip insert assembled formation in metal molybdenum cup, obtain assembled block;
2) by step 1) gained assembled block first reduction treatment 1 ~ 2h under an atmosphere of hydrogen, then after vacuum drying 1 ~ 2h carries out pretreatment, synthesize in the diamond Thermodynamically stable district of carbon, obtain synthetic;
3) by step 2) gained synthetic is placed in after mixed acid carries out heating 24 ~ 48h, and cleaning, to obtain final product.
10. the application of nonmetal catalyst according to claim 9 in artificially synthesizing diamond, is characterized in that: step 3) in, described mixed acid is the mixture of any two kinds in nitric acid, sulfuric acid, hydrochloric acid, hydrofluoric acid.
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Cited By (6)
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| CN108585855A (en) * | 2018-01-26 | 2018-09-28 | 西南交通大学 | A kind of grain polycrystalline diamond compact and preparation method thereof of selenium catalyst |
| CN112371148A (en) * | 2020-10-22 | 2021-02-19 | 河南工业大学 | Preparation method of novel catalyst for synthesizing diamond at high temperature and high pressure |
| CN112899776A (en) * | 2021-01-19 | 2021-06-04 | 吉林大学 | Method for synthesizing boron-hydrogen co-doped diamond single crystal |
| CN113797852A (en) * | 2021-10-20 | 2021-12-17 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN113968736A (en) * | 2021-12-01 | 2022-01-25 | 西南交通大学 | Polycrystalline diamond sintered body of tellurium catalyst and preparation method thereof |
| CN115318204A (en) * | 2022-07-26 | 2022-11-11 | 湖南良诚新材料科技有限公司 | Method for artificially synthesizing diamond |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108585855A (en) * | 2018-01-26 | 2018-09-28 | 西南交通大学 | A kind of grain polycrystalline diamond compact and preparation method thereof of selenium catalyst |
| CN112371148A (en) * | 2020-10-22 | 2021-02-19 | 河南工业大学 | Preparation method of novel catalyst for synthesizing diamond at high temperature and high pressure |
| CN112899776A (en) * | 2021-01-19 | 2021-06-04 | 吉林大学 | Method for synthesizing boron-hydrogen co-doped diamond single crystal |
| CN113797852A (en) * | 2021-10-20 | 2021-12-17 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN113797852B (en) * | 2021-10-20 | 2024-04-09 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN113968736A (en) * | 2021-12-01 | 2022-01-25 | 西南交通大学 | Polycrystalline diamond sintered body of tellurium catalyst and preparation method thereof |
| CN115318204A (en) * | 2022-07-26 | 2022-11-11 | 湖南良诚新材料科技有限公司 | Method for artificially synthesizing diamond |
| CN115318204B (en) * | 2022-07-26 | 2024-05-10 | 湖南良诚新材料科技有限公司 | Method for artificially synthesizing diamond |
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