CN1099906C - Preparation method of bortz body by using superfine carbon powder through synthesis process - Google Patents
Preparation method of bortz body by using superfine carbon powder through synthesis process Download PDFInfo
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- CN1099906C CN1099906C CN99110845A CN99110845A CN1099906C CN 1099906 C CN1099906 C CN 1099906C CN 99110845 A CN99110845 A CN 99110845A CN 99110845 A CN99110845 A CN 99110845A CN 1099906 C CN1099906 C CN 1099906C
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- ultrafine carbon
- carbonaceous
- powder
- colloidal sol
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 title claims description 7
- 238000003786 synthesis reaction Methods 0.000 title claims description 6
- 238000000034 method Methods 0.000 title description 4
- 239000000843 powder Substances 0.000 claims abstract description 41
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 26
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 24
- 239000010432 diamond Substances 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 13
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 9
- 238000000352 supercritical drying Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 150000003857 carboxamides Chemical group 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910001867 inorganic solvent Inorganic materials 0.000 claims description 2
- 239000003049 inorganic solvent Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000010439 graphite Substances 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 2
- 229910001573 adamantine Inorganic materials 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 239000002010 green coke Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 208000001840 Dandruff Diseases 0.000 description 1
- 206010016825 Flushing Diseases 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 150000003948 formamides Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a preparation method for synthesizing diamond powder particles by superfine carbon powders. Superfine carbon powders are prepared from carbon water mesophase collosol by solvent treatment, supercritical drying and heat treatment and mixed with alloy powders according to the weight ratio of 98 to 60:2 to 40; the mixture is prepressed into a cylinder; pyrophyllite blocks are filled in the cylinder and synthesized under 5 to 6 Gpa at 1350 to 1450 DEG C for 1 to 12 minutes to prepare diamond with the particle diameter of 1 to 200 mu m. The diamond of the present invention has nucleation rate and crystal shape integrity rate superior to those of diamond prepared from graphite raw materials and has the characteristics of high conversion rate, controllable particle diameter, homogeneous distribution of the particle diameter, etc.
Description
The invention belongs to a kind of preparation method of diamond powder, relate in particular to a kind of method for preparing the bortz powder plastochondria by ultrafine carbon powder.
Diamond has been widely used in numerous industries such as geological drilling, cutting marble as a kind of desirable superhard material.Owing to the resource-constrained of natural diamond, be difficult to satisfy the needs of industrial development, utilize the graphite artificially synthesizing diamond to become main source.
The method of artificially synthesizing diamond is a lot, but industrial production mainly adopts static pressure catalyst method.Static pressure catalyst synthetic method is that pack into the powder of 380 ℃ of roastings of carbon source graphite material and catalyst alloy layering is pressed in the synthetic chamber of pyrophyllite and formed briquetting, synthetic chamber is the transverse sheet structure, after 120 ℃ of oven dry, under the pressure of 5.5-5.7Gpa and about 1450 ℃-1500 ℃ temperature, the heating regular hour is synthetic.The many employings of its carbon source graphite are base-material with graphited forging back petroleum coke powder, with molten asphalt as binding agent, handle through operations such as mixing, roll, abrasive dust, compacting, roasting, dipping, graphitizations, at last at the disk that finish grindes or be machined into required gauge thickness.Catalyst material is the alloy disk.
Have not yet to see and utilize the ultrafine carbon powder that makes mutually in the middle of the carbonaceous water-based to prepare adamantine report.
Preparation method of the present invention comprises the steps:
1. be raw material with phase colloidal sol in the middle of the carbonaceous water-based, with in the middle of the carbonaceous water-based with organic solvent or inorganic alkaline solution by weight 1: 5-50 mixes, and obtains the carbonaceous sol-gel after the dissolving;
2. ethanol is added in carbonaceous colloidal sol-gel, remove organic solvent or inorganic solvent in carbonaceous colloidal sol-gel, obtain clean carbonaceous colloidal sol;
3. with clean carbonaceous colloidal sol, put into autoclave,, carry out supercritical drying under the 4.0-8.5MPa at 200-280 ℃, emit supercritical medium after, purge and be cooled to room temperature with inert gas, make primary ultrafine carbon powders;
4. with the primary ultrafine carbon powders that makes, heating rate with (0.1-3) ℃/minute under the condition of inert atmosphere or secluding air is heated to 1000 ℃-1300 ℃, holding temperature 2 hours, being warmed up to 1700 ℃-3000 ℃ with the heating rate of (20-100) ℃/minute then heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
5. be catalyst material with 300 orders～400 purpose alloy powders,, and then be pressed into the cylinder of φ 18 * 20mm in advance ultrafine carbon powder and the alloy powder proportioning mixed grinding by weight 98～60: 2～40 1 hour;
6. 32.5 * 32.5 * 32.5mm pyrophyllite square of carbon-catalytic alloy cylinder being packed under the temperature of the pressure of 5-6GPa and about 1350-1450 ℃, synthesized 1-12 minute, and the diamond particle diameter that makes is 1-200 μ m.
The present invention has following advantage:
1. diamond nucleation and complete in crystal formation rate are better than the diamond of graphite raw material growth.
2. adamantine conversion ratio height.
3. the controlled system of diamond particle diameter, particle diameter is evenly distributed.
Described ultrafine carbon prepares by supercritical drying by in the middle of the carbonaceous water-based.
Described organic solvent is organic amide, ethylene glycol, glycerine, acetone.
Described inorganic alkaline solution be potassium,, soda solution or ammoniacal liquor.
Described catalytic alloy powder is Ni
67Mn
3Fe
30, Ni
70Mn
25Co
5, Ni
70Mn
30
Embodiment 1
(1) with phase in the middle of the 10 gram coal tar pitch charcoal processing matter water-baseds, is dissolved in the 50 gram ammoniacal liquor, obtains the carbonaceous gel;
(2) with carbonaceous colloidal sol, put into the glass sintering funnel, remove wherein ammoniacal liquor with 1000 gram alcohol flushings, make clean carbonaceous colloidal sol;
(3) with clean carbonaceous colloidal sol, put into the stainless steel cylinder of the 50ml of 0.5 liter of autoclave, in still, add 300ml ethanol, be warming up to 280 ℃, 8.5MPa, holding temperature, pressure 120 minutes.Emit ethanol, purge with nitrogen and be cooled to room temperature, make primary ultrafine carbon powders;
(4) with the primary ultrafine carbon powders that makes, heating rate with 0.1 ℃/minute under the condition of secluding air is heated to 1000 ℃, and holding temperature 2 hours is warmed up to 1700 ℃ with 20 ℃/minute heating rate then and heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(5) with 300 order Ni
67Mn
3Fe
30Alloy powder is a catalyst material, and ultrafine carbon powder and alloy powder by weight 60: 40 proportioning mixed grinding 1 hour, and then are pressed into the cylinder of φ 18 * 20mm in advance;
(6) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square, under the pressure of 6GPa and about 1450 ℃ temperature, synthetic 12 minutes, the diamond particle diameter that makes was 40-50 μ m.
Embodiment 2
(1) makes primary ultrafine carbon powders as embodiment 1 step (1), (2), (3);
(2) with the primary ultrafine carbon powders that makes mutually in the middle of the water-based, heating rate with 2 ℃/minute under the condition of argon gas atmosphere is heated to 1200 ℃, and holding temperature 2 hours is warmed up to 2400 ℃ with 50 ℃/minute heating rate then and heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(3) with about 350 purpose Ni
70Mn
30Alloy powder is a catalyst material, and ultrafine carbon powder and alloy powder by weight 70: 30 proportioning mixed grinding 1 hour, and then are pressed into the cylinder of φ 18 * 20mm in advance;
(4) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square, under the pressure of 5GPa and about 1350 ℃ temperature, synthetic 6 minutes, the diamond particle diameter that makes was 20-100 μ m.
Embodiment 3
(1) with phase in the middle of the 5 gram oil green coke charcoal processing matter water-baseds, under room temperature, is dissolved in the 250 gram acetone, makes carbonaceous colloidal sol;
(2) carbonaceous colloidal sol is heated remove wherein most of acetone, add 50 gram ethanol again, divides three addings, continue to add thermal distillation, remove acetone wherein, must clean carbonaceous colloidal sol;
(3) with clean carbonaceous colloidal sol, put into the 50ml metal cylinder of 0.5 liter of autoclave, feed CO
2Gas is warming up to 200 ℃ to 7.5MPa, and holding temperature, pressure 120 minutes are emitted CO
2Gas.Be cooled to room temperature with the nitrogen purging, make primary ultrafine carbon powders;
(4) with the primary ultrafine carbon powders that makes, heating rate with 0.5 ℃/minute under the condition of argon gas atmosphere is heated to 1300 ℃, and holding temperature 2 hours is warmed up to 3000 ℃ with 100 ℃/minute heating rate then and heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(5) with about 400 purpose Ni
70Mn
25Co
5Alloy powder is a catalyst material, and ultrafine carbon powder and alloy powder by weight 98: 2 proportioning mixed grinding 1 hour, and then are pressed into the cylinder of φ 18 * 20mm in advance;
(6) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square, under the pressure of 5.5GPa and about 1400 ℃ temperature, synthetic 9 minutes, the diamond particle diameter that makes was 100-200 μ m.
Embodiment 4
(1) with phase in the middle of the 10 gram coal tar pitch charcoal processing matter water-baseds, under 100 ℃ temperature, is dissolved in second
In the glycol, make the carbonaceous gel;
(2) with the carbonaceous gel, put into the centrifuge Centrifuge Cup, divide four times with 800ml ethanol, carry out centrifugation, remove wherein ethylene glycol, centrifugal sediment is clean carbonaceous colloidal sol.
(3) make primary ultrafine carbon powders as step (3), (4) among the embodiment 1;
(4) with the primary ultrafine carbon powders that makes, heating rate with 3 ℃/minute under the condition of argon gas atmosphere is heated to 1100 ℃, and holding temperature 2 hours is warmed up to 2400 ℃ with 40 ℃/minute heating rate then and heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(5) with about 300 purpose Ni
70Mn
25Co
5Alloy powder is a catalyst material, and ultrafine carbon powder and alloy powder by weight 80: 20 proportioning mixed grinding 1 hour, and then are pressed into the cylinder of φ 18 * 20mm in advance;
(6) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square, under the pressure of 5.5GPa and about 1400 ℃ temperature, synthetic 1 minute, the diamond particle diameter that makes was 1-10 μ m.
Embodiment 5
(1) phased soln in the middle of the 10 gram oil green coke charcoal processing matter water-baseds is made the carbonaceous gel in 100 gram formamides;
(2) make clean carbonaceous colloidal sol as step (2) among the embodiment 4.Supercritical drying and charing are carried out to above-mentioned clean carbonaceous colloidal sol in step (3), (4) among the embodiment 1 for another example, make ultra-fine grain charcoal;
(3) with the primary ultrafine carbon powders that makes mutually in the middle of the water-based, heating rate with 0.5 ℃/minute under the condition of argon gas atmosphere is heated to 1300 ℃, and holding temperature 2 hours is warmed up to 3000 ℃ with 70 ℃/minute heating rate then and heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(4) with about 400 purpose Ni
70Mn
25Co
5Alloy powder is a catalyst material, and ultrafine carbon powder and alloy powder by weight 95: 5 proportioning mixed grinding 1 hour, and then are pressed into the cylinder of Φ 18 * 20mm in advance;
(5) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square, under the pressure of 5.0GPa and about 1400 ℃ temperature, synthetic 3 minutes, the diamond particle diameter that makes was 5-20 μ m.
Claims (4)
1. the preparation method by ultrafine carbon powder diamond synthesis powder body is characterized in that comprising the steps:
(1) be raw material with phase colloidal sol in the middle of the carbonaceous water-based, with in the middle of the carbonaceous water-based with organic solvent or inorganic alkaline solution by weight 1: 5-50 mixes, and obtains the carbonaceous sol-gel after the dissolving;
(2) ethanol is added in carbonaceous colloidal sol-gel, remove organic solvent or inorganic solvent in carbonaceous colloidal sol-gel, obtain clean carbonaceous colloidal sol;
(3) with clean carbonaceous colloidal sol, put into autoclave,, carry out supercritical drying under the 4.0-8.5MPa at 200-280 ℃, emit supercritical medium after, purge and be cooled to room temperature with inert gas, make primary ultrafine carbon powders;
(4) with the primary ultrafine carbon powders that makes, heating rate with (0.1-3) ℃/minute under the condition of inert atmosphere or secluding air is heated to 1000 ℃-1300 ℃, holding temperature 2 hours, being warmed up to 1700 ℃-3000 ℃ with the heating rate of (20-100) ℃/minute then heat-treats, holding temperature 30 minutes obtains ultrafine carbon powder after the cooling;
(5) be catalyst material with 300 orders～400 purpose alloy powders,, and then be pressed into the cylinder of φ 18 * 20mm in advance ultrafine carbon powder and the alloy powder proportioning mixed grinding by weight 98～60: 2～40 1 hour;
(6) carbon-catalytic alloy cylinder is packed into 32.5 * 32.5 * 32.5mm pyrophyllite square under the temperature of the pressure of 5-6GPa and about 1350-1450 ℃, synthesized 1-12 minute, and the diamond particle diameter that makes is 1-200 μ m.
2. a kind of preparation method by ultrafine carbon powder diamond synthesis powder body according to claim 1 is characterized in that described organic solvent is organic amide, ethylene glycol, glycerine or acetone.
3. a kind of preparation method by ultrafine carbon powder diamond synthesis powder body according to claim 1 is characterized in that described inorganic alkaline solution is potassium, soda solution or ammoniacal liquor.
4. a kind of preparation method by ultrafine carbon powder diamond synthesis powder body according to claim 1 is characterized in that described catalytic alloy powder is Ni
67Mn
3Fe
30, Ni
70Mn
25Co
5Or Ni
70Mn
30
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99110845A CN1099906C (en) | 1999-07-21 | 1999-07-21 | Preparation method of bortz body by using superfine carbon powder through synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99110845A CN1099906C (en) | 1999-07-21 | 1999-07-21 | Preparation method of bortz body by using superfine carbon powder through synthesis process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1281748A CN1281748A (en) | 2001-01-31 |
| CN1099906C true CN1099906C (en) | 2003-01-29 |
Family
ID=5274735
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99110845A Expired - Fee Related CN1099906C (en) | 1999-07-21 | 1999-07-21 | Preparation method of bortz body by using superfine carbon powder through synthesis process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1099906C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006061672A1 (en) * | 2004-12-09 | 2006-06-15 | Element Six (Production) (Pty) Ltd | Synthesis of diamond |
| CN104264210B (en) * | 2014-09-12 | 2016-08-24 | 河南省力量钻石股份有限公司 | A kind of synthetic method of ultra-fine grain diamond single crystal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106030A (en) * | 1985-08-13 | 1986-05-10 | 国家建筑材料工业局人工晶体研究所 | The method of directly synthesizing microns diamond |
-
1999
- 1999-07-21 CN CN99110845A patent/CN1099906C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106030A (en) * | 1985-08-13 | 1986-05-10 | 国家建筑材料工业局人工晶体研究所 | The method of directly synthesizing microns diamond |
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| Publication number | Publication date |
|---|---|
| CN1281748A (en) | 2001-01-31 |
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