CN1281748A - 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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- CN1281748A CN1281748A CN 99110845 CN99110845A CN1281748A CN 1281748 A CN1281748 A CN 1281748A CN 99110845 CN99110845 CN 99110845 CN 99110845 A CN99110845 A CN 99110845A CN 1281748 A CN1281748 A CN 1281748A
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Abstract
The preparation method for synthesizing diamond particle body by using superfine carbon powder includes the following steps: using carbon water mesophase sol as raw material, solvent treatment, supercritical drying, heat treatment to obtain superfine carbon powder, mixing the superfine carbon powder with alloy powder according to the weight ratio of 98-60:2-40, prepressing to make the above-mentioned materials into cylinder, then placing pyrauxite block and synthesizing for 1-12 min. at 5-6 GPa and 1350-1450 deg.C to obtain the diamond whose grain size is 1-200 micrometers. As compared with diamond grown on graphite as raw material its nucleation and crystal form perfection are high, conversion rate is high, grain size can be controlled and grain size distribution is uniform, 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 the carbonaceous sol-gel, remove organic solvent or inorganic solvent in the carbonaceous 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 ammoniacal liquor 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 atmosphere of calming the anger 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 the ethylene glycol, makes 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 ℃, holding temperature 2 hours, being warmed up to 3000 ℃ with 70 ℃/minute heating rate then 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 (5)
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 the carbonaceous sol-gel, remove organic solvent or inorganic solvent in the carbonaceous 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 ultrafine carbon is for making through supercritical drying by in the middle of the carbonaceous water-based.
3. 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.
4. 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.
5. 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 |
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|---|---|---|---|
| CN99110845A CN1099906C (en) | 1999-07-21 | 1999-07-21 | Preparation method of bortz body by using superfine carbon powder through synthesis process |
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| CN1281748A true CN1281748A (en) | 2001-01-31 |
| CN1099906C CN1099906C (en) | 2003-01-29 |
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| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101094807B (en) * | 2004-12-09 | 2010-09-29 | 六号元素（产品）（控股）公司 | 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106030B (en) * | 1985-08-13 | 1987-09-16 | 国家建筑材料工业局人工晶体研究所 | The directly method of synthetic microns diamond |
-
1999
- 1999-07-21 CN CN99110845A patent/CN1099906C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101094807B (en) * | 2004-12-09 | 2010-09-29 | 六号元素（产品）（控股）公司 | 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 |
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| Publication number | Publication date |
|---|---|
| CN1099906C (en) | 2003-01-29 |
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