CN101734660A - Method for preparing carbonized titanium powder by vacuum carbothermal reduction - Google Patents
Method for preparing carbonized titanium powder by vacuum carbothermal reduction Download PDFInfo
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- CN101734660A CN101734660A CN200910218390A CN200910218390A CN101734660A CN 101734660 A CN101734660 A CN 101734660A CN 200910218390 A CN200910218390 A CN 200910218390A CN 200910218390 A CN200910218390 A CN 200910218390A CN 101734660 A CN101734660 A CN 101734660A
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- 238000000034 method Methods 0.000 title claims abstract description 25
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000000571 coke Substances 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910034327 TiC Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000003407 synthetizing effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing carbonized titanium powder by vacuum carbothermal reduction. A method of vacuum metallurgy is adopted, and the method comprises the following steps: taking titanium dioxide and carbon as raw materials, wherein the mass ratio of the titanium dioxide to the carbon powder is 20:9-21; after crushing and briquetting, entering a vacuum furnace; heating the materials to the temperature of between 1,300 and 1,600 DEG C at a heating rate of 10-15 DEG C per minute; and keeping the temperature for 2 to 10 hours, and controlling the pressure in the furnace to between 10 and 100 Pa. Therefore, the materials undergo vacuum carbothermal reduction reaction, and ultra-fine carbonized titanium powder is prepared.
Description
One, technical field
The present invention relates to a kind of method of preparing carbonized titanium powder by vacuum carbothermal reduction, belong to the vacuum metallurgy technology field,
Two, background technology
Titanium carbide carbon containing 20.05% is the grey powder, has NaCl type cubic crystal structure. density is 4.93 gram per centimeters
3Fusing point: 3160 ℃, boiling point: 4300 ℃; Have high-melting-point, high strength, high rigidity and high elastic coefficient, good heat-shock resistance and chemical stability, high-temperature oxidation resistance only is lower than silicon carbide, it is the important source material of Wimet, therefore in structured material, be widely used in making high-abrasive material, cutter material, mould manufacturing, mechanical component etc. mutually as hard, also can make the crucible of metals such as melting tin, lead, cadmium, zinc, transparent titanium carbide pottery is good optical material; The thermal shock resistance that titanium carbide is good makes it be suitable for being used as special refractory materials in neutrality or reducing atmosphere; The TiC based ceramic metal, it is a kind of heterogeneous matrix material of being formed by metal or alloy and TiC ceramic phase, it had both maintained characteristics such as the high strength, high rigidity of pottery, wear-resistant, high temperature resistant, anti-oxidant and chemical stability, preferred metal toughness is arranged again, and therefore the composite diphase material for preparing with titanium carbide has a wide range of applications in fields such as mechanical workout, metallurgical mineral products, space industry, fusion reactors.
The method of synthesizing titanium carbide powder mainly contains both at home and abroad: (1) TiO
2Carbothermic method; (2) the high temperature cabonization method of titanium and carbon; (3) the self-propagating combustion synthesis method of titanium and carbon (SHS method).Industrial titanium carbide powder is carbon black reduction TiO at first
2Synthetic, temperature of reaction are 1700 ℃～2100 ℃, and the time is 10～24h, carry out in tube furnace or electric arc furnace under the gas atmosphere, because mixing of materials is inhomogeneous, carbon source is at TiO
2Middle distribution is restricted, and material is influenced by diffusion gradient during reaction, and unreacted TiO is arranged after the reaction
2And carbon, usually make synthetic powder pure inadequately.Direct reaction method reaction needs 5～20h, and in exothermal reaction process difficult controlled temperature, reactant is easily reunited, and must attrition process just can prepare micron order TiC powder.Though and the self-propagating combustion synthesis method synthetic TiC that can burn at short notice, moment liberated heat can make product particle agglomeration and grain growth, seldom arrive thin powder.
Document [Koc R, Folmer J.S.Carbothermal synthesis of titanium carbide usingultrafine titania powders[J] .Journal of Materials science, 1997,32 (12): 1301-1311] reported a kind of novel method of superfine titanium carbide powdered preparation, utilize the carbothermic reduction reaction principle, at first with propylene gas C3H6 cracking, the carbon after the cracking is deposited on nano level TiO equably
2The surface, make TiO
2Increase with the carbon contact area, so the kinetics obstacle of material reaction reduces, temperature of reaction is low, reacts more abundant, has obtained submicron grade titanium carbide at 1550 ℃ of carbothermic reduction reactions after 4 hours.Document [Young-Chul Woo, Ho-Jae Kang, Deug J.Kim.Formation of TiC particle during carbothermalreduction of TiO
2[J] .Journal of European Ceramic Society.2007,27:719-722] reported carbothermic reduction TiO
2The method for preparing titanium carbide powder, this method is mainly with TiO
2With resin carbon be raw material; add behind the solvent methanol ball milling mixing 2h on ball mill; dry behind the ball milling, put into graphite heater furnace then and be heated to 1500 ℃ carbothermic reduction reactions take place prepare titanium carbide powder under the argon shield environment, soaking time is 0-45 minute.A kind of refinery coke and TiO of utilizing disclosed among China patent CN1511804A
2Chemical reaction prepares the method for TiC ceramic powder, mainly with TiO
2Powder, a small amount of Ti powder and refinery coke are raw material, make base substrate at 1-3Mpa pressure lower lock block at ball milling on the planetary ball mill after 5 hours, under 800～1100 ℃, light base substrate with the tungsten filament electric ignition in the inert atmosphere then, prepare the TiC ceramic powder.A kind of method of microwave synthetizing nano level titanium carbide is disclosed among the patent CN1348919A, after titanium dioxide and acetylene carbon black oven dry, according to material: zirconium ball: the quality of dehydrated alcohol=1: 1～5: 3～6 mixes than ball milling, oven dry utilizes microwave heating to make raw material generation carbothermic reduction reaction prepare nano titanium carbide.The present invention utilizes under the vacuum condition, can reduce the characteristics of temperature of reaction, minimizing contaminating impurity, has developed the novel method at preparing carbonized titanium powder by vacuum carbothermal reduction end.
Three, summary of the invention
The object of the present invention is to provide a kind of method of preparing carbonized titanium powder by vacuum carbothermal reduction, adopt the method for vacuum metallurgy, with TiO
2With carbon be raw material, in vacuum oven, finish carbothermic reduction reaction and make the superfine titanium carbide powder.It adopts following steps to finish:
1,20: 9～21 weighing mixings of 100-200 purpose titanium dioxide and carbon dust being pressed mass ratio; Described carbon dust is a kind of in charcoal, gac, refinery coke, coal and the carbon black;
2, added in the ball mill ball milling 6～24 hours, drum's speed of rotation is 100～400rpm;
3 make the piece material of Ф 2cm * 1-4cm with the material behind the ball milling at tabletting machine;
4, the piece material is put into vacuum oven, is heated to 1300～1600 ℃, be incubated 2～10 hours, make the reaction of material generation vacuum carbothermal reduction with the temperature rise rate of 10 ℃/min～15 ℃/min, during vacuum oven pressure keep 10Pa～100Pa;
5, the reacted product of vacuum carbothermal reduction is ground, prepare the titanium carbide powder of the granularity that requires.
The present invention has following advantage:
1. but raw material titanium dioxide and carbon are by ball mill ball milling uniform mixing, and the cylinder material behind briquetting fully reacts the generation titanium carbide, can not have unreacted titanium dioxide and carbon simultaneously, and there is not the material spray problem in the material behind the briquetting in vacuum oven;
2. temperature of reaction of the present invention is at 1300 ℃～1600 ℃, and soaking time is 2～10 hours, with preparation method (the carbon black reduction TiO of industrial titanium carbide powder
2, temperature of reaction is 1700 ℃～2100 ℃, the time is 10～24h) to compare the power saving that saves time, save energy.And without any need for shielding gas, product is difficult for oxidized under vacuum condition;
3. the titanium carbide block for preparing is loose, obtains after the grinding＜sub-micron powder of 1 μ m.
Four, embodiment
Embodiment 1: 100-200 purpose titanium dioxide and gac are pressed 20: 9 weighing mixings of mass ratio, contain TiO in the titanium dioxide
2For 〉=98.5wt%, ball milling is 8 hours on the adding planetary ball mill, drum's speed of rotation is 400rpm, and the material behind the ball milling is made the piece material of Ф 2cm * 1.5-2.5cm at tabletting machine, and the piece material is put into vacuum oven, temperature rise rate with 15 ℃/min is heated to 1500 ℃, be incubated 5 hours, make material generation vacuum carbothermal reduction reaction, during vacuum oven pressure keep 10Pa～100Pa, with the reacted material fragmentation of vacuum carbothermal reduction, prepare the titanium carbide powder of granularity＜1 μ m.
Embodiment 2: 100-200 purpose titanium dioxide and carbon black are pressed 20: 12 weighing mixings of mass ratio, contain TiO in the titanium dioxide
2Be 99wt%, ball milling is 20 hours in the adding planetary ball mill, drum's speed of rotation is 200rpm, and the material behind the ball milling is made the piece material of Ф 2 * 2-3cm at tabletting machine, and the piece material is put into vacuum oven, temperature rise rate with 12 ℃/min is heated to 1300 ℃, be incubated 8 hours, make material generation vacuum carbothermal reduction reaction, during vacuum oven pressure keep 50Pa～100Pa, with the reacted material fragmentation of vacuum carbothermal reduction, prepare the titanium carbide powder of granularity＜1 μ m.
Claims (3)
1. the method for a preparing carbonized titanium powder by vacuum carbothermal reduction, it is characterized in that: it adopts following steps to finish,
1) be 20: 9～21 weighing mixings by mass ratio, with 100-200 purpose titanium dioxide and carbon dust;
2), added in the ball mill ball milling 6～24 hours, drum's speed of rotation is 100～400rpm;
3), the material behind the ball milling is made the piece material of Φ 2cm * 1-4cm at tabletting machine;
4), the piece material is put into vacuum oven, be heated to 1300～1600 ℃, be incubated 2～10 hours, make the reaction of material generation vacuum carbothermal reduction with the temperature rise rate of 10 ℃/min～15 ℃/min, during vacuum oven pressure keep 10Pa～100Pa;
5), the reacted product of vacuum carbothermal reduction is ground, prepare the titanium carbide powder of the granularity that requires.
2. the method for preparing carbonized titanium powder by vacuum carbothermal reduction according to claim 1 is characterized in that: described carbon dust is a kind of in charcoal, gac, refinery coke, coal and the carbon black.
3. the method for preparing carbonized titanium powder by vacuum carbothermal reduction according to claim 1 and 2 is characterized in that: contain TiO in the described titanium dioxide
2For 〉=98.5wt%.
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| CN200910218390A CN101734660A (en) | 2009-12-18 | 2009-12-18 | Method for preparing carbonized titanium powder by vacuum carbothermal reduction |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153084A (en) * | 2011-02-28 | 2011-08-17 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing submicron titanium carbide powder |
| CN102719720A (en) * | 2011-03-29 | 2012-10-10 | 厦门钨业股份有限公司 | Method for preparing (Ti, Mo, W(Ta, Nb)) (C, N) solid-solution powder |
| CN102976759A (en) * | 2012-12-17 | 2013-03-20 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing titanium carbonitride by use of vacuum reduction nitriding method |
| CN103193231A (en) * | 2013-04-01 | 2013-07-10 | 攀枝花学院 | Method for preparing titanium carbide or titanium carbonitride |
| CN103265032A (en) * | 2013-06-16 | 2013-08-28 | 桂林理工大学 | Method for preparing TiC powder by respectively using TiOSO4 and pentaerythritol as titanium source and carbon source |
| CN104129994A (en) * | 2014-07-29 | 2014-11-05 | 攀枝花学院 | Preparation method of vanadium titanium carbide |
| CN106587063A (en) * | 2016-12-19 | 2017-04-26 | 北方民族大学 | Method for synthesizing titanium carbide through soft mechanical force chemical auxiliary microwaves |
| CN106784729A (en) * | 2017-01-20 | 2017-05-31 | 武汉科技大学 | Carbide-derived carbon/charcoal composite energy-storage material and preparation method and application |
| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
| CN110257756A (en) * | 2019-07-23 | 2019-09-20 | 海南中航特玻科技有限公司 | A kind of preparation method of surface carbonation titanium metal products |
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2009
- 2009-12-18 CN CN200910218390A patent/CN101734660A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153084B (en) * | 2011-02-28 | 2012-11-14 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing submicron titanium carbide powder |
| CN102153084A (en) * | 2011-02-28 | 2011-08-17 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing submicron titanium carbide powder |
| CN102719720B (en) * | 2011-03-29 | 2015-08-05 | 厦门钨业股份有限公司 | A kind of preparation method of (Ti, Mo, W (Ta, Nb)) (C, N) solid-solution powder |
| CN102719720A (en) * | 2011-03-29 | 2012-10-10 | 厦门钨业股份有限公司 | Method for preparing (Ti, Mo, W(Ta, Nb)) (C, N) solid-solution powder |
| CN102976759A (en) * | 2012-12-17 | 2013-03-20 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing titanium carbonitride by use of vacuum reduction nitriding method |
| CN103193231B (en) * | 2013-04-01 | 2015-12-09 | 攀枝花学院 | Prepare the method for titanium carbide or titanium carbonitride |
| CN103193231A (en) * | 2013-04-01 | 2013-07-10 | 攀枝花学院 | Method for preparing titanium carbide or titanium carbonitride |
| CN103265032A (en) * | 2013-06-16 | 2013-08-28 | 桂林理工大学 | Method for preparing TiC powder by respectively using TiOSO4 and pentaerythritol as titanium source and carbon source |
| CN104129994A (en) * | 2014-07-29 | 2014-11-05 | 攀枝花学院 | Preparation method of vanadium titanium carbide |
| CN104129994B (en) * | 2014-07-29 | 2016-05-04 | 攀枝花学院 | The preparation method of vanadium carbide titanium |
| CN106587063A (en) * | 2016-12-19 | 2017-04-26 | 北方民族大学 | Method for synthesizing titanium carbide through soft mechanical force chemical auxiliary microwaves |
| CN106784729A (en) * | 2017-01-20 | 2017-05-31 | 武汉科技大学 | Carbide-derived carbon/charcoal composite energy-storage material and preparation method and application |
| CN106784729B (en) * | 2017-01-20 | 2019-07-30 | 武汉科技大学 | Carbide-derived carbon/charcoal composite energy-storage material and the preparation method and application thereof |
| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
| CN110257756A (en) * | 2019-07-23 | 2019-09-20 | 海南中航特玻科技有限公司 | A kind of preparation method of surface carbonation titanium metal products |
| CN110257756B (en) * | 2019-07-23 | 2021-08-31 | 海南海控特玻科技有限公司 | Preparation method of surface titanium carbide metal product |
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Open date: 20100616 |