CN104649269A - Method for preparing titanium carbide powder by high frequency induction furnace - Google Patents
Method for preparing titanium carbide powder by high frequency induction furnace Download PDFInfo
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- CN104649269A CN104649269A CN201410755754.8A CN201410755754A CN104649269A CN 104649269 A CN104649269 A CN 104649269A CN 201410755754 A CN201410755754 A CN 201410755754A CN 104649269 A CN104649269 A CN 104649269A
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Abstract
The invention relates to the technical field of semiconductor material preparation, and specifically relates to a method for preparing titanium carbide powder by high frequency induction furnace. The method comprises the following steps: mixing pigment titanium dioxide powder and charcoal powder together, adding the mixture into a ball milling pot, performing ball milling, and then, pressing the material subjected to ball milling into blocks on a tablet press; finally, adding the material into a crucible, placing the crucible into a high-frequency induction heating device, gradually regulating current of the high-frequency induction heating device to 500A to cause carbothermal reduction reaction of the material, and preserving heat for 20 minutes; and after heat preservation, naturally cooling the reduction product to room temperature, taking out the reduction product, and grinding the production product to obtain the ultrafine titanium carbide powder. The powder prepared by the method has uniform grain shape, even grain distribution and no big agglomeration phenomenon.
Description
Technical field
The present invention relates to technical field of semiconductor material preparation, be specifically related to a kind of method that carbonized titanium powder prepared by high frequency furnace.
Background technology
Titanium carbide has NaCl type cubic crystal structure, its characteristic is: high-melting-point (3067 DEG C), high strength, high Vickers' hardness (29 ~ 34GPa), high elastic coefficient (410 ~ 450GPa), excellent conductivity (30 × 10
6w
-1cm) and thermal conductivity, high-temperature oxidation resistance only lower than silicon carbide, and has excellent compatibility with other carbide.Be widely used in the fields such as cutter material, wearing-proof refractory material, aviation and metallurgical mineral products.
At present both at home and abroad the method for synthesizing titanium carbide powder mainly contains: (1) is with carbon or carbonaceous organic material carbothermic reduction titanium dioxide powder; (2) sol-gel method prepares the polymeric precursor of inorganics and carbonaceous organic material, and then titanium carbide powder is prepared in carbothermic reduction.(3) titanium and carbon direct reaction method (SHS or MA method); (4) TiCI
4with gaseous hydrocarbons gas-phase reaction method.Wherein carbothermic reduction titanium dioxide method is applied to industrial production, and it has cheaper starting materials and the simple advantage of technological process.Under argon atmosphere, in tube furnace or resistance furnace, carbothermic reduction titanium dioxide needs very high temperature of reaction (1700 ~ 2100 DEG C) and very long reaction times (10 ~ 24h), therefore occurs that particle agglomeration, particle shape are uneven, has the problems such as unreacted raw material in product.
Summary of the invention
The present invention is intended to propose the novel method that a kind of high-frequency induction carbothermic reduction titanium dioxide prepares superfine titanium carbide powder.
Technical program of the present invention lies in:
A method for carbonized titanium powder prepared by high frequency furnace, adopts following steps:
By pigmentary titanium dioxide powder and wood charcoal powder mixing, add in ball grinder, carry out ball milling, then ball milling material is pressed into block on tabletting machine, finally material loaded crucible and put into HF induction heating apparatus, regulate the electric current of HF induction heating apparatus to make material generation carbothermic reduction reaction to 500A gradually, and be incubated 20min; Insulation terminates rear reduzate and naturally cools to room temperature, takes out reduzate, obtains superfine titanium carbide powder after grinding fragmentation.
Preferably, the mol ratio of described titanium dioxide powder and wood charcoal powder mixing is 1:3 and 1:4.
Preferably, described ball milling adopts planetary ball mill, and Ball-milling Time is 6 ~ 10h, and rotating speed during ball milling is 300 ~ 400r/min.
Preferably, describedly need with argon gas to be protective atmosphere when material being put into HF induction heating apparatus.
Preferably, describedly need to complete under an argon atmosphere when reduzate being cooled to room temperature.
Or preferably, the temperature regulating range of described adjustment HF induction heating apparatus is 100-500 DEG C, and regulations speed is 10 DEG C/30min.
Or the block of preferably, described compression moulding is of a size of F2cm × 2cm ~ F2cm × 4cm.
Or plumbago crucible selected by preferably, described crucible.
Technique effect of the present invention is:
The present invention adopts high-frequency induction carbothermic method to prepare titanium carbide powder novel process, raw material titanium dioxide is read interior abundant reaction and prepares the very low superfine titanium carbide powder of foreign matter content when very short, temperature of reaction is 1490 ~ 1510 DEG C, size-grade distribution (D50) is between l ~ lOum, this powder particle shape is consistent, is evenly distributed and without bulk agglomeration.
Embodiment
A method for carbonized titanium powder prepared by high frequency furnace, adopts following steps:
By pigmentary titanium dioxide powder and wood charcoal powder mixing, add in ball grinder, carry out ball milling, then ball milling material is pressed into block on tabletting machine, finally material loaded crucible and put into HF induction heating apparatus, regulate the electric current of HF induction heating apparatus to make material generation carbothermic reduction reaction to 500A gradually, and be incubated 20min; Insulation terminates rear reduzate and naturally cools to room temperature, takes out reduzate, obtains superfine titanium carbide powder after grinding fragmentation.
Wherein, the mol ratio of titanium dioxide powder and wood charcoal powder mixing is 1:3 and 1:4.Ball milling adopts planetary ball mill, and Ball-milling Time is 6 ~ 10h, and rotating speed during ball milling is 300 ~ 400r/min.Need with argon gas to be protective atmosphere when material being put into HF induction heating apparatus.Need when reduzate being cooled to room temperature to complete under an argon atmosphere.The temperature regulating range regulating HF induction heating apparatus is 100-500 DEG C, and regulations speed is 10 DEG C/30min.The block of compression moulding is of a size of F2cm × 2cm ~ F2cm × 4cm.Plumbago crucible selected by crucible.
The present invention adopts High Frequency Solid State induction heating equipment to heat, can in heat-processed
By infrared thermometer, material reduction reaction temperature is monitored.
Claims (8)
1. a method for carbonized titanium powder prepared by high frequency furnace, it is characterized in that: adopt following steps:
By pigmentary titanium dioxide powder and wood charcoal powder mixing, add in ball grinder, carry out ball milling, then ball milling material is pressed into block on tabletting machine, finally material loaded crucible and put into HF induction heating apparatus, regulate the electric current of HF induction heating apparatus to make material generation carbothermic reduction reaction to 500A gradually, and be incubated 20min; Insulation terminates rear reduzate and naturally cools to room temperature, takes out reduzate, obtains superfine titanium carbide powder after grinding fragmentation.
2. as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: the mol ratio of described titanium dioxide powder and wood charcoal powder mixing is 1:3 and 1:4.
3. as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: described ball milling adopts planetary ball mill, and Ball-milling Time is 6 ~ 10h, and rotating speed during ball milling is 300 ~ 400r/min.
4., as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: described when material being put into HF induction heating apparatus needs be protective atmosphere with argon gas.
5. as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: described need to complete under an argon atmosphere when reduzate being cooled to room temperature.
6., as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: the temperature regulating range of described adjustment HF induction heating apparatus is 100-500 DEG C, regulations speed is 10 DEG C/30min.
7., as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: the block of described compression moulding is of a size of F2cm × 2cm ~ F2cm × 4cm.
8., as the method for carbonized titanium powder prepared by claim 1 high frequency furnace, it is characterized in that: plumbago crucible selected by described crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410755754.8A CN104649269A (en) | 2014-12-11 | 2014-12-11 | Method for preparing titanium carbide powder by high frequency induction furnace |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410755754.8A CN104649269A (en) | 2014-12-11 | 2014-12-11 | Method for preparing titanium carbide powder by high frequency induction furnace |
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| CN104649269A true CN104649269A (en) | 2015-05-27 |
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| CN201410755754.8A Pending CN104649269A (en) | 2014-12-11 | 2014-12-11 | Method for preparing titanium carbide powder by high frequency induction furnace |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055534A (en) * | 2017-03-20 | 2017-08-18 | 锦州博德新金属材料有限公司 | The method that high-purity titanium carbide is prepared using low-purity titanium material |
| CN108823445A (en) * | 2018-07-19 | 2018-11-16 | 佛山陵朝新材料有限公司 | A kind of preparation method of high-strength corrosion-resisting cermet |
| CN114890423A (en) * | 2022-04-30 | 2022-08-12 | 浙江万畅环保科技有限公司 | Method for synthesizing titanium carbide/carbon at low temperature |
-
2014
- 2014-12-11 CN CN201410755754.8A patent/CN104649269A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055534A (en) * | 2017-03-20 | 2017-08-18 | 锦州博德新金属材料有限公司 | The method that high-purity titanium carbide is prepared using low-purity titanium material |
| CN108823445A (en) * | 2018-07-19 | 2018-11-16 | 佛山陵朝新材料有限公司 | A kind of preparation method of high-strength corrosion-resisting cermet |
| CN114890423A (en) * | 2022-04-30 | 2022-08-12 | 浙江万畅环保科技有限公司 | Method for synthesizing titanium carbide/carbon at low temperature |
| CN114890423B (en) * | 2022-04-30 | 2024-04-09 | 浙江万畅环保科技有限公司 | Method for synthesizing titanium carbide/carbon at low temperature |
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Application publication date: 20150527 |