CN103601188A - Preparation method for high-melting point conductive hard ceramic material carbide of tantalum - Google Patents
Preparation method for high-melting point conductive hard ceramic material carbide of tantalum Download PDFInfo
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- CN103601188A CN103601188A CN201310636225.1A CN201310636225A CN103601188A CN 103601188 A CN103601188 A CN 103601188A CN 201310636225 A CN201310636225 A CN 201310636225A CN 103601188 A CN103601188 A CN 103601188A
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Abstract
The invention provides a preparation method for a high-melting point conductive hard ceramic material--carbide of tantalum, which belongs to the technical field of ceramic materials. The main component of the carbide of tantalum is TaC or Ta2C. The material is prepared from tantalum powder and carbon powder through mixing, briquetting, assembling, high-temperature high-pressure synthesis and cooling and pressure relief; high-temperature high-pressure synthesis is carried out on a high pressure apparatus, and a pressure of 5.2 to 6.0 GPa and a temperature of 2000 to 2200 K are maintained for 60 to 180 min. The method provided by the invention is simple, uses no fluxing agent and can be easily carried out; single-phase high-purity TaC or Ta2C is prepared; prepared TaC has a high melting point, high conductivity and high hardness; generation of tantalum steam is effectively inhibited in the process of preparation, and damage and pollution to personnel and the environment are eradicated; an obsolete small-cavity cubic hydraulic press can be effectively utilized, the service life period of the press is prolonged, and energy consumption is saved.
Description
Technical field
The invention belongs to a kind of high-melting-point and conduct electricity the technical field of hard stupalith, particularly main ingredient is tantalum carbide (TaC) or tantalium carbide (Ta
2the preparation method of the carbide of tantalum C).
Background technology
Stupalith has that fusing point is high, high temperature resistant, hardness is high, wear-resistant, and chemical stability is high, resistance to oxidation and corrosion and lightweight, the premium properties such as Young's modulus is large, intensity is high, is widely used in tool and mould, the aspects such as engine, computer optics device.And conducting ceramic material also has good conductive capability, be widely used in electrode of the negative electrode of high-temperature electric hot body in oxidizing atmosphere, high-temperature fuel cell (HTFC) and interconnection material, magnetohydrodynamic generator (MHD) etc.High-melting-point conducts electricity hard stupalith, mainly contains carbide, boride and nitride.As Wimet wolfram varbide, be widely used in a plurality of industrial circles.Tantalum carbide (3880 ℃ of fusing points) is another important cermet material, the cutter made from it, can resistance to 3800 ℃ of high temperature, also can be used as Wimet grain-refining agent, effectively improve alloy property, its industrial consumption has reached the 0.5-5% of Wimet output.
In traditional preparing in tantalum carbon compound method, be all to adopt carborization substantially, take tantalum pentoxide and carbon black and prepare tantalum carbide as raw material.Typical preparation process is: 1 mole of tantalum pentoxide and 7 moles of carbon blacks are fully mixed, put into reduction furnace, in hydrogen or vacuum at 1500 ℃ heat reduction 1h, make tantalum carbide powder.In the method, the product obtaining is Powdered.Pulverous sample, can't form ceramic (as cutter, electrode materials etc.), realizes its industrialized application.If the hard ceramic body material product of preparation conduction, also need to powder body material granular size process, the technological process of a plurality of complexity such as the moulding of powder body material and high temperature sintering.Total institute is known, and tantalum steam is for the toxic effect of human body.The generation that how to suppress tantalum steam in preparation process is very important.Take C and Ta simple substance powder during as raw material reaction sintering generation self-propagating reaction, and product is loose porous, can not obtain fine and close TaC pottery.In addition, tantalum carbon compound also has the electronic structure of similar precious metal and good katalysis.The general transition metal carbides that synthesizes, adopts ball milled, vapour deposition process or ion scorification etc., but the carbide that reaction generates is all powdery substance, and character measurement, industrial application are all caused to difficulty.Therefore, research and develop the preparation method of new tantalum carbon compound, to opening up the application of wide such material, tool is of great significance.
Summary of the invention
The technical problem to be solved in the present invention is the carbide body material that one time to produce goes out tantalum, and the method for employing is high pressure synthesis method.In the method, do not adopt any fusing assistant, mainly by proportioning (being mainly the chemical composition of carbon, tantalum), synthesis temperature and the pressure of raw material, adjust material component and the purity of the carbide of tantalum, effectively suppress the generation of tantalum steam, prepare the tantalum carbon compound body material of higher degree.The method is easy to implement, has greatly shortened the preparation cycle of traditional method, there is no environmental pollution (release of tantalum steam).
The carbide main ingredient of tantalum of the present invention is TaC(tantalum carbide) or Ta
2c(tantalium carbide).
As described below during the concrete technical scheme of synthetic TaC of the present invention.
A high temperature and high pressure preparation process for the carbide of tantalum, the carbide main ingredient of described tantalum is TaC; Preparation method is: take tantalum powder (Ta) and carbon dust (C) is raw material, through batch mixing briquetting, assembling, High Temperature High Pressure technological process synthetic, cooling release, makes the carbide material of tantalum; Described batch mixing briquetting, is that tantalum powder and carbon dust are mixed for 1: 1 in molar ratio, by synthetic cavity size, is pressed into bulk; Said assembling, is to pack block raw material into heating container, puts into synthetic cavity; Said High Temperature High Pressure is synthetic, is to carry out on high-tension unit, at pressure, is that 2.0～6.0GPa, temperature are heat-insulation pressure keeping 10～180 minutes under 2000～2500K; Described cooling release is to stop naturally cooling to release after room temperature after heating.
The optimum material proportion of synthetic TaC is that tantalum powder and carbon dust are 1: 1 in molar ratio, and best synthesis pressure scope is 5.2～6.0GPa, and optimum synthesising temperature scope is 2000～2200K, heat-insulation pressure keeping 60～120 minutes.
Described cooling release, can also be to stop heating rear first pressurize release after 3～8 minutes, then naturally cool to room temperature.The service efficiency that is conducive to like this protection to equipment, the duration of service that reduces press, raising pressure.
Synthetic Ta of the present invention
2as described below during the concrete technical scheme of C.
A high temperature and high pressure preparation process for the carbide of tantalum, the carbide main ingredient of described tantalum is Ta
2c; Preparation method is: take tantalum powder (Ta) and carbon dust (C) is raw material, through batch mixing briquetting, assembling, High Temperature High Pressure technological process synthetic, cooling release, makes the carbide material of tantalum; Described batch mixing briquetting, is that tantalum powder and carbon dust are mixed for 2: 1 in molar ratio, by synthetic cavity size, is pressed into bulk; Said assembling, is to pack block raw material into heating container, puts into synthetic cavity; Said High Temperature High Pressure is synthetic, is to carry out on high-tension unit, at pressure, is that 5.2GPa, temperature are heat-insulation pressure keeping 60 minutes under 2100K; Described cooling release is to stop naturally cooling to release after room temperature after heating.
Described cooling release, can also be to stop heating rear first pressurize release after 3～8 minutes, then naturally cool to room temperature.The service efficiency that is conducive to like this protection to equipment, the duration of service that reduces press, raising pressure.
Compound experiment of the present invention can complete on domestic DS029B type six-plane piercer.Experiment shows, the size of synthesis pressure, temperature, raw-material proportioning are to affect the carbide material phase of tantalum and the important factor of purity thereof.In order to keep sample chamber temperature homogeneity, assembling can be heater-type type of heating; In order to make carbide material and the raw material of synthetic tantalum not oxidized in preparation, can applying argon gas protection in synthetic cavity.
The inventive method is simple, easy to implement; Do not adopt any (such as metallic aluminium etc.) fusing assistant; Proportioning, synthesis temperature and pressure by raw material are adjusted TaC or Ta
2the component of C material and purity thereof, and prepare TaC or the Ta of the higher degree of single-phase
2c.The synthetic product of the present invention is body material, can directly to material character, measure, industrial, directly process goods, and avoided product test and added the moulding in man-hour and the complicated technological process such as high temperature sintering.The TaC material of preparing has high-melting-point (3880 ℃), high conductivity (0.72 * 10
6s/m) and high rigidity (seeing Fig. 7).And in preparation process, effectively suppressed the generation of tantalum steam, stopped personnel and environment damage and pollute.The present invention also can effectively utilize the superseded loculus body cubic hydraulic press high-tension apparatus of China's China superhard material Industry as production unit, extends the working life of existing installation.There is a plurality of superhard material manufacturer in China, and along with the development of pressure technique and the development of superhard material technology, original cubic hydraulic press high-tension apparatus, because cavity is little, yields poorly, and superhard material production industry is gradually eliminated out.The unique method of processing at present this kind equipment reclaims exactly this equipment and again melts down melting to be processed.This technological invention will bring extra profit for enterprise, and is that country saves energy consumption.
Accompanying drawing explanation
Fig. 1 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 1 preparation.
Fig. 2 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 2 preparations.
Fig. 3 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 3 preparations.
Fig. 4 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 4 preparations.
Fig. 5 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 5 preparations.
Fig. 6 is the tantalum carbon compound X-ray diffractogram of the embodiment of the present invention 6 preparations.
Fig. 7 is the hardness test of the embodiment of the present invention 2 tantalum carbon compound TaC.
Embodiment
Following examples all complete on domestic DS029B type six-plane piercer.
The tantalum powder (Ta) of 1～5 micron of analytically pure granularity is mixed with the carbon dust (C) of 1～5 micron of granularity for 1: 1 in molar ratio, after powder is molded, sample is packed in high-pressure chamber.Assembling is made heating tube with graphite in cavity, with agalmatolite, does insulation tube, and synthesis pressure is 2GPa, temperature 2000K, and 180 minutes pressure-maintaining and heat-preservation time, stop heating rear sample and naturally cool to release after room temperature, the component that this condition is prepared is mainly TaC.Concrete X-ray the results are shown in Figure 1.
Adopt the starting material powder identical with embodiment 1, within 1: 1 in molar ratio, mix, after powder is molded, adopt the assembling identical with embodiment 1, synthesis pressure is 5.2GPa, temperature 2200K, 60 minutes pressure-maintaining and heat-preservation time, stop heating rear sample and naturally cool to release after room temperature, it is best that this condition is prepared the TaC(crystallization degree of pure phase).Concrete X-ray the results are shown in Figure 2.
Adopt assembling and the starting material identical with embodiment 1, within 1: 1 in molar ratio, mix, synthesis pressure is 5.2GPa, temperature 2200K, 120 minutes pressure-maintaining and heat-preservation time, stops heating rear sample and naturally cools to release after room temperature, and the tantalum carbon compound that this condition is prepared is that TaC(crystallization degree is fine).Concrete X-ray the results are shown in Figure 3.
Embodiment 4
Adopt assembling and the starting material identical with embodiment 1, within 1: 1 in molar ratio, mix, synthesis pressure is 6GPa, temperature 2200K, 180 minutes pressure-maintaining and heat-preservation time, stops heating rear sample and naturally cools to release after room temperature, and the tantalum carbon compound that this condition is prepared is that TaC(crystallization degree is better).Concrete X-ray the results are shown in Figure 4.
Adopt assembling and the starting material identical with embodiment 1, within 1: 1 in molar ratio, mix, synthesis pressure is 6GPa, temperature 2500K, 10 minutes pressure-maintaining and heat-preservation time, stops heating rear sample and naturally cools to release after room temperature, and it is general that the component that this condition is prepared is mainly TaC(crystallization degree).Concrete X-ray the results are shown in Figure 5.
Embodiment 6
Adopt assembling and the starting material identical with embodiment 1, within 2: 1 in molar ratio, mix, synthesis pressure is 5.2GPa, temperature 2100K, and 60 minutes pressure-maintaining and heat-preservation time, stop heating rear sample and naturally cool to release after room temperature, the component that this condition is prepared is mainly Ta
2c(crystallization degree is general).Concrete X-ray the results are shown in Figure 6.
Embodiment 7
Adopt the inventive method to prepare TaC, it is shown to carry out after polished finish, can directly carry out hardness test (testing with AHVD-1000XY type microhardness instrument at normal temperatures and pressures).Embodiment 2 and the synthetic TaC of embodiment 3 have identical test result, and concrete test result is shown in Fig. 7.
Claims (7)
1. a high temperature and high pressure preparation process for the carbide of tantalum, the carbide main ingredient of described tantalum is TaC; Preparation method is: take tantalum powder and carbon dust as raw material, through batch mixing briquetting, assembling, High Temperature High Pressure technological process synthetic, cooling release, make the carbide material of tantalum; Described batch mixing briquetting, is that tantalum powder and carbon dust are mixed for 1: 1 in molar ratio, by synthetic cavity size, is pressed into bulk; Described assembling, is to pack block raw material into heating container, puts into synthetic cavity; Described High Temperature High Pressure is synthetic, is to carry out on high-tension unit, at pressure, is that 2.0～6.0GPa, temperature are heat-insulation pressure keeping 10～180 minutes under 2000～2500K; Described cooling release is to stop naturally cooling to release after room temperature after heating.
2. the high temperature and high pressure preparation process of the carbide of tantalum according to claim 1, is characterized in that, described High Temperature High Pressure is synthetic, is to be that 5.2～6.0GPa, temperature are heat-insulation pressure keeping 60～120 minutes under 2000～2200K at pressure.
3. the high temperature and high pressure preparation process of the carbide of tantalum according to claim 1 and 2, is characterized in that, described cooling release is to stop heating rear first pressurize release after 3～8 minutes, then naturally cools to room temperature.
4. the high temperature and high pressure preparation process of the carbide of tantalum according to claim 1 and 2, is characterized in that, described assembling, applying argon gas protection in synthetic cavity.
5. a high temperature and high pressure preparation process for the carbide of tantalum, the carbide main ingredient of described tantalum is Ta
2c; Preparation method is: take tantalum powder and carbon dust as raw material, through batch mixing briquetting, assembling, High Temperature High Pressure technological process synthetic, cooling release, make the carbide material of tantalum; Described batch mixing briquetting, is that tantalum powder and carbon dust are mixed for 2: 1 in molar ratio, by synthetic cavity size, is pressed into bulk; Said assembling, is to pack block raw material into heating container, puts into synthetic cavity; Said High Temperature High Pressure is synthetic, is to carry out on high-tension unit, at pressure, is that 5.2GPa, temperature are heat-insulation pressure keeping 60 minutes under 2100K; Described cooling release is to stop naturally cooling to release after room temperature after heating.
6. the high temperature and high pressure preparation process of the carbide of tantalum according to claim 5, is characterized in that, described cooling release is to stop heating rear first pressurize release after 3～8 minutes, then naturally cools to room temperature.
7. according to the high temperature and high pressure preparation process of the carbide of the tantalum described in claim 5 or 6, it is characterized in that described assembling, applying argon gas protection in synthetic cavity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886838A (en) * | 2016-05-03 | 2016-08-24 | 中国有色桂林矿产地质研究院有限公司 | Grid-structure TiB2-Ti composite metal-ceramic material and preparation method thereof |
| CN111423100A (en) * | 2020-04-01 | 2020-07-17 | 北京理工大学 | Method for carrying out rapid heating and imprinting on surface of micro-nano structure by using tantalum coating |
| CN112939569A (en) * | 2021-03-19 | 2021-06-11 | 哈尔滨化兴软控科技有限公司 | Method for recycling tantalum carbide crucible material for PVT (physical vapor transport) method |
| CN114907125A (en) * | 2022-06-20 | 2022-08-16 | 北方民族大学 | Preparation method of tantalum carbide ceramic composite material |
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| JPS56145109A (en) * | 1980-04-12 | 1981-11-11 | Mitsui Mining & Smelting Co Ltd | Preparation of tantalum carbide or niobium carbide |
| CN101328064A (en) * | 2007-06-22 | 2008-12-24 | 中国科学院金属研究所 | In situ reaction heat synthesized TaC-TaSi2 ceramic composite material and preparation thereof |
-
2013
- 2013-11-30 CN CN201310636225.1A patent/CN103601188B/en not_active Expired - Fee Related
Patent Citations (2)
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|---|---|---|---|---|
| JPS56145109A (en) * | 1980-04-12 | 1981-11-11 | Mitsui Mining & Smelting Co Ltd | Preparation of tantalum carbide or niobium carbide |
| CN101328064A (en) * | 2007-06-22 | 2008-12-24 | 中国科学院金属研究所 | In situ reaction heat synthesized TaC-TaSi2 ceramic composite material and preparation thereof |
Non-Patent Citations (3)
| Title |
|---|
| C.L.YEH: "Combustion synthesis of tantalum carbides TaC and Ta2C", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 415, no. 12, 18 May 2006 (2006-05-18), pages 66 - 72 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886838A (en) * | 2016-05-03 | 2016-08-24 | 中国有色桂林矿产地质研究院有限公司 | Grid-structure TiB2-Ti composite metal-ceramic material and preparation method thereof |
| CN111423100A (en) * | 2020-04-01 | 2020-07-17 | 北京理工大学 | Method for carrying out rapid heating and imprinting on surface of micro-nano structure by using tantalum coating |
| CN111423100B (en) * | 2020-04-01 | 2021-07-23 | 北京理工大学 | Method for carrying out rapid heating and imprinting on surface of micro-nano structure by using tantalum coating |
| CN112939569A (en) * | 2021-03-19 | 2021-06-11 | 哈尔滨化兴软控科技有限公司 | Method for recycling tantalum carbide crucible material for PVT (physical vapor transport) method |
| CN114907125A (en) * | 2022-06-20 | 2022-08-16 | 北方民族大学 | Preparation method of tantalum carbide ceramic composite material |
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