CN103601188B - The preparation method of the carbide of high-melting-point conductive hard ceramic material tantalum - Google Patents
The preparation method of the carbide of high-melting-point conductive hard ceramic material tantalum Download PDFInfo
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Abstract
The preparation method of the carbide of high-melting-point conductive hard ceramic material tantalum of the present invention, belongs to the technical field of stupalith.The carbide main ingredient of tantalum is TaC or Ta
2c.With tantalum powder and carbon dust for raw material, the technological process through batch mixing briquetting, assembling, HP-HT synthesize, cooling release obtains the carbide material of tantalum; Described HP-HT synthesize carries out on high-tension unit, pressure be 5.2 ~ 6.0GPa, temperature be 2000 ~ 2200K under heat-insulation pressure keeping 60 ~ 180 minutes.The inventive method is simple, does not adopt any fusing assistant, easy to implement; Prepare TaC or Ta of the higher degree of single-phase
2c; The TaC material prepared has high-melting-point, high conductivity and high rigidity; Restrained effectively the generation of tantalum steam in preparation process, stopped personnel and environmental pollution and pollution; The little cavity cubic hydraulic press be eliminated can be effectively utilized, extend its working life, save energy consumption.
Description
Technical field
The invention belongs to a kind of technical field of high-melting-point conductive hard ceramic material, 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 the electrode etc. of the high-temperature electric hot body in oxidizing atmosphere, the negative electrode of high-temperature fuel cell (HTFC) and interconnection material, magnetohydrodynamic generator (MHD).High-melting-point conductive hard ceramic material, mainly contains carbide, boride and nitride.As Wimet wolfram varbide, be widely used in multiple industrial circle.Tantalum carbide (fusing point 3880 DEG C) is another important cermet material, with the cutter that it is made, can resistance to 3800 DEG C of high temperature, also can be used as Wimet grain-refining agent, effective raising alloy property, its industrial consumption has reached the 0.5-5% of Wimet output.
Preparing in tantalum carbon compound method traditional, is all adopt carborization substantially, namely with tantalum pentoxide and carbon black for tantalum carbide prepared by 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 DEG C heat reduction 1h, i.e. obtained tantalum carbide powder.In the method, the product obtained 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 process powder body material granular size, the technological process of multiple complexity such as the shaping and high temperature sintering of powder body material.Total institute is known, and tantalum steam is for the toxic effect of human body.How to suppress the generation of tantalum steam very important in preparation process.During with C and Ta elemental powders for raw material reaction sintering generation self-propagating reaction, product 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.General synthesis transition metal carbides, adopts ball milled, vapour deposition process or ion scorification etc., but the carbide that reaction generates is all powdery substance, all causes difficulty to character measurement, industrial application.Therefore, research and develop the preparation method of new tantalum carbon compound, to the application of opening up such material wide, 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, adjust material component and the purity of the carbide of tantalum mainly through the proportioning (mainly the chemical composition of carbon, tantalum) of raw material, synthesis temperature and pressure, effectively suppress the generation of tantalum steam, prepare the tantalum carbon compound body material of higher degree.The method is easy to implement, substantially reduces the preparation cycle of traditional method, does not have 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).
Of the present invention synthesis TaC concrete technical scheme time as described below.
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: with tantalum powder (Ta) and carbon dust (C) for raw material, the technological process through batch mixing briquetting, assembling, HP-HT synthesize, cooling release obtains the carbide material of tantalum; Described batch mixing briquetting, is tantalum powder and carbon dust to be mixed at 1: 1 in molar ratio, is pressed into bulk by synthetic cavity size; Said assembling, is that block stock is loaded heating container, puts into synthetic cavity; Said HP-HT synthesize carries out on high-tension unit, pressure be 2.0 ~ 6.0GPa, temperature be 2000 ~ 2500K under heat-insulation pressure keeping 10 ~ 180 minutes; Described cooling release naturally cools to release after room temperature after stopping heating.
The optimum material proportion of synthesis TaC is tantalum powder and carbon dust is 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 stop the rear first pressurize release after 3 ~ 8 minutes of heating, then naturally cool to room temperature.The service efficiency being conducive to the protection to equipment like this, reducing the duration of service of press, improve pressure.
Synthesis 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: with tantalum powder (Ta) and carbon dust (C) for raw material, the technological process through batch mixing briquetting, assembling, HP-HT synthesize, cooling release obtains the carbide material of tantalum; Described batch mixing briquetting, is tantalum powder and carbon dust to be mixed at 2: 1 in molar ratio, is pressed into bulk by synthetic cavity size; Said assembling, is that block stock is loaded heating container, puts into synthetic cavity; Said HP-HT synthesize carries out on high-tension unit, pressure be 5.2GPa, temperature be 2100K under heat-insulation pressure keeping 60 minutes; Described cooling release naturally cools to release after room temperature after stopping heating.
Described cooling release, can also be stop the rear first pressurize release after 3 ~ 8 minutes of heating, then naturally cool to room temperature.The service efficiency being conducive to the protection to equipment like this, reducing the duration of service of press, improve 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 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 the carbide material of synthesis tantalum and raw material 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; TaC or Ta is adjusted by the proportioning of raw material, synthesis temperature and pressure
2the component of C material and purity thereof, and TaC or Ta preparing the higher degree of single-phase
2c.The product of the present invention's synthesis is body material, directly can measure material character, industrially directly process goods, and avoids product test and add the complicated technological process such as the shaping of man-hour and high temperature sintering.The TaC material prepared has high-melting-point (3880 DEG C), high conductivity (0.72 × 10
6and high rigidity (see Fig. 7) S/m).And in preparation process, restrained effectively the generation of tantalum steam, stopped personnel and environmental pollution and pollution.The present invention also can effectively utilize the superseded little cavity 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 multiple 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 is little due to cavity, yields poorly, and be eliminated out superhard material production industry gradually.The unique method of current this kind equipment of process reclaims this equipment exactly and again melts down melting process.This technological invention will bring extra profit for enterprise, and is that country saves energy consumption.
Accompanying drawing explanation
Fig. 1 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 1.
Fig. 2 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 2.
Fig. 3 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 3.
Fig. 4 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 4.
Fig. 5 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 5.
Fig. 6 is tantalum carbon compound X-ray diffractogram prepared by the embodiment of the present invention 6.
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.
Embodiment 1
The carbon dust (C) of the tantalum powder (Ta) of analytically pure granularity 1 ~ 5 micron and granularity 1 ~ 5 micron to be mixed in molar ratio at 1: 1, after powder is molded, sample is loaded in high-pressure chamber.Make heating tube with graphite in assembling cavity, do insulation tube with agalmatolite, synthesis pressure is 2GPa, temperature 2000K, 180 minutes pressure-maintaining and heat-preservation time, and after stopping heating, sample naturally cools to release after room temperature, and the component that this condition is prepared is mainly TaC.Concrete X-ray the results are shown in Figure 1.
Embodiment 2
Adopt the starting material powder identical with embodiment 1,1: 1 mixing in molar ratio, 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, after stopping heating, sample naturally cools to release after room temperature, and the TaC(crystallization degree that this condition prepares pure phase is best).Concrete X-ray the results are shown in Figure 2.
Embodiment 3
Adopt the assembling identical with embodiment 1 and starting material, in molar ratio 1: 1 mixing, synthesis pressure is 5.2GPa, temperature 2200K, 120 minutes pressure-maintaining and heat-preservation time, after stopping heating, sample 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 the assembling identical with embodiment 1 and starting material, in molar ratio 1: 1 mixing, synthesis pressure is 6GPa, temperature 2200K, 180 minutes pressure-maintaining and heat-preservation time, after stopping heating, sample 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.
Embodiment 5
Adopt the assembling identical with embodiment 1 and starting material, in molar ratio 1: 1 mixing, synthesis pressure is 6GPa, temperature 2500K, 10 minutes pressure-maintaining and heat-preservation time, after stopping heating, sample 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 the assembling identical with embodiment 1 and starting material, in molar ratio 2: 1 mixing, synthesis pressure is 5.2GPa, temperature 2100K, 60 minutes pressure-maintaining and heat-preservation time, and stop the rear sample of heating to 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, after it is shown to carry out polished finish, directly can carry out hardness test (at normal temperatures and pressures, testing with AHVD-1000XY type microhardness instrument).The TaC that embodiment 2 and embodiment 3 are synthesized has 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: with tantalum powder and carbon dust for raw material, the technological process through batch mixing briquetting, assembling, HP-HT synthesize, cooling release obtains the carbide material of tantalum; Described batch mixing briquetting, is tantalum powder and carbon dust to be mixed at 1: 1 in molar ratio, is pressed into bulk by synthetic cavity size; Described assembling, is that block stock is loaded heating container, puts into synthetic cavity; Described HP-HT synthesize carries out on high-tension unit, pressure be 2.0 ~ 6.0GPa, temperature be 2000 ~ 2500K under heat-insulation pressure keeping 10 ~ 180 minutes; Described cooling release naturally cools to release after room temperature after stopping heating.
2. the high temperature and high pressure preparation process of the carbide of tantalum according to claim 1, is characterized in that, described HP-HT synthesize, be pressure be 5.2 ~ 6.0GPa, temperature be 2000 ~ 2200K under heat-insulation pressure keeping 60 ~ 120 minutes.
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 the rear first pressurize release after 3 ~ 8 minutes of heating, 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: with tantalum powder and carbon dust for raw material, the technological process through batch mixing briquetting, assembling, HP-HT synthesize, cooling release obtains the carbide material of tantalum; Described batch mixing briquetting, is tantalum powder and carbon dust to be mixed at 2: 1 in molar ratio, is pressed into bulk by synthetic cavity size; Said assembling, is that block stock is loaded heating container, puts into synthetic cavity; Said HP-HT synthesize carries out on high-tension unit, pressure be 5.2GPa, temperature be 2100K under heat-insulation pressure keeping 60 minutes; Described cooling release naturally cools to release after room temperature after stopping 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 the rear first pressurize release after 3 ~ 8 minutes of heating, then naturally cools to room temperature.
7. the high temperature and high pressure preparation process of the carbide of the tantalum according to claim 5 or 6, is characterized in that, described assembling, applying argon gas protection in synthetic cavity.
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| 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 |
| 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 |
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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| Combustion synthesis of tantalum carbides TaC and Ta2C;C.L.Yeh;《Journal of Alloys and Compounds》;20060518;第415卷(第1-2期);66-72 * |
| Structure and some properties of sintered tantalun carbide;S.A.Shvab;《Powder Metallurgy and Metal Ceramics》;19821130;第21卷(第11期);894-897 * |
| 自蔓延高温合成TaC粉末;谭卫宁;《湖南化工》;19980430;第28卷(第2期);27-29 * |
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