CN114790112A - High-hardness and high-heat-stability tantalum nitride block prepared based on domestic cubic press - Google Patents
High-hardness and high-heat-stability tantalum nitride block prepared based on domestic cubic press Download PDFInfo
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- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 3
- 239000007858 starting material Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005553 drilling Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 229910002804 graphite Inorganic materials 0.000 description 15
- 239000010439 graphite Substances 0.000 description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052903 pyrophyllite Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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Abstract
The invention discloses a preparation method for preparing a large-size tantalum nitride block based on a domestic cubic press, which comprises the following steps of (1) grinding a tantalum nitride initial material; (2) and carrying out vacuum treatment on the tantalum nitride powder obtained by grinding, and prepressing into a cylindrical block. (3) Putting the pressed cylindrical block into a high-pressure synthesis block; (4) placing the high-pressure synthesis block in a synthesis cavity of a domestic cubic press to perform high-temperature high-pressure phase-change sintering; the sintering pressure is 2-6 GPa; the temperature is 600-1800 ℃; the heat preservation time is 5-60 minutes; (5) and after sintering, cooling and decompressing, and taking out the tantalum nitride sintered body with the block diameter of 10 mm. The tantalum nitride block prepared by the method has the characteristics of uniform microstructure, few pores and hardness and thermal stability superior to those of the traditional pure-phase tungsten carbide, and can be widely applied to the fields of machinery manufacturing, geological drilling, grinding tool industry and the like.
Description
Technical Field
The invention relates to a preparation method of a superhard block material, in particular to a large-size tantalum nitride block prepared based on a domestic cubic press.
Background
A large number of researches show that the tantalum nitride (TaN) has excellent heat resistance, chemical stability and hardness, so that the tantalum nitride (TaN) can be used in the fields of industrial production and the like. In particular, theoretical studies have shown that tantalum nitride of the tungsten carbide type (WC-type) is a superhard material, with a theoretical hardness of up to 37.1 GPa, and has a bulk modulus (400 GPa) similar to that of cubic boron nitride (cBN). In 1972, WC-type tantalum nitride was first synthesized by Brauer et al at 1073-1233K and a temperature pressure of 2-10 GPa. Two decades later, Mashimo et al also successfully prepared single phase bodies of WC-type tantalum nitride at static high pressures of 0.8-3 GPa. But the hardness of WC-type tantalum nitride prepared by the method is far lower than the theoretical hardness of 37.1 GPa. Recently, Yusa et al prepared WC-type tantalum nitride blocks again by high temperature and high pressure methods, with Vickers hardness of only 11.3 + -2.2 GPa (1 Kg load), size of only 5 mm, and also much lower than the theoretical hardness of WC-type tantalum nitride (37.1 GPa). WC-type tantalum nitride is not a true superhard material. In order to solve the problems, the WC-type tantalum nitride with the Vickers hardness of 30 GPa (1 Kg load) and the thermal stability of 1077K is successfully prepared by using the high-temperature and high-pressure conditions of a domestic cubic press, and the diameter of a block body of the WC-type tantalum nitride reaches 10 mm.
Disclosure of Invention
The method for preparing the tantalum nitride block with high hardness and high thermal stability by using the domestic cubic press comprises the following steps:
(1) grinding a tantalum nitride initial material (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure);
(2) carrying out vacuum treatment on the tantalum nitride powder obtained by grinding, and prepressing the tantalum nitride powder into a cylindrical block;
(3) putting the pressed cylinder into a high-pressure synthesis block;
(4) placing the assembled high-pressure synthesis block into a synthesis cavity of a domestic cubic press to perform high-temperature high-pressure phase change sintering, wherein the sintering pressure is not lower than 2 GPa; the sintering temperature is not lower than 600 ℃, and the sintering time is not less than 5 min; (ii) a
(5) And after sintering, cooling, relieving pressure and removing the inclusion to obtain the large-size tantalum nitride block with high hardness and high thermal stability.
Compared with the prior art, the invention has the following beneficial effects:
(1) the WC-type tantalum nitride single-phase body is successfully prepared by adopting a domestic cubic apparatus large-cavity press.
(2) The WC-type tantalum nitride block prepared by the invention has Vickers hardness of 30 GPa under the loading of 1 Kg, thermal stability of 1077K, and performance superior to that of the traditional pure-phase tungsten carbide (26 GPa, 800K). In addition, the size of the WC-type tantalum nitride block prepared by the method reaches 10 mm, and the industrial application prospect of the WC-type tantalum nitride is widened.
(3) The invention fully utilizes the advantages of the domestic cubic apparatus large cavity press, has simple preparation process, applies pressure of 2-6 GPa, temperature of 800-1700 ℃, heat preservation time of 5-60 min and lower temperature and pressure conditions during sintering, and is completely suitable for domestic industrial production.
Drawings
Figure 1 shows a schematic diagram of a domestic cubic press based synthesis assembly.
FIG. 2 shows XRD patterns of WC-type tantalum nitride prepared in example 3 and the starting material.
FIG. 3 shows an optical photograph and microstructure morphology of WC-type tantalum nitride as prepared in example 4.
FIG. 4 shows the Vickers hardness of WC-type tantalum nitride prepared in example 4 under different loadings.
FIG. 5 shows a differential thermogram of WC-type tantalum nitride prepared in example 5.
Detailed Description
The first embodiment is as follows: taking tantalum nitride powder (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure) for grinding, putting the ground tantalum nitride powder into a vacuum furnace, introducing hydrogen into the vacuum furnace for vacuum treatment at 1000-1600 ℃, taking out the tantalum nitride powder after the vacuum treatment, prepressing the tantalum nitride into a cylindrical block by using a mold, putting the pressed cylindrical block into graphite in a pyrophyllite synthesis block, and sequentially assembling a graphite flake, a molybdenum flake and a conductive steel ring at the upper end and the lower end of a graphite tube. And after the assembly, putting the synthetic block into a large-press synthetic cavity, keeping the temperature and pressure at about 1000 ℃ and the pressure at about 2 GPa for about 20 min, cooling and reducing the pressure, and taking out the synthetic sintered block, namely the WC-type tantalum nitride block.
The second embodiment: taking tantalum nitride powder (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure) for grinding, putting the ground powder into a vacuum furnace, introducing hydrogen into the vacuum furnace for vacuum sintering at 1000-1600 ℃, taking out the tantalum nitride powder after vacuum sintering, prepressing the tantalum nitride into a cylindrical block by using a mold, putting the pressed cylindrical block into graphite in a pyrophyllite synthesis block, and sequentially assembling a graphite sheet, a molybdenum sheet and a conductive steel ring at the upper end and the lower end of a graphite tube. And after the assembly, putting the synthetic block into a large-press synthetic cavity, keeping the temperature and pressure at about 1400 ℃ and the pressure at about 4 GPa for about 45 min, cooling and depressurizing, and taking out the sintered block, wherein the block is WC-type tantalum nitride.
Example three: taking tantalum nitride powder (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure) for grinding, putting the ground tantalum nitride powder into a vacuum furnace, introducing hydrogen into the vacuum furnace for vacuum sintering at 1000-1600 ℃, taking out the tantalum nitride powder after vacuum sintering, prepressing the tantalum nitride into a cylindrical block by using a die, putting the pressed cylindrical block into graphite in a pyrophyllite synthetic block, and sequentially assembling a graphite sheet, a molybdenum sheet and a conductive steel ring at the upper end and the lower end of a graphite tube. And after the assembly, putting the synthetic block into a large-press synthetic cavity, keeping the temperature and pressure at about 1600 ℃ and the pressure at about 5 GPa for about 30 min, cooling and reducing the pressure, and taking out the sintered block, wherein the block is WC-type tantalum nitride.
Example four: taking tantalum nitride powder (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure) for grinding, putting the ground powder into a vacuum furnace, introducing hydrogen into the vacuum furnace for vacuum sintering at 1000-1600 ℃, taking out the tantalum nitride powder after vacuum sintering, prepressing the tantalum nitride into a cylindrical block by using a mold, putting the pressed cylindrical block into graphite in a pyrophyllite synthesis block, and sequentially assembling a graphite sheet, a molybdenum sheet and a conductive steel ring at the upper end and the lower end of a graphite tube. And after the assembly, putting the synthetic block into a large-press synthetic cavity, keeping the temperature and pressure at 1800 ℃ and the pressure at about 5.5 GPa for about 20 min, cooling and depressurizing, and taking out the sintered block, namely the WC-type tantalum nitride block.
Example five: taking tantalum nitride powder (CoSn-type tantalum nitride with a hexagonal structure or WC-type tantalum nitride with a cubic structure) for grinding, putting the ground tantalum nitride powder into a vacuum furnace, introducing hydrogen into the vacuum furnace for vacuum sintering at 1000-1600 ℃, taking out the tantalum nitride powder after vacuum sintering, prepressing the tantalum nitride into a cylindrical block by using a die, putting the pressed cylindrical block into graphite in a pyrophyllite synthetic block, and sequentially assembling a graphite sheet, a molybdenum sheet and a conductive steel ring at the upper end and the lower end of a graphite tube. And after the assembly, putting the synthetic block into a large-press synthetic cavity, keeping the temperature and pressure at 1700 ℃ and the pressure at about 5 GPa, and taking out the sintered block after cooling and pressure reduction for 30 min, wherein the block is WC-type tantalum nitride.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. Based on a domestic cubic press, a tantalum nitride block with high hardness and high thermal stability is prepared, and relates to a method for preparing the tantalum nitride block by utilizing the domestic cubic press under the conditions of high temperature and high pressure, which is characterized by comprising the following steps:
(1) grinding the tantalum nitride initial material;
(2) carrying out vacuum treatment on the tantalum nitride powder obtained by grinding, and prepressing the tantalum nitride powder into a cylindrical block;
(3) putting the pressed cylinder into a high-pressure synthesis block;
(4) placing the assembled high-pressure synthesis block in a synthesis cavity of a domestic cubic press to perform high-temperature high-pressure phase change sintering;
(5) and after sintering, cooling, relieving pressure and removing the inclusion to obtain the large-size tantalum nitride block with high hardness and high thermal stability.
2. The tantalum nitride starting material according to claim 1 (1), wherein the tantalum nitride starting material is in the form of powder, granules or blocks.
3. The tantalum nitride starting material of claim 1 (1); the method is characterized in that the nitrogen initial material is CoSn-type with a hexagonal structure (P6/mmm) or WC-type tantalum nitride with a cubic structure (P-6 m 2).
4. The high-temperature high-pressure sintering according to claim 1 (4), wherein the sintering temperature is 600-1800 ℃; the pressure is 2-6 GPa; the heat preservation time is 5-60 min.
5. The high-temperature high-pressure phase-change sintering according to claim 1 (4); the method is characterized in that the phase change is the conversion of hexagonal phase CoSn-type tantalum nitride to cubic phase WC-type tantalum nitride under the conditions of high temperature and high pressure.
6. The high hardness and high thermal stability tantalum nitride mass of claim 1 (5); the high hardness is Vickers hardness of 30 GPa, thermal stability of 1077K, and block diameter of 10 mm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06305732A (en) * | 1993-04-27 | 1994-11-01 | Toshiba Tungaloy Co Ltd | Wc type tantalum nitride and method for synthesizing the same |
| CN105339516A (en) * | 2013-05-31 | 2016-02-17 | 山特维克知识产权股份有限公司 | New process of manufacturing cemented carbide and a product obtained thereof |
| CN107311663A (en) * | 2017-04-01 | 2017-11-03 | 四川大学 | A kind of new tantalum nitride hard alloy and preparation method thereof |
| CN110922192A (en) * | 2019-11-20 | 2020-03-27 | 天津大学 | Polycrystalline cubic boron nitride cutter material |
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- 2021-01-26 CN CN202110104832.8A patent/CN114790112A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06305732A (en) * | 1993-04-27 | 1994-11-01 | Toshiba Tungaloy Co Ltd | Wc type tantalum nitride and method for synthesizing the same |
| CN105339516A (en) * | 2013-05-31 | 2016-02-17 | 山特维克知识产权股份有限公司 | New process of manufacturing cemented carbide and a product obtained thereof |
| CN107311663A (en) * | 2017-04-01 | 2017-11-03 | 四川大学 | A kind of new tantalum nitride hard alloy and preparation method thereof |
| CN110922192A (en) * | 2019-11-20 | 2020-03-27 | 天津大学 | Polycrystalline cubic boron nitride cutter material |
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