CN107164680A - A kind of preparation method of metal carbides solid solution - Google Patents
A kind of preparation method of metal carbides solid solution Download PDFInfo
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- CN107164680A CN107164680A CN201710409843.0A CN201710409843A CN107164680A CN 107164680 A CN107164680 A CN 107164680A CN 201710409843 A CN201710409843 A CN 201710409843A CN 107164680 A CN107164680 A CN 107164680A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/055—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using carbon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation method of metal carbides solid solution；Micro-nano tungsten carbide/molybdenum/tantalate solid solution the composite powder is with tungsten, molybdenum and tantalum carburet and solid solution forms (W, Mo, Ta) C solid solution；The preparation method of the micro-nano tungsten carbide/molybdenum/tantalate solid solution composite powder includes the steps such as dispensing, high-energy ball milling solid phase reaction, hot combination reaction.Tungsten carbide/molybdenum/tantalate solid solution composite powder that the present invention is prepared is micro/nano level and is evenly distributed.
Description
The present invention is Application No. 201610061685.X, at 29 on the applying date 2016 year 01 month, entitled " micro-nano
The divisional application of tungsten carbide/molybdenum/tantalate solid solution composite powder and preparation method thereof ".
Technical field
The present invention relates to powder metallurgical technology, and in particular to a kind of preparation side of metal carbides solid solution composite powder
Method.
Background technology
Metal carbides have higher fusing point, hardness, and good anticorrosive, heat endurance are widely used in industrial each
Individual field, the particularly common rapidoprint in modern manufacturing industry.Hard phase Ti (C, N) in cermet material) it is polycrystalline sintering
Material, its deadly defect is that fragility is big, toughness is not enough, and hard phase is not yet obtained at present with the wetting out problems that match of Binder Phase
Solve, cause its obdurability not enough, be the crucial problem faced in cermet material practical engineering application.Therefore to high-performance
The design Main way of cermet material is to overcome fragility and raising toughness.At present, by adding Equations of The Second Kind metal carbides
To improve wetabilitys of the Ti (C, N) between Binder Phase, reinforced structure, and corresponding metallic element solid solution is set to enter hard phase and viscous
Tie in phase, reach certain solution strengthening purpose.Tungsten carbide (WC), molybdenum carbide (Mo2C), ramet (TaC) belongs to transition gold
Belong to carbide, the features such as with higher hardness, fusing point.Substantial amounts of research shows, appropriate WC is added in cermet, can be changed
Kind Binder Phase is to the wetability of hard phase, and the opposing party can be such that hard phase crystal grain substantially refines, so that the mechanical property of alloy is carried
It is high.And Mo or Mo2C can improve wetability of the liquid metal Binder Phase to TiC particles, under conditions of complete wetting, TiC particles
Occur without accumulative crystallization, it is suppressed that Carbide Phases crystal grain grows up during sintering.Adding TaC in cermet can be significantly thin
Change the particle of hard phase, improve the wearability of material, oxidation resistance and thermal conductivity, and the red hard of cermet can be improved
Property and thermal shock resistance, so as to improve the interrupted cut performance of ceramic tool.
The Adding Way of metal carbides determines the distribution of metallic element.The scattered of Equations of The Second Kind metal carbides adds
Plus, each element in cermet is disperseed uneven, cause heavy metal segregation, so that the structure of bulk ceramics body is influenceed,
The purpose of solution strengthening is not reached.Experiment shows, is combined by the certain proportion of carbon, tungsten, molybdenum, tantalum, then by tungsten carbide/molybdenum/
Tantalate solid solution composite powder is added in metal ceramic powder, except the dispersion-strengthened of above-mentioned metal carbides, wetting, crystal grain refinement
Effect is outer, and the metallic element such as Mo, W, Ta will uniformly spread to TiC particles at a sintering temperature, and replaces the Ti in TiC lattices,
(Ti, W, Mo, Ta) C solid solution is formed on TiC particle surfaces, the contact between TiC particles will be reduced, prevent them from occurring poly-
Collection is grown up, and makes TiC based ceramic metal crystal grain thinner, organizes more uniform, the raising for cermet overall performance has significantly
Effect.Therefore the preparation research of tungsten carbide/molybdenum/tantalate solid solution composite powder is significant to improving cermet performance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of metal carbides solid solution, micro/nano level can be prepared
Uniform tungsten carbide/molybdenum/tantalate solid solution composite powder.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of metal carbides solid solution, it is with tungsten, molybdenum and tantalum carburet and solid solution formation (W, Mo, Ta) C is solid
Molten composite powder；Tungsten in the solid solution composite powder, molybdenum, the atomic molar ratio of tantalum and carbon are 3~5:2~3:1.5~2:6.5~
10；The average grain diameter of the solid solution composite powder is 80~300nm.
The preparation method of above-mentioned metal carbides solid solution, comprises the following steps：
(1) dispensing：Tungsten powder, molybdenum powder, tantalum powder and graphite powder are weighed, and it is that cerium race is dilute to add rare earth Re, the rare earth Re
The oxide of at least one of soil；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter be 20~
100μm.Rare earth Re weight accounts for the 4%~6% of raw material gross weight, 20 μm of rare earth Re average grain diameter ＜.
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball together with tungsten-carbide ball
Grinding jar carries out high-energy ball milling；Ratio of grinding media to material is 6~10:1, ball milling speed is 200~300 turns/min, and Ball-milling Time is 24~48h.
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas
Under atmosphere, hot combination reaction is carried out under the conditions of 800~900 DEG C, micro-nano tungsten carbide/molybdenum/tantalate solid solution composite powder is obtained.Heat
The combination reaction time is 60~120min.Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained micro-nano tungsten carbide/
Molybdenum/tantalate solid solution composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
Most preferably, a kind of preparation method of metal carbides solid solution, comprises the following steps：
(1) dispensing：Tungsten powder 850g, molybdenum powder 420g, tantalum powder 420g and graphite powder 150g are weighed, and adds 75g cerium oxide
Powder；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter is 20~100 μm；Ceria oxide powder it is flat
Equal 20 μm of particle diameter ＜；
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball together with tungsten-carbide ball
Grinding jar carries out high-energy ball milling, and ratio of grinding media to material is 10:1, ball milling speed is 300 turns/min, and Ball-milling Time is 36h, obtains (Mo, Ta) C
Solid solution powder and W+C+ (W, Mo, Ta) C mixed-powders；
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas
Under atmosphere, hot combination reaction 60min, the carbonization for obtain average grain diameter 100nm or so, being evenly distributed are carried out under the conditions of 800 DEG C
Tungsten/molybdenum/tantalate solid solution composite powder；Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained tungsten carbide/molybdenum/tantalate solid solution
Composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
The beneficial effects of the present invention are：
The present invention is by tungsten powder, molybdenum powder, tantalum powder, graphite powder and rare earth Re high-energy ball milling solid phase reaction together, in high energy
In the presence of the mechanical force of ball milling, metal Mo and Ta will react with graphite (C), generate (Mo, Ta) C solid solution, simultaneously few
(Mo, Ta) C compounds formation (W, Mo, Ta) C solid solution is entered in part W atom solid solutions；Then in conjunction with hot combination reaction, tungsten powder and
Graphite powder will complete reaction generation WC, and (Mo, Ta) C enters solid solution in WC, completely generation (W, Mo, Ta) C solid solution composite powders.
Tungsten carbide/molybdenum/tantalate solid solution composite powder that the present invention is prepared is micro/nano level and is evenly distributed.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is the XRD spectrum for tungsten carbide/molybdenum/tantalate solid solution composite powder that embodiment 1 is obtained.
Embodiment
The preferred embodiments of the present invention are described in detail below.
Embodiment 1
(1) dispensing：Tungsten powder 850g, molybdenum powder 420g, tantalum powder 420g and graphite powder 150g are weighed, and adds 75g cerium oxide
Powder；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter is 20~100 μm；Ceria oxide powder it is flat
Equal 20 μm of particle diameter ＜；
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball together with tungsten-carbide ball
Grinding jar carries out high-energy ball milling, and ratio of grinding media to material is 10:1, ball milling speed is 300 turns/min, and Ball-milling Time is 36h, obtains (Mo, Ta) C
Solid solution powder and W+C+ (W, Mo, Ta) C mixed-powders；
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas
Under atmosphere, hot combination reaction 60min, the carbonization for obtain average grain diameter 100nm or so, being evenly distributed are carried out under the conditions of 800 DEG C
Tungsten/molybdenum/tantalate solid solution composite powder；Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained tungsten carbide/molybdenum/tantalate solid solution
Composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
Fig. 1 is the XRD spectrum for tungsten carbide/molybdenum/tantalate solid solution composite powder that embodiment 1 is obtained, and Fig. 1 shows, embodiment 1
Tungsten carbide/molybdenum/tantalate solid solution the composite powder arrived is (W, Mo, Ta) C solid solution that tungsten, molybdenum and tantalum carburet and solid solution are formed.
Embodiment 2
(1) dispensing：Tungsten powder 1050g, molybdenum powder 410g, tantalum powder 510g and graphite powder 130g are weighed, and adds 90g cerium oxide
Powder；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter is 20~100 μm；Ceria oxide powder it is flat
Equal 20 μm of particle diameter ＜；
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball together with tungsten-carbide ball
Grinding jar carries out high-energy ball milling, and ratio of grinding media to material is 6:1, ball milling speed is 200 turns/min, and Ball-milling Time is 24h, obtains (Mo, Ta) C solid
Solution powder and W+C+ (W, Mo, Ta) C mixed-powders；
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas
Under atmosphere, hot combination reaction 120min, the carbonization for obtain average grain diameter 300nm or so, being evenly distributed are carried out under the conditions of 900 DEG C
Tungsten/molybdenum/tantalate solid solution composite powder；Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained tungsten carbide/molybdenum/tantalate solid solution
Composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
Embodiment 3
(1) dispensing：Tungsten powder 1150g, molybdenum powder 360g, tantalum powder 450g and graphite powder 140g are weighed, and adds 90g cerium oxide
Powder；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter is 20~100 μm；Ceria oxide powder it is flat
Equal 20 μm of particle diameter ＜；
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball together with tungsten-carbide ball
Grinding jar carries out high-energy ball milling, and ratio of grinding media to material is 9:1, ball milling speed is 300 turns/min, and Ball-milling Time is 36h, obtains (Mo, Ta) C solid
Solution powder and W+C+ (W, Mo, Ta) C mixed-powders；
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas
Under atmosphere, hot combination reaction 90min, the carbonization for obtain average grain diameter 200nm or so, being evenly distributed are carried out under the conditions of 850 DEG C
Tungsten/molybdenum/tantalate solid solution composite powder；Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained tungsten carbide/molybdenum/tantalate solid solution
Composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (1)
1. a kind of preparation method of metal carbides solid solution, it is characterised in that：Comprise the following steps：
(1) dispensing：About tungsten powder 850g, molybdenum powder 420g, tantalum powder 420g and graphite powder 150g are weighed, and adds 75g cerium oxide powders
End；Tungsten powder, molybdenum powder, the purity of tantalum powder and graphite powder>99.9%, average grain diameter is 20~100 μm；Ceria oxide powder is averaged
20 μm of particle diameter ＜；
(2) high-energy ball milling solid phase reaction：The raw material that step (1) is matched somebody with somebody is loaded into stainless-steel vacuum ball grinder together with tungsten-carbide ball
High-energy ball milling is carried out, ratio of grinding media to material is 10:1, ball milling speed is 300 turns/min, and Ball-milling Time is 36h, obtains (Mo, Ta) C solid solutions
Body powder and W+C+ (W, Mo, Ta) C mixed-powders；
(3) hot combination reaction：The reaction product that step (2) is obtained is put into high-temperature atmosphere furnace, in nitrogen hydrogen mixeding gas atmosphere
Under, hot combination reaction 60min or so, the carbonization for obtain average grain diameter 100nm or so, being evenly distributed are carried out under the conditions of 800 DEG C
Tungsten/molybdenum/tantalate solid solution composite powder；Hydrogen is closed after the completion of reaction, under nitrogen protection by obtained tungsten carbide/molybdenum/tantalate solid solution
Composite powder is cooled to after room temperature, is vacuum-packed under nitrogen protection.
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| CN201610061685.XA CN105483488B (en) | 2016-01-29 | 2016-01-29 | Micro-nano tungsten/molybdenum/tantalum carbide solid-solution composite powder and preparation method thereof |
| CN201710409843.0A CN107164680B (en) | 2016-01-29 | 2016-01-29 | A kind of preparation method of metal carbides solid solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758666A (en) * | 2017-10-16 | 2018-03-06 | 四川理工学院 | A kind of (Ti, M) C nano solid-solution powder and preparation method thereof |
| CN110029261A (en) * | 2019-05-10 | 2019-07-19 | 重庆文理学院 | A kind of preparation method of Micro-Nano Hardmetal cutter material |
| EP4119524A4 (en) * | 2020-03-12 | 2023-10-25 | Institute Of Chemistry, Chinese Academy Of Sciences | Carbide-based high-entropy ceramic, rare-earth-containing carbide-based high-entropy ceramic and fibers and precursor thereof, and preparation method therefor |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107177767A (en) * | 2017-06-12 | 2017-09-19 | 成都众鑫达超硬工具材料科技有限公司 | A kind of TiC ceramic tools material and preparation method thereof |
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| CN101090786A (en) * | 2004-12-27 | 2007-12-19 | 优米科尔公司 | Composite powder products for hard metals |
| CN101838766A (en) * | 2010-06-22 | 2010-09-22 | 华中科技大学 | Metal ceramic cutter with gradient structure and preparation method thereof |
| CN102834210A (en) * | 2010-04-08 | 2012-12-19 | 株式会社图格莱 | Composite body |
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| US5746803A (en) * | 1996-06-04 | 1998-05-05 | The Dow Chemical Company | Metallic-carbide group VIII metal powder and preparation methods thereof |
| 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 |
| CN105177568B (en) * | 2015-10-13 | 2018-04-06 | 四川科力特硬质合金股份有限公司 | Hot melt knot other carbide solid solution alloy coatings of tungsten carbide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101090786A (en) * | 2004-12-27 | 2007-12-19 | 优米科尔公司 | Composite powder products for hard metals |
| CN102834210A (en) * | 2010-04-08 | 2012-12-19 | 株式会社图格莱 | Composite body |
| CN101838766A (en) * | 2010-06-22 | 2010-09-22 | 华中科技大学 | Metal ceramic cutter with gradient structure and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758666A (en) * | 2017-10-16 | 2018-03-06 | 四川理工学院 | A kind of (Ti, M) C nano solid-solution powder and preparation method thereof |
| CN107758666B (en) * | 2017-10-16 | 2020-06-23 | 四川理工学院 | (Ti, M) C nano solid solution powder and preparation method thereof |
| CN110029261A (en) * | 2019-05-10 | 2019-07-19 | 重庆文理学院 | A kind of preparation method of Micro-Nano Hardmetal cutter material |
| CN110029261B (en) * | 2019-05-10 | 2020-07-14 | 重庆文理学院 | Preparation method of micro-nano hard alloy cutter material |
| EP4119524A4 (en) * | 2020-03-12 | 2023-10-25 | Institute Of Chemistry, Chinese Academy Of Sciences | Carbide-based high-entropy ceramic, rare-earth-containing carbide-based high-entropy ceramic and fibers and precursor thereof, and preparation method therefor |
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| CN105483488A (en) | 2016-04-13 |
| CN107164680B (en) | 2018-07-13 |
| CN105483488B (en) | 2017-05-17 |
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