CN102925728B - Preparation method of binderless nanometer tungsten carbide cemented carbide - Google Patents
Preparation method of binderless nanometer tungsten carbide cemented carbide Download PDFInfo
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- CN102925728B CN102925728B CN201110231828.4A CN201110231828A CN102925728B CN 102925728 B CN102925728 B CN 102925728B CN 201110231828 A CN201110231828 A CN 201110231828A CN 102925728 B CN102925728 B CN 102925728B
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- preparation
- tungsten carbide
- binder phase
- sintering
- hard alloy
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 9
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 9
- 239000006229 carbon black Substances 0.000 claims abstract description 8
- -1 tungsten nitride Chemical class 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims description 30
- 239000011230 binding agent Substances 0.000 claims description 30
- 229910045601 alloy Inorganic materials 0.000 claims description 29
- 239000012298 atmosphere Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 238000002490 spark plasma sintering Methods 0.000 abstract 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 238000009413 insulation Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a preparation method of a binderless nanometer tungsten carbide cemented carbide. The method comprises the following steps: carrying out ball milling mixing of tungsten nitride and carbon black to prepare a W2N/C powder mixture; and sintering the prepared W2N/C powder mixture in a spark plasma sintering (SPS) furnace: heating to 700-1000DEG C according to a rate of 10-500DEG C/min, maintaining the temperature for 1-20min, pressurizing to 10-200MPa, heating to 1200-1800DEG C, and maintaining the temperature for 1-20min. The preparation method which adopts a reaction SPS technique enables the sintering temperature to be substantially reduced and the raw material cost and the energy consumption to be reduced; the prepared binderless nanometer tungsten carbide cemented carbide has the advantages of fine crystal grains, high density and good mechanical performances; and the preparation method has the advantages of simplicity, practicality, strong controllability, and easy realization of the large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method without Binder Phase nano tungsten carbide hard alloy, specifically, relate to a kind of reaction discharge plasma sintering technology preparation based on nitride conversion method without the method for Binder Phase nano tungsten carbide hard alloy, belong to Hardmetal materials preparing technical field.
Background technology
Tungsten carbide base carbide alloy has the advantages that hardness is high, bending strength is high and fracture toughness property is good, at aspects such as modern tool material, high-abrasive material, high temperature resistant and corrosion resistant materials, has application very widely.The most representative is that it can replace rapid steel to a great extent, thereby has caused the technological revolution of metal-processing industry, is described as " tooth of industry ".In Wimet system, adding of metallic binding phase (as cobalt, nickel) can increase the toughness of alloy and intensity, but inevitably makes its hardness and erosion resistance reduce.Under some specific use occasion, as the nozzle that high-pressure water cutting is used, the reduction of hardness has limited its application.Therefore,, for putting forward heavy alloyed hardness and wear resistance, often, by reducing the content of metallic binding phase in component, even do not add Binder Phase and realize.At present, about the research without Binder Phase carboloy, be day by day subject to domestic and international attention.
Raising is that the grain-size of material is decreased to even nanoscale of submicron without the effective way of Binder Phase carboloy performance, and its gordian technique is the preparation of superfine powder and the sintering of material.The Production Flow Chart of tradition Wimet is generally: ammonium paratungstate (APT) obtains the oxide compound of tungsten through calcining, through reduction and carbonization, obtain WC again, need afterwards to experience the steps such as batching, ball milling, compacting, dewaxing, high temperature sintering, can find out not only long flow path of this technique, and energy consumption is large, repetitious high-temperature process causes the crystal particle scale of material wayward.Ultra-fine or the nano hard alloy material of at present both at home and abroad development is still continued to use above-mentioned traditional technique, although obtained larger progress at ultra-fine or nano powder of tungsten carbide aspect preparing, but because above-mentioned technique sintering temperature is high, the time is long, cause nano powder of tungsten carbide crystal grain in sintering process sharply to be grown up, even if interpolation grain growth inhibitor, can not avoid grain growth completely.
Summary of the invention
The problems referred to above and the deficiency that for prior art, exist; the object of this invention is to provide a kind of preparation technology simple, practical; can be handling strong; easily accomplish scale production; sintering temperature is low; material grains is tiny, the preparation method without Binder Phase nano tungsten carbide hard alloy of good mechanical performance.
For achieving the above object, the technical solution used in the present invention is as follows:
A preparation method without Binder Phase nano tungsten carbide hard alloy, comprises the steps:
A) tungsten nitride and carbon black are carried out to ball milling and mix, preparation W
2n/C mixed powder;
B) W step a) being made
2n/C mixed powder is placed in discharge plasma sintering stove and carries out sintering: first the speed with 10～500 ℃/min is warmed up to 700～1000 ℃, be incubated and after 1～20 minute, be forced into again 10～200MPa and be warming up to 1200～1800 ℃, be incubated 1～20 minute, obtain without Binder Phase nano tungsten carbide hard alloy.
The mol ratio of the tungsten nitride of step in a) and carbon black is preferably 1: 2～and 1: 3.
The ball milling solvent of step in a) is preferably ethanol.
The ball-milling medium of step in a) is preferably tungsten-carbide ball.
The Ball-milling Time of step in a) is preferably 6～48 hours.
Step b) sintering atmosphere in is preferably vacuum or inert atmosphere.
Step b) temperature rise rate in is preferably 50～200 ℃/min.
Step b) sintering pressure in is preferably 50～200MPa.
Compared with prior art, tool of the present invention has the following advantages:
1) adopt reaction SPS sintering technology, greatly reduce sintering temperature, reduced raw materials cost and energy consumption.
2) prepared material grains is tiny, and density is high, and has good mechanical property.
3) preparation technology simple, practical, can be handling strong, easily accomplish scale production.
Accompanying drawing explanation
Fig. 1 is the figure of the SEM without Binder Phase nano tungsten carbide hard alloy polished surface that embodiment 1 makes.
Specific implementation method
Below in conjunction with embodiment, the present invention is described in further detail and completely, but do not limit content of the present invention.
Embodiment 1
Take 10mol tungsten nitride and 25mol carbon black, take ethanol as solvent, tungsten-carbide ball are ball-milling medium, mix 24 hours on roll-type ball mill, rotary evaporation, is placed in baking oven inner drying, sieves, and obtains W
2n/C mixed powder;
By the W after sieving
2n/C mixed powder is placed in discharge plasma sintering stove and carries out sintering: under vacuum condition, first the temperature rise rate with 100 ℃/min rises to 800 ℃, is incubated and again pressure is increased to 90MPa after 5 minutes, and be warming up to 1250 ℃, after insulation 3min, obtain without Binder Phase nano tungsten carbide hard alloy.
Fig. 1 is the figure of the SEM without Binder Phase nano tungsten carbide hard alloy polished surface that the present embodiment makes, as seen from Figure 1: the grain-size without Binder Phase nano tungsten carbide hard alloy making is tiny, and median size is 270nm, and density is higher than 98%.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only: taking 10mol tungsten nitride and 20mol carbon black is raw material, and secondary temperature elevation to 1450 ℃ is also incubated 5 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 410nm, and density is higher than 98%.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only: taking 10mol tungsten nitride and 30mol carbon black is raw material, and secondary temperature elevation to 1250 ℃ is also incubated 3 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 220nm, and density is higher than 98%.
Embodiment 4
The difference of the present embodiment and embodiment 1 is only: Ball-milling Time is 6 hours, secondary temperature elevation to 1500 ℃ insulation 5 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 450nm, and density is higher than 98%.
Embodiment 5
The difference of the present embodiment and embodiment 1 is only: Ball-milling Time is 48 hours, and secondary temperature elevation to 1250 ℃ is also incubated 5 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 250nm, and density is higher than 98%.
Embodiment 6
The difference of the present embodiment and embodiment 1 is only: sintering atmosphere is nitrogen atmosphere, is once warming up to 900 ℃ and be incubated 10 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 300nm, and density is higher than 98%.
Embodiment 7
The difference of the present embodiment and embodiment 1 is only: sintering atmosphere is argon gas atmosphere, is once warming up to 900 ℃ and be incubated 15 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 320nm, and density is higher than 98%.
Embodiment 8
The difference of the present embodiment and embodiment 1 is only: be once warming up to 1000 ℃ of insulations 1 minute.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 320nm, and density is higher than 98%.
Embodiment 9
The difference of the present embodiment and embodiment 1 is only: be once warming up to 700 ℃ and be incubated 20 minutes.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 220nm, and density is higher than 98%.
Embodiment 10
The difference of the present embodiment and embodiment 1 is only: a temperature rise rate is 10 ℃/min; Secondary temperature elevation to 1500 ℃ insulation 10min.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 460nm, and density is higher than 98%.
Embodiment 11
The difference of the present embodiment and embodiment 1 is only: a temperature rise rate is 500 ℃/min; Secondary temperature elevation to 1200 ℃ insulation 10min.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 210nm, and density is higher than 98%.
Embodiment 12
The difference of the present embodiment and embodiment 1 is only: during secondary temperature elevation, institute's applied pressure is 10MPa, secondary temperature elevation to 1800 ℃ insulation 1min.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 670nm, and density is higher than 98%.
Embodiment 13
The difference of the present embodiment and embodiment 1 is only: during secondary temperature elevation, institute's applied pressure is 200MPa, secondary temperature elevation to 1200 ℃ insulation 20min.
All the other contents are all with described in embodiment 1.
Analyze and learn after testing: the grain-size without Binder Phase nano tungsten carbide hard alloy that the present embodiment makes is tiny, and median size is 200nm, and density is higher than 98%.
In sum, utilize prepared by the inventive method without Binder Phase nano tungsten carbide hard alloy, to have sintering temperature low, consuming time short; Prepared material grains is tiny, and density is high, good mechanical performance.
Claims (3)
1. without a preparation method for Binder Phase nano tungsten carbide hard alloy, it is characterized in that, comprise the steps:
A) tungsten nitride and carbon black are carried out to ball milling and mix, preparation W
2n/C mixed powder; The mol ratio of tungsten nitride and carbon black is 1:2～1:3; Ball milling solvent is ethanol, and ball-milling medium is tungsten-carbide ball, and Ball-milling Time is 6～48 hours;
B) W step a) being made
2n/C mixed powder is placed in discharge plasma sintering stove and carries out sintering: first the speed with 10～500 ℃/min is warmed up to 700～1000 ℃, be incubated and after 1～20 minute, be forced into again 10～200MPa and be warming up to 1200～1800 ℃, be incubated 1～20 minute, obtain without Binder Phase nano tungsten carbide hard alloy.
2. the preparation method without Binder Phase nano tungsten carbide hard alloy according to claim 1, is characterized in that: the sintering atmosphere step b) is vacuum or inert atmosphere.
3. the preparation method without Binder Phase nano tungsten carbide hard alloy according to claim 1, is characterized in that: the temperature rise rate step b) is 50～200 ℃/min.
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| CN102925728B true CN102925728B (en) | 2014-11-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088044A (en) * | 2015-09-30 | 2015-11-25 | 株洲水箭硬质合金有限责任公司 | Preparation method of nanometer unbonded phase ultra-hard cemented carbide product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459353B (en) * | 2017-07-04 | 2020-06-09 | 江苏大学 | Method for enhancing performance of WC-based hard alloy without binding phase by VC and TiC |
| CN114315358B (en) * | 2021-12-27 | 2023-01-24 | 海南大学 | Fully-compact binderless tungsten carbide ceramic and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609053A (en) * | 2004-11-11 | 2005-04-27 | 上海交通大学 | Sintering process of superfine pure WC without adhering phase |
| CN101020971A (en) * | 2007-04-06 | 2007-08-22 | 北京科技大学 | Process of making superfine crystal hard alloy without adhesive |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609053A (en) * | 2004-11-11 | 2005-04-27 | 上海交通大学 | Sintering process of superfine pure WC without adhering phase |
| CN101020971A (en) * | 2007-04-06 | 2007-08-22 | 北京科技大学 | Process of making superfine crystal hard alloy without adhesive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088044A (en) * | 2015-09-30 | 2015-11-25 | 株洲水箭硬质合金有限责任公司 | Preparation method of nanometer unbonded phase ultra-hard cemented carbide product |
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Effective date of registration: 20161230 Address after: 215499 Changchun South Road, Jiangsu, Suzhou, No. 238, No. Patentee after: SUZHOU Research Institute SHANGHAI INSTITUTE OF CERAMICS CHINESE ACADEMY OF SCIENCES Address before: 200050 Dingxi Road, Shanghai, Changning District, No. 1295 Patentee before: SHANGHAI INSTITUTE OF CERAMICS, CHINESE ACADEMY OF SCIENCES |
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Address after: 215400 No.6 Liangfu Road, Taicang City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Institute of advanced inorganic materials Address before: No. 238 Changchun South Road, Taicang City, Suzhou City, Jiangsu Province, 215499 Patentee before: SUZHOU Research Institute SHANGHAI INSTITUTE OF CERAMICS CHINESE ACADEMY OF SCIENCES |