CN100348482C - Production method of needle-shaped tungsten carbide powder - Google Patents
Production method of needle-shaped tungsten carbide powder Download PDFInfo
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- CN100348482C CN100348482C CNB200410040330XA CN200410040330A CN100348482C CN 100348482 C CN100348482 C CN 100348482C CN B200410040330X A CNB200410040330X A CN B200410040330XA CN 200410040330 A CN200410040330 A CN 200410040330A CN 100348482 C CN100348482 C CN 100348482C
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- 239000000843 powder Substances 0.000 title claims abstract description 69
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 238000010000 carbonizing Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 10
- 239000000956 alloy Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract 2
- 238000005299 abrasion Methods 0.000 abstract 1
- 230000006978 adaptation Effects 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 12
- 238000005245 sintering Methods 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 229910009043 WC-Co Inorganic materials 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
The present invention belongs to a production method of needle-shaped tungsten carbide powder for hard alloy production. The production method comprises the steps: raw material mixture, reducing treatment, carbon and cobalt mixture, primary carbonizing treatment, carbon and cobalt mixture for the second time, secondary carbonizing treatment and ball milling operation, and thus, crystal needle-shaped WC powder is obtained. In the production method, because WO3 is used as raw material, Ni and Na or K are used as catalysts for reducing treatment, and reduced W powder is carbonized through two steps under the condition of adding the catalysts, WC crystal grains grow in a needle shape. The production method has the advantages of advanced production process, high stability and reliability, high needle-shaped degree of WC powder metallographic structure, wide adaptation range of producing hard alloy and obvious effect on fiber reinforcement of alloy. Compared with hard alloy products prepared from the conventional WC powder under the corresponding condition, the hard alloy product prepared by the production method has the characteristics of high strength and hardness, high toughness and abrasion resistance, excellent integrative mechanical property, etc. The production method overcomes the defects of WC crystal grains which are equiaxial triangular prisms or polygon prisms through a one-step carbonization method, and alloy product defects caused by the WC crystal grains.
Description
Technical field
The invention belongs to the production method of a kind of CEMENTED CARBIDE PRODUCTION with raw material powder, particularly a kind of crystal grain is the production method of acicular wolfram varbide (WC) powder.The WC powder that adopts this method to produce can be widely used in produces cutting tool, wear resistant tools and mine probing, exploitation with instrument etc.
Background technology
WC-Co base binary alloy not only has good anti-breaking tenacity, and has high rigidity, thereby is widely used as instruments such as cutting, wear-resisting and mine probing, exploitation.In the production of this type of alloy, determined the overall performance of alloy largely as the inner quality of the WC powder of main raw material.Conventional WC powder is used for producing WC-Co base binary alloy, its metallographic structure WC grain and axle triangular prism or multiedge cylinder such as is generally.Its production method is to adopt blue tungsten (WO
2.9) be main raw material, after handling, reduction forms through disposable carbonizing treatment again.Characteristics such as batching is simple though this method has, technical process is short; But owing to adopt a step carbonization, its carbonization speed is too fast, and the WC of generation more easily makes WC grain explosion in process of growth because of the density variation between itself and the W, thereby the WC grain pattern that generates under this condition can not form (growing into) needle-like or tabular.Thereby the Wimet that adopts this type of WC powder production in use WC grain is easily transferred to the wear resistance that has reduced alloy, and its hardness is relative with toughness relatively poor, has also shortened work-ing life.At this defective, the Masaki Kobayashi of Japan etc. disclose a kind of use " Co-W-C mixture ten carbon " powder mix in " development of pan enhanced Wimet " (" external refractory metal and mechanically resistant material " in December, 2000, the 16th volume 12 phase P41-45) or " W+ graphite+Co " powder mix is made raw material, in sintering process, form plate-like WC by chemical reaction, have higher hardness, toughness, intensity and cutting ability though this Wimet with WC of plate-like crystal morphology is compared with conventional Wimet.But it is to adopt the raw material powder mix of fixing (uniqueness) that this type of WC crystalline phase is organized as discous Wimet, in sintering process, form, thereby there is an one. the composition of alloy (composition) scope and product category are subjected to great restriction, as not adding compositions such as TiC, NC, otherwise the preferential growth that will stop WC grain crystal face in sintering process causes its crystal grain can not plate-likeization; Its two, poor stability forms owing to the plate-like WC grain makes its crystal face grow up unusually according to qualifications in sintering process, it is bigger that the ratio that the plate-like WC grain generates is influenced by sintering process and proportioning raw materials, defectives such as constant product quality difference.
Summary of the invention
The objective of the invention is the production method that a kind of WC grain pattern of research and development is acicular needle-shaped tungsten carbide powder on the basis of conventional WC powder production method, the length-to-diameter ratio of the crystal grain of the WC powder of being produced is generally more than 4: 1; To reach production technique advanced person, reliable, WC powder Functionality, quality and appealing design, stable performance, be convenient to suitability for industrialized production, and adopt that this powder production Wimet has that production technique is simple, reliable, applied range, constant product quality and have arch bridge and make fiber reinforcement effect such as crackle kinking, hardness, toughness, intensity height, purpose such as wear resistance is good.
Solution of the present invention is to adopt WO
3(yellow tungsten) is for raw material and add the catalyst reduction processing, step (level) carbonization with background technology simultaneously changes two step (level) carbonization techniques into, the mixed carbon comtent of the carbonization first time is reduced to the 60-78% of theoretical carbon amount, avoid crystal grain explosion in process of growth to reduce carburizing reagent speed; Carbonizing treatment makes residual tungsten nuclear and W more for the second time
2C is transformed into WC and impels its grain growing to become needle-like; Thereby realize its purpose.Therefore, method of the present invention comprises:
A, batching: with WO
3Raw material powder and catalyzer are sent in the mixing tank and are mixed; Catalyzer and add-on thereof are with WO
3Weight is counted the Ni of 30-300ppm and Na or the K of 150-650ppm;
B, reduction are handled: pack into the mixed powder that is made in the graphite boat and send in the reduction furnace, at H
2Reduction was handled 5-8 hour under protection and the 980-1270 ℃ of temperature, and the 40-100 mesh sieve is crossed in gained W powder cooling back, to remove impurity;
C, join carbon and catalyst cobalt: above-mentioned gained W powder is sent in the ball mill together with C powder (being roughly equal to the 60-78% that whole W generate the required theoretical carbon amount of WC) and the Co powder of 150-650ppm of its weight 3.7-4.7%, is mixed, the W+C+Co mixed powder;
D, carbonizing treatment: above-mentioned mixed powder packed into send in the carbon tube furnace behind the graphite boat, under 1750-2150 ℃ of temperature carbonizing treatment 8-10 hour, cooling back ball milling became the powder of 40-100 mesh sieve, must contain W nuclear, W
2The tungsten carbide powder of C.
E, secondary are joined carbon and cobalt: will send in the ball mill through the powder of above-mentioned carbonizing treatment, and supply the C amount by the 93.0-101.1% of the theoretical carbon content of total WC, and add the Co powder of 150-350ppm, ball milling mixes;
F, secondary carbonization and ball-milling processing: will prepare pack into graphite boat and sending in the carbon tube furnace of gained mixed powder by E, under 1650-2050 ℃ of temperature carbonizing treatment 5-10 hour; Gained WC piece is crossed the 40-200 sieve behind ball milling, promptly getting crystal morphology is acicular WC powder.
In order to help mixing, in the batching before reduction is handled, catalyst n i that is added and Na or K all add with the aqueous solution of its soluble salt, and the solution amount that is added is by the heavy WO of every kg
3Powder adds preparation of mixed aqueous solution amount and the adding of Ni and Na or the K of 100-150ml, and is fashionable when adding with the aqueous solution, again with the compound oven dry, stand-by after mixing.And the soluble salt of described Ni and Na or K, wherein the soluble salt of Ni is Ni (NO
3)
2, the soluble salt of Na, K is respectively NaCl, KCl.And described reduction furnace is the molybdenum filament electric reduction furnace.
The present invention is owing to change conventional one step of WC powder process for carbonization production two step carbonizations into and add different catalyzer in reduction processing and carbonizing treatment process, both avoided causing crystal grain explosion fragmentation, promoted effectively again that WC grain grew into needle-like because of carbonization speed is too fast.The WC powder that adopts production method of the present invention to produce is used to produce hart metal product, regardless of its prescription, all can not change WC intrinsic crystalline-granular texture in sintering process, its product has fiber reinforcement effects such as the crackle of making kinking, arch bridge effect, and in use WC grain also is difficult for being transferred to.Thereby, the present invention has production technique advanced person, reliable and stable, WC flour gold phase structure spiculation degree height, the fiber reinforcement effect that is used to produce Wimet wide accommodation, product is obvious, the hart metal product of being produced with conventional WC powder has intensity, hardness height more again under corresponding situation, characteristics such as toughness and wear resistance are good, and comprehensive mechanical performance is better.
Accompanying drawing and description of drawings
Fig. 1 is embodiment 1, WC powder (500 times) metallograph;
Fig. 2 is embodiment 2, WC powder (500 times) metallograph;
White is WC grain among the figure, and black part is divided into the copper base.
Embodiment 1
A, batching: with 10kgFSSS (Fisher particle size) 18.8 μ m, concentration class is 18.43 WO
3Raw material powder places the double cone mixing tank, with 1.56gNi (NO
3)
2And 6.36gNaCl be dissolved in altogether be made into the aqueous solution in the 1.5L water after, under agitation condition, spray in the mixing tank, send into drying in oven to bulky powder after mixing, stand-by.
B, reduction are handled: above-mentioned powder is packed into send in the molybdenum filament electric reduction furnace, at H in the graphite boat
2Reduction was handled 6.5 hours under protection and the 1100 ℃ of temperature, and 80 mesh sieves are crossed to remove impurity in the cooling back.
C, join carbon and catalyst cobalt: the W powder 7kg of back gained is handled in the reduction of learning from else's experience, and adds in the ball mill together with the carbon black powders and the 1.75gCo powder of 267.3 grams, and ball milling mixes, the W+C+Co mixed powder.
D, carbonizing treatment: above-mentioned mixed powder is sent in the carbon tube furnace, and carbonizing treatment is 9 hours under 1950 ℃ of temperature; Ball milling became the powder of 80 mesh sieves behind the furnace cooling, must contain W nuclear, W
2The tungsten carbide powder of C.
E, secondary are joined carbon and cobalt: the powder 7kg of the above-mentioned carbonizing treatment of learning from else's experience sends in the ball mill and adds 182g carbon black powder and 2.19Co powder, and ball milling mixes.
F, secondary carbonization and ball-milling processing: above-mentioned preparation gained mixed powder is reinstalled graphite boat and send in the carbon tube furnace, carbonizing treatment is 8 hours under 1800 ℃ of temperature; Treat the cooling of WC piece after ball milling is crossed 100 mesh sieves, promptly getting crystal morphology is acicular WC powder product.Accompanying drawing 1, be 500 times of metallographs of present embodiment product.
Implement 2
Present embodiment batching and reduction are handled and adopted FSSS (Fisher particle size) is 20.2 μ m, and concentration class is 46.47 WO
310kg is a raw material, adds catalyst n i (NO
3)
26.22g and the mixed aqueous solution 1.5L of NaCl 12.72g, mix and be dried into loose mixed powder after, send in the reduction furnace at H in the boat of packing into
2Reduction was handled 7 hours under protection and the 1150 ℃ of temperature, after the removal of impurities of sieving the W powder.
Join carbon, add catalyst cobalt and carbonizing treatment: get above-mentioned tungsten powder 7kg, carbon black powder 322g, Co powder 3.15g goes in the ball mill altogether, ball milling mixes back dress boat, and carbonizing treatment is 9 hours under 2000 ℃ of temperature, and cooling back ball milling sieves, and must contain W nuclear and W
2The tungsten carbide powder of C.
Secondary is joined carbon, cobalt and carbonizing treatment: get above-mentioned powder 7kg through the carbonizing treatment gained first time, carbon black powder 159kg, Co powder 2.5g, ball milling mixes back dress boat, goes in the carbon tube furnace, and carbonizing treatment is 7.5 hours under 1850 ℃ of temperature, gets the WC piece.
All the other technologies are all same with embodiment 1.Fig. 2 is 500 times of metallographs of present embodiment gained WC powder product.
Claims (4)
1, a kind of production method of needle-shaped tungsten carbide powder, this method comprises:
A, batching: with WO
3Raw material powder and catalyzer are sent in the mixing tank, mix; Catalyzer and add-on thereof are with WO
3Weight is counted the Ni of 30-300ppm and Na or the K of 150-650ppm;
B, reduction are handled: pack into the mixed powder that is made in the graphite boat and send in the reduction furnace, at H
2Reduction was handled 5-8 hour under protection and the 980-1270 ℃ of temperature, and the 40-100 mesh sieve is crossed in gained W powder cooling back, to remove impurity;
C, join carbon and catalyst cobalt: above-mentioned gained W powder is sent in the ball mill together with the C powder of its weight 3.7-4.7% and the Co powder of 150-650ppm, is mixed, the W+C+Co mixed powder;
D, carbonizing treatment: above-mentioned mixed powder is packed into behind the graphite boat, send in the carbon tube furnace, under 1750-2150 ℃ of temperature carbonizing treatment 8-10 hour, cooling back ball milling became the powder of 40-100 mesh sieve, must contain W nuclear, W
2The tungsten carbide powder of C;
E, secondary are joined carbon and cobalt: will send in the ball mill through the powder of above-mentioned carbonizing treatment, and supply C and add the Co powder of 150-350ppm by the 93.0-101.1% of the theoretical carbon content of total WC, ball milling mixes;
F, secondary carbonization and ball-milling processing: will prepare pack into graphite boat and sending in the carbon tube furnace of gained mixed powder by E, under 1650-2050 ℃ of temperature carbonizing treatment 5-10 hour; Gained WC piece is crossed the 40-200 mesh sieve behind ball milling, promptly getting crystal morphology is acicular WC powder.
2, by the described production method of claim 1, the catalyst n i of adding and Na or K all add with the aqueous solution of its soluble salt, and the solution amount that is added is by the heavy WO of every kg
3Powder adds preparation of mixed aqueous solution amount and the adding of Ni and Na or the K of 100-150ml; Fashionable when adding with the above-mentioned aqueous solution,, stand-by after mixing again with the mixed powder oven dry.
3, by the described production method of claim 2, the soluble salt of described Ni and Na or K, wherein the soluble salt of Ni is Ni (NO
3)
2, the soluble salt of Na, K then is respectively NaCl, KCl.
4, by the described production method of claim 1, its reduction furnace is the molybdenum filament electric reduction furnace.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331810C (en) * | 2005-11-03 | 2007-08-15 | 武汉化工学院 | Preparation method of nano-carbon tube-nano tungston carbide composite powder |
| CN101298328B (en) * | 2008-01-02 | 2011-12-21 | 长沙伟徽高科技新材料股份有限公司 | Preparation process of metallic carbide fine powder |
| CN102069002B (en) * | 2010-12-31 | 2012-05-30 | 浙江工业大学 | Preparation method of wolfram carbide-carbon (WC-C) composite material with large specific surface area |
| CN103183347A (en) * | 2011-12-29 | 2013-07-03 | 北京有色金属研究总院 | Preparation method of crude tungsten carbide powder |
| CN102583381B (en) * | 2012-03-21 | 2013-08-28 | 浏阳市鑫利粉末冶金有限公司 | Method for preparing tungsten carbide by using regeneration tungsten powder |
| CN103922341B (en) * | 2014-05-06 | 2016-03-23 | 重庆市科学技术研究院 | The preparation method of nanometer WC whisker |
| CN106270536A (en) * | 2016-08-23 | 2017-01-04 | 沈阳思忆纳米材料有限公司 | A kind of Diamondization tungsten powder and the preparation method of block |
| CN107089662B (en) * | 2017-06-16 | 2019-05-31 | 重庆大学 | A kind of method that CH4 reduction and carbonization WO3 prepares WC powder |
| CN107973299B (en) * | 2017-11-30 | 2020-06-12 | 株洲三鑫硬质合金生产有限公司 | Production system and production process of high-temperature-base WC powder |
| CN107867691B (en) * | 2017-11-30 | 2020-07-31 | 株洲三鑫硬质合金生产有限公司 | Preparation method and application of high-quality coarse grain WC powder |
| CN107867690B (en) * | 2017-11-30 | 2019-09-24 | 株洲三鑫硬质合金生产有限公司 | A kind of high temperature base WC powder and its preparation method and application |
| CN109264722A (en) * | 2018-10-17 | 2019-01-25 | 东北大学 | A method of superfine tungsten carbide powder is prepared using tungsten powder and nickel powder as raw material |
| CN110240163B (en) * | 2019-07-30 | 2022-09-06 | 株洲硬质合金集团有限公司 | Method for preparing fine-grain WC powder by using medium-coarse-grain tungsten powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5882620A (en) * | 1995-06-07 | 1999-03-16 | International Carbitech Industries, Inc. | Pyrometallurgical process for forming tungsten carbide |
| CN1424252A (en) * | 2003-01-03 | 2003-06-18 | 浙江大学 | Preparation of tungsten carbide powder |
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2004
- 2004-07-30 CN CNB200410040330XA patent/CN100348482C/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5882620A (en) * | 1995-06-07 | 1999-03-16 | International Carbitech Industries, Inc. | Pyrometallurgical process for forming tungsten carbide |
| CN1424252A (en) * | 2003-01-03 | 2003-06-18 | 浙江大学 | Preparation of tungsten carbide powder |
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