CN102534277A - New preparation method for coarse particles and super coarse particle hard alloy - Google Patents
New preparation method for coarse particles and super coarse particle hard alloy Download PDFInfo
- Publication number
- CN102534277A CN102534277A CN2010105883510A CN201010588351A CN102534277A CN 102534277 A CN102534277 A CN 102534277A CN 2010105883510 A CN2010105883510 A CN 2010105883510A CN 201010588351 A CN201010588351 A CN 201010588351A CN 102534277 A CN102534277 A CN 102534277A
- Authority
- CN
- China
- Prior art keywords
- coarse particles
- powder
- wimet
- sintering
- hard phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a new preparation method for coarse particles and a super coarse particle hard alloy. The method comprises the following steps: (1) crushing the hard phase raw material, and carrying out particle size grading to obtain the hard phase powder with the desired average particle size and the desired particle size distribution; (2) placing the pre-treated hard phase powder in a physical vapor deposition powder film plating machine to plate a binding phase on the surface of the hard phase powder to obtain a mixing material with a bonding phase content of 3-20%; (3) introducing argon to the obtained mixing material to carry out passivation, screening, adding 1-8 wt% of a forming agent, drying, and screening; (4) adopting a method of mold pressing, isostatic pressing, injection forming or extrusion forming to obtain the required shape; (5) carrying out a dewaxing treatment on the formed product, removing the forming agent in the product, and sintering for 1-2 hours at a temperature of 1300-1450 DEG C. The hard alloy prepared by using the method of the present invention has characteristics of uniform binding phase distribution, low adjacency degree of the hard phase, coarse particles, and no impurity contamination.
Description
Technical field
The present invention relates to a kind of novel preparation method of wimet, the novel preparation method of particularly a kind of coarse particles and ultra coarse particles wimet.
Background technology
Wimet has purposes widely with its high firmness and HS.According to current international practice standard, grain fineness number is that 2.5～6.0 μ m are the coarse particles wimet, and grain fineness number is an extra-coarse grained carbide alloy greater than 6.0 μ m.A series of premium propertiess such as coarse particles and ultra coarse particles wimet have under the high temperature that hardness is high, wear-resisting, intensity and good toughness, creep strain are little, heat-resisting, corrosion-resistant are widely used in mine instrument, petroleum drilling and mining instrument, coal winning machine cutting bit instrument, Tunnel Engineering and spray etc. with shield machine cutter, press tool, stiff dough are surperficial.
The technology of traditional preparation process wimet is with raw material powder wet-milling, drying, moulding, sintering.Mix mutually with hard in order to bond, the ball milling time is generally several hrs to time of several days.In mechanical milling process, be difficult to keep the grain fineness number of coarse particles hard phase, the long ball milling time can be reduced the crystal grain skewness of alloy behind grain fineness number and the sintering of hard phase, therefore is difficult to prepare the ultra coarse particles wimet of mean grain size >=6 μ m.Adopt the method for chemistry to prepare compound for shortcoming U.S. Pat 5505902, US5529804 and the English Patent 346473 that overcomes ball-milling technology discloses, adopt conventional compacting, sintering process to prepare wimet again at wolfram varbide (WC) powder surface cobalt plating.Patent US5505902 adopts sol-gel method, and patent US5529804 adopts the polyvalent alcohol method, and English Patent 346473 adopts electric plating method.Because these chemical processes all will adopt chemical agent, and complex process, give in the compound easily in the cobalt coating procedure and bring impurity into, also pollute environmental pollution easily.。
Summary of the invention
To the deficiency of prior art, the present invention provides the novel preparation method of a kind of coarse particles and ultra coarse particles wimet.It is low to utilize this method can prepare the adjacent degree of hard, and particle is thick, the hart metal product of H.T..
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The novel preparation method of a kind of coarse particles and ultra coarse particles wimet may further comprise the steps:
(1) pre-treatment of hard phase raw material: behind hard phase raw material crushing, carry out size classification, obtain the hard phase powder of required mean particle size and size-grade distribution;
(2) physical vapor deposition powder plated film: will put into physical vapor deposition powder coating equipment through pretreated hard phase powder, and, obtain bonding phase weight percentage at 3%～20% compound in hard phase powder surface plating bonding phase;
(3) mix forming agent: sieve after in the compound that obtains, feeding the argon gas passivation, mix 1～8wt% forming agent then, sieve after the drying;
(4) moulding: adopt mold pressing, etc. the method for static pressure, injection molding or extrusion molding obtain needed shape.
(5) dewaxing and sintering: the product after the moulding is carried out dewaxing treatment, deviate from forming agent wherein, carry out sintering then, sintering temperature is 1300～1450 ℃, sintering time 1～2 hour.
The Fsss granularity of coarse particles and ultra coarse grained hard phase raw material all more than 10 μ m, generally all is made up of hard agglomeration mostly.When the preparation wimet, at first hard phase raw material is carried out pre-treatment, the pre-treatment of hard phase raw material can be adopted the hard agglomeration in the broken hard phase of modes such as rolling ball milling, stirring ball-milling or the airflow milling raw material; Adopt method cyclone classified or that sieve to carry out size classification then, remove tiny and thick especially particle, obtain the hard phase powder of required mean particle size and size-grade distribution.
Hard of the present invention is the sosoloid of a kind of or two or more formation among WC, TiC, TaC and the NbC mutually.
Said bonding be the sosoloid of any one or two or more formation among Co, Ni and the Fe mutually.
Said physical vapor deposition powder plated film is vacuum-evaporation powder plated film, vacuum sputtering powder plated film or vacuum ionic powder plated film, is preferably magnetron sputtering plating.The target that adopts is sosoloid target or Single Phase Metal target in the magnetron sputtering membrane process.
Forming agent described in the step (3) is paraffin, rubber or PEG.
Dewaxing treatment described in the step (5) can be hydrogen dewaxing, vacuum dewaxing or negative pressure carrier gas dewaxing.
Be sintered to hydrogen sintering, vacuum sintering, low pressure sintering or HIP sintering described in the step (5).
The invention has the advantages that:
Adopt the wimet of method preparation of the present invention, bonding is evenly distributed mutually, the adjacent degree of hard phase is low, and particle is thick.Under identical cobalt contents and identical hard phase particle sizes, the toughness of alloy is high.Adopt the compound of magnetron sputtering membrane prepare totally not have contaminating impurity, the alloy voidage that is prepared into through sintering is low, and the bending strength of alloy is high.Prepared wimet is particularly suitable for mine instrument, petroleum drilling and mining instrument, coal winning machine cutting bit instrument, Tunnel Engineering with shield machine cutter, heavy type cutting tools etc.
Embodiment
Below through embodiment the present invention is described further.
Embodiment 1:
With the Fsss granularity is 15 μ m, and carbon content is 6.17% WC powder, and ball milling was separated reunion in 8 hours in rotary mill, and ball-to-powder weight ratio is 3: 1, crosses 200 eye mesh screens then, removes thicker WC particle.Put into the magnetron sputtering coater cobalt plating then and prepare the WC/Co compound, make the quality of powder increase by 11% through cobalt plating, promptly the cobalt contents of alloy is about 10%.After the logical argon gas passivation of powder with cobalt plating, took out 100 mesh sieves, mixed the spirituous solution that concentration is the PEG of 60g/L then, mixed the spirituous solution of 30mlPEG in every 100gWC/Co compound, behind the mixing, in vacuum drying oven, removed alcohol through 80 ℃ of dryings.80 mesh sieves are crossed in dry back, then with powder extrusion molding under 200MPa.Product is put into dewaxing furnace carry out the negative pressure carrier gas and sloughed PEG and 600 ℃ of pre-burnings 1 hour, waiting static pressure stove sintering then, sintering temperature is 1430 ℃, and sintering time is 1 hour.The mean grain size of WC is 9.5 μ m in the ultra coarse-grain WC-10Co wimet of preparation, and bending strength is 3300MPa, HV
30Hardness is 850, and fracture toughness property is 25MNm
-3/2
Embodiment 2:
With the Fsss granularity is 15 μ m, and carbon content is 6.17% WC powder, and ball milling was separated reunion in 8 hours in rotary mill, and ball-to-powder weight ratio is 4: 1, crosses 200 eye mesh screens then, removes thicker WC particle.Put into magnetron sputtering coater cosputtering cobalt plating then, nickel prepares the 90WC5Co5Ni compound, makes the quality of powder increase by 11%, promptly the bonding phase content of alloy is about 10wt%.After the logical argon gas passivation of composite powder of having plated bonding phase metal, took out 100 mesh sieves, mix paraffin gasoline solution then, behind the mixing, in vacuum drying oven, remove gasoline through 80 ℃ of dryings.80 mesh sieves are crossed in dry back, then with powder in the inferior static pressure compression moulding of 200MPa.Product is put into dewaxing and sintering integrated stove carry out vacuum sintering, sintering temperature is 1420 ℃, and sintering time is 1 hour.The mean grain size of WC is 9.5 μ m in the ultra coarse-grain 90WC5Co5Ni wimet of preparation, and bending strength is 2000MPa, HV
30Hardness is 870, and fracture toughness property is 20MNm
-3/2
Embodiment 3:
With the 113.2KgFsss granularity is 3 μ m, and carbon content is (W, Ti) the C solid-solution powder that 6.15% WC powder and 16.2KgFsss granularity are 3 μ m; Ball milling was separated reunion in 8 hours in rotary mill; Ball-to-powder weight ratio is 3: 1, crosses 200 eye mesh screens then, removes thicker particle.Put into the magnetron sputtering coater cobalt plating then and prepare YT14 alloy compound, make the quality of powder increase by 8.7% through cobalt plating, promptly the bonding phase content of alloy is about 8wt%.After the logical argon gas passivation of the powder that has plated cobalt, took out 100 mesh sieves, mix gasoline rubber solution then, behind the mixing, in vacuum drying oven, remove gasoline through 80 ℃ of dryings.80 mesh sieves are crossed in dry back, then with powder compression molding under 200MPa.Product is put into the low pressure sintering stove slough rubber, sintering, sintering temperature is 1420 ℃, and sintering time is 1 hour, and argon pressure is 6MPa.The mean grain size of WC is 2.5 μ m in the coarse-grain YT14 alloy of preparation, and bending strength is 2900MPa, and HRA hardness is 90.
Embodiment 4:
With the 132.6KgFsss granularity is 3.5 μ m; Carbon content is TiC-WC-TaC (NbC) solid-solution powder that 6.15% WC powder and 32.8KgFsss granularity are 4 μ m, and ball milling was separated reunion in 8 hours in rotary mill, and ball-to-powder weight ratio is 3: 1; Cross 200 eye mesh screens then, remove thicker particle.Put into the magnetron sputtering coater cobalt plating then and prepare YW alloy compound, make the quality of powder increase by 8.7% through cobalt plating, promptly the bonding phase content of alloy is 8wt%.After the logical argon gas passivation of the powder that has plated cobalt, took out 100 mesh sieves, mix the spirituous solution that concentration is the PEG of 60g/L then, mix the spirituous solution of 30mlPEG in every 100gYW alloy compound, behind the mixing, in vacuum drying oven, remove alcohol through 80 ℃ of dryings.80 mesh sieves are crossed in dry back, then powder are shaped in the 100MPa injected.Product is put into dewaxing and sintering integrated stove carry out vacuum sintering, sintering temperature is 1430 ℃, and sintering time is 1 hour.The mean grain size of WC is 2.7 μ m in the coarse-grain YW2 alloy of the preparation of preparation, and bending strength is 2100MPa, and hardness HRA is 89.
Claims (10)
1. the novel preparation method of a coarse particles and ultra coarse particles wimet is characterized in that, may further comprise the steps:
(1) pre-treatment of hard phase raw material: behind hard phase raw material crushing, carry out size classification, obtain the hard phase powder of required mean particle size and size-grade distribution;
(2) physical vapor deposition powder plated film: will put into physical vapor deposition powder coating equipment through pretreated hard phase powder, and, obtain bonding phase weight percentage at 3%～20% compound in hard phase powder surface plating bonding phase;
(3) mix forming agent: sieve after in the compound that obtains, feeding the argon gas passivation, mix 1～8wt% forming agent then, sieve after the drying;
(4) moulding: adopt the method for compression molding, isostatic pressing, injection molding or extrusion molding to obtain needed shape.
(5) dewaxing and sintering: the product after the moulding is carried out dewaxing treatment, deviate from forming agent wherein, carry out sintering then, sintering temperature is 1300～1450 ℃, sintering time 1～2 hour.
2. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that described hard is the sosoloid of a kind of or two or more formation among WC, TiC, TaC and the NbC mutually.
3. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that, said bonding be the sosoloid of any one or two or more formation among Co, Ni and the Fe mutually.
4. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that, adopts the broken hard phase of the mode raw material of rolling ball milling, stirring ball-milling or airflow milling in the said step (1); Adopt method cyclone classified or that sieve to carry out size classification.
5. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that said physical vapor deposition powder plated film is vacuum-evaporation powder plated film, vacuum sputtering powder plated film or vacuum ionic powder plated film.
6. the novel preparation method of coarse particles according to claim 5 and ultra coarse particles wimet is characterized in that said physical vapor deposition powder plated film is a magnetron sputtering plating.
7. the novel preparation method of coarse particles according to claim 6 and ultra coarse particles wimet is characterized in that, the target that said magnetron sputtering plating adopts is sosoloid target or Single Phase Metal target.
8. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that the forming agent described in the step (3) is paraffin, rubber or PEG.
9. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that, the dewaxing treatment described in the step (5) is hydrogen dewaxing, vacuum dewaxing or negative pressure carrier gas dewaxing.
10. the novel preparation method of coarse particles according to claim 1 and ultra coarse particles wimet is characterized in that, is sintered to hydrogen sintering, vacuum sintering, low pressure sintering or HIP sintering described in the step (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010588351.0A CN102534277B (en) | 2010-12-07 | 2010-12-07 | New preparation method for coarse particles and super coarse particle hard alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010588351.0A CN102534277B (en) | 2010-12-07 | 2010-12-07 | New preparation method for coarse particles and super coarse particle hard alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102534277A true CN102534277A (en) | 2012-07-04 |
| CN102534277B CN102534277B (en) | 2014-01-08 |
Family
ID=46342296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010588351.0A Active CN102534277B (en) | 2010-12-07 | 2010-12-07 | New preparation method for coarse particles and super coarse particle hard alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102534277B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102990303A (en) * | 2012-12-03 | 2013-03-27 | 浙江东钨实业有限公司 | Manufacturing method of hard alloy special-shaped product |
| CN104357696A (en) * | 2014-12-01 | 2015-02-18 | 技锋精密刀具（马鞍山）有限公司 | Sintering process of products obtained by hard alloy paraffin production process |
| CN105274415A (en) * | 2015-10-10 | 2016-01-27 | 西安交通大学 | Manufacturing method for porous titanium carbide ceramics |
| CN105950935A (en) * | 2016-05-05 | 2016-09-21 | 苏州新锐合金工具股份有限公司 | Hard alloy mold material for fastener formed through cold upsetting and preparation method of hard alloy mold material |
| CN106031949A (en) * | 2015-09-02 | 2016-10-19 | 洛阳新巨能高热技术有限公司 | Preparation method of complex-shaped cemented carbide products |
| CN107385255A (en) * | 2017-07-13 | 2017-11-24 | 四川大学 | The preparation method of solid solution based ceramic metal blade material and obtained blade material |
| CN111154993A (en) * | 2019-12-25 | 2020-05-15 | 株洲鸿达实业有限公司 | Preparation method of tungsten carbide-titanium carbide solid solution |
| WO2021189798A1 (en) * | 2020-03-23 | 2021-09-30 | 陕西斯瑞新材料股份有限公司 | Method for preparing cuw90 material by using spherical tungsten powder |
| JP7392423B2 (en) | 2019-11-26 | 2023-12-06 | 住友電気工業株式会社 | Cemented carbide and cutting tools containing it as a base material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313150A (en) * | 1997-05-13 | 2001-09-19 | 理查德.埃德蒙多.托特 | Hard powder for toughness material coating |
| CN101648213A (en) * | 2009-08-31 | 2010-02-17 | 株洲硬质合金集团有限公司 | Hard alloy roll collar for finished frame of high-speed wire mill and preparation method thereof |
-
2010
- 2010-12-07 CN CN201010588351.0A patent/CN102534277B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313150A (en) * | 1997-05-13 | 2001-09-19 | 理查德.埃德蒙多.托特 | Hard powder for toughness material coating |
| CN101648213A (en) * | 2009-08-31 | 2010-02-17 | 株洲硬质合金集团有限公司 | Hard alloy roll collar for finished frame of high-speed wire mill and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102990303A (en) * | 2012-12-03 | 2013-03-27 | 浙江东钨实业有限公司 | Manufacturing method of hard alloy special-shaped product |
| CN104357696A (en) * | 2014-12-01 | 2015-02-18 | 技锋精密刀具（马鞍山）有限公司 | Sintering process of products obtained by hard alloy paraffin production process |
| CN104357696B (en) * | 2014-12-01 | 2016-04-27 | 技锋精密刀具（马鞍山）有限公司 | A kind of sintering process of carbide paraffin production technique goods |
| CN106031949A (en) * | 2015-09-02 | 2016-10-19 | 洛阳新巨能高热技术有限公司 | Preparation method of complex-shaped cemented carbide products |
| CN105274415A (en) * | 2015-10-10 | 2016-01-27 | 西安交通大学 | Manufacturing method for porous titanium carbide ceramics |
| CN105274415B (en) * | 2015-10-10 | 2017-04-19 | 西安交通大学 | Manufacturing method for porous titanium carbide ceramics |
| CN105950935A (en) * | 2016-05-05 | 2016-09-21 | 苏州新锐合金工具股份有限公司 | Hard alloy mold material for fastener formed through cold upsetting and preparation method of hard alloy mold material |
| CN107385255A (en) * | 2017-07-13 | 2017-11-24 | 四川大学 | The preparation method of solid solution based ceramic metal blade material and obtained blade material |
| JP7392423B2 (en) | 2019-11-26 | 2023-12-06 | 住友電気工業株式会社 | Cemented carbide and cutting tools containing it as a base material |
| CN111154993A (en) * | 2019-12-25 | 2020-05-15 | 株洲鸿达实业有限公司 | Preparation method of tungsten carbide-titanium carbide solid solution |
| WO2021189798A1 (en) * | 2020-03-23 | 2021-09-30 | 陕西斯瑞新材料股份有限公司 | Method for preparing cuw90 material by using spherical tungsten powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102534277B (en) | 2014-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102534277B (en) | New preparation method for coarse particles and super coarse particle hard alloy | |
| CN109252081B (en) | High-entropy alloy binding phase superfine tungsten carbide hard alloy and preparation method thereof | |
| CN102990069B (en) | A kind of preparation method utilizing useless tungsten-cobalt alloy to make coarse-grain carbide alloy pick | |
| CN101664809B (en) | Uniform macromeritic tungsten powder and method for preparing tungsten carbide powder | |
| CN101985717B (en) | Method for preparing high-tenacity super-coarse-grained tungsten and cobalt hard alloy | |
| CN101967593A (en) | Ultrafine grain solid carbide material containing rare earth and preparation method thereof | |
| WO2015169132A1 (en) | Method for preparing wc-co powder used for thermal spraying | |
| CN102676902A (en) | Ultra-thick hard alloy, and preparation method and application thereof | |
| CN101301686A (en) | Fe/Ni-based carbide alloy coating cutter material for cutting rolled steel and preparation thereof | |
| CN102719720A (en) | Method for preparing (Ti, Mo, W(Ta, Nb)) (C, N) solid-solution powder | |
| CN103189155A (en) | Method for producing a sintered composite body | |
| CN103866172B (en) | A kind of super thick and stiff matter Alloy And Preparation Method of narrow particle size distribution | |
| CN102517467A (en) | Method for preparing coarse-grain hard alloy | |
| CN105296834B (en) | High-hardness and high-tenacity hard alloy and preparation method thereof | |
| CN114318040B (en) | Rare earth-added hard alloy and preparation method thereof | |
| CN107973299B (en) | Production system and production process of high-temperature-base WC powder | |
| CN107265458A (en) | Tungsten powder grading system for extra-coarse grained carbide alloy method | |
| CN106735244A (en) | A kind of oil field with WC Co hard alloy series tooth preparation method | |
| CN101255557B (en) | Synthetic reaction plasma cladding powder and preparation technique thereof | |
| CN1861295A (en) | Cobalt powder contg. rare-earth nano-crystal enhancement phase and its prepn. method | |
| CN102162058B (en) | Hard alloy taking nickel-aluminum intermetallic compound Ni3Al as binding phase and preparation method thereof | |
| KR100700197B1 (en) | Process for Manufacturing Sintered Materials Containing Cobalt Component | |
| JP7157887B1 (en) | Grinding, stirring, mixing, kneading machine parts | |
| CN110358961B (en) | Preparation method of WC-Co hard alloy with average grain size larger than 15 mu m | |
| CN112359241B (en) | Bicrystal heterogeneous hard alloy and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190626 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |