CN101397615A - Method for preparing cemented carbides with nearly equiaxed WC crystal particle - Google Patents
Method for preparing cemented carbides with nearly equiaxed WC crystal particle Download PDFInfo
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- CN101397615A CN101397615A CNA2008100464532A CN200810046453A CN101397615A CN 101397615 A CN101397615 A CN 101397615A CN A2008100464532 A CNA2008100464532 A CN A2008100464532A CN 200810046453 A CN200810046453 A CN 200810046453A CN 101397615 A CN101397615 A CN 101397615A
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Abstract
The invention discloses a preparation method of a hard alloy with approximately isometric WC crystal grains, which is characterized by comprising the following steps: firstly, the mixing powder of WC and Co is subjected to wet grinding, drying and pressing in absolute ethyl alcohol, and then subjected to vacuum sintering at the temperature of 1400 DEG C to 1440 DEG C; when the sintering is finished, nitrogen is introduced to a furnace simultaneously for carrying out vacuum quenching, the pressure of the nitrogen is 0.1MPa to 0.4MPa, and the quenching time is 5min to 10min; then tapping is carried out for deep cooling treatment in liquid nitrogen, the treatment temperature is 150 DEG C to 196 DEG C, and the heat-preservation time is: the hard alloy weight multiplied by weight factor plus the Co percent content of the hard alloy multiplied by component factor, wherein, the weight factor is 5min/g to 25min/g and the component factor is 10min to 20min; and drawing temper is carried out in a vacuum furnace at the temperature of 120 DEG C to 200 DEG C, the temperature-preservation time is 1h to 3h. By adopting the method for preparing the WC group hard alloy, the dissolving and precipitation processes of the WC can be controlled, the triangular prism shape thereof is changed, the approximately isometric WC crystal grains are obtained, the stress concentration and dissevering effect to the substrate caused by the WC crystal grains are reduced, and the surface stress condition of the alloy after treatment is compressive stress, therefore, the toughness and the shock resistance capability of the hard alloy are improved.
Description
Technical field
The present invention is a kind of Wimet preparation method, particularly has the preparation method of nearly equiaxed WC grain hard alloy.
Background technology
With WC, TiC, TaC etc. is main hard phase, serves as main bonding phase with Co, Ni, Fe etc., and the Wimet by powder metallurgy liquid phase sintering is prepared into owing to have high rigidity, high-wearing feature, mainly is used as cutting tool, wear part etc.Prepare in the Wimet process in liquid phase sintering, the WC solid phase has limited solubleness in liquid phase, and according to minimum free enthalpy principle, the protrusion corner angle of tiny WC grain and thick WC particle part is preferentially dissolved in liquid phase.And dissolved WC separates out on coarse particles WC surface, thereby WC particle is grown up.And WC is a hexagonal, be tesseral system not, thereby the dissolving in the liquid phase sintering process and separate out and have directivity, thereby make the WC grain in the Wimet present angular (rhizoma sparganic column), the existence of corner angle causes stress distribution extremely inhomogeneous, cause stress concentration, be unfavorable for the toughness of Wimet.
Improve toughness at present and mainly contain three kinds of methods, promptly adopt ultrafine WC crystal grain or increase wc grain size or raising bonding phase content, but effect is still undesirable.And these methods have higher requirement to raw material, have perhaps changed the composition of design, have perhaps increased cost.Preparation method of the present invention, the non-axle property that waits by the control WC grain changes its rhizoma sparganic column pattern, obtains nearly equiaxial WC grain.The effect of isolating that the stress concentration that WC grain causes reaches matrix reduces, so the toughness of Wimet is improved.
Summary of the invention
The toughness that the present invention is directed to present Wimet has much room for improvement, and present method has certain circumscribed present situation, invented the preparation method that a kind of vacuum air-quenching and sub-zero treatment combine, obtained to have nearly equiaxed WC grain hard alloy, its toughness is improved.
Preparation method with nearly equiaxed WC grain hard alloy of the present invention is characterized in that will carrying out vacuum sintering after the wet-milling of raw material mixed powder process, drying, the compacting earlier; Feed nitrogen when sintering is finished in the stove and carry out vacuum hardening; Come out of the stove then and in liquid nitrogen, carry out sub-zero treatment, and in vacuum oven, carry out temper;
Preparation method with nearly equiaxed WC grain hard alloy of the present invention, it is further characterized in that:
(1) wet-milling of raw material powder mix is carried out in the roller milling machine, and rotational speed of ball-mill is 50～80r/min, and milling time is 48～56h, and mill ball is the WC-8wt%Co sintered carbide ball of diameter of phi 10mm, and ratio of grinding media to material (wt%) is 5:1; Wet grinding media is a dehydrated alcohol, and adds the forming agent polyoxyethylene glycol of 1.0～2.0wt%, and the dehydrated alcohol dosage is 250～300ml/Kg; Powder behind the filtration drying is at the forming under the pressure of 300～400MPa; Sintering carries out in vacuum oven, takes off forming agent and is higher than under 10～15Pa in vacuum tightness and carries out, and is incubated 2～4h between 400 ℃～600 ℃; Sintering vacuum tightness is higher than 1～5 * 10
-2Carry out under the Pa, sintering temperature is 1400 ℃～1440 ℃, and soaking time is 1～1.5h.
(2) nitrogen pressure is 0.1～0.4MPa during vacuum hardening, and the cool time is 5～10 minutes;
(3) during sub-zero treatment, be cooled to 150-196 ℃ with the speed of 20～60 ℃/min; Soaking time is: the bonding phase percentage composition * composition coefficient of the weight * weight coefficient of Wimet+Wimet, and the wherein wt coefficient is 5～25min/g, the composition coefficient is 10～20min; Speed with 20～60 ℃/min after insulation finishes is raised to room temperature; The temperature that vacuum tempering is handled is 120～200 ℃, and soaking time is 1～3h, and vacuum tightness is 2～5 * 10
-2Pa.
The invention has the advantages that:
The employing vacuum nitrogen quenches, and cooling is controlled the dissolving precipitation process of WC grain fast, and WC grain can too not grown up; Sub-zero treatment can make the solubleness of WC in binding agent improve, and improve the strengthening effect of WC, and the alloy surface stressed condition is a stress after handling, and the alloy impact resistance is improved.
Description of drawings
The microtexture pattern (1500X) of the WC base cemented carbide of example 1 among Fig. 1 the present invention
The microtexture pattern (1500X) of the WC base cemented carbide of example 2 among Fig. 2 the present invention
Embodiment
Example 1: composition is that the powder mix of WC-6wt%Co carries out wet-milling in the roller milling machine, and rotational speed of ball-mill is 50～80r/min, and milling time is 48～56h, and mill ball is the WC-8wt%Co sintered carbide ball of diameter of phi 10mm, and ratio of grinding media to material (wt%) is 5:1; Wet grinding media is a dehydrated alcohol, and adds the forming agent polyoxyethylene glycol of 1.0～2.0wt%, and the dehydrated alcohol dosage is 250～300ml/Kg; Powder behind the filtration drying becomes VBMT160408-V under the pressure of 300～400MPa, its weight is 9.5g; Sintering carries out in vacuum oven, takes off forming agent and is higher than under 10～15Pa in vacuum tightness and carries out, and is incubated 2-4h between 400 ℃～600 ℃; Sintering vacuum tightness is higher than 1～5 * 10
-2Carry out under the Pa, sintering temperature is 1400 ℃～1440 ℃, and soaking time is 1～1.5h.Nitrogen pressure is 0.1～0.4MPa during vacuum hardening, and the cool time is 5～10 minutes; During sub-zero treatment, be cooled to 150～196 ℃ with the speed of 20～60 ℃/min; Soaking time is 120～150min; Speed with 20-60 ℃/min after insulation finishes is raised to room temperature; The temperature that vacuum tempering is handled is 120～200 ℃, and soaking time is 1～3h, and vacuum tightness is 2～5 * 10
-2Pa.Its hardness is 91.81HRA, and microtexture is seen Fig. 1.
Example 2: composition is that the powder mix of WC-8wt%Co carries out wet-milling in the roller milling machine, and rotational speed of ball-mill is 50～80r/min, and milling time is 48～56h, and mill ball is the WC-8wt%Co sintered carbide ball of diameter of phi 10mm, and ratio of grinding media to material (wt%) is 5:1; Wet grinding media is a dehydrated alcohol, and adds the forming agent polyoxyethylene glycol of 1.0～2.0wt%, and the dehydrated alcohol dosage is 250～300ml/Kg; Powder behind the filtration drying becomes VBMT160404-V under the pressure of 300～400MPa, its weight is 9.3g; Sintering carries out in vacuum oven, takes off forming agent and is higher than under 10～15Pa in vacuum tightness and carries out, and is incubated 2-4h between 400 ℃～600 ℃; Sintering vacuum tightness is higher than 1～5 * 10
-2Carry out under the Pa, sintering temperature is 1400 ℃～1440 ℃, and soaking time is 1～1.5h.Nitrogen pressure is 0.1～0.4MPa during vacuum hardening, and the cool time is 5～10 minutes; During sub-zero treatment, be cooled to 150～196 ℃ with the speed of 20～60 ℃/min; Soaking time is 100～140min; Speed with 20-60 ℃/min after insulation finishes is raised to room temperature; The temperature that vacuum tempering is handled is 120～200 ℃, and soaking time is 1～3h, and vacuum tightness is 2～5 * 10
-2Pa.Its hardness is 91.0HRA, and microtexture is seen Fig. 2.
Claims (2)
1. the preparation method with nearly equiaxed WC grain hard alloy is characterized in that will carrying out vacuum sintering after the wet-milling of raw material mixed powder process, drying, the compacting earlier; Feed nitrogen when sintering is finished in the stove and carry out vacuum hardening; Come out of the stove then and in liquid nitrogen, carry out sub-zero treatment, and in vacuum oven, carry out temper.
2. the preparation method with nearly equiaxed WC grain hard alloy according to claim 1, it is further characterized in that:
(1) wet-milling of raw material powder mix is carried out in the roller milling machine, and rotational speed of ball-mill is 50～80r/min, and milling time is 48～56h, and mill ball is the WC-8wt%Co sintered carbide ball of diameter of phi 10mm, and ratio of grinding media to material (wt%) is 5:1; Wet grinding media is a dehydrated alcohol, and adds the forming agent polyoxyethylene glycol of 1.0～2.0wt%, and the dehydrated alcohol dosage is 250～300ml/Kg; Powder behind the filtration drying is at the forming under the pressure of 300～400MPa; Sintering carries out in vacuum oven, takes off forming agent and is higher than under 10～15Pa in vacuum tightness and carries out, and is incubated 2～4h between 400 ℃～600 ℃; Sintering vacuum tightness is higher than 1～5 * 10
-2Carry out under the Pa, sintering temperature is 1400 ℃～1440 ℃, and soaking time is 1～1.5h;
(2) nitrogen pressure is 0.1～0.4MPa during vacuum hardening, and the cool time is 5～10 minutes;
(3) during sub-zero treatment, be cooled to 150-196 ℃ with the speed of 20～60 ℃/min; Soaking time is: the bonding phase percentage composition * composition coefficient of the weight * weight coefficient of Wimet+Wimet, and the wherein wt coefficient is 5～25min/g, the composition coefficient is 10～20min; Speed with 20～60 ℃/min after insulation finishes is raised to room temperature; The temperature that vacuum tempering is handled is 120～200 ℃, and soaking time is 1～3h, and vacuum tightness is 2～5 * 10
-2Pa.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019424A (en) * | 2010-10-14 | 2011-04-20 | 浙江恒成硬质合金有限公司 | Method for manufacturing hard alloy numerical control blade |
| CN106834618A (en) * | 2016-12-06 | 2017-06-13 | 太原科技大学 | A kind of cryogenic treating process for improving coal mining cutting pick mechanical property |
| CN107475548A (en) * | 2017-06-28 | 2017-12-15 | 沈阳寰博磁电科技有限公司 | A kind of preparation method of nanometer of toughness reinforcing Ultra-fine Grained WC Co hard alloy |
| CN110102769A (en) * | 2019-05-14 | 2019-08-09 | 株洲特利亚硬质合金有限公司 | A kind of wet milling process conducive to high bonding phase cemented carbide uniform texture |
| CN111394556A (en) * | 2020-04-19 | 2020-07-10 | 苏州思传电子测量技术有限公司 | Heat treatment process of strain type force sensor stainless steel elastomer |
| CN114031392A (en) * | 2021-12-15 | 2022-02-11 | 烁光特晶科技有限公司 | Method for sintering magnesia-alumina spinel transparent ceramic in inert atmosphere |
-
2008
- 2008-11-04 CN CN2008100464532A patent/CN101397615B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019424A (en) * | 2010-10-14 | 2011-04-20 | 浙江恒成硬质合金有限公司 | Method for manufacturing hard alloy numerical control blade |
| CN106834618A (en) * | 2016-12-06 | 2017-06-13 | 太原科技大学 | A kind of cryogenic treating process for improving coal mining cutting pick mechanical property |
| CN107475548A (en) * | 2017-06-28 | 2017-12-15 | 沈阳寰博磁电科技有限公司 | A kind of preparation method of nanometer of toughness reinforcing Ultra-fine Grained WC Co hard alloy |
| CN110102769A (en) * | 2019-05-14 | 2019-08-09 | 株洲特利亚硬质合金有限公司 | A kind of wet milling process conducive to high bonding phase cemented carbide uniform texture |
| CN111394556A (en) * | 2020-04-19 | 2020-07-10 | 苏州思传电子测量技术有限公司 | Heat treatment process of strain type force sensor stainless steel elastomer |
| CN114031392A (en) * | 2021-12-15 | 2022-02-11 | 烁光特晶科技有限公司 | Method for sintering magnesia-alumina spinel transparent ceramic in inert atmosphere |
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