CN102628138A - Trace cobalt-containing tungsten carbide without bonding phase and preparation method thereof - Google Patents
Trace cobalt-containing tungsten carbide without bonding phase and preparation method thereof Download PDFInfo
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- CN102628138A CN102628138A CN2012100829523A CN201210082952A CN102628138A CN 102628138 A CN102628138 A CN 102628138A CN 2012100829523 A CN2012100829523 A CN 2012100829523A CN 201210082952 A CN201210082952 A CN 201210082952A CN 102628138 A CN102628138 A CN 102628138A
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Abstract
The invention belongs to the field of powder metallurgy sintering, in particular refers to a trace cobalt-containing tungsten carbide without bonding phase and preparation method thereof. A hard alloy comprises components, by weight, as follows: 0.20-1.00% of Co, 0.01-0.50% of Cr3C2, 0.01-0.50% of VC and the balance of WC with grain size of 0.2-0.8 mum. The preparation method comprises the steps of: carrying out feeding and high energy ball milling according to the above raw material powder ratio, until WC powder in the ball milling powder has an average grain size refined to less than 200nm; then sintering the cemented carbide powder rapidly after the high energy ball milling by discharge plasma. The tungsten carbide base cemented carbide powder of the invention has reasonably designed components and a simple preparation method; the powder gives out heat uniformly and has fast heating and cooling speed, low sintering temperature and short sintering time to save the energy greatly; and the obtained ultrafine-grained WC cemented carbide has excellent integrated properties.
Description
Technical field
The invention belongs to powder metallurgy sintered shaping field, specifically be meant a kind of nothing bonding phase wolfram varbide (WC) wimet that contains trace cobalt (Co) and preparation method thereof.
Background technology
The tradition wimet is to be matrix with the insoluble metal hard compounds, serves as the bonding phase with metals such as cobalt, nickel, iron.Bonding is divided by and is had outside the function that promotes the full densification of alloy sintering, has also given alloy toughness and intensity, but has also made reductions such as its corrosion resistance nature, resistance to elevated temperatures, wear resisting property, thermal conductivity, thereby made its Application Areas receive certain limitation.No metal bonding phase cemented carbide; Be called for short no bonding phase cemented carbide; Belong to one type of special wimet, can be divided into two big series, one type for pure WC series with refractory carbide sosoloid serve as bonding series mutually; Another kind of " not having the bonding phase " WC wimet for mentioning in some document refers to metal bonding phase massfraction≤1%.Owing to have the higher hardness of more traditional wimet, wear resistance and erosion resistance; Through precise polished; Its surfaceness can reach≤15nm, and no bonding phase cemented carbide can be used as extraordinary sealing material, high-pressure medium nozzle material, sliding material, precision die material, high abrasion resisting material etc.
Not having bonding phase WC wimet is just becoming an important development direction of high-anti-friction hard alloy.Yet the fusing point of pure WC is up to 2860 ℃, and the sintering temperature of nothing bonding phase WC wimet for preparing full densification is very high, and growing up unusually of WC grain is taken place in sintering process easily.In the prior art; Preparation nothing bonding phase WC Study of Cemented Carbide mainly concentrates on preparation and does not add the pure WC wimet of any sticker and the pure WC wimet aspect that carbon is joined in preparation; There is following problem in the preparation process: 1, sintering temperature is too high; Sintering time is longer, and the sintering temperature of pure WC wimet for preparing full densification is more than 1800 ℃; 2, the alloy phenomenon that exists WC grain to grow up unusually of preparation can't be prepared the nothing bonding phase WC wimet of ultra-fine crystalline substance; 3, owing to do not contain any sticker, the alloy strength of preparation and fracture toughness property are very low.Up to now, Shang Weijian adopts the discharge plasma sintering preparation to add the report of the nothing bonding phase WC wimet of micro-Co.
Summary of the invention
The objective of the invention is to weak point, a kind of nothing bonding phase WC wimet that contains micro-Co with excellent comprehensive performance is provided to prior art.
Another object of the present invention also is to combine through reasonable component design and optimal preparation technology, and a kind of preparation method that can further improve the nothing bonding phase WC wimet that contains micro-Co that over-all properties, technology are easy, sintering temperature is low, sintering time is short of material is provided.
The object of the invention can be realized through following measure:
A kind of nothing bonding phase carboloy that contains trace cobalt, it is characterized in that: the component and the mass percentage content thereof of this alloy are following: Co:0.20-1.00%, Cr
3C
2: 0.01-0.50%, VC:0.01-0.50%, surplus is grain-size 0.2-0.8 μ m WC.
A kind of preparation method who contains the nothing bonding phase carboloy of trace cobalt, it is characterized in that: this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
Raw material wolfram varbide, cobalt, chromium carbide and vanadium carbide powder are carried out proportioning: Co:0.20-1.00%, Cr by following mass percent consumption
3C
2: 0.01-0.50%, VC:0.01-0.50%, surplus is grain-size 0.2-0.8 μ m WC;
Step 2: high-energy ball milling
Feed intake by above-mentioned raw materials powder quality per-cent consumption and to carry out high-energy ball milling, the WC powder average grain size is refined to less than 200nm in ball-milled powder;
Step 3: discharge plasma sintering ball-milled powder
With the discharge plasma sintering mould of packing into of the cemented carbide powder behind the high-energy ball milling, adopt the plasma discharging Fast Sintering, the sintering process condition is following:
Sintering pressure: 30～50MPa
Sintering heating rate: 100～200 ℃/min
Sintering temperature: 1500～1700 ℃
The sintered heat insulating time: 1～5min
Sintering vacuum tightness :≤6Pa
Obtain a kind of ultra-fine brilliant bonding phase carboloy that do not have tiny, that contain trace cobalt uniformly of organizing through Fast Sintering.
The present invention compared with prior art has the following advantages:
1, the composition of tungsten carbide base carbide alloy powder of the present invention is reasonable in design, owing to add micro-Co, greatly reduces sintering temperature again, has quickened the sintering densification process significantly, has shortened sintering time, and whole sintering process can be short to has only several minutes; And reduce the sintering temperature that the full densification of preparation does not have bonding phase WC wimet, thereby practiced thrift the energy greatly, in save energy, there is very important meaning the aspect of enhancing productivity.
2, need not compression moulding in the preparation process, do not add any sintering aid, simplified technical process.
3, in the sintering process of the present invention, there is liquid phase Co film between the part WC particle, strengthened intergranular strength of joint, improved the toughness of alloy, can obtain to have the nothing bonding phase WC wimet of the ultra-fine crystalline substance of excellent over-all properties.
4, powder of the present invention evenly generates heat, and heats up, cooling rate is fast, and sintering temperature is low, the time is short, can suppress grain growth, and the block grain-size behind the sintering is tiny even.
The practical implementation form
Through following embodiment the present invention is described further, but embodiment of the present invention is not limited only to this.
Embodiment 1
A kind of preparation method who contains the nothing bonding phase carboloy of trace cobalt, this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
With WC, Co, Cr
3C
2, the VC powder carries out proportioning by following mass percent consumption: grain-size is the WC:98.70% of 0.2 μ m; Co:0.50%, Cr
3C
2: 0.50%, VC:0.30%;
Step 2: high-energy ball milling
The powder stock of a said tungsten carbide base carbide alloy powder mixture ratio places planetary ball mill to carry out high-energy ball milling set by step; Ball grinder and abrading-ball material adopt the WC wimet; Ball-milling medium is an ethanol, and ball-to-powder weight ratio is 5: 1, and ball milling speed is 200r/min; And adopt high-purity Ar gas as protective atmosphere, ball milling after 40 hours the WC powder average grain size be refined to about 150nm;
Step 3: discharge plasma sintering ball-milled powder
Getting wimet ball-milled powder 30g behind the high-energy ball milling diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mold of φ 20mm; Wherein sintering pressure is 50MPa; Sintering temperature is 1500 ℃; The sintering heating rate is 200 ℃/min, and the sintered heat insulating time is 5min, and sintering vacuum tightness is 6Pa.Obtain a kind of ultra-fine brilliant nothing bonding phase carboloy block materials that contains trace cobalt tiny, even, the about 350nm of WC average grain size of organizing after the Fast Sintering, the specific density of this sample reaches 98.67%, and hardness is 2368HV
10, bending strength is 985MPa, fracture toughness property is 7.54MPam
1/2
Embodiment 2
A kind of preparation method who contains the nothing bonding phase carboloy of trace cobalt, this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
With WC, Co, Cr
3C
2, the VC powder carries out proportioning by following mass percent consumption: grain-size is the WC:98.69% of 0.2 μ m; Co:0.80%, Cr
3C
2: 0.01%, VC:0.50%;
Step 2: high-energy ball milling
The consumption of a said tungsten carbide base carbide alloy powder mixture ratio set by step; Place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and abrading-ball material adopt the WC wimet, and ball-milling medium is an ethanol; Ball-to-powder weight ratio is 5: 1; Ball milling speed is 200r/min, and adopts high-purity Ar gas as protective atmosphere, ball milling after 40 hours the WC powder average grain size be refined to about 150nm;
Step 3: discharge plasma sintering ball-milled powder
Get the wimet ball-milled powder 30g behind the high-energy ball milling; The diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mold of φ 20mm; Wherein sintering pressure is 50MPa, and sintering temperature is 1500 ℃, and the sintering heating rate is 200 ℃/min; The sintered heat insulating time is 5min, and sintering vacuum tightness is 5Pa.Obtain a kind of ultra-fine brilliant nothing bonding phase carboloy block materials that contains trace cobalt tiny, even, the about 380nm of WC average grain size of organizing after the Fast Sintering, the specific density of this sample reaches 99.41%, and hardness is 2546HV
10, bending strength is 1146MPa, fracture toughness property is 8.01MPam
1/2
Embodiment 3
A kind of preparation method who contains the nothing bonding phase carboloy of trace cobalt, this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
With WC, Co, Cr
3C
2, the VC powder carries out proportioning by following mass percent consumption: grain-size is the WC:99.00% of 0.4 μ m; Co:0.20%, Cr
3C
2: 0.50%, VC:0.30%;
Step 2: high-energy ball milling
The consumption of a said tungsten carbide base carbide alloy powder mixture ratio set by step; Place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and abrading-ball material adopt the WC wimet, and ball-milling medium is an ethanol; Ball-to-powder weight ratio is 5: 1; Ball milling speed is 200r/min, and adopts high-purity Ar gas as protective atmosphere, ball milling after 50 hours the WC powder average grain size be refined to about 170nm;
Step 3: discharge plasma sintering ball-milled powder
Get the wimet ball-milled powder 30g behind the high-energy ball milling; The diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mold of φ 20mm; Wherein sintering pressure is 40MPa, and sintering temperature is 1700 ℃, and the sintering heating rate is 150 ℃/min; The sintered heat insulating time is 1min, and sintering vacuum tightness is 4Pa.Obtain a kind of ultra-fine brilliant nothing bonding phase carboloy block materials that contains trace cobalt tiny, even, the about 410nm of WC average grain size of organizing after the Fast Sintering, the specific density of this sample reaches 99.53%, and hardness is 2605HV
10, bending strength is 1027MPa, fracture toughness property is 7.83MPam
1/2
Embodiment 4
A kind of preparation method who contains the nothing bonding phase carboloy of trace cobalt, this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
With WC, Co, Cr
3C
2, the VC powder carries out proportioning by following mass percent consumption: grain-size is the WC:98.69% of 0.8 μ m; Co:1.00%, Cr
3C
2: 0.30%, VC:0.01%;
Step 2: high-energy ball milling
The consumption of a said tungsten carbide base carbide alloy powder mixture ratio set by step; Place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and abrading-ball material adopt the WC wimet, and ball-milling medium is an ethanol; Ball-to-powder weight ratio is 5: 1; Ball milling speed is 200r/min, and adopts high-purity Ar gas as protective atmosphere, ball milling after 60 hours the WC powder average grain size be refined to about 180nm;
Step 3: discharge plasma sintering ball-milled powder
Get the wimet ball-milled powder 30g behind the high-energy ball milling, the diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mold of φ 20mm, and wherein sintering pressure is 30MPa; Sintering temperature is 1550 ℃; Heating rate is 100 ℃/min, and soaking time is 3min, and vacuum tightness is 6Pa.Obtain a kind of ultra-fine brilliant nothing bonding phase carboloy block materials that contains trace cobalt tiny, even, the about 400nm of WC average grain size of organizing after the Fast Sintering, the specific density of this sample reaches 99.92%, and hardness is 2511HV
10, bending strength is 1225MPa, fracture toughness property is 8.22MPam
1/2
Claims (2)
1. nothing bonding phase carboloy that contains trace cobalt, it is characterized in that: the component and the mass percentage content thereof of this alloy are following: Co:0.20-1.00%, Cr
3C
2: 0.01-0.50%, VC:0.01-0.50%, surplus is grain-size 0.2-0.8 μ m WC.
2. the preparation method of a nothing bonding phase carboloy that contains trace cobalt, it is characterized in that: this method adopts discharge plasma sintering technique, specifically comprises the steps and processing condition:
Step 1: the composition design of tungsten carbide base carbide alloy powder
Raw material wolfram varbide, cobalt, chromium carbide and vanadium carbide powder are carried out proportioning: Co:0.20-1.00%, Cr by following mass percent consumption
3C
2: 0.01-0.50%, VC:0.01-0.50%, surplus is grain-size 0.2-0.8 μ m WC;
Step 2: high-energy ball milling
Feed intake by above-mentioned raw materials powder quality per-cent consumption and to carry out high-energy ball milling, the WC powder average grain size is refined to less than 200nm in ball-milled powder;
Step 3: discharge plasma sintering ball-milled powder
With the discharge plasma sintering mould of packing into of the cemented carbide powder behind the high-energy ball milling, adopt the plasma discharging Fast Sintering, the sintering process condition is following:
Sintering pressure: 30～50MPa
Sintering heating rate: 100～200 ℃/min
Sintering temperature: 1500～1700 ℃
The sintered heat insulating time: 1～5min
Sintering vacuum tightness :≤6Pa
Obtain a kind of ultra-fine brilliant bonding phase carboloy that do not have tiny, that contain trace cobalt uniformly of organizing through Fast Sintering.
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| CN115821099A (en) * | 2022-11-28 | 2023-03-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of hard alloy |
| CN116752024A (en) * | 2023-08-21 | 2023-09-15 | 包头市新盛粉末冶金制品科技有限公司 | Tungsten carbide super wear-resistant hard alloy and preparation method and application thereof |
| CN116924804A (en) * | 2023-09-18 | 2023-10-24 | 成都金钨硬质合金有限公司 | Binding phase-free ultrafine ultra-fine grain hard alloy and preparation method thereof |
| CN116924804B (en) * | 2023-09-18 | 2023-11-21 | 成都金钨硬质合金有限公司 | Binding phase-free ultrafine ultra-fine grain hard alloy and preparation method thereof |
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Effective date of registration: 20181214 Address after: 331800 Hatching Garden Area of Xiaogang Town Economic Development Zone, Dongxiang District, Fuzhou City, Jiangxi Province Patentee after: Jiangxi Changyu Hard New Materials Co., Ltd. Address before: 510640 No. five, 381 mountain road, Guangzhou, Guangdong, Tianhe District Patentee before: South China University of Technology |