CN102628138B - 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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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 refer to a kind of contain trace cobalt (Co) without Binder Phase wolfram varbide (WC) Wimet and preparation method thereof.
Background technology
The tradition Wimet is take the insoluble metal hard compounds as matrix, take metals such as cobalt, nickel, iron as Binder Phase.Binder Phase has also been given alloy toughness and intensity, but has also been made the reductions such as its corrosion resistance nature, resistance to elevated temperatures, wear resisting property, thermal conductivity, thereby made its Application Areas be subject to certain limitation except having the function that promotes the full densification of alloy sintering.Without the metal bonding phase cemented carbide, be called for short non-bond cemented carbide, belong to the special Wimet of a class, can be divided into two large series, one class is pure WC series and serial take refractory carbide sosoloid as Binder Phase, another kind of " without Binder Phase " WC Wimet for mentioning in some document refers to metallic binding phase massfraction≤1%.Owing to have the higher hardness of more traditional Wimet, wear resistance and erosion resistance, by precise polished, its surfaceness can reach≤15nm, and non-bond cemented carbide can be used as extraordinary sealing material, high-pressure medium nozzle material, sliding material, precision die material, high abrasion resisting material etc.
Just becoming an important development direction of high-anti-friction hard alloy without Binder Phase WC Wimet.Yet the fusing point of pure WC is up to 2860 ℃, and the sintering temperature without Binder Phase WC Wimet for preparing full densification is very high, and the abnormal growth of WC grain occurs in sintering process easily.In the prior art, preparation mainly concentrates on preparation without the research of Binder Phase WC Wimet and does not add the pure WC Wimet of any binding agent and the pure WC Wimet aspect that carbon is joined in preparation, there are the following problems for preparation process: 1, sintering temperature is too high, sintering time is longer, prepares the sintering temperature of pure WC Wimet of full densification more than 1800 ℃; 2, there is the phenomenon of WC grain abnormal growth in the alloy of preparation, can't prepare Ultra-fine Grained without Binder Phase WC Wimet; 3, owing to do not contain any binding agent, the alloy strength of preparation and fracture toughness property are very low.Up to now, there is not yet the report without Binder Phase WC Wimet that adopts the discharge plasma sintering preparation to add micro-Co.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art part, provide a kind of have excellent comprehensive performance contain micro-Co without Binder Phase WC Wimet.
Another object of the present invention also is to combine by reasonable component design and optimal preparation technology, and a kind of preparation method without Binder Phase WC Wimet who contains micro-Co that over-all properties, simple process, sintering temperature are low, sintering time is short that can further improve material is provided.
Purpose of the present invention can be achieved by the following measures:
A kind of contain trace cobalt without the Binder Phase carboloy, it is characterized in that: component and the mass percentage content thereof of this alloy are as follows: 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 without the Binder Phase carboloy who contains trace cobalt is characterized in that: the 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, until the WC powder average grain size is refined to less than 200nm in the 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, sintering process conditions is as follows:
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 fine microstructures, contain the Ultra-fine Grained of trace cobalt without the Binder Phase carboloy uniformly through Fast Sintering.
The present invention compared with prior art has the following advantages:
1, the Composition Design of tungsten carbide base carbide alloy powder of the present invention is reasonable, owing to add micro-Co, greatly reduces sintering temperature again, has accelerated significantly the sintering densification process, has shortened sintering time, and whole sintering process can be short to only has several minutes; And reduce the full densification of preparation without the sintering temperature of Binder Phase WC Wimet, thereby greatly saved the energy, 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, have liquid phase Co film between the part WC particle, strengthened intergranular strength of joint, improved the toughness of alloy, can obtain to have Good All-around Property Ultra-fine Grained without Binder Phase WC Wimet.
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 inhibiting grain growth, and the block grain-size behind the sintering is tiny even.
The implementation form
The invention will be further described by following embodiment, but embodiments of the present invention are not limited only to this.
Embodiment 1
A kind of preparation method without the Binder Phase carboloy who contains trace cobalt, the 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
Powder stock by the described tungsten carbide base carbide alloy powder mixture ratio of step 1 places planetary ball mill to carry out high-energy ball milling, ball grinder and Material quality of grinding balls adopt the WC Wimet, ball-milling medium is ethanol, ratio of grinding media to material is 5: 1, 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 milling powder end 30g behind the high-energy ball milling diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mould of φ 20mm, wherein sintering pressure is 50MPa, sintering temperature is 1500 ℃, the sintering heating rate is 200 ℃/min, the sintered heat insulating time is 5min, and sintering vacuum tightness is 6Pa.Obtain after the Fast Sintering a kind of fine microstructures, evenly, the Ultra-fine Grained that contains trace cobalt of the about 350nm of WC average grain size is without Binder Phase carboloy block materials, the relative density of this sample reaches 98.67%, hardness is 2368HV
10, bending strength is 985MPa, fracture toughness property is 7.54MPam
1/2
Embodiment 2
A kind of preparation method without the Binder Phase carboloy who contains trace cobalt, the 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
Consumption by the described tungsten carbide base carbide alloy powder mixture ratio of step 1, place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and Material quality of grinding balls adopt the WC Wimet, ball-milling medium is ethanol, ratio of grinding media to material 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 milling powder end 30g behind the high-energy ball milling, the diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mould of φ 20mm, wherein sintering pressure is 50MPa, sintering temperature is 1500 ℃, the sintering heating rate is 200 ℃/min, the sintered heat insulating time is 5min, and sintering vacuum tightness is 5Pa.Obtain after the Fast Sintering a kind of fine microstructures, evenly, the Ultra-fine Grained that contains trace cobalt of the about 380nm of WC average grain size is without Binder Phase carboloy block materials, the relative density of this sample reaches 99.41%, hardness is 2546HV
10, bending strength is 1146MPa, fracture toughness property is 8.01MPam
1/2
Embodiment 3
A kind of preparation method without the Binder Phase carboloy who contains trace cobalt, the 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
Consumption by the described tungsten carbide base carbide alloy powder mixture ratio of step 1, place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and Material quality of grinding balls adopt the WC Wimet, ball-milling medium is ethanol, ratio of grinding media to material 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 milling powder end 30g behind the high-energy ball milling, the diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mould of φ 20mm, wherein sintering pressure is 40MPa, sintering temperature is 1700 ℃, the sintering heating rate is 150 ℃/min, the sintered heat insulating time is 1min, and sintering vacuum tightness is 4Pa.Obtain after the Fast Sintering a kind of fine microstructures, evenly, the Ultra-fine Grained that contains trace cobalt of the about 410nm of WC average grain size is without Binder Phase carboloy block materials, the relative density of this sample reaches 99.53%, hardness is 2605HV
10, bending strength is 1027MPa, fracture toughness property is 7.83MPam
1/2
Embodiment 4
A kind of preparation method without the Binder Phase carboloy who contains trace cobalt, the 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
Consumption by the described tungsten carbide base carbide alloy powder mixture ratio of step 1, place planetary ball mill to carry out high-energy ball milling powder stock, ball grinder and Material quality of grinding balls adopt the WC Wimet, ball-milling medium is ethanol, ratio of grinding media to material 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 milling powder end 30g behind the high-energy ball milling, the diameter of packing into is to carry out discharge plasma sintering in the graphite sintering mould 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 after the Fast Sintering a kind of fine microstructures, evenly, the Ultra-fine Grained that contains trace cobalt of the about 400nm of WC average grain size is without Binder Phase carboloy block materials, the relative density of this sample reaches 99.92%, hardness is 2511HV
10, bending strength is 1225MPa, fracture toughness property is 8.22MPam
1/2
Claims (2)
1. preparation method without the Binder Phase carboloy who contains trace cobalt is characterized in that: the 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, until the WC powder average grain size is refined to less than 200nm in the 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, sintering process conditions is as follows:
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 fine microstructures, contain the Ultra-fine Grained of trace cobalt without the Binder Phase carboloy uniformly through Fast Sintering.
2. a kind of preparation method without the Binder Phase carboloy who contains trace cobalt according to claim 1, prepared a kind of component and mass percentage content thereof are Co:0.20-1.00%, Cr
3C
2: 0.01-0.50%, VC:0.01-0.50%, surplus be grain-size 0.2-0.8 μ m WC contain trace cobalt without the Binder Phase carboloy.
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