CN102234729A - Preparation method for hard metal - Google Patents
Preparation method for hard metal Download PDFInfo
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Abstract
The invention discloses a preparation method for a hard metal. The method comprises the following steps: adding hard phase powder to a jet mill to carry out crushing; carrying out stirring and grinding in a stirring ball mill to form slurry; carrying out filtering, drying and screening; finally carrying out a forming treatment through molding, extruding and injection molding to prepare the hard metal. According to the present invention, a high-energy crushing and air classification method is adopted for providing a strength crushing for the hard metal powder with internal defects, followed by carrying out powder shaping, such that surface of the hard phase powder is endowed with high energy so as to reduce the defects of the hard metal powder and improve the energy of the powder; all components are mixed more uniformly through adopting high-speed and high-performance mixing shaping so as to improve a concordance of the powder appearance, such that the alloy microstructure grain has characteristics of uniform particle size, good concordance of the grain appearance, no refining particles and no specially massive particles, centralized granularity, no internal defects, so as to finally improve performance of the hard metal material.
Description
Technical field
The present invention relates to Wimet, be specifically related to a kind of manufacture method of Wimet.
Background technology
Wimet is that the carbide micron powder with the high rigidity refractory metal is a main component, is binding agent with cobalt or nickel, molybdenum, the sintered metal product that sintering forms in vacuum oven or hydrogen reducing furnace.Wimet is the material of a kind of high rigidity, high strength, high abrasion, has obtained using widely at modern industry, and the manufacturing critical process of Hardmetal materials is the manufacturing of carbide alloy mixture.The manufacture method of traditional Wimet exists the powder defective to remove difficulties, mix that inequality, mixing efficiency are low, there is coarse grain in the finished product.
Summary of the invention
The crystal grain of the technical problem to be solved in the present invention Wimet is thick, and a kind of manufacture method of Wimet is provided.
Technical scheme of the present invention is: a kind of manufacture method of Wimet, and it is operated by following step:
(1) hard phase powder is added in the micronizer mill, carry out 1~5 time and pulverize, the pulverizing time is 0.2~3.0 hour, and size classification is handled then, and making size range is the hard phase powder of 0.4~30 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, weight with hard phase powder is benchmark, add 1~35% bonded metal powder, 0.01~5.00% micro-powder, 25~45% grinding medium, 0.01~2% dispersion agent, 1~8% forming agent, carry out 2~5 agitation grindings, the agitation grinding time is 0.5~8.0 hour, form slip, filter then, dry under 50~250 ℃ condition, sieve, the order number of sieve is 20~200 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1350 ℃~1500 ℃ condition is incubated 30~150 minutes then, makes Wimet.
Hard phase powder in the described step (1) is tungsten, wolfram varbide, tungsten nitride, molybdenum, molybdenum carbide, molybdenum nitride, shield, carbonization is shielded, nitrogenize is shielded, any one or at least two kinds in the niobium, niobium carbide, niobium nitride, titanium, titanium carbide, titanium nitride.
The mean particle size of described hard phase powder is 0.8~25 μ m.
The gas of micronizer mill is N in the described step (1)
2, Ar, airborne any one or at least two kinds, stream pressure is 0.6~12Mpa.
Bonded metal powder in the described step (2) is any one or two or three the mixture in nickel, iron, the cobalt; The trace element powder is that carbonization is shielded, in the titanium carbide, vanadium carbide, chromium carbide any one; Grinding medium is any one in ethanol, hexane, heptane, acetone or the water; Dispersion agent is any one in oleic acid, the stearic acid; Forming agent is any one in paraffin, the polyoxyethylene glycol.
The agitator shaft speed of described step (2) agitating ball mill is 80~3500 rev/mins.
The mill ball diameter of described step (2) agitating ball mill is 2~8mm, and mill ball and the hard ratio of the weight of powder mutually are 3~10: 1.
The present invention selects for use high pressure draft to spray fragmentation and is classified as the beginning of technology, selects for use high speed high-energy stirring mixing machine to substitute existing rolling ball milling, stirring at low speed ball mill then; By the high energy unit, finish the function of powerful fragmentation, classification, uniform mixing, shaping, by spray-drying process, all kinds of compacting, sintering process, finish the production of hart metal product again.
Major equipment among the present invention: high pressure draft injection and stepped mixing unit, high speed stirred ball mill group;
(1) high pressure draft sprays broken classification unit
High pressure N
2The agitation vat of the container of (dust-free air, other are single or mixed gas) equipment, 2~5 at high abrasion nozzle, band high hardness spray coating (Mo, W or Mo, W mixture), band cooling jacket, powder circulation unit, vibration motor, electrical equipment control, air classification unit etc. are partly formed.
Owing to adopt high pressure draft, drive hard phase (metal or metallic carbide or nitride such as WC, TaC) high-speed motion, streams is intersected impact mutually, impact again on the hard sphere at last, hard accelerates to high speed (100~500m/s) by air-flow, single particle possesses high kinetic energy, air flow stream is by special nozzle form and angle, carry out intersection-type collision, friction, shearing, reach powder particle from crushing effect, especially to there being the hard-phase particles of subsurface defect, its crushing effect is especially outstanding.
By the material Cycle Unit, make hard phase (metal or metallic carbide or nitride such as WC, TaC) material carry out above-mentioned processing repeatedly for 1~5 time again, thereby reach the purpose of abundant fragmentation, removal defective.By the air classification unit,, go out powder size composition powder (the powder size scope 0.4~30um) that the user needs at last thereby reach classification by adjusting parameters at different levels.
(2) high speed stirred ball mill
The agitation vat of band cooling jacket, stirring main shaft, band wear-resistant protection agitator arm, bung, motor, electrical control part.Owing to adopt high speed stirred ball mill (150~5000 rev/mins) initiatively to drive the mill ball high-speed motion by main shaft, also there is velocity contrast between the mill ball, special in addition material movement is so mill ball and agitator arm carry out effects such as impact grinding, high efficient mixed, powder shaping together to polycomponent Wimet powder; Its speed and energy height are existing rolling ball milling or agitating ball mill 30~200 times, have about 30~150 times so mixing efficiency improves, and can shorten the production cycle significantly.By the material Cycle Unit, each component of material is circulated again, carry out above-mentioned processing repeatedly, thereby reach the purpose of abundant fragmentation, removal defective.
The invention has the beneficial effects as follows: the present invention is by the method for high energy fragmentation with air classification, to there be the cemented carbide powder of latent defect to carry out the brute force fragmentation, conducting powder end shaping, thereby give hard phase surface high-energy such as WC, thereby reach the defective that reduces hard phase powder, improve the powder energy; Pass through the mixing shaping of high-speed and high-efficiency again, reach and respectively organize more uniform mixing, improve powder profile consistence, thereby reach alloy structure crystallite size size evenly, the grain shape high conformity, no refinement and extraordinarily thick macrobead, and granularity is concentrated, no subsurface defect, finally reaches the performance that improves Hardmetal materials.
Specific embodiment:
Embodiment 1
A kind of manufacture method of Wimet, it is operated by following step:
(1) tungsten-carbide powder with 1200g mean particle size 2.0 μ m adds in the micronizer mill, through the N of high pressure draft pulverizer
2Air pressure 2Mpa carries out 1 time and pulverizes, and the pulverizing time is 0.4 hour, finishes powder classification simultaneously and handles, and making size range is the hard phase powder of 0.4~2.0 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the cobalt dust that the 60g mean particle size is 1.2 μ m again, 2g titanium carbide powder, 0.24g oleic acid, 24g polyoxyethylene glycol, 400g ethanol is as grinding medium, 500 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, the quality of mill ball is 7200g, carry out agitation grinding, ground 2.0 hours, and formed slip, filter then, dry under 50~250 ℃ condition, sieve, the order number is 20 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1400 ℃ condition is incubated 60 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 1.2um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 2
A kind of manufacture method of Wimet, it is operated by following step:
(1) tungsten powder with 1200g mean particle size 2.0 μ m adds in the micronizer mill, through the Ar air pressure 12Mpa of high pressure draft pulverizer, to carry out 5 times and pulverize, the pulverizing time is 3 hours, finish size classification simultaneously and handle, making size range is the hard phase powder of 20~30 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the nickel by powder that the 420g mean particle size is 1.2 μ m again, 0.12g tantalum carbide powder, 24g stearic acid, 96g polyoxyethylene glycol, 540g ethanol is as grinding medium, 3500 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, mill ball weight is 12kg, carry out agitation grinding, ground 8 hours, and formed slip, filter then, dry under 200 ℃ condition, sieve, the order number of sieve is 200 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1500 ℃ condition is incubated 150 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 1.0um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 3
A kind of manufacture method of Wimet, it is operated by following step:
(1) the molybdenum nitride powder with 1200g mean particle size 25 μ m adds in the micronizer mill, and through the high pressure draft pulverizer, gas is N
2With Air mixing gas, air pressure 0.6Mpa carries out 1 time and pulverizes, and the pulverizing time is 0.3 hour, finishes size classification simultaneously and handles, and making size range is the hard phase powder of 5~25 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the iron powder that the 12g mean particle size is 1.2 μ m again, 60g vanadium carbide powder, 24g oleic acid, 12g polyoxyethylene glycol, the 300g hexane is as grinding medium, 80 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, mill ball weight is 3600g, carry out agitation grinding, ground 0.5 hour, and formed slip, filter then, dry under 50~250 ℃ condition, sieve, the order number is 140 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1350 ℃ condition is incubated 30 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 5.0um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 4
A kind of manufacture method of Wimet, it is operated by following step:
(1) niobium powder with 1200g mean particle size 0.8 μ m adds in the micronizer mill, through the air pressure 3Mpa of high pressure draft pulverizer, to carry out 2 times and pulverize, the pulverizing time is 1 hour, finish size classification simultaneously and handle, making size range is the hard phase powder of 0.4~0.8 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, adding cobalt dust and the 150g mean particle size that the 150g mean particle size is 1.2 μ m again is the nickel by powder of 1.2 μ m, 20g chromium carbide powder, 1g stearic acid, 50g paraffin, the 400g heptane is as grinding medium, 500 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, the mill ball quality is 5kg, carry out agitation grinding, ground 2.0 hours, and formed slip, filter then, dry under 150 ℃ condition, sieve, the order number is 120 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1400 ℃ condition is incubated 60 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 0.6um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 5
A kind of manufacture method of Wimet, it is operated by following step:
(1) titanium carbide powder with 1200g mean particle size 5.0 μ m adds in the micronizer mill, through the N of high pressure draft pulverizer
2Air pressure 10Mpa carries out 3 times and pulverizes, and the pulverizing time is 2.0 hours, finishes powder classification simultaneously and handles, and making size range is the hard phase powder of 0.4~1.0 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the cobalt dust that the 12g mean particle size is 1.0 μ m again, 0.12g chromium carbide powder, 0.12g oleic acid, 12g polyoxyethylene glycol, 300g water is as grinding medium, 80 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, mill ball weight is 7200g, carry out agitation grinding, ground 2.0 hours, and formed slip, filter then, dry under 120 ℃ condition, sieve, the order number of sieve is 160 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1350 ℃ condition is incubated 100 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 1.2um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 6
A kind of manufacture method of Wimet, it is operated by following step:
(1) titanium nitride powder of 600g mean particle size 2.0 μ m and the ti powder of 600g mean particle size 2.0 μ m are added in the micronizer mill, Ar air pressure 8Mpa through the high pressure draft pulverizer, carrying out 5 times pulverizes, the pulverizing time is 3 hours, finish size classification simultaneously and handle, making size range is the hard phase powder of 10~15 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the nickel by powder that the 540g mean particle size is 1.2 μ m again, 18g vanadium carbide powder, 2g stearic acid, 20g polyoxyethylene glycol, 480g acetone is as grinding medium, 800 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, mill ball weight is 6kg, carry out agitation grinding, ground 8 hours, and formed slip, filter then, dry under 100 ℃ condition, sieve, the order number of sieve is 60 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1380 ℃ condition is incubated 50 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 1.0um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 7
A kind of manufacture method of Wimet, it is operated by following step:
(1) the molybdenum nitride powder with 1200g mean particle size 25 μ m adds in the micronizer mill, through the N of high pressure draft pulverizer
2Air pressure 8Mpa carries out 2 times and pulverizes, and the pulverizing time is 1.5 hours, finishes size classification simultaneously and handles, and making size range is the hard phase powder of 25~30 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the iron powder that the 200g mean particle size is 1.2 μ m again, 10g vanadium carbide powder, 6g stearic acid, 80g polyoxyethylene glycol, 450g ethanol is as grinding medium, 3000 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, mill ball weight is 4800g, carry out agitation grinding, ground 6 hours, and formed slip, filter then, dry under 80 ℃ condition, sieve, the order number of sieve is 180 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1350 ℃ condition is incubated 120 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 5.0um, uniform crystal particles, grain shape high conformity, no big particle.
Embodiment 8
A kind of manufacture method of Wimet, it is operated by following step:
(1) tantalum nitride powder with 1200g mean particle size 0.8 μ m adds in the micronizer mill, through the air pressure 3Mpa of high pressure draft pulverizer, to carry out 4 times and pulverize, the pulverizing time is 2.5 hours, finish size classification simultaneously and handle, making size range is the hard phase powder of 5~10 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, add the cobalt dust that the 500g mean particle size is 1.2 μ m again, 200g vanadium carbide powder, 8g stearic acid, 15g paraffin, 520g water is as grinding medium, 3500 rev/mins of stirring velocitys, stacking factor 0.65, mill ball diameter D4, the mill ball quality is 8kg, carry out agitation grinding, ground 8 hours, and formed slip, filter then, dry under 150 ℃ condition, sieve, the order number of sieve is 40 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1400 ℃ condition is incubated 150 minutes then, makes Wimet.
Through detecting, hard phase average grain-size is 0.6um, uniform crystal particles, grain shape high conformity, no big particle.
In the foregoing description, hard phase powder can be for tungsten, wolfram varbide, tungsten nitride, molybdenum, molybdenum carbide, molybdenum nitride, shield, carbonization is shielded, nitrogenize is shielded, in the niobium, niobium carbide, niobium nitride, titanium, titanium carbide, titanium nitride any one or two or more.
Claims (7)
1. the manufacture method of a Wimet is characterized in that, it is operated by following step:
(1) hard phase powder is added in the micronizer mill, carry out 1~5 time and pulverize, the pulverizing time is 0.2~3.0 hour, and size classification is handled then, and making size range is the hard phase powder of 0.4~30 μ m;
(2) the hard phase powder in the step (1) is added in the agitating ball mill, weight with hard phase powder is benchmark, add 1~35% bonded metal powder, 0.01~5.00% micro-powder, 25~45% grinding medium, 0.01~2% dispersion agent, 1~8% forming agent, carry out 2~5 agitation grindings, the agitation grinding time is 0.5~8.0 hour, form slip, filter then, dry under 50~250 ℃ condition, sieve, the order number of sieve is 20~200 orders, makes the carbide alloy mixture grain;
(3) the carbide alloy mixture grain in the step (2) is carried out forming processes by mold pressing, extruding, injection moulding, sintering under 1350 ℃~1500 ℃ condition is incubated 30~150 minutes then, makes Wimet.
2. the manufacture method of Wimet according to claim 1 is characterized in that: the hard phase powder in the described step (1) is tungsten, wolfram varbide, tungsten nitride, molybdenum, molybdenum carbide, molybdenum nitride, shield, carbonization is shielded, nitrogenize is shielded, any one or at least two kinds in the niobium, niobium carbide, niobium nitride, titanium, titanium carbide, titanium nitride.
3. the manufacture method of Wimet according to claim 2, it is characterized in that: the mean particle size of described hard phase powder is 0.8~25 μ m.
4. the manufacture method of Wimet according to claim 1 is characterized in that: the gas of micronizer mill is N in the described step (1)
2, Ar, airborne any one or at least two kinds, stream pressure is 0.6~12Mpa.
5. the manufacture method of Wimet according to claim 1 is characterized in that: the bonded metal powder in the described step (2) is any one or two or three the mixture in nickel, iron, the cobalt; The trace element powder is that carbonization is shielded, in the titanium carbide, vanadium carbide, chromium carbide any one; Grinding medium is any one in ethanol, hexane, heptane, acetone or the water; Dispersion agent is any one in oleic acid, the stearic acid; Forming agent is any one in paraffin, the polyoxyethylene glycol.
6. the manufacture method of Wimet according to claim 1, it is characterized in that: the agitator shaft speed of described step (2) agitating ball mill is 80~3500 rev/mins.
7. the manufacture method of Wimet according to claim 1, it is characterized in that: the mill ball diameter of described step (2) agitating ball mill is 2~8mm, mill ball and the hard weight ratio of powder mutually are 3~10: 1.
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