CN102382997B - Method for preparing WC-Co cemented carbide through microwave sintering - Google Patents
Method for preparing WC-Co cemented carbide through microwave sintering Download PDFInfo
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Abstract
The invention provides a method for preparing WC-Co cemented carbide through microwave sintering. The method comprises the steps of WC powder and Co powder batching and mixing, compacting and sintering, wherein in the step of sintering, compacts, SiC chips, carbon black and alumina powder are put in an alumina fiber insulating bag sleeve and then the alumina fiber insulating bag sleeve is put in a microwave high temperature furnace, the products in the furnace are heated to 500-600 DEG C at a heating speed of 5-10 DEG C/min and the heat is preserved and then the products are heated to 1400-1500 DEG C at a heating speed of 30-80 DEG C/min and the heat is preserved, thus obtaining the WC-Co cemented carbide. The method has the advantages of simple process, convenience in operation, short sintering period and low energy consumption, can replace the existing WC-Co cemented carbide processes, is used for producing the WC-Co cemented carbide by adopting the intermittent or continuous microwave sintering mode and is suitable for industrial application. The prepared WC-Co cemented carbide has excellent performances.
Description
Technical field:
The invention discloses the method that a kind of microwave prepares the WC-Co Wimet.Belong to microwave application and Wimet prepares technical field.
Technical background:
Wimet is produced with powder metallurgy process, is made of cermet material with Binder Phase coating hard phase microstructure feature refractory metal compound (WC, TiC etc.) and matrix metal (Co, Ni, Fe etc.).Wimet is widely used in various cutting tools, drilling tool, wear part, shaping dies etc. because having the performances such as good wear resistance, resistance to deformation impact resistance, erosion resistance.Usually adopt the modes such as vacuum sintering, low pressure sintering to prepare the WC-Co Wimet, the WC-Co alloy of preparation has the characteristics such as relative density is high, over-all properties is good, and the production cycle is long, technical process is complicated, energy consumption is large, the high in cost of production shortcoming but this type of sintering method exists.
Summary of the invention:
The object of the present invention is to provide that a kind of technical process is simple, easy to operate, the sintering period is short, sintering rate is fast, energy consumption is few, the method for the preparing WC-Co cemented carbide through microwave sintering of prepared WC-Co alloy microscopic structure and mechanical property excellence.Adopt the inventive method degreasing, sintering and thermal treatment process can be combined as a whole, can carry out intermittent type or continous way and produce the WC-Co Wimet.
The method of a kind of preparing WC-Co cemented carbide through microwave sintering of the present invention comprises the steps:
The first step: adopt WC powder, Co powder, behind the ball milling combination drying, obtain the WC-Co compound; Wherein Co accounts for the 3-30% of WC-Co compound total mass; WC powder Fisher particle size is the 6.0-7.0 micron, and it is the 1.0-2.0 micron that purity is higher than 99.9%, Co powder Fisher particle size, and purity is higher than 99.9%;
Second step: add in the first step gained compound account for described mixture quality 0.6-0.8% sodium butadiene rubber as forming agent, compression moulding under 200-500MPa pressure after dry, the screening obtains the WC-Co pressed compact;
The 3rd step: second step gained WC-Co pressed compact and boosting material SiC sheet are placed in the sapphire whisker insulation jacket simultaneously, and the filler that filling is comprised of carbon black and aluminum oxide powder around pressed compact, then, sapphire whisker is incubated jacket puts into microwave high-temperature stove furnace chamber, the vacuum tightness of furnace chamber is evacuated to 20-50Pa; In the microwave high-temperature stove, pass into pure N
2Protective atmosphere, keeping furnace chamber pressure is (0.8-1.5) * 10
5Pa; The output rating of regulation and control microwave source, the heat-up rate of 5-10 ℃/min is heated to 500-600 ℃, behind the insulation 30-60min, temperature rise rate with 30-80 ℃/min is heated to sintering temperature 1400-1500 ℃, insulation 1-10min, close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min, can obtain the WC-Co Wimet; Or
Place hydrogen furnace to be heated to 500-600 ℃ second step gained WC-Co pressed compact, behind the 6-8h that comes unstuck, be cooled to room temperature; Then place simultaneously in the sapphire whisker insulation jacket with boosting material SiC sheet, and around pressed compact, fill the filler that is formed by carbon black and aluminum oxide powder; Sapphire whisker is incubated jacket puts into microwave high-temperature stove furnace chamber, the vacuum tightness of furnace chamber is evacuated to 40-42Pa; In the microwave high-temperature stove, pass into pure N
2Protective atmosphere, keeping furnace chamber pressure is 1.01 * 10
5Pa; The output rating of regulation and control microwave source, temperature rise rate with 30-80 ℃/min is heated to sintering temperature 1400-1500 ℃, and insulation 1-10min closes microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min, can obtain the WC-Co Wimet.
Among the present invention, described ball milling adopts planetary ball mill, and ball-milling medium is dehydrated alcohol, rotating speed 120rpm, ratio of grinding media to material 2: 1, Ball-milling Time 6-8h.
Among the present invention, described sodium butadiene rubber adds after take gasoline as dissolution with solvents.
Among the present invention, the WC-Co pressed compact volume calculation that described boosting material SiC sheet addition is pressed sintering, every cubic centimetre of WC-Co pressed compact adds the 10-20gSiC sheet.
Among the present invention, described N
2The purity of shielding gas 〉=99.99%.
Among the present invention, carbon black and aluminum oxide powder mass ratio are (1-10) in the described filler: (99-90).
Among the present invention, during described compression moulding, smear the Zinic stearas spirituous solution at shaping grinding apparatus, to improve its oilness and compactibility.
Among the present invention, adopt vacuum pump to vacuumize in the described microwave high-temperature stove furnace chamber.
The present invention utilizes the whole heating of microwave, selects the characteristics such as heating, non-thermal effect owing to adopting above-mentioned processing method, makes sintering process have that heat-up rate is fast, the sintering period is short, the energy utilization rate high.The alloy mean grain size that studies have shown that microwave sintering method preparation is tiny, tissue distribution evenly, performance improves; And with short production cycle, save energy; Because the whole heating property of microwave sintering has overcome the slow heating of conventional sintering process using and repeatedly has been incubated to avoid the shortcomings such as the excessive distortion that causes of thermograde, bubbling; Simultaneously, in microwave heating process, add an amount of SiC as the boosting material, effectively promoted being rapidly heated and the even distribution of furnace chamber temperature field of sample.Compare with existing sintering technology, the present invention has following advantage:
1. simple, the consuming little energy of production technique of the present invention, preparation cost are low.Since microwave can with powder compact in the structural unit direct-coupling produce heat, the characteristic that therefore has whole heating and be rapidly heated.Adopt the alloy of microwave sintering preparation only to need just can finish about one hour whole sintering process from the room temperature to the sintering temperature; In addition because there is low inside and high outside thermograde in the object of microwave heating, so alloy sample carries out fast degumming and the bubbling phenomenon can not occur in microwave oven, and sodium butadiene rubber can remove fully; Reasonably insulation design can guarantee that also the shape of alloy sample can not change, and therefore can be chilled under 100 ℃ and can take out with stove after the shorter time of insulation, and the whole sintering period is the 1/3-1/6 of existing production cycle.
The present invention in the microwave high-temperature stove, adopt faster temperature rise rate (30-80 ℃/min) heating can make the rapid densification of alloy because microwave has the essential characteristics such as the heating of selection and non-thermal effect, the alloy relative density of preparation is all more than 99.0%.And, compare the alloy that the normal sintering method prepares, the WC-Co Wimet sample that microwave sintering goes out has more tiny grain fineness number because WC grain has little time to grow up, and microstructure also can be more even, and performance also increases.
3. the present invention adopts behind the sintering flow that passes into cooling gas by control to control speed of cooling, can realize that sintering and thermal treatment process are integrated; Simplify the Wimet subsequent treatment process, be beneficial to control and the optimization of WC-Co Wimet microstructure and structure.
In sum, the WC-Co Cemented Carbide Properties that technique of the present invention is simple, easy to operate, the sintering period is short, energy consumption is low, prepared is excellent, can replace existing WC-Co hard alloy process, adopt intermittent type or continuous-type microwave sintering processing to produce.
Embodiment:
Embodiment 1:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-6Co, adopt planetary ball mill in anhydrous ethanol medium, to mix drying behind the 8h, obtain the WC-Co compound, rotating speed is 150rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 500MPa pressure, be compressed to respectively cylinder sample and the high 42mm of being respectively of length and width that diameter is 18mm, 6.5mm, 6.5mm the rectangular parallelepiped bending test specimen, then be heated to 500 ℃ in hydrogen furnace, 8h comes unstuck; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.6% in the described gasoline solution;
The 3rd step: will take off the pressed compact of glue and the SiC boosting material of 80g and be positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 94% aluminum oxide powder and 6% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 20Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere is regulated microwave output power, is heated to 1460 ℃ with the heat-up rate of 30 ℃/min; the control microwave output power; make temperature at 1460 ℃ of insulation 1min, then close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.2%, Rockwell hardness HR is 90.1, bending strength is 1900MPa.
Embodiment 2:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-23Co, adopt planetary ball mill in anhydrous ethanol medium, will mix drying behind the 7h, obtain the WC-Co compound, rotating speed is 120rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 200MPa pressure, be compressed to respectively cylinder sample and the high respectively rectangular parallelepiped bending test specimen of 42mm * 6.5mm * 6.5mm of length and width that diameter is 18mm, then in hydrogen furnace, be heated to 550 ℃ of 7h that come unstuck; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.7% in the described gasoline solution;
The 3rd step: will take off the pressed compact of glue and the SiC boosting material of 80g and be positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 95% aluminum oxide powder and 5% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 35Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere is regulated microwave output power, is heated to 1420 ℃ with the heat-up rate of 30 ℃/min; the control microwave output power; make temperature at 1420 ℃ of insulation 1min, then close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.4%, Rockwell hardness HR is 88.0, bending strength is 3100MPa.
Embodiment 3:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-8Co, adopt planetary ball mill in anhydrous ethanol medium, will mix drying behind the 8h, obtain the WC-Co compound, rotating speed is 150rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 400MPa pressure, be compressed to respectively cylinder sample and the high 42mm of being respectively of length and width that diameter is 18mm, 6.5mm, 6.5mm the rectangular parallelepiped bending test specimen, then be heated to 600 ℃ in hydrogen furnace, 6h comes unstuck; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.8% in the described gasoline solution;
The 3rd step: will take off the pressed compact of glue and the SiC boosting material of 160g and be positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 95% aluminum oxide powder and 5% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 50Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere is regulated microwave output power, is heated to 1450 ℃ with the heat-up rate of 80 ℃/min; the control microwave output power; make temperature at 1450 ℃ of insulation 10min, then close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.2%, Rockwell hardness HR is 89.2, bending strength is 2600MPa.
Embodiment 4:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-8Co, adopt planetary ball mill in anhydrous ethanol medium, will mix drying behind the 6h, obtain the WC-Co compound, rotating speed is 120rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 400MPa pressure, be compressed to respectively cylinder sample and the high 42mm of being respectively of length and width that diameter is 18mm, 6.5mm, the rectangular parallelepiped bending test specimen of 6.5mm; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.6% in the described gasoline solution;
The 3rd step: the SiC boosting material of the pressed compact that suppresses and 80g is positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 99% aluminum oxide powder and 1% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 36Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere; regulate microwave output power; heat-up rate with 5 ℃/min is heated to 525 ℃; insulation 1h; then the heat-up rate with 30 ℃/min is heated to 1450 ℃, and the control microwave output power makes temperature at 1450 ℃ of insulation 5min; then close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.0%, Rockwell hardness HR is 88.7, bending strength is 2600MPa.
Embodiment 5:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-8Co, adopt planetary ball mill in anhydrous ethanol medium, will mix drying behind the 6h, obtain the WC-Co compound, rotating speed is 120rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 400MPa pressure, be compressed to respectively cylinder sample and the high 42mm of being respectively of length and width that diameter is 18mm, 6.5mm, the rectangular parallelepiped bending test specimen of 6.5mm; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.7% in the described gasoline solution;
The 3rd step: the SiC boosting material of the pressed compact that suppresses and 100g is positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 98% aluminum oxide powder and 2% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 45Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere; regulate microwave output power; heat-up rate with 8 ℃/min is heated to 580 ℃; insulation 1h, then the heat-up rate with 50 ℃/min is heated to 1450 ℃, the control microwave output power; make temperature at 1475 ℃ of insulation 5min; then close microwave source, pass into flowing nitrogen, sintered blank was cooled to below 100 ℃ in 60 minutes comes out of the stove.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.4%, Rockwell hardness HRA is 89.0, bending strength is 2800MPa.
Embodiment 6:
The first step: with purity greater than 99.9%, the WC powder of Fisher particle size 6.0-7.0 micron, purity greater than 99.9%, the Co powder of Fisher particle size 1-2 micron presses the mass percent batching of WC-8Co, adopt planetary ball mill in anhydrous ethanol medium, will mix drying behind the 6h, obtain the WC-Co compound, rotating speed is 120rpm, and ratio of grinding media to material is 2: 1;
Second step: in compound, add the gasoline solution final vacuum drying that is dissolved with sodium butadiene rubber, sieve, under 500MPa pressure, be compressed to respectively cylinder sample and the high 42mm of being respectively of length and width that diameter is 18mm, 6.5mm, the rectangular parallelepiped bending test specimen of 6.5mm; Be dissolved with the sodium butadiene rubber that accounts for described mixture quality 0.8% in the described gasoline solution;
The 3rd step: the SiC boosting material of the pressed compact that suppresses and 80g is positioned in the sapphire whisker insulation jacket, with the pressed compact landfill in the compound of 97% aluminum oxide powder and 3% carbon black, and jacket is put into the effective heating area territory of microwave high-temperature furnace chamber, use vacuum pump that the vacuum tightness in the furnace chamber is evacuated to 48Pa;
The 4th step: in the microwave high-temperature furnace chamber, pass into pure N
2The gas protective atmosphere; regulate microwave output power; heat-up rate with 10 ℃/min is heated to 600 ℃; insulation 1h, then the heat-up rate with 30 ℃/min is heated to 1450 ℃, the control microwave output power; make temperature at 1450 ℃ of insulation 5min; then close microwave source, pass into flowing nitrogen, sintered blank was cooled to below 100 ℃ in 60 minutes comes out of the stove.
The alloy property parameter that obtains after the cooling is: relative density reaches 99.0%, Rockwell hardness HR is 88.9, bending strength is 2400MPa.
Claims (8)
1. the method for a preparing WC-Co cemented carbide through microwave sintering comprises the steps:
The first step: adopt WC powder, Co powder, behind the ball milling combination drying, obtain the WC-Co compound; Wherein Co accounts for the 3-30% of WC-Co compound total mass; WC powder Fisher particle size is the 6.0-7.0 micron, and it is the 1.0-2.0 micron that purity is higher than 99.9%, Co powder Fisher particle size, and purity is higher than 99.9%;
Second step: add in the first step gained compound account for described mixture quality 0.6-0.8% sodium butadiene rubber as forming agent, compression moulding under the 200-500MPa pressure obtains the WC-Co pressed compact after dry, the screening;
The 3rd step: second step gained WC-Co pressed compact and boosting material SiC sheet are placed in the sapphire whisker insulation jacket simultaneously, and the filler that filling is comprised of carbon black and aluminum oxide powder around pressed compact, then, sapphire whisker is incubated jacket puts into microwave high-temperature stove furnace chamber, the vacuum tightness of furnace chamber is evacuated to 20-50Pa; In the microwave high-temperature stove, pass into pure N
2Protective atmosphere, keeping furnace chamber pressure is (0.8-1.5) * 10
5Pa; The output rating of regulation and control microwave source, heat-up rate with 5-10 ℃/min is heated to 500-600 ℃, behind the insulation 30-60min, temperature rise rate with 30-80 ℃/min is heated to sintering temperature 1400-1500 ℃, insulation 1-10min, close microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min, can obtain the WC-Co Wimet; The WC-Co pressed compact volume calculation that described boosting material SiC sheet addition is pressed sintering, every cubic centimetre of WC-Co pressed compact adds the 10-20gSiC sheet.
2. the method for a preparing WC-Co cemented carbide through microwave sintering comprises the steps:
The first step: adopt WC powder, Co powder, behind the ball milling combination drying, obtain the WC-Co compound; Wherein Co accounts for the 3-30% of WC-Co compound total mass; WC powder Fisher particle size is the 6.0-7.0 micron, and it is the 1.0-2.0 micron that purity is higher than 99.9%, Co powder Fisher particle size, and purity is higher than 99.9%;
Second step: add in the first step gained compound account for described mixture quality 0.6-0.8% sodium butadiene rubber as forming agent, compression moulding under 100-500MPa pressure after dry, the screening obtains the WC-Co pressed compact;
The 3rd step: place hydrogen furnace to be heated to 500-600 ℃ second step gained WC-Co pressed compact, behind the 6-8h that comes unstuck, be cooled to room temperature; Then place simultaneously in the sapphire whisker insulation jacket with boosting material SiC sheet, and around pressed compact, fill the filler that is formed by carbon black and aluminum oxide powder; Sapphire whisker is incubated jacket puts into microwave high-temperature stove furnace chamber, the vacuum tightness of furnace chamber is evacuated to 20-35Pa; In the microwave high-temperature stove, pass into pure N
2Protective atmosphere, keeping furnace chamber pressure is (0.8-1.5) * 10
5Pa; The output rating of regulation and control microwave source, temperature rise rate with 30-80 ℃/min is heated to sintering temperature 1400-1500 ℃, and insulation 1-10min closes microwave source, come out of the stove after being cooled to below 100 ℃ with the rate of temperature fall of 24-28 ℃/min, can obtain the WC-Co Wimet; The WC-Co pressed compact volume calculation that described boosting material SiC sheet addition is pressed sintering, every cubic centimetre of WC-Co pressed compact adds the 10-20gSiC sheet.
3. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 1 and 2 is characterized in that: described ball milling adopts planetary ball mill, and ball-milling medium is dehydrated alcohol, rotating speed 120rpm, ratio of grinding media to material 2:1, Ball-milling Time 6-8h.
4. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 3 is characterized in that: described sodium butadiene rubber adds after take gasoline as dissolution with solvents.
5. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 4 is characterized in that: described N
2The purity of shielding gas 〉=99.99%.
6. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 5 is characterized in that: carbon black and aluminum oxide powder mass ratio are (1-10) in the described filler: (99-90).
7. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 6 is characterized in that: during described compression moulding, smear the Zinic stearas spirituous solution at shaping grinding apparatus, to improve its oilness and compactibility.
8. the method for a kind of preparing WC-Co cemented carbide through microwave sintering according to claim 7 is characterized in that: adopt vacuum pump to vacuumize in the described microwave high-temperature stove furnace chamber.
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| 微波多模腔快速烧结WC-8%Co硬质合金;鲍瑞等;《中国钨业》;20090630;第24卷(第03期);32-35 * |
| 微波烧结制备WC-12Co硬质合金;杨亚杰等;《粉末冶金材料科学与工程》;20100228;第15卷(第1期);84-88 * |
| 杨亚杰等.微波烧结制备WC-12Co硬质合金.《粉末冶金材料科学与工程》.2010,第15卷(第1期),84-88. |
| 鲍瑞等.微波多模腔快速烧结WC-8%Co硬质合金.《中国钨业》.2009,第24卷(第03期),32-35. |
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| CN102382997A (en) | 2012-03-21 |
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