CN104131208A - Aluminium oxide-titanium carbide micron composite ceramic cutter material and microwave sintering method thereof - Google Patents
Aluminium oxide-titanium carbide micron composite ceramic cutter material and microwave sintering method thereof Download PDFInfo
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- CN104131208A CN104131208A CN201410382490.6A CN201410382490A CN104131208A CN 104131208 A CN104131208 A CN 104131208A CN 201410382490 A CN201410382490 A CN 201410382490A CN 104131208 A CN104131208 A CN 104131208A
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Abstract
The invention belongs to the technical field of microwave sintered material sciences and relates to an aluminium oxide-titanium carbide micron composite ceramic cutter material and a microwave sintering method thereof. The method is characterized by comprising the following steps: mixing submicron alpha-Al2O3, micron TiC, molybdenum powder and nickel powder, balance being MgO and Y2O3 according to certain proportion and carrying out microwave sintering process under the protection of high-purity argon to successfully prepare the aluminium oxide-titanium carbide micrometer composite ceramic cutter material. The composite material is high in compactness and good in mechanical property; the Vickers hardness and the fracture toughness of the material are respectively up to 19.6GPa and 4.8MPa.m1/2; therefore, the material is suitable for the manufacturing and the processing of cutters made from difficult-to-machine materials. The microwave sintering method of the aluminium oxide-titanium carbide micrometer composite ceramic cutter material, provided by the invention, is high in prepared material property, simple in process, energy-saving and time-saving, low in cost and easy for industrialization.
Description
Technical field
The invention belongs to microwave sintering materials science field, relate to a kind of alumina-titanium carbide micron composite ceramic tool material and microwave sintering method thereof.
Background technology
Al
2o
3-TiC matrix material has the character such as high conductivity, high rigidity, high strength and high-fracture toughness, these good performances make it tool and have been widely used, in particular as sintex (A.G. King. Ceramics for Cutting Materls.Am.Ceram.Soc.Bull, 1965.43 (5): 395-401).So far the Al as cutter of report
2o
3-TiC composite ceramics great majority obtain by hot pressed sintering, hot pressed sintering pressurizes simultaneously, heat and contribute to intergranular contact, diffusion and the mass transfer process such as flow, can reduce sintering temperature and shorten sintering time, suppress grain growing, do not need sintering agent. easily obtain approaching the sintered compact of theoretical density, the material property obtaining is high.But hot pressed sintering efficiency is lower, be difficult to production in enormous quantities and cost also high.
Al
2o
3the sintering temperature of-TiC composite ceramic material is very high, conventionally use the temperature range of pressureless sintering at 1673 DEG C ~ 1800 DEG C (Tian D Xia, Zuhair A, Yan L. Tang et al. Structure Formation in the Combustion synthesis of Al
2o
3-TiC Composites. J. Am. Ceram.Soc, 2000.83 (3): 507-512).But Al
2o
3-TiC can react under high temperature (>1500 DEG C): Al
2o
3+ TiC=Al
2o ↑+TiO+ CO ↑, in sintered specimen, produce gas and can make its fine and close reduction, finally affect its mechanical property.
Adrian Goldstein thinks under high temperature (>1500 DEG C) to Al
2o
3-TiC sample is carried out Fast Sintering, can suppress Al
2o
3with TiC reaction, found that the Al after microwave sintering
2o
3-TiC stupalith density at 1800 DEG C can reach 95-97%, can meet service requirements (Goldstein A, the Singurindi A. Al of cutter through HIP sintering material property after treatment
2o
3/ TiC based metal cutting tools by microwave sintering followed by hot isostatic pressing[J]. Journal of the American Ceramic Society, 2000,83 (6): 1530-1532.).But hot isostatic apparatus expense is somewhat expensive, be difficult to realize mass production.
As from the foregoing, existing hot pressing and sintering technique efficiency is lower, the corresponding Al that makes
2o
3the cost of-TiC sintex is higher, pressureless sintering Al
2o
3the ceramic sintering temperature needing of-TiC is higher, soaking time is long, and sintering cutter material density is out not high, and performance is not high.Therefore, existing technology is difficult to successfully realize high performance Al
2o
3the low cost of-TiC composite ceramic cutting tool, batch production.
Summary of the invention
The object of the present invention is to provide a kind of alumina-titanium carbide micron composite ceramic tool material and microwave sintering method thereof, be easy to realize Al
2o
3the scale production of-TiC composite ceramic cutting tool.
Realize the object of the invention technical scheme as follows: a kind of alumina-titanium carbide micron composite ceramic tool material, the composition of this material is by mass percentage: submicron ɑ-Al
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3.
Described submicron ɑ-Al
2o
3powder particle particle diameter is 0.5 ~ 0.8 μ m.
Described micron TiC powder particle particle diameter is 1 ~ 3 μ m.
A method for the above-mentioned alumina-titanium carbide micron composite ceramic tool material of microwave sintering, comprises the following steps:
Step 1, batching: submicron ɑ-Al by mass percentage
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3prepare burden;
Step 2, batch mixing; The mixed powder that step 1 is prepared mixes 30 ~ 60h taking dehydrated alcohol as medium ball milling, ball milling post-drying is sieved; Described abrading-ball is aluminum oxide abrading-ball; In batch mixing process, ball material mass ratio is 5:1 ~ 10:1.
Step 3, granulation: will in mixed powder, add polyvinyl alcohol water solution granulation; The concentration of described polyvinyl alcohol water solution is 3% ~ 5%.
Step 4, moulding: by dry-pressing formed the powder that granulation is good, pressure is 150 ~ 250MPa, and the dwell time is 1 ~ 5min;
Step 5, binder removal: the blank of step 3 moulding is placed in to microwave agglomerating furnace, open vacuum pump, vacuum in body of heater is evacuated to 0.07MPa ~ 0.09 MPa, then open microwave power supply and heat, blank is heated to 600 DEG C ~ 800 DEG C by the speed of 20 ~ 30 DEG C/min, at this insulation 5 ~ 20min;
Step 6, sintering: after binder removal finishes, vacuum in body of heater is evacuated to 0.004 MPa ~ 0.006MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 30 ~ 40 DEG C/min, be heated to 1600 DEG C ~ 1700 DEG C, at this temperature, be incubated 10 ~ 30min, then furnace cooling makes ceramic cutting tool material.The purity of argon gas used is 99.99%.
Compared with prior art, its remarkable advantage is in the present invention: 1) compared with conventional sintering mode, the sintering temperature that microwave of the present invention burns sintering process is low, and soaking time is short, can greatly enhance productivity, reduce production costs; 2) the microwave sintering method sintering velocity of alumina-titanium carbide micron composite ceramic tool material provided by the invention is fast, can suppress Al
2o
3with TiC reaction, refinement material grains at high temperature, prepare the alumina-titanium carbide micron composite ceramic tool material of excellent property; 3) the present invention proposes a kind of alumina-titanium carbide micron composite ceramic tool material and microwave sintering method thereof are easy to scale production.
Embodiment
A kind of alumina-titanium carbide micron composite ceramic tool material of the present invention, the composition of this material is by mass percentage: submicron ɑ-Al
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3.
Described submicron ɑ-Al
2o
3powder particle particle diameter is 0.5 ~ 0.8 μ m.
Described micron TiC powder particle particle diameter is 1 ~ 3 μ m.
A method for the above-mentioned alumina-titanium carbide micron of microwave sintering composite ceramic tool material, comprises the following steps:
Step 1, batching: submicron ɑ-Al by mass percentage
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3prepare burden;
Step 2, batch mixing; The mixed powder that step 1 is prepared mixes 30 ~ 60h taking dehydrated alcohol as medium ball milling, ball milling post-drying is sieved; Described abrading-ball is aluminum oxide abrading-ball; In batch mixing process, ball material mass ratio is 5:1 ~ 10:1.
Step 3, granulation: will in mixed powder, add polyvinyl alcohol water solution granulation; The concentration of polyvinyl alcohol water solution is 3% ~ 5%.
Step 4, moulding: by dry-pressing formed the powder that granulation is good, pressure is 150 ~ 250MPa, and the dwell time is 1 ~ 5min;
Step 5, binder removal: the blank of step 3 moulding is placed in to microwave agglomerating furnace, open vacuum pump, vacuum in body of heater is evacuated to 0.07MPa ~ 0.09 MPa, then open microwave power supply and heat, blank is heated to 600 DEG C ~ 800 DEG C by the speed of 20 ~ 30 DEG C/min, at this insulation 5 ~ 20min;
Step 6, sintering: after binder removal finishes, vacuum in body of heater is evacuated to 0.004 MPa ~ 0.006MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 30 ~ 40 DEG C/min, be heated to 1600 DEG C ~ 1700 DEG C, at this temperature, be incubated 10 ~ 30min, then furnace cooling makes ceramic cutting tool material.The purity of argon gas used is 99.99%.
Below in conjunction with embodiment, the present invention is done to further detailed description:
Embodiment 1
A method for microwave sintering alumina-titanium carbide micron composite ceramic tool material, is specially: submicron ɑ-Al by mass percentage
2o
3be 55%, a micron TiC is 35%, molybdenum powder and nickel powder are 5%, surplus is MgO and Y
2o
3prepare burden, described submicron ɑ-Al
2o
3powder particle particle diameter is 0.5 μ m, and micron TiC powder particle particle diameter is 1 μ m, and by the mixed powder of preparation, taking dehydrated alcohol as medium ball milling mixing 30h, ball material mass ratio is 5:1; Ball milling post-drying is sieved, and adding concentration is 3% polyvinyl alcohol water solution granulation; By dry-pressing formed the powder that granulation is good, pressure is 150MPa, and the dwell time is 5min; Moulding sample is placed in to microwave agglomerating furnace, opens vacuum pump, vacuum in body of heater is evacuated to 0.07MPa, then open microwave power supply and heat, sample is heated to 600 DEG C by the speed of 20 DEG C/min, be incubated 5min at this.After binder removal finishes, vacuum in body of heater is evacuated to 0.004MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 30 DEG C/min, be heated to 1600 DEG C, at this temperature, be incubated 10min, then cool to room temperature with the furnace.
Can obtain after tested, the density of material is 99%, and Vickers' hardness is 18.86GPa(HV20), fracture toughness is 4.14MPam
1/2, can meet the service requirements of cutter.
Embodiment 2
A method for microwave sintering alumina-titanium carbide micron composite ceramic tool material, is specially: submicron ɑ-Al by mass percentage
2o
3be 60%, a micron TiC is 30%, molybdenum powder and nickel powder are 8%, surplus is MgO and Y
2o
3prepare burden, described submicron ɑ-Al
2o
3powder particle particle diameter is 0.7 μ m, and micron TiC powder particle particle diameter is 2 μ m, and by the mixed powder of preparation, taking dehydrated alcohol as medium ball milling mixing 48h, ball material mass ratio is 8:1; Ball milling post-drying is sieved, and adding concentration is 4% polyvinyl alcohol water solution granulation; By dry-pressing formed the powder that granulation is good, pressure is 200MPa, and the dwell time is 3min; Moulding sample is placed in to microwave agglomerating furnace, opens vacuum pump, vacuum in body of heater is evacuated to 0.08MPa, then open microwave power supply and heat, sample is heated to 700 DEG C by the speed of 25 DEG C/min, be incubated 15min at this.After binder removal finishes, vacuum in body of heater is evacuated to 0.005MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 35 DEG C/min, be heated to 1650 DEG C, at this temperature, be incubated 20min, then cool to room temperature with the furnace.
The density that records material is 99.2%, and Vickers' hardness is 19 GPa(HV20), fracture toughness is 4.63MPam
1/2, can meet the service requirements of cutter.
Embodiment 3
A method for microwave sintering alumina-titanium carbide micron composite ceramic tool material, is specially: submicron ɑ-Al by mass percentage
2o
3be 65%, a micron TiC is 25%, molybdenum powder and nickel powder are 10%, surplus is MgO and Y
2o
3prepare burden, described submicron ɑ-Al
2o
3powder particle particle diameter is 0.8 μ m, and micron TiC powder particle particle diameter is 3 μ m, and by the mixed powder of preparation, taking dehydrated alcohol as medium ball milling mixing 60h, ball material mass ratio is 10:1; Ball milling post-drying is sieved, and adding concentration is 5% polyvinyl alcohol water solution granulation; By dry-pressing formed the powder that granulation is good, pressure is 250MPa, and the dwell time is 1min; Moulding sample is placed in to microwave agglomerating furnace, opens vacuum pump, vacuum in body of heater is evacuated to 0.09MPa, then open microwave power supply and heat, sample is heated to 800 DEG C by the speed of 30 DEG C/min, be incubated 20min at this.After binder removal finishes, vacuum in body of heater is evacuated to 0.006MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 40 DEG C/min, be heated to 1700 DEG C, at this temperature, be incubated 30min, then cool to room temperature with the furnace.
The density that records material is 99.5%, and Vickers' hardness is 19 .5GPa(HV20), fracture toughness is 4.5MPam
1/2, can meet the service requirements of cutter.
As from the foregoing, the microwave sintering method sintering velocity of alumina-titanium carbide micron composite ceramic tool material provided by the invention is fast, can prepare the alumina-titanium carbide micron composite ceramic tool material of excellent property.
Claims (7)
1. an alumina-titanium carbide micron composite ceramic tool material, is characterized in that, the composition of this material is by mass percentage: submicron ɑ-Al
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3.
2. alumina-titanium carbide micron composite ceramic tool material according to claim 1, is characterized in that described submicron ɑ-Al
2o
3powder particle particle diameter is 0.5 ~ 0.8 μ m.
3. alumina-titanium carbide micron composite ceramic tool material according to claim 1, is characterized in that, described micron TiC powder particle particle diameter is 1 ~ 3 μ m.
4. a method for the alumina-titanium carbide micron composite ceramic tool material described in microwave sintering claim 1,2 or 3, is characterized in that, comprises the following steps:
Step 1, batching: submicron ɑ-Al by mass percentage
2o
3be 55% ~ 65%, a micron TiC is 25% ~ 35%, molybdenum powder and nickel powder are 5% ~ 10%, surplus is MgO and Y
2o
3prepare burden;
Step 2, batch mixing; The mixed powder that step 1 is prepared mixes 30 ~ 60h taking dehydrated alcohol as medium ball milling, ball milling post-drying is sieved; Described abrading-ball is aluminum oxide abrading-ball;
Step 3, granulation: will in mixed powder, add polyvinyl alcohol water solution granulation;
Step 4, moulding: by dry-pressing formed the powder that granulation is good, pressure is 150 ~ 250MPa, and the dwell time is 1 ~ 5min;
Step 5, binder removal: the blank of step 3 moulding is placed in to microwave agglomerating furnace, open vacuum pump, vacuum in body of heater is evacuated to 0.07MPa ~ 0.09 MPa, then open microwave power supply and heat, blank is heated to 600 DEG C ~ 800 DEG C by the speed of 20 ~ 30 DEG C/min, at this insulation 5 ~ 20min;
Step 6, sintering: after binder removal finishes, vacuum in body of heater is evacuated to 0.004 MPa ~ 0.006MPa, then pours the argon gas of 0.03MPa, with the heat-up rate of 30 ~ 40 DEG C/min, be heated to 1600 DEG C ~ 1700 DEG C, at this temperature, be incubated 10 ~ 30min, then furnace cooling makes ceramic cutting tool material.
5. the microwave sintering method of alumina-titanium carbide micron composite ceramic tool material according to claim 4, is characterized in that: in step 2, in batch mixing process, ball material mass ratio is 5:1 ~ 10:1.
6. the microwave sintering method of alumina-titanium carbide micron composite ceramic tool material according to claim 4, is characterized in that: in step 3 granulation process, the concentration of polyvinyl alcohol water solution is 3% ~ 5%.
7. the microwave sintering method of alumina-titanium carbide micron composite ceramic tool material according to claim 4, is characterized in that: in step 6, the purity of argon gas used is 99.99%.
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Cited By (6)
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| CN104446482A (en) * | 2014-11-11 | 2015-03-25 | 合肥皖为电气设备工程有限责任公司 | Ceramic for nano titanium carbide cutting tools and preparation method of ceramic |
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| CN105236943A (en) * | 2015-11-13 | 2016-01-13 | 南京理工大学 | A composite Al2O3/Ti (C, N) ceramic cutter material and its microwave sintering tech |
| CN106187259A (en) * | 2016-07-18 | 2016-12-07 | 南京理工大学 | Composite ceramic cutting tool that a kind of graphene nanometer sheet is toughness reinforcing and microwave preparation technology thereof |
| CN106348777A (en) * | 2016-09-04 | 2017-01-25 | 南京理工大学 | Alumina-based composite ceramic knife material and microwave preparation method thereof |
| CN107140974A (en) * | 2017-04-11 | 2017-09-08 | 陕西科技大学 | A kind of unleaded high energy storage density ST NBT ceramic materials of microwave sintering and preparation method thereof |
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| CN106348777A (en) * | 2016-09-04 | 2017-01-25 | 南京理工大学 | Alumina-based composite ceramic knife material and microwave preparation method thereof |
| CN107140974A (en) * | 2017-04-11 | 2017-09-08 | 陕西科技大学 | A kind of unleaded high energy storage density ST NBT ceramic materials of microwave sintering and preparation method thereof |
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Application publication date: 20141105 |