CN102491775B - In-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material and preparation process thereof - Google Patents
In-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material and preparation process thereof Download PDFInfo
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- CN102491775B CN102491775B CN 201110401147 CN201110401147A CN102491775B CN 102491775 B CN102491775 B CN 102491775B CN 201110401147 CN201110401147 CN 201110401147 CN 201110401147 A CN201110401147 A CN 201110401147A CN 102491775 B CN102491775 B CN 102491775B
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Abstract
The invention relates to a ceramic-based composite and a preparation process thereof, in particular to an in-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material and a preparation process thereof. The in-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material comprises the following material compositions in percentage by mass: 25.4 to 38.0 percent of Ta2O5, 4.8 to 7.2 percent of C, 1.7 to 2.5 percent of NaCl, 1.7 to 2.5 percent of Ni and 49.8 to 66.4 percent of Al2O3. The preparation process comprises the following steps of: putting raw materials prepared in a ratio into a jar type ball mill, and performing wet milling by using alumina balls for 24 hours; drying a mixture at the temperature of between 100 and 120 DEGC under vacuum, and sieving with a 100-mesh sieve; putting powder into a graphite container of which the end part is provided with a cover, the lower part is closed and the middle is provided with a plurality of holes, and culturing in-situ growth whiskers in a high-temperature furnace; keeping the temperature at the temperature of between 1,350 and 1,500 DEG C at a heating speed of 100 DEG C/minute under the protection of argon atmosphere for 50 to 80 minutes, and cooling to room temperature at a speed of 20 DEG C/minute to synthesize complex phase powder; and removing residual impurities, pressurizing to 32 MPa at the temperature of 1,600 and 1,800 DEG C under vacuum, keeping the temperature for 15 to 45 minutes, and sintering for forming. The ceramic cutting tool material prepared by a two-step process is uniform in dispersion of the whiskers, high in comprehensive mechanical property, low in cost, environment-friendly and safe, and the process is simple.
Description
One, technical field
The present invention relates to ceramic matric composite and preparation technology thereof, especially a kind of for the preparation of growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material and preparation technology thereof, belong to new material technology field.
Two, background technology
The advanced ceramics cutter material has the hardness height, wear resistance is good, chemical stability is good and advantage such as good high-temperature performance, but its intrinsic fragility has limited its large-scale application.Add a certain amount of whisker with high elastic coefficient and can improve fracture toughness property and the bending strength of ceramic cutting tool material greatly.The technology of the crystal whisker toughened ceramic matric composite of traditional preparation process generally adopts the outside method that a certain amount of whisker adds the mechanical stirring mixing of adding, but have that whisker is expensive, whisker disperses shortcoming such as whisker performance degradation and complex process in inhomogeneous, the high temperature use, and this technology contaminate environment is detrimental to health.
Three, summary of the invention
The objective of the invention is to overcome the defective that existing ceramic cutting tool material preparation technology exists, for the good ceramic cutting tool material of preparation comprehensive mechanical property provides a kind of, can make whisker evenly growth in ceramic matrix material, growth in situ tantalum carbide (TaC) crystal whisker toughened aluminum oxide base ceramics cutting tool material and preparation technology thereof best in quality, that technology is simple, with low cost, safe add crystal whisker toughened ceramic cutting tool material and preparation technology thereof in order to replace tradition.
Basic design of the present invention is with α-Al
2O
3Particle is matrix, adds the required persursor material of whisker growth, adopts certain technology and passes through processing parameters such as control whiskerization temperature, soaking time, and original position generates the tantalum carbide whisker-alumina substrate complex phase ceramic powder with certain mass content.Through behind certain impurity removal process, by control sintering temperature, soaking time and pressure and other parameters, prepare the tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material with higher comprehensive mechanical property.
The starting material of preparation growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material are by α-Al
2O
3The required persursor material of particle and whisker growth is formed, and the quality proportioning of material composition is wt%:Ta
2O
525.4%-38.0%; C 4.8%-7.2%; NaCl 1.7%-2.5%; Ni 1.7%-2.5%; Al
2O
349.8%-66.4%.
Concrete preparation were established is: the starting material that (1) will proportionally prepare are packed in the iar mill, and as ball-milling medium, with alumina balls ball milling 24h, ball material weight ratio is 10: 1 with dehydrated alcohol; (2) compound behind the ball milling is put into vacuum drying oven, adopt 100 mesh sieves screening powder after the drying down at 100-120 ℃; (3) end of packing into of the powder after will screening has lid, below sealing, centre to have in the graphite reaction vessel of porous, and this reaction vessel is put into high temperature sintering furnace carry out the growth in situ whisker and cultivate; (4) be that the protection of 100 ℃/min, argon gas atmosphere, temperature are 1350-1500 ℃ of insulation 50-80min and be cooled to the synthetic complex phase powder that contains tantalum carbide whisker and alumina substrate under the room temperature condition with the rate of cooling of 20 ℃/min down at temperature rise rate; (5) adopt ultrasonic agitation to add the deionized water precipitator method and remove impurity such as sodium-chlor residual in the complex phase powder and carbon black; (6) the complex phase powder after the removal of impurities is incubated the 15-45min sinter molding in vacuum, after being forced into 32MPa under the 1600-1800 ℃ of temperature.
The mass content of the tantalum carbide whisker of technology growth in situ of the present invention (including a spot of tantalum carbide particle) in aluminum oxide base ceramics cutting tool material is: 25%-40%.The bending strength of the growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material after synthetic is 485-638MPa, and fracture toughness property is 5.82-6.47MPam
1/2, Vickers' hardness is 17.0-17.4GPa.
The present invention is novel, has the growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material of higher comprehensive mechanical property by the growth of tantalum carbide whisker in-situ and the powder sintered two step process preparation of complex phase.This technology has that whisker is uniformly dispersed, technology is simple, advantage such as good, the with low cost and environmental protection of synthesis material quality, safety.
Four, embodiment:
Being mixed with starting material by listed composition in the embodiment parameter subordinate list, in the iar mill of packing into, is ball-milling medium with the dehydrated alcohol, and with alumina balls ball milling 24h, ball material weight ratio is 10: 1; Sieve with 100 mesh sieves after the drying down at 100-120 ℃; The end of packing into has the sealing of lid, below, centre to have in the graphite reaction vessel of porous, again graphite reaction vessel is put into high temperature sintering furnace; Temperature rise rate is 100 ℃/min, argon gas atmosphere protection; undertaken that whisker is cultivated and be cooled to the synthetic complex phase powder that contains tantalum carbide whisker and alumina substrate under the room temperature condition with the rate of cooling of 20 ℃/min by the parameter in the embodiment parameter subordinate list; again after ultrasonic agitation adds the deionized water precipitator method and removes impurity such as residual sodium-chlor and carbon black, with the complex phase powder in vacuum, press the parameter sinter molding in the embodiment parameter subordinate list.
Embodiment parameter subordinate list
The bending strength of the growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material after synthetic is 485-638MPa, and fracture toughness property is 5.82-6.47MPam
1/2, Vickers' hardness is 17.0-17.4GPa.
Claims (1)
1. the preparation technology of growth in situ tantalum carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material is characterized in that composition of raw material quality proportioning is wt%:Ta
2O
525.4%-38.0%; C4.8%-7.2%; NaCl1.7%-2.5%; Ni1.7%-2.5%; Al
2O
349.8%-66.4%; Preparation process: the starting material that (1) will proportionally prepare are packed in the iar mill, and as ball-milling medium, with alumina balls ball milling 24h, ball material weight ratio is 10:1 with dehydrated alcohol; (2) compound behind the ball milling is put into vacuum drying oven, adopt 100 mesh sieves screening powder after the drying down at 100-120 ℃; (3) end of packing into of the powder after will screening has lid, below sealing, centre to have in the graphite reaction vessel of porous, and this reaction vessel is put into high temperature sintering furnace carry out the growth in situ whisker and cultivate; (4) be that the protection of 100 ℃/min, argon gas atmosphere, temperature are 1350-1500 ℃ of insulation 50-80min and be cooled to the synthetic complex phase powder that contains tantalum carbide whisker and alumina substrate under the room temperature condition with the rate of cooling of 20 ℃/min down at temperature rise rate; (5) adopt ultrasonic agitation to add the deionized water precipitator method and remove residual sodium-chlor and carbon black impurity in the complex phase powder; (6) the complex phase powder after the removal of impurities is incubated the 15-45min sinter molding in vacuum, after being forced into 32MPa under the 1600-1800 ℃ of temperature.
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| CN 201110401147 CN102491775B (en) | 2011-12-06 | 2011-12-06 | In-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material and preparation process thereof |
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| CN 201110401147 CN102491775B (en) | 2011-12-06 | 2011-12-06 | In-situ growth tantalum carbide whisker toughened alumina-based ceramic cutting tool material and preparation process thereof |
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| CN102491775B true CN102491775B (en) | 2013-07-03 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054290A (en) * | 2006-04-14 | 2007-10-17 | 山东大学 | In-situ growth titanium carbonitride crystal whisker toughened aluminum oxide base ceramics cutting tool material powder and preparation technique thereof |
| CN101058503A (en) * | 2006-04-17 | 2007-10-24 | 山东大学 | In-situ growth titanium carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material powder and preparation technique thereof |
| CN101723367A (en) * | 2009-12-23 | 2010-06-09 | 北京科技大学 | Method for preparing powder of nanometer tantalum carbide |
| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054290A (en) * | 2006-04-14 | 2007-10-17 | 山东大学 | In-situ growth titanium carbonitride crystal whisker toughened aluminum oxide base ceramics cutting tool material powder and preparation technique thereof |
| CN101058503A (en) * | 2006-04-17 | 2007-10-24 | 山东大学 | In-situ growth titanium carbide crystal whisker toughened aluminum oxide base ceramics cutting tool material powder and preparation technique thereof |
| CN101723367A (en) * | 2009-12-23 | 2010-06-09 | 北京科技大学 | Method for preparing powder of nanometer tantalum carbide |
| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
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