CN104163630B - A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito - Google Patents
A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito Download PDFInfo
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- CN104163630B CN104163630B CN201410381862.3A CN201410381862A CN104163630B CN 104163630 B CN104163630 B CN 104163630B CN 201410381862 A CN201410381862 A CN 201410381862A CN 104163630 B CN104163630 B CN 104163630B
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Abstract
The invention discloses the first nano composite ceramic mould of a kind of aluminum oxide and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 60-80 part, aluminum oxide 10-20 part, titanium carbide 10-20 part, silicon nitride 15-25 part, yttrium oxide 2-6 part, hafnium boride 4-8 part, chromium 2-4 part, cobalt 1-3 part, manganese 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering.This mould resistance to deterioration and defect support ability by force, have good comprehensive mechanical property and excellent properties of antifriction and wear resistance.
Description
Technical field
The present invention relates to a kind of ceramic die material, specifically a kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito.
Background technology
Sintex has high hardness and wear resistance, and showing excellent cutting ability when high speed cutting and dry cutting, is the cutter material that a class has development prospect.But the ceramic cutting tool material of application is at present confined to a micron composite ceramics mostly, and especially intensity, toughness still await further raising to the mechanical property of material.According to Hall-petch relation: grain-size is less, the intensity of stupalith is higher.Therefore, the research and development of nano modification, nano-micrometre composite ceramic tool material one of the Main way that will be cutter material development from now on.
Current nano composite ceramic cutter material after deliberation mainly comprises Si
3n
4/ TiNn, Si
3n
4/ TiCn, Si
3n
4-Ai
2o
3n-TiC-Y
2o
3, Al
2o
3/ TiC/SiCn, Al
2o
3/ TiCn, Al
2o
3/ Al
2o
3n/SiCn, Al
2o
3/ Ti (C
0.7n
0.3) n/SiCn, Al
2o
3/ SiC/SiCn, Al
2o
3/ TiC/TiNn, etc., all have than the better mechanical property of micron composite ceramic tool material and cutting ability.But up to the present, not yet find with zirconium boride ceramic the report of the nano composite ceramic cutter material being matrix.
On the other hand, thermostability and the wear resistance of stupalith are splendid, are the ideal materials manufacturing shaping dies, have development prospect very much, but its toughness are very poor, are not therefore also used widely in mould industry.From status both at home and abroad, the research of ceramic die is still in the research and development stage, and little, the applicable mould applications of kind being applied to the stupalith of mould industry is very narrow, and the report of this respect is also few.At present, the applied research of stupalith in all kinds of mould is confined to a micron composite ceramic material, mostly as ZrO
2toughness reinforcing Al
2o
3base composite ceramic ZTA wortle, TZP/TiC/Al
2o
3, Al
2o
3/ TiC composite ceramics wortle, (Ce-TZP)-Al
2o
3hot-extrusion mold, 3Y-TZP-Al
2o
3pottery drawing die, PSZ pottery hot extruding die, Al
2o
3/ Cr
3c
2/ (W, Ti) C etc.Although nano composite ceramic is less in the research of moulding stock application aspect, as compound UP ceramic die, Al
2o
3/ Ti (C, N) etc., but also achieve good effect.
As can be seen from existing research, performance, the price advantage of nano combined especially nano-micron compound pottery could not be not fully exerted in mould applications.With regard to current general status, the kind of ceramic die material, performance and application scope all await expanding further and improving.
Summary of the invention
The object of the present invention is to provide the first nano composite ceramic mould of a kind of aluminum oxide and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, this mould resistance to deterioration and defect support ability by force, have good comprehensive mechanical property and excellent properties of antifriction and wear resistance.
For achieving the above object, the invention provides following technical scheme:
A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 60-80 part, aluminum oxide 10-20 part, titanium carbide 10-20 part, silicon nitride 15-25 part, yttrium oxide 2-6 part, hafnium boride 4-8 part, chromium 2-4 part, cobalt 1-3 part, manganese 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium boride 99.5004323A8ure, aluminum oxide, titanium carbide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the first suspension simultaneously;
Step 3: yttrium oxide, hafnium boride, chromium, cobalt and manganese are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the second suspension simultaneously;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with rare gas element, take dehydrated alcohol as medium, and diameter is the iron ball of 1-2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: by lapping liquid vacuum-drying at 110-120 DEG C of temperature, sieve in inert gas flow after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
As the further scheme of the present invention: described aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 65-75 part, aluminum oxide 14-16 part, titanium carbide 14-16 part, silicon nitride 18-22 part, yttrium oxide 3-5 part, hafnium boride 5-7 part, chromium 2.5-3.5 part, cobalt 1.5-2.5 part.
As the further scheme of the present invention: described in step 2 and step 3, the volume ratio of dehydrated alcohol and polyoxyethylene glycol is 1: 0.5-2.
As the further scheme of the present invention: described in step 5 and step 6, rare gas element is nitrogen or rare gas.
As the further scheme of the present invention: in step 7, pressure sintering sintering process parameter is: heating-up time 20-30min, holding temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, soaking time 40-60min, be then cooled to room temperature.
Compared with prior art, the invention has the beneficial effects as follows: polynary nanometer composite ceramic die of the present invention, by adding nano aluminium oxide in nanometer zirconium boride 99.5004323A8ure matrix, nano titanium carbide and nano-silicon nitride realize the nano combined of different-grain diameter as wild phase, adding of nano titanium carbide and nano-silicon nitride, typical intracrystalline/intergranular hybrid architecture can be defined with nanometer zirconium boride 99.5004323A8ure, cause along crystalline substance/transcrystalline mixed-mode crack pattern thus, the multiple toughening and strengthening such as these strengthened mechanism and zirconium boride 99.5004323A8ure transformation toughening act synergistically, common mechanical property and the use properties improving material, and research shows: yttrium oxide and hafnium boride add as the compound of stablizer, material is not only made to have quite high resistance to deterioration and defect resistivity, and crystal grain phase transformation critical size is larger, requires lower to material fineness, thus make material have good over-all properties.Finally, utilize the little abrading-ball of metallic, what occur after metal is subject to microwave exposure is dissipated in whole reaction system micro-wave reflection and refraction, serves the effect of microwave heating, can accelerated reaction carry out.Compared with existing ceramic die material, this polynary nanometer composite ceramic die material has better comprehensive mechanical property and excellent properties of antifriction and wear resistance, can be used for making potter's moulds such as overflow mould, drawing die and cutting tool.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 60 parts, 10 parts, aluminum oxide, titanium carbide 10 parts, silicon nitride 15 parts, yttrium oxide 2 parts, hafnium boride 4 parts, chromium 2 parts, cobalt 1 part, 1 part, manganese; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium boride 99.5004323A8ure, aluminum oxide, titanium carbide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 3: yttrium oxide, hafnium boride, chromium, cobalt and manganese are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 10 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with nitrogen, take dehydrated alcohol as medium, and diameter is the iron ball of 1mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10;
Step 6: by lapping liquid vacuum-drying at 110 DEG C of temperature, sieve in stream of nitrogen gas after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The processing parameter of pressure sintering sintering: heating-up time 20min, holding temperature 1400 DEG C, hot pressing pressure 30MPa, soaking time 40min, be then cooled to room temperature.
Embodiment 2
A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 70 parts, 15 parts, aluminum oxide, titanium carbide 15 parts, silicon nitride 20 parts, yttrium oxide 4 parts, hafnium boride 6 parts, chromium 3 parts, cobalt 2 parts, 2 parts, manganese; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium boride 99.5004323A8ure, aluminum oxide, titanium carbide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 25 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 3: yttrium oxide, hafnium boride, chromium, cobalt and manganese are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 25 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 15 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with nitrogen, take dehydrated alcohol as medium, and diameter is the iron ball of 1.5mm is mill ball, and under the microwave environment of 2450MHz, ball milling 18 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 15;
Step 6: by lapping liquid vacuum-drying at 115 DEG C of temperature, sieve in stream of nitrogen gas after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The processing parameter of pressure sintering sintering: heating-up time 25min, holding temperature 1500 DEG C, hot pressing pressure 35MPa, soaking time 50min, be then cooled to room temperature.
Embodiment 3
A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 80 parts, 20 parts, aluminum oxide, titanium carbide 20 parts, silicon nitride 25 parts, yttrium oxide 6 parts, hafnium boride 8 parts, chromium 4 parts, cobalt 3 parts, 3 parts, manganese; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium boride 99.5004323A8ure, aluminum oxide, titanium carbide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 30 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 3: yttrium oxide, hafnium boride, chromium, cobalt and manganese are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 30 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 20 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with argon gas, take dehydrated alcohol as medium, and diameter is the iron ball of 2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 24 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 20;
Step 6: by lapping liquid vacuum-drying at 120 DEG C of temperature, sieve in an argon stream after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The processing parameter of pressure sintering sintering: heating-up time 30min, holding temperature 1600 DEG C, hot pressing pressure 40MPa, soaking time 60min, be then cooled to room temperature.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. the preparation method of an aluminum oxide and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito unit nano composite ceramic mould, it is characterized in that, described aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 60-80 part, aluminum oxide 10-20 part, titanium carbide 10-20 part, silicon nitride 15-25 part, yttrium oxide 2-6 part, hafnium boride 4-8 part, chromium 2-4 part, cobalt 1-3 part, manganese 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium boride 99.5004323A8ure is 10-100 nanometer, and the footpath grain size of aluminum oxide, titanium carbide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium boride 99.5004323A8ure as matrix, adds aluminum oxide and titanium carbide and silicon nitride as wild phase, with yttrium oxide and hafnium boride for stablizer, using chromium, cobalt and manganese as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium boride 99.5004323A8ure, aluminum oxide, titanium carbide and silicon nitride and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the first suspension simultaneously;
Step 3: yttrium oxide, hafnium boride, chromium, cobalt and manganese are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the second suspension simultaneously;
Step 4: by the first suspension and the mixing of the second suspension, then fully stir, ultrasonic disperse 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with rare gas element, take dehydrated alcohol as medium, and diameter is the iron ball of 1-2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: by lapping liquid vacuum-drying at 110-120 DEG C of temperature, sieve in inert gas flow after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
2. the preparation method of aluminum oxide according to claim 1 and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito unit nano composite ceramic mould, it is characterized in that, described aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito, according to the raw material of weight part be: zirconium boride 99.5004323A8ure 65-75 part, aluminum oxide 14-16 part, titanium carbide 14-16 part, silicon nitride 18-22 part, yttrium oxide 3-5 part, hafnium boride 5-7 part, chromium 2.5-3.5 part, cobalt 1.5-2.5 part, manganese 1.5-2.5 part.
3. the preparation method of aluminum oxide according to claim 1 and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito unit nano composite ceramic mould, is characterized in that, described in step 2 and step 3, the volume ratio of dehydrated alcohol and polyoxyethylene glycol is 1: 0.5-2.
4. the preparation method of aluminum oxide according to claim 1 and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito unit nano composite ceramic mould, is characterized in that, described in step 5 and step 6, rare gas element is nitrogen or rare gas.
5. the preparation method of aluminum oxide according to claim 1 and titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito unit nano composite ceramic mould, it is characterized in that, in step 7, pressure sintering sintering process parameter is: heating-up time 20-30min, holding temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, soaking time 40-60min, is then cooled to room temperature.
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| CN105734386B (en) * | 2016-01-11 | 2017-12-08 | 东莞市松湖科技有限公司 | A kind of zirconium diboride composite ceramic material and preparation method thereof |
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| CN101164963A (en) * | 2007-09-26 | 2008-04-23 | 山东轻工业学院 | Micro-nano composite ceramic die material and preparation method thereof |
| CN101767989A (en) * | 2009-10-26 | 2010-07-07 | 山东轻工业学院 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
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| CN101164963A (en) * | 2007-09-26 | 2008-04-23 | 山东轻工业学院 | Micro-nano composite ceramic die material and preparation method thereof |
| CN101767989A (en) * | 2009-10-26 | 2010-07-07 | 山东轻工业学院 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
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