CN105503197A - Preparation method of zirconium nitride reinforced aluminum oxynitride composite ceramic material - Google Patents
Preparation method of zirconium nitride reinforced aluminum oxynitride composite ceramic material Download PDFInfo
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- CN105503197A CN105503197A CN201410498729.6A CN201410498729A CN105503197A CN 105503197 A CN105503197 A CN 105503197A CN 201410498729 A CN201410498729 A CN 201410498729A CN 105503197 A CN105503197 A CN 105503197A
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Abstract
The invention relates to a preparation method of a zirconium nitride reinforced aluminum oxynitride composite ceramic material. The preparation method consists of: batching, ultrasonic dispersion of nano-zirconia powder, preparation of a mixed slurry composed of aluminum nitride and zirconia, preparation of mixed powder composed of aluminum oxynitride and zirconia, and preparation of the zirconium nitride reinforced aluminum oxynitride composite ceramic material. The zirconium nitride reinforced aluminum oxynitride ceramic material prepared by the method has the characteristic of high bending strength.
Description
Technical field
The present invention relates to the preparation method of the high performance zirconium-nitride enhanced aluminum-oxynitride composite ceramic material of a kind of technical field of inorganic nonmetallic materials.
Background technology
γ-aluminum oxynitride spinel (Alon) is the solid-solution ceramic materials of a kind of more stable aluminum oxide and aluminium nitride.Because it has excellent optics, physics and chemistry character, receive extensive concern at Material Field.Aluminum oxynitride material is not only a kind of desirable high-temperature structural ceramics and advanced refractory materials, and the preferred material of high-purity, fine and close aluminum oxynitride material or a kind of high temperature resistant infrared window and head-shield.Conventional preparation method mainly comprises normal pressure-sintered, hot pressed sintering and reaction sintering.Wherein, normal pressure-sintered is in sintering process, and sintered body is placed in heatable kiln, under heat energy effect under normal pressure (i.e. natural atmosphere condition), make base substrate become crystal grain combination by powder aggregates, porous insert becomes the preparation technology of DB.Hot pressed sintering a kind ofly in mould, applies pressure, the preparation technology simultaneously heated up to compared with the powder of hard-to-sinter or green compact.Reaction sintering is a kind of preparation technology along with solid phase, liquid phase or gas-phase reaction in a kind of process sintering.No matter be normal pressure-sintered or hot pressed sintering, or reaction sintering method, the bending strength of the aluminium oxynitride stupalith obtained is on the low side, can not meet the demand that modern science and technology develops rapidly.For many years, in order to improve and improve the mechanical property of aluminium oxynitride stupalith further, many research workers by adding the second-phases such as boron nitride, Sai Long, silicon carbide respectively, to strengthen the mechanical property of aluminium oxynitride base ceramic material in aluminium oxynitride matrix.But, DeGrain up to now.
Main purpose of the present invention take zirconium nitride as wild phase, the aluminium oxynitride stupalith that preparation mechanical property is higher.Not yet there is any report prepared about zirconium-nitride enhanced aluminum-oxynitride composite ceramic material at present.Thus the present invention has promoter action to applying of aluminium oxynitride stupalith.
Summary of the invention
Main purpose of the present invention is to provide a kind of preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material, and zirconium nitride prepared by the method strengthens aluminium oxynitride stupalith and has the high feature of bending strength.
The object of the present invention is achieved like this: the preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material
:
1, prepare burden: raw material is aluminium oxynitride and Zirconium powder.Wherein the mass percent of aluminium oxynitride is 80,8%, and zirconic mass percent is that 2 (T2%, utilizes precision electronic balance to take appropriate powder respectively according to mentioned component proportioning, stand-by.Weigh appropriate ethanolic soln again, stand-by.
2, ultrasonic disperse nano zirconium oxide powder: above-mentioned load weighted Zirconium powder is put into the beaker of certain capacity, pour appropriate ethanolic soln again into, carry out supersound process to it, the time of ultrasonic disperse is 2 15 minutes, can zirconia solution be obtained, stand-by.
3, the mixed slurry of aluminium oxynitride and zirconium white formation is prepared: pour in ball grinder by above-mentioned load weighted aluminum oxynitride powder, then in this ball grinder, scattered zirconia solution is poured into, finally pour ethanol in proper amount solution into, after stirring with glass stick, put into zirconium oxide balls again, the ratio of the total mass of the total mass of zirconium oxide balls and feed oxygen aluminium nitride and zirconium white mixed powder is 4 5:1, capping, ball milling is after 12 48 hours, the mixed slurry be made up of aluminium oxynitride and zirconium white can be obtained, stand-by.
4, the mixed powder of aluminium oxynitride and zirconium white formation is prepared: by the above-mentioned oxygen nitrogen obtained
changealuminium and zirconium white mixed slurry are in 6 (the baking oven inner drying process 12 48 of T100 degree Celsius
hour,and milled processed is carried out to the mixed powder of drying, the mixed powder mixed be made up of aluminium oxynitride and zirconium white can be obtained.
5, prepare aluminium nitride and strengthen aluminium oxynitride composite ceramic material: the above-mentioned ground mixed powder be made up of aluminium oxynitride and zirconium white is put into graphite grinding tool; and carried out first pressing forming processes; then put it in hot-pressed sintering furnace; first with vacuum pump, the air in hot pressing furnace is extracted out before heating; pass into nitrogen again as shielding gas, carry out in a nitrogen atmosphere sintering and prepare aluminium nitride enhancing aluminium oxynitride composite ceramic material.Wherein, sintering temperature is 17001900 degrees Celsius, and soaking time is that 2 (T90 minute, heat-up rate is per minute 5 30 degrees Celsius, and institute's plus-pressure is 1 (T40 MPa at a sintering temperature.
The present invention for raw material, under nitrogen atmosphere, makes zirconium white original position generation chemical reaction be transformed into zirconium nitride with aluminum oxynitride powder and Zirconium powder, and the preparation method utilizing hot pressing and reaction sintering to combine obtains zirconium nitride and strengthens aluminium oxynitride composite ceramics
material.due to second-phase nitrogen
changezirconium grain boundary sites be uniformly distributed and in sintering process to the inhibition of crystal boundary movement, effectively inhibit growing up of crystal grain, serve the effect of crystal grain thinning.Zirconium-nitride enhanced aluminum-oxynitride composite ceramic material prepared by the method significantly reduces sintering temperature, improves the bending strength of material.
Embodiment
Embodiment 1
Aluminium nitride strengthens the preparation of aluminium oxynitride composite ceramic material
:
Batching: weigh micron aluminum oxynitride powder 85 grams respectively stand-by with nano zirconium oxide powder 15 grams; Weigh ethanol in proper amount solution again, stand-by.
Ultrasonic disperse nano zirconium oxide powder: the beaker above-mentioned load weighted nm-class powder of zirconium oxide being put into 50 milliliters, then pour ethanol in proper amount solution into, ultrasonic disperse 5 minutes, can obtain zirconia solution, stand-by.
Prepare the mixed slurry that aluminium oxynitride and zirconium white are formed: by above-mentioned oneself pour in ball grinder through load weighted aluminum oxynitride powder, then in this ball grinder, scattered nano oxidized zirconium solution is poured into, finally pour ethanol in proper amount solution into, after stirring with glass stick, then put into 500 grams
'szirconium oxide balls, capping, ball milling 24
hour,can obtain by oxygen nitrogen
changethe mixed slurry that aluminium and zirconium white are formed, stand-by.
systemstandby oxygen nitrogen
changethe mixed powder that aluminium and zirconium white are formed: by the above-mentioned own oxygen nitrogen through obtaining
changealuminium and zirconium white mixed slurry carry out drying treatment 24 in the baking oven of 80 degrees Celsius
hour,and milled processed is carried out to the mixed powder of drying, the mixed powder mixed be made up of aluminium oxynitride and zirconium white can be obtained.
Prepare zirconium-nitride enhanced aluminum-oxynitride composite ceramic material: the above-mentioned ground mixed powder be made up of aluminium oxynitride and zirconium white is put into graphite grinding tool; and carried out first pressing forming processes; then put it in hot-pressed sintering furnace; first with vacuum pump, the air in hot pressing furnace is extracted out before heating; pass into nitrogen again as shielding gas; sintering temperature is 1800 degrees Celsius; soaking time is 70 minutes; heat-up rate is per minute 10 degrees Celsius; institute's plus-pressure is 35 MPas at a sintering temperature, has sintered rear sample furnace cooling.
Embodiment 2
Aluminium nitride strengthens the preparation of aluminium oxynitride composite ceramic material
:
Batching: weigh micron aluminum oxynitride powder 175 grams respectively and weigh ethanol in proper amount solution for later use again with nano zirconium oxide powder 25 grams is stand-by.
Ethanol in proper amount solution ultrasonic disperse poured again into by the beaker that above-mentioned load weighted nm-class powder of zirconium oxide is put into 100 milliliters by ultrasonic disperse nano zirconium oxide powder, and within 5 minutes, can to obtain zirconia solution stand-by.
Prepare the mixed slurry of aluminium oxynitride and zirconium white formation: pour in ball grinder by above-mentioned load weighted aluminum oxynitride powder, then in this ball grinder, scattered nano oxidized zirconium solution is poured into, finally pour ethanol in proper amount solution into, after stirring with glass stick, put into the zirconium oxide balls of 900 grams again, capping, ball milling 36 hours, the mixed slurry be made up of aluminium oxynitride and zirconium white can be obtained, stand-by.
Prepare mixed powder that aluminium oxynitride and zirconium white form and the above-mentioned aluminium oxynitride that obtained and zirconium white mixed slurry are carried out drying treatment 36 hours in the baking oven of 70 degrees Celsius, and milled processed is carried out to the mixed powder of drying, the mixed powder mixed be made up of aluminium oxynitride and zirconium white can be obtained.
Prepare zirconium-nitride enhanced aluminum-oxynitride composite ceramic material and the above-mentioned ground mixed powder be made up of aluminium oxynitride and zirconium white is put into graphite grinding tool; and carried out first pressing forming processes; then put it in hot-pressed sintering furnace; first with vacuum pump, the air in hot pressing furnace is extracted out before heating; pass into nitrogen again as shielding gas; sintering temperature is 1900 degrees Celsius; soaking time is 30 minutes; heat-up rate is per minute 10 degrees Celsius; institute's plus-pressure is 20 MPas at a sintering temperature, has sintered rear sample furnace cooling.
Claims (1)
1. a preparation method for zirconium-nitride enhanced aluminum-oxynitride composite ceramic material, is characterized in that: preparation method is: (1), batching: raw material is aluminium oxynitride and Zirconium powder; Wherein the mass percent of aluminium oxynitride is 80,8%, and zirconic mass percent is that 2 (T2%, utilizes precision electronic balance to take appropriate powder respectively according to mentioned component proportioning, stand-by; Weigh appropriate ethanolic soln again, stand-by; (2), ultrasonic disperse nano zirconium oxide powder: above-mentioned load weighted Zirconium powder is put into the beaker of certain capacity, pour appropriate ethanolic soln again into, carry out supersound process to it, the time of ultrasonic disperse is 2 15 minutes, can zirconia solution be obtained, stand-by; (3) mixed slurry of aluminium oxynitride and zirconium white formation, is prepared: pour in ball grinder by above-mentioned load weighted aluminum oxynitride powder, then in this ball grinder, scattered zirconia solution is poured into, finally pour ethanol in proper amount solution into, after stirring with glass stick, put into zirconium oxide balls again, the ratio of the total mass of the total mass of zirconium oxide balls and feed oxygen aluminium nitride and zirconium white mixed powder is 4 5:1, capping, ball milling is after 12 48 hours, the mixed slurry be made up of aluminium oxynitride and zirconium white can be obtained, stand-by; (4) mixed powder that aluminium oxynitride and zirconium white are formed, is prepared: by the above-mentioned aluminium oxynitride that obtained and zirconium white mixed slurry in 6 (the baking oven inner drying process of T100 degree Celsius 12 48 hours, and milled processed is carried out to the mixed powder of drying, the mixed powder mixed be made up of aluminium oxynitride and zirconium white can be obtained; (5), prepare aluminium nitride and strengthen aluminium oxynitride composite ceramic material: the above-mentioned ground mixed powder be made up of aluminium oxynitride and zirconium white is put into graphite grinding tool, and carried out first pressing forming processes, then put it in hot-pressed sintering furnace, first with vacuum pump, the air in hot pressing furnace is extracted out before heating, pass into nitrogen again as shielding gas, carry out in a nitrogen atmosphere sintering and prepare aluminium nitride enhancing aluminium oxynitride composite ceramic material; Wherein, sintering temperature is 1700 ~ 1900 degrees Celsius, soaking time is that 2 (T90 minute, heat-up rate is per minute 5 30 degrees Celsius, and institute's plus-pressure is the making method handkerchief of a kind of watermelon health-care wine of making method of 10 40 million 1 kinds of watermelon health-care wines at a sintering temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540429A (en) * | 2019-08-29 | 2019-12-06 | 南充三环电子有限公司 | aluminum nitride sintered body and application |
| CN115650730A (en) * | 2022-05-31 | 2023-01-31 | 广东工业大学 | Aluminum nitride ceramic substrate and preparation method and application thereof |
-
2014
- 2014-09-26 CN CN201410498729.6A patent/CN105503197A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540429A (en) * | 2019-08-29 | 2019-12-06 | 南充三环电子有限公司 | aluminum nitride sintered body and application |
| CN110540429B (en) * | 2019-08-29 | 2022-06-14 | 南充三环电子有限公司 | Aluminum nitride sintered body and application |
| CN115650730A (en) * | 2022-05-31 | 2023-01-31 | 广东工业大学 | Aluminum nitride ceramic substrate and preparation method and application thereof |
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