CN1304903A - Process for preparing high-toughness alumina ceramics - Google Patents
Process for preparing high-toughness alumina ceramics Download PDFInfo
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- CN1304903A CN1304903A CN 00136835 CN00136835A CN1304903A CN 1304903 A CN1304903 A CN 1304903A CN 00136835 CN00136835 CN 00136835 CN 00136835 A CN00136835 A CN 00136835A CN 1304903 A CN1304903 A CN 1304903A
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Abstract
A high-toughness alumina ceramics is prepared from Al(OH)3 and AlOOH through wet ball grinding with alpha-Al2O balls and deionized water, drying, calcining in muffle furnace, adding alcohol, ball grinding, shaping, vacuum high-pressure calcining. Its advantages are low cost, easy control of process and high toughness and strength of the ceramics.
Description
The present invention relates to a kind of novel method for preparing high-toughness alumina ceramics, belong to technical field of material.
Alumina ceramic material is because of having excellent mechanical property and electrical property, and low cost of manufacture; Therefore be present most widely used a kind of advanced ceramics material.Adopt high purity submicron order ultra-fine alumina powder can prepare bending resistance by force up to the aluminum oxide high technology ceramics of 700～1000MPa.Yet the fracture toughness property of alumina ceramic material is very low, has only 3MPam usually
1/2Therefore, improve the target that the aluminium oxide ceramics fracture toughness is ceramic material scientist expectation and effort always.
In order to improve the fracture toughness property of alumina-ceramic, people grow second phase with toughening effect by adding a little auxiliary in the sintering process of aluminum oxide.As people such as the I-w Cheng of Michigan, United States university successfully in alumina sintering original position grow LaAl with tabular crystal formation
11O
18And LaMgAl
11O
19Toughness reinforcing phase makes this alumina-based ceramic material fracture toughness property reach 4.4MPam
1/2The people such as Japan Masaki Yasuoka are by adding the SiO of hundreds of ppm
2Auxiliary agent can be induced
Al
2O
3The matrix anisotropic grain growth goes out long column shape and tabular crystalline substance.They are with the high-purity Al of commerce
2O
3Synthetic LaAlO
3With silicon sol as initial feed, in 1600 ℃ of high temperature sinterings, growth in situ goes out to have simultaneously α-Al after the low temperature calcination
2O
3Long column shape and LaAl
11O
18Tabular crystalline substance, its bending strength is 600MPa, the tough 5.6MPam of reaching ruptures
1/2In sum, the method that improves at present aluminium oxide toughness mainly is the toughness reinforcing phase that has tabular crystalline form by growing in alumina substrate.A kind of Al
2O
3The complex phase ceramic of base.
The object of the invention proposes a kind of new method for preparing high-toughness alumina ceramics, and its principle is different from existing method.Not by adding sintering aid, but by introducing α-Al
2O
3Crystal seed is induced other Al
2O
3The long column shape alumina grain of (or claiming bar-shaped) is grown, grown to crystal grain anisotropy (mainly along the C axle) direction.These bar-like grains disperses are distributed in the normal Al of axle shapes such as being
2O
3Among the crystal grain.Because bar-shaped Al
2O
3Crystalline substance has crackle to be compiled and to turn to and transfer to effect, thus but the fracture toughness of Effective Raise material.
The preparation method of high-toughness alumina ceramics of the present invention comprises following each step:
1, initial ceramic raw material adopts three water aluminium compounds [Al (OH)
3] or boehmite [AlOOH], with α-Al
2O abrading-ball and deionized water are put into together ball grinder and carried out wet ball grinding, and addition is: ceramic raw material: the aluminium oxide abrading-ball: deionized water=1: 2-6: 1-2, Ball-milling Time are 30-90 hour; α-Al in mechanical milling process
2O
3α-Al that the abrading-ball surface is ground
2O
3Fine grained is as Al
2O
3Crystal seed is introduced.Crystal seed introducing amount is that 15-50wt% is (with Al (OH)
3Be base), can control α-Al by changing Ball-milling Time
2O
3Crystal seed introducing amount.
2, the mixed slurry behind the wet ball grinding after drying, calcination in high temperature Muffle furnace (1100-1300 ℃) makes three water aluminium compounds or boehmite change Al into
2O
3Crystalline phase.
3, the Al that obtains after the calcination
2O
3Material adds alcohol and carries out ball milling again, and Ball-milling Time is 10-20 hour, makes block material fully levigate.
4, the Al behind the ball milling
2O
3The powder drying is for subsequent use.
5, with the above-mentioned α-Al that introduced
2O
3The Al of crystal seed
2O
3The powder moulding, vacuum heating-press sintering then, sintering temperature is 1500～1650 ℃, temperature retention time namely got ceramic material of the present invention at 1～4 hour.α-Al in the sintering process
2O
3Crystal seed is induced part A l
2O
3Development growth is bar-shaped crystalline substance, is had simultaneously bar-shaped crystal alumina and the microstructure that waits axle shape crystal alumina, and this microstructure is given the aluminium oxide ceramics high-fracture toughness.
The advantage of the inventive method is:
1) initial feed adopts industrial gibbsite mineral or boehmite, low, the aboundresources of raw materials cost.
2) introducing of crystal seed is by α-Al in mechanical milling process
2O
3Wearing and tearing on abrading-ball surface when abrading-ball and former abrasive lapping and introducing, thereby technology is simple, is convenient to control.
3) under the condition that crystal seed exists, gibbsite mineral or boehmite can change Al into fully at 1100～1200 ℃
2O
3Crystalline phase, phase inversion temperature is lower.
4) behind the hot pressed sintering, alumina ceramic material has higher fracture toughness property (61～7.1 MPam simultaneously
1/2) and higher intensity (610～660MPa).
Introduce embodiments of the invention below:
Embodiment 1
Get industrial three water aluminum compound Al (OH)
3Powder 500 grams, the powder median size is 2.84 microns, purity is 98%.Alumina balls are 1500 grams, and its purity is 99.9%, and directly through being about 1 centimetre, other removes ionized water 600 grams, puts into together and carries out wet ball grinding in the alumina balls grinding jar 48 hours, and slip is separated with abrading-ball.Dry putting into drying box with slip behind the abrading-ball wash clean.To the Al behind the ball milling
2O
3Abrading-ball is weighed, and learns that abrading-ball weighs 1380 grams, and 120 gram α-Al are namely arranged
2O
3Be incorporated into Al (OH) as crystal seed
3In the powder, α-Al
2O
3Crystal seed is Al (OH)
3The 24wt% of weight.To contain α-Al
2O
3The Al of crystal seed (OH)
3Powder calcination 2 hours in 1150 ℃ of high temperature furnaces makes Al (OH)
3Change Al into
2O
3Again with the powder after the calcination with ethanol ball milling 17 hours, powder is scatter, dry then, vaporized alcohol is obtained fine powder, with powder dry-pressing formed be the garden bulk of 10 millimeters of 50 ≌, in vacuum hotpressing stove, carry out high temperature sintering in 1550 ℃ of down insulations 2 hours, pressure is 40MPa.Alumina-ceramic behind the sintering is carried out Mechanics Performance Testing, and the fracture toughness property value is 6.4MPam
1/2Fracture toughness property value than general alumina-ceramic exceeds one times.Bending strength is carried out scanning electron microscope observation to the alumina ceramic material microstructure and is confirmed also up to 653MPa, is waiting axle shape Al
2O
3Intergranule grows diameter 1-15 micron, and length is the long column shape Al of 3-6 micron
2O
3Brilliant.
Embodiment 2
Three water aluminum compound Al (OH)
3Raw material is the same, and with this powder of 300 grams, 1500 gram alumina balls and 350 gram deionized waters are put into together in the aluminum oxide ball milling jar and carried out wet ball grinding 72 hours, then slip are separated with abrading-ball.Dry putting into drying box with slip behind the aluminium oxide abrading-ball wash clean.Al behind the ball milling
2O
3Weightless 146 grams of abrading-ball namely have 146 gram α-Al
2O
3In mechanical milling process, be incorporated into Al (OH) as crystal seed
3In the powder, account for Al (OH)
3The 41.7wt% of weight.To contain α-Al
2O
3The Al of crystal seed (OH)
3Powder calcination 2 hours in 1100 ℃ of high temperature furnaces makes Al (OH)
3Change Al into
2O
3Again with the powder after the calcination with ethanol ball milling 15 hours, powder is scatter, dry then, vaporized alcohol is obtained fine powder, with powder dry-pressing formed be the garden bulk of 10 millimeters of 50 ≌, in vacuum hotpressing stove, carry out high temperature sintering in 1600 ℃ of down insulations 1.5 hours, pressure is 30MPa.Alumina-ceramic behind the sintering is carried out Mechanics Performance Testing, and the fracture toughness property value is 7.1MPam
1/2, bending strength is also up to 625MPa.
Embodiment 3
It is 1.8 microns boehmite [AlOOH] powder 300 gram with industrial, average grain diameter, the high purity aluminium oxide ball of 800 grammes per square metres and 500 gram deionized waters are put into together the nylon ball milling and were filled with wet ball grinding 58 hours, then the aluminium oxide abrading-ball of cleaning and slip are put into fully drying of drying box, to the Al of oven dry
2O
3Abrading-ball is weighed, and its weight is 705 grams, namely has the aluminium oxide abrasion of 95 grammes per square metres to be introduced in the AlOOH powder α-Al
2O
3Crystal seed is the 31.6wt% of AlOOH weight.The aluminium oxide abrasion that are introduced in the AlOOH powder are α-Al
2O
3Fine powder is as crystal seed.To contain the AlOOH powder of crystal seed 1200 ℃ of calcination 1 hour, this moment, AlOOH transferred Al fully to
2O
3Phase.Al with the powder agglomates shape after this calcination
2O
3With ethanol (ratio is 1: 1) ball milling 10 hours, obtain average grain diameter after the oven dry and be 0.6 micron Al
2O
3Powder.With the part powder dry-pressing formed be the nahlock shape of 15 millimeters of 60 ≌, high temperature sintering in vacuum hotpressing stove, pressure is 30MPa, is warmed up to 1550 ℃ of insulations 2 hours, the fracture toughness property of stupalith behind the sintering is measured reach 6.1MPam
1/2, bending strength is promptly had high tenacity and high-intensity alumina ceramic material simultaneously also up to 632MPa.
Embodiment 4
Adopt boehmite [AlOOH] powder 400 grams among the embodiment 3, put into the nylon ball milling and irritated wet ball grinding 70 hours with alumina balls 1000 grams, deionized water 500 grams.Then the aluminium oxide abrading-ball of cleaning and slip are put into fully drying of drying box, the Al of survey
2O
3Weightless 182 grams of abrading-ball.Namely with respect to α-Al of boehmite [AlOOH] powder weight 45.5wt%
2O
3Fine powder is introduced in the AlOOH powder as crystal seed.To contain the AlOOH powder of crystal seed 1200 ℃ of calcination 1 hour, this moment, AlOOH transferred Al fully to
2O
3Phase.With the blocky Al of the powder after this calcination
2O
3With ethanol (ratio is 1: 1) ball milling 12 hours, the oven dry back is dry-pressing formed to be the nahlock shape of 15 millimeters of 60 ≌, and high temperature sintering in vacuum hotpressing stove, pressure are 35MPa, be warmed up to 1600 ℃ of insulations 1 hour, the fracture toughness property of stupalith is 6.7MPam behind the mensuration sintering
1/2, prepare high-toughness alumina ceramics.Scanning electron microscope observation confirms, exists in this aluminium oxide ceramics microstructure improving the favourable long column shape Al of toughness
2O
3Brilliant.
Claims (1)
1, a kind of preparation method of high-toughness alumina ceramics is characterized in that this method comprises following each step:
(1) initial ceramic raw material adopts three water aluminum compound or boehmites, with α-Al
2O abrading-ball and deionized water are put into ball grinder together and are carried out wet ball grinding, and add-on is: ceramic raw material: the aluminum oxide abrading-ball: deionized water=1: 2-6: 1-2, and the ball milling time is 30-90 hour;
(2) mixed slurry behind the wet ball grinding after drying, calcination under 1100-1300 ℃ of temperature makes three water aluminium compounds or boehmite change Al in high temperature Muffle furnace
2O
3Crystalline phase;
(3) Al that obtains after the calcination
2O
3Material adds alcohol and carries out ball milling again, and Ball-milling Time is 10-20 hour, makes block material fully levigate;
(4) Al behind the ball milling
2O
3The powder drying is for subsequent use;
(5) with the above-mentioned α-Al that introduced
2O
3The Al of crystal seed
2O
3The powder moulding, vacuum heating-press sintering then, sintering temperature is 1500～1650 ℃, temperature retention time is 1～4 hour, namely gets ceramic material of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00136835 CN1131185C (en) | 2000-12-29 | 2000-12-29 | Process for preparing high-toughness alumina ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00136835 CN1131185C (en) | 2000-12-29 | 2000-12-29 | Process for preparing high-toughness alumina ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1304903A true CN1304903A (en) | 2001-07-25 |
| CN1131185C CN1131185C (en) | 2003-12-17 |
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ID=4597528
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|---|---|---|---|
| CN 00136835 Expired - Fee Related CN1131185C (en) | 2000-12-29 | 2000-12-29 | Process for preparing high-toughness alumina ceramics |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378002C (en) * | 2006-01-13 | 2008-04-02 | 中国科学院上海硅酸盐研究所 | Plate-like aluminum oxide granule preparation method |
| CN101817693A (en) * | 2010-04-22 | 2010-09-01 | 武汉楚熊科技有限公司 | Method for preparing foamed ceramics based on nano-alumina |
| CN102030518A (en) * | 2010-10-26 | 2011-04-27 | 余建平 | Alumina/graphite composite ceramic material and preparation method thereof |
| CN105819834A (en) * | 2016-03-03 | 2016-08-03 | 刘佩佩 | Alumina ceramic material with good toughness, and preparation method thereof |
| CN110844928A (en) * | 2019-12-06 | 2020-02-28 | 湖北工业大学 | Method for preparing micro-nano aluminum oxide from aluminum alloy hydrolysate |
| CN111620691A (en) * | 2020-05-11 | 2020-09-04 | 华南理工大学 | Al based on azeotropic distillation2O3/ZrO2Composite ceramic and preparation method and application thereof |
| CN113416064A (en) * | 2021-04-21 | 2021-09-21 | 郑州航空工业管理学院 | Zirconia/alumina ceramic composite material and preparation method thereof |
| CN115872727A (en) * | 2023-01-31 | 2023-03-31 | 无锡特科精细陶瓷有限公司 | Method for preparing ceramic material by isostatic pressing |
| CN116217255A (en) * | 2023-03-02 | 2023-06-06 | 新化县顺达电子陶瓷有限公司 | High-precision ceramic material for 5G signal base station and preparation method thereof |
-
2000
- 2000-12-29 CN CN 00136835 patent/CN1131185C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378002C (en) * | 2006-01-13 | 2008-04-02 | 中国科学院上海硅酸盐研究所 | Plate-like aluminum oxide granule preparation method |
| CN101817693A (en) * | 2010-04-22 | 2010-09-01 | 武汉楚熊科技有限公司 | Method for preparing foamed ceramics based on nano-alumina |
| CN101817693B (en) * | 2010-04-22 | 2012-03-21 | 武汉吉耐德科技有限公司 | Method for preparing foamed ceramics based on nano-alumina |
| CN102030518A (en) * | 2010-10-26 | 2011-04-27 | 余建平 | Alumina/graphite composite ceramic material and preparation method thereof |
| CN102030518B (en) * | 2010-10-26 | 2013-03-13 | 江西华烨节能照明股份有限公司 | Alumina/graphite composite ceramic material and preparation method thereof |
| CN105819834A (en) * | 2016-03-03 | 2016-08-03 | 刘佩佩 | Alumina ceramic material with good toughness, and preparation method thereof |
| CN110844928A (en) * | 2019-12-06 | 2020-02-28 | 湖北工业大学 | Method for preparing micro-nano aluminum oxide from aluminum alloy hydrolysate |
| CN111620691A (en) * | 2020-05-11 | 2020-09-04 | 华南理工大学 | Al based on azeotropic distillation2O3/ZrO2Composite ceramic and preparation method and application thereof |
| CN111620691B (en) * | 2020-05-11 | 2021-09-21 | 华南理工大学 | Al based on azeotropic distillation2O3/ZrO2Composite ceramic and preparation method and application thereof |
| CN113416064A (en) * | 2021-04-21 | 2021-09-21 | 郑州航空工业管理学院 | Zirconia/alumina ceramic composite material and preparation method thereof |
| CN115872727A (en) * | 2023-01-31 | 2023-03-31 | 无锡特科精细陶瓷有限公司 | Method for preparing ceramic material by isostatic pressing |
| CN116217255A (en) * | 2023-03-02 | 2023-06-06 | 新化县顺达电子陶瓷有限公司 | High-precision ceramic material for 5G signal base station and preparation method thereof |
| CN116217255B (en) * | 2023-03-02 | 2023-12-15 | 新化县顺达电子陶瓷有限公司 | High-precision ceramic material for 5G signal base station and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1131185C (en) | 2003-12-17 |
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