CN1303037C - Preparation method of mullite whiskers - Google Patents
Preparation method of mullite whiskers Download PDFInfo
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- CN1303037C CN1303037C CNB2005100449079A CN200510044907A CN1303037C CN 1303037 C CN1303037 C CN 1303037C CN B2005100449079 A CNB2005100449079 A CN B2005100449079A CN 200510044907 A CN200510044907 A CN 200510044907A CN 1303037 C CN1303037 C CN 1303037C
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- mullite
- crystal whisker
- sol
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- mullite crystal
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Abstract
The present invention relates to a preparation method of mullite whiskers, which belongs to the technical field of new material. The mullite whiskers of the present invention takes commercially pure aluminium sol and silicon collosol as raw material and adopts the colloidal sol-gel technology to prepare mullite precursor dried gel, and then dried gel powder and commercially pure aluminium fluoride are mixed. The mullite whiskers of the present invention is prepared by calcination at high temperature in a hermetic alumina ceramic crucible, so that the mullite whiskers with low cost and good performance are obtained. The present invention has simple manufacturing process and is easy to realize industrial production.
Description
(1) technical field
The present invention relates to a kind of preparation method who is used for the mullite crystal whisker of toughened and reinforced high-temperature structural ceramics, metal and plastics, belong to new material technology field.
(2) background technology
High temperature resistant, anti-oxidant, corrosion-resistant, performances such as thermal expansivity is less, hot strength height that mullite crystal whisker has are a kind of metal, pottery and plastic toughening strengthening agent of excellence, also can be used for fields such as friction materials.
About existing many documents of the preparation of mullite crystal whisker and patent report.Japan Okada etc. are raw material with tetraethoxy and aluminum nitrate, adopt sol-gel method to prepare Al
2O
3-SiO
2Xerogel, and with xerogel and AlF
3Mix, mullite crystal whisker has been synthesized in calcining in airtight container then, referring to Materials science communication .8[9] and (1989): 1052-1054 (J.Matter.Sci.Lett., 8[9] (1989): 1052-1054).Chinese patent application CN 1064713A discloses a kind of preparation method of highly pure mullite crystal whisker, and this method is dissolved in aluminium salt in the alcoholic solution, presses SiO
2: Al
2O
3=2: 3 mol ratio drips the alkoxide of silicon, and adds HF solution, with the gel oven dry that obtains, broken, sieve, calcine, obtain the mullite crystal whisker of various length-to-diameter ratios at last.United States Patent (USP) 4910172 and 4948766 (US Patent 4910172 and US Patent 4948766) discloses with powder method (Al
2O
3, SiO
2, AlF
3) prepare the method for mullite crystal whisker.It is raw material that Yuan Jianjun etc. delivered with chemical pure tetraethoxysilance, water, aluminum nitrate and aluminum fluoride in 1996, and ethanol is solvent, and hydrochloric acid and ammoniacal liquor are for the Preparation of Catalyst mullite crystal whisker of preparation gel, referring to silicate journal .24[3] (1996): 342-346.Yuan Jianjun etc. have proposed with Al
2O
3-SiO
2Glass powder and AlF
3Novel process for the feedstock production mullite crystal whisker, compound is warming up to 950 ℃ with the temperature rise rate of 2 ℃/min, insulation 1h, then be warming up to 1250 ℃ of insulation 4h again, the diameter of gained mullite crystal whisker is 0.4～1.2 μ m, length-to-diameter ratio is 10～40, referring to Journal of Inorganic Materials .11[1] (1996): 101-106).
The technology of above-mentioned preparation mullite crystal whisker is a kind of to be that alkoxide with aluminium and silicon is a raw material, another kind of then be raw material with the oxide powder of aluminium and silicon, is catalyzer with the fluorochemical, prepares mullite crystal whisker under the high temperature in encloses container.The complex technical process and the raw materials cost of preceding a kind of prepared mullite crystal whisker are higher relatively; Then a kind of technology is difficult to reach uniform mixing owing to adopt the powder raw material of aluminum oxide, silicon oxide, and therefore whisker morphology, the composition of preparation are even inadequately.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of mullite crystal whisker preparation method who is suitable for producing in batches is provided.
The invention is characterized in that mullite crystal whisker is is raw material with commercial-purity aluminium colloidal sol and silicon sol, adopt sol-gel technology to prepare the mullite precursor xerogel, then dry gel powder is mixed with the technical pure aluminum fluoride, high-temperature calcination is prepared from airtight alumina-ceramic crucible, thereby can obtain mullite crystal whisker with low cost, excellent property.
The preparation method of mullite crystal whisker of the present invention, step is as follows:
1, commercial-purity aluminium colloidal sol is joined in the deionized water aluminium colloidal sol and deionized water weight ratio 1: 1～3, heating in water bath to 70～90 ℃ when stirring;
2, the technical pure silicon sol is joined the deionized water for stirring of 1～3 times of weight;
3, press SiO
2: Al
2O
3=2: 3 mol ratio is added drop-wise to the silicon sol of step 2 in the alumina sol of step 1, fully stirs 1～2 hour.
4, step 3 heavy-gravity mixed sols is dried down at 60～80 ℃, pulverize, cross 100～200 mesh sieves, obtain mullite precursor xerogel powder.
5, according to 3: 1～4: 1 ratio the mullite precursor xerogel is mixed with the technical pure aluminum fluoride, in 1350～1550 ℃ temperature lower calcination, obtain the mullite crystal whisker powder in the airtight alumina crucible of packing into.
Above-mentioned mullite crystal whisker powder is ball milling more as required, sieves, and can get the mullite crystal whisker product of required granularity.
The commercial-purity aluminium colloidal sol of above-mentioned steps 1, wherein the mass percent of aluminum oxide is 8～10%, all the other are water;
The technical pure silicon sol of above-mentioned steps 2, wherein the mass percent of silicon-dioxide is 20～30%, all the other are water;
The technical pure aluminum fluoride of above-mentioned steps 5, wherein the aluminum fluoride mass percent is 95～98%, all the other are impurity.
Compared with prior art, excellent results of the present invention is as follows:
1, owing to adopt industrial pure material and sol-gel technology, mullite crystal whisker of the present invention not only has characteristics with low cost but also has good performance.
2, technology of the present invention is simple, is easy to realize suitability for industrialized production, and productive rate can reach 100%.
(4) embodiment
The invention will be further described below in conjunction with embodiment, but be not limited thereto.Among the embodiment in the used aluminium colloidal sol mass percent of aluminum oxide be 8～10%, all the other are water; The mass percent of silicon-dioxide is 20～30% in the silicon sol, and all the other are water; The aluminum fluoride mass percent is 95～98%, and all the other are impurity.
Embodiment 1:
1, commercial-purity aluminium colloidal sol is joined in the deionized water aluminium colloidal sol and deionized water weight ratio 1: 2, heating in water bath to 90 ℃ when stirring;
2, the technical pure silicon sol is joined 2 times deionized water for stirring;
3, press SiO
2: Al
2O
3=2: 3 mol ratio is added drop-wise to the silicon sol of step 2 in the alumina sol of step 1, fully stirs 1.5 hours.
4, step 3 heavy-gravity mixed sols is dried down at 70 ℃, pulverize, cross 100 mesh sieves, obtain mullite precursor xerogel powder.
5, according to 3: 1 ratio the mullite precursor xerogel is mixed with the technical pure aluminum fluoride, in 1400 ℃ temperature lower calcination, obtain the mullite crystal whisker powder in the airtight alumina crucible of packing into.The diameter of mullite crystal whisker is 0.3～1 μ m, and length-to-diameter ratio is 30～100.Productive rate 100%.Ball milling sieves again, can get the mullite crystal whisker product of required granularity.
Embodiment 2:
1, commercial-purity aluminium colloidal sol is joined in the deionized water aluminium colloidal sol and deionized water weight ratio 1: 3, heating in water bath to 90 ℃ when stirring;
2, the technical pure silicon sol is joined 3 times deionized water for stirring;
3, press SiO
2: Al
2O
3=2: 3 mol ratio is added drop-wise to the silicon sol of step 2 in the alumina sol of step 1, fully stirs 2 hours.
4, step 3 heavy-gravity mixed sols is dried down at 80 ℃, pulverize, cross 180 mesh sieves, obtain mullite precursor xerogel powder.
5, according to 4: 1 ratio the mullite precursor xerogel is mixed with the technical pure aluminum fluoride, in 1500 ℃ temperature lower calcination, obtain the mullite crystal whisker powder in the airtight alumina crucible of packing into.The diameter of mullite crystal whisker is 0.3～1 μ m, and length-to-diameter ratio is 30～100.Productive rate 100%.Ball milling sieves again, can get the mullite crystal whisker product of required granularity.
Claims (4)
1, a kind of preparation method of mullite crystal whisker, step is as follows:
(1) commercial-purity aluminium colloidal sol is joined in the deionized water aluminium colloidal sol and deionized water weight ratio 1: 1～3, heating in water bath to 70～90 ℃ when stirring;
(2) the technical pure silicon sol is joined the deionized water for stirring of 1～3 times of weight;
(3) press SiO
2: Al
2O
3=2: 3 mol ratio is added drop-wise to the silicon sol of step (2) in the alumina sol of step (1), fully stirs 1～2 hour;
(4) step (3) heavy-gravity mixed sols is dried down at 60～80 ℃, pulverize, cross 100～200 mesh sieves, obtain mullite precursor xerogel powder;
(5) according to 3: 1～4: 1 ratio the mullite precursor xerogel is mixed with the technical pure aluminum fluoride, in 1350～1550 ℃ temperature lower calcination, obtain the mullite crystal whisker powder in the airtight alumina crucible of packing into.
2, the preparation method of mullite crystal whisker as claimed in claim 1 is characterized in that, the commercial-purity aluminium colloidal sol of described step (1), and wherein the mass percent of aluminum oxide is 8～10%, all the other are water.
3, the preparation method of mullite crystal whisker as claimed in claim 1 is characterized in that, the technical pure silicon sol of described step (2), and wherein the mass percent of silicon-dioxide is 20～30%, all the other are water.
4, the preparation method of mullite crystal whisker as claimed in claim 1 is characterized in that, the technical pure aluminum fluoride of described step (5), and wherein the aluminum fluoride mass percent is 95～98%, all the other are impurity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100449079A CN1303037C (en) | 2005-10-18 | 2005-10-18 | Preparation method of mullite whiskers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100449079A CN1303037C (en) | 2005-10-18 | 2005-10-18 | Preparation method of mullite whiskers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1785893A CN1785893A (en) | 2006-06-14 |
| CN1303037C true CN1303037C (en) | 2007-03-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100449079A Expired - Fee Related CN1303037C (en) | 2005-10-18 | 2005-10-18 | Preparation method of mullite whiskers |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206865B (en) * | 2011-05-09 | 2012-11-14 | 中国地质大学（武汉） | Method for preparing mullite whisker from cyanite ore |
| CN103614808B (en) * | 2013-10-24 | 2015-05-27 | 西安交通大学 | Mullite fiber with villous whisker and preparation method thereof |
| CN103803568B (en) * | 2013-12-23 | 2016-08-17 | 天津大学 | A kind of method utilizing microwave catalysis synthesis acicular mullite |
| CN105088345B (en) * | 2015-07-28 | 2017-09-19 | 景德镇陶瓷大学 | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker |
| CN106915749B (en) * | 2017-04-07 | 2019-03-01 | 武汉科技大学 | A kind of rod-like mullite-tabular alumina composite granule and preparation method thereof |
| CN107827442A (en) * | 2017-11-21 | 2018-03-23 | 常州创索新材料科技有限公司 | A kind of preparation method of crack-resistant ceramic base frication material |
| CN108315810B (en) * | 2018-02-24 | 2020-09-22 | 陕西大秦钾业有限公司 | Method for synthesizing mullite whisker by taking kaliophilite as raw material |
| CN108863430A (en) * | 2018-08-17 | 2018-11-23 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of high temperature resistant aeroge heat-barrier material |
| CN110183244B (en) * | 2019-06-19 | 2022-06-03 | 长安大学 | Hollow mullite spherical material and preparation method thereof |
| CN110512310B (en) * | 2019-09-03 | 2021-12-21 | 哈尔滨工业大学 | Preparation method of micron-scale alumina fiber |
| CN111943699B (en) * | 2020-08-24 | 2022-06-28 | 宜兴瑞泰耐火材料有限公司 | Large length-diameter ratio mullite whisker-combined andalusite refractory brick for propane dehydrogenation device and preparation process thereof |
| CN112280538B (en) * | 2020-10-28 | 2021-11-16 | 武汉科技大学 | Whisker toughened phase change heat storage microcapsule and preparation method thereof |
| CN116444279A (en) * | 2022-01-06 | 2023-07-18 | 辽宁科技大学 | Mullite whisker reinforced mullite composite material and preparation method thereof |
| CN115161759B (en) * | 2022-08-03 | 2023-06-16 | 湖北工业大学 | Method for preparing high-length-diameter-ratio radiation-proof mullite whisker from solid waste precursor at low temperature |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990001471A1 (en) * | 1988-08-05 | 1990-02-22 | THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY | Method of preparing rigid mullite-whisker felt |
| WO1990009360A1 (en) * | 1989-02-08 | 1990-08-23 | THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY | PREPARATION OF MULLITE WHISKERS FROM AlF3, SiO2, AND Al2O3 POWDERS |
| CN1064713A (en) * | 1992-04-30 | 1992-09-23 | 清华大学 | The preparation method of highly pure mullite crystal whisker |
-
2005
- 2005-10-18 CN CNB2005100449079A patent/CN1303037C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990001471A1 (en) * | 1988-08-05 | 1990-02-22 | THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY | Method of preparing rigid mullite-whisker felt |
| WO1990009360A1 (en) * | 1989-02-08 | 1990-08-23 | THE GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by, THE SECRETARY OF THE DEPARTMENT OF THE NAVY | PREPARATION OF MULLITE WHISKERS FROM AlF3, SiO2, AND Al2O3 POWDERS |
| CN1064713A (en) * | 1992-04-30 | 1992-09-23 | 清华大学 | The preparation method of highly pure mullite crystal whisker |
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|---|---|
| CN1785893A (en) | 2006-06-14 |
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Assignee: Zibo forever anda Industry & Trade Co., Ltd. Assignor: Shandong University Contract fulfillment period: 2008.10.10 to 2013.10.10 contract change Contract record no.: 2009370000147 Denomination of invention: Preparation method of mullite whiskers Granted publication date: 20070307 License type: Exclusive license Record date: 2009.7.7 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.10 TO 2013.10.10; CHANGE OF CONTRACT Name of requester: ZIBO YONGANDA INDUSTRY AND TRADE CO., LTD. Effective date: 20090707 |
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Granted publication date: 20070307 Termination date: 20091118 |