CN1803629A - Method for preparing modified aluminium titanate material - Google Patents
Method for preparing modified aluminium titanate material Download PDFInfo
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- CN1803629A CN1803629A CN 200610005315 CN200610005315A CN1803629A CN 1803629 A CN1803629 A CN 1803629A CN 200610005315 CN200610005315 CN 200610005315 CN 200610005315 A CN200610005315 A CN 200610005315A CN 1803629 A CN1803629 A CN 1803629A
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- alcohol
- ticl
- modified aluminium
- low
- titanate material
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Abstract
The invention discloses a preparation method for modified aluminum titanates material. Wherein, with titanium tetrachloride and aluminum nitrate as predecessor material to dissolve in anhydrous low-carbon alcohol and form mixed liquid; stirring acutely, adding composite stabilizer and reinforcing agent to prepare mixed alcohol liquid; finally, obtaining the product with heating hydrolysis sol-gel method. This invention realizes the synthesis and modifying in one step, improves material performance, and needs low cost with short period.
Description
Technical field the present invention relates to inorganic material-modified technical field, is specifically related to a kind of method for preparing the material of aluminum titanate of intensity height, Heat stability is good.
The background technology aluminum titanate ceramic material is a kind of collection high-melting-point (1860 ℃), low bulk (0.5～1.5 * 10
-6/ ℃) excellent inorganic materials, have broad application prospects.But this material also exists two big deadly defects: the one, and crystal expansion coefficient difference on each crystalline axis direction is very big, produces a large amount of tiny cracks when cooling, causes physical strength very low; It two is easily to resolve into rutile and corundum mutually in 800～1280 ℃ of intervals, has lost the premium properties of aluminium titanates, has therefore limited the practical application of material of aluminum titanate greatly.Prepare and modification with regard to the material of aluminum titanate that begun one's study in the seventies in last century both at home and abroad, between 800 ℃～1280 ℃, easily decompose and be difficult to dense sintering two hang-ups at it and done number of research projects, obtained very big progress.As stablize the lattice of aluminium titanates, thereby reach the purpose of raising aluminium titanates stability by introducing additives such as ferric oxide, magnesium oxide, silicon-dioxide, yttrium oxide, lanthanum trioxide; Introducing Gao Ling, triphane, silicon-dioxide improve the sintering character of aluminium titanates, promote the densification of material of aluminum titanate.Also the someone studies by introducing second performance of improving aluminium titanates mutually, as preparation aluminium titanates and mullite Multiphase pottery, adds zirconium dioxide and strengthens alumina titanate ceramics etc.Yet,, often do not reach the effect of anticipation because existing research mainly concentrates on and utilizes solid phase method doping vario-property alumina titanate ceramics.And the research of being carried out or be to be primarily aimed at the intensity that improves aluminium titanates, it is the thermostability of paying attention to improving aluminium titanates, do not see the achievement report that above-mentioned two aspects is combined research is arranged, promptly seldom study under the prerequisite that keeps the aluminium titanates low bulk, improve the physical strength and the thermostability of aluminium titanates simultaneously.
Summary of the invention the object of the present invention is to provide a kind of preparation method of modified aluminium titanate material.Adopt the prepared material of aluminum titanate of this method under the prerequisite that keeps the aluminium titanates low bulk, its physical strength and thermostability all are significantly improved.Overcome solid phase method and introduced the unfavorable shortcoming of additive agent modified effect, made aluminium titanates become a kind of material of practicability.
For realizing goal of the invention, the preparation method of a kind of modified aluminium titanate material of the present invention comprises successively: (1) is with titanium tetrachloride (TiCl
4) and aluminum nitrate (Al (NO
3)
39H
2O) be presoma, they are dissolved in the anhydrous low-carbon alcohol, obtain both alcohol mixture solution A; (2) under vigorous stirring, be benchmark with the alcohol mixture solution A, 0.5～3wt% glycerine or/and molecular weight is 600～10000 polyoxyethylene glycol adds in the alcohol mixture solution A, is obtained mixed liquid B; (3) with titanium tetrachloride (TiCl
4) mole number be benchmark, with one package stabilizer (12mol%Mg (NO
3)
26H
2O and 8mol%Fe (NO
3)
39H
2O) and 6～10mol% toughener (ZrOCl
28H
2O is or/and Y (NO
3)
39H
2O) join in the mixed liquid B, stirring obtains mixed solution C; (4) mixed solution C is heated under 60～90 ℃ condition, refluxes, produce hydrolysis, polycondensation, form gel D, (5) can obtain modified aluminium titanate material of the present invention with gel D drying, grinding, low temperature calcination, compression moulding, sintering.
Described anhydrous low-carbon alcohol is meant one or more mixture of methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol.
The best proportioning of described presoma and anhydrous low-carbon alcohol is: the mol ratio of presoma and anhydrous low-carbon alcohol is 1: 10～25, wherein, and TiCl
4With Al (NO
3)
39H
2The mol ratio of O is 1: 2.
The optimum temperature range of described drying treatment is 60～85 ℃, and best low temperature calcination system is: calcine 15～30min down at 400～500 ℃, sintering preferably carries out under 1380～1450 ℃, and is incubated 1～2h.
The present invention is by introducing toughener and stablizer simultaneously in titanium tetrachloride and aluminum nitrate alcohol mixture solution, one step of synthetic and modification of aluminium titanates is finished, aluminium titanates intensity is greater than 50MPa after the modification, and have good thermostability and low bulk performance, solved two hang-ups of puzzlement material of aluminum titanate practical application.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 has shown at aluminium titanates and has decomposed the rule that the coefficient of expansion of 1100 ℃ of the most violent following embodiment 1～3 synthetic modified aluminium titanate materials changes with soaking time, also listed among the figure and used the trend of the coefficient of expansion of solid phase method and the unmodified material of aluminum titanate of present method synthetic respectively, as a means of comparing with the soaking time variation.
Embodiment
Embodiment 1
With 0.036molAl (NO
3)
39H
2O (analytical pure), 0.018molTiCl
4The precursor material of (chemical pure) is dissolved in the anhydrous C of 0.735mol
2H
5OH (analytical pure) obtains the alcohol mixture solution A of titanium tetrachloride and aluminum nitrate, under vigorous stirring, 1.5wt% glycerine (analytical pure) is added wherein, obtains mixed liquid B, with 10mol% toughener ZrOCl
28H
2O (chemical pure) and one package stabilizer Mg (NO
3)
26H
2O (12mol%, chemical pure) and Fe (NO
3)
39H
2O (8mol%, chemical pure) joins in the mixed liquid B, and stirring obtains mixed solution C, and the water-bath that places 70 ℃ is heated, refluxed, and makes it to take place hydrolysis condensation reaction, forms gel D.Then through 65 ℃ of dry xerogel E that form, grind then at 450 ℃ of following low temperature calcination 25min, obtain modified aluminium titanate precursor powder F, the PVA of 2wt% is mixed with modified aluminium titanate precursor powder F as binding agent, compression moulding, dry back is at 1400 ℃ of following sintering, and insulation 1.5h obtains modified aluminium titanate material of the present invention.
Embodiment 2
With 10mol% toughener ZrOCl among the embodiment 1
28H
2O (chemical pure) changes 6mol% toughener Y (NO into
3)
39H
2O (chemical pure), other condition is constant, obtains modified aluminium titanate material.
Embodiment 3
With 10mol% toughener ZrOCl among the embodiment 1
28H
2O (chemical pure) changes 6mol%ZrOCl into
28H
2O (chemical pure) and 3mol%Y (NO
3)
39H
2O's (chemical pure) is compound, and other condition is constant, obtains modified aluminium titanate material.
The prepared powder of solid phase method and present method means and does not add synthetic aluminium titanates powder under the properties-correcting agent condition among Fig. 2, the sintering temperature of the synthetic aluminium titanates powder of solid phase method is 1520 ℃, soaking time is 4h, and the sintering temperature of the synthetic aluminium titanates powder of present method is 1420 ℃, and soaking time is 2h.As can be seen from Figure 2, the coefficient of expansion of embodiment 1～3 synthetic modified aluminium titanate material is very little with soaking time prolongation amplification, compares with the unmodified material of aluminum titanate of present method synthetic with solid phase method, and the material of aluminum titanate thermostability after the modification improves greatly.The folding strength of modified aluminium titanate material, water-intake rate and thermal expansivity data are listed in table 1, for ease of relatively, have provided the corresponding data of using solid phase method and the unmodified material of aluminum titanate of present method synthetic respectively in the table 1.
The test result of the folding strength of table 1 material of aluminum titanate, water-intake rate and thermal expansivity
Claims (4)
1, a kind of preparation method of modified aluminium titanate material comprises successively: (1) is with titanium tetrachloride (TiCl
4) and aluminum nitrate (Al (NO
3)
39H
2O) be presoma, they are dissolved in the anhydrous low-carbon alcohol, obtain both alcohol mixture solution A; (2) under vigorous stirring, be benchmark with the alcohol mixture solution A, 0.5～3wt% glycerine or/and molecular weight is 600～10000 polyoxyethylene glycol adds in the alcohol mixture solution A, is obtained mixed liquid B; (3) with titanium tetrachloride (TiCl
4) mole number be benchmark, with 12mol%Mg (NO
3)
26H
2O and 8mol%Fe (NO
3)
39H
2O and 6～10mol%ZrOCl
28H
2O is or/and Y (NO
3)
39H
2O joins in the mixed liquid B, stirs to obtain mixed solution C; (4) mixed solution C is heated under 60～90 ℃ condition, refluxes, produce hydrolysis, polycondensation, form gel D, (5) can obtain modified aluminium titanate material of the present invention with gel D drying, grinding, low temperature calcination, compression moulding, sintering.
2, method according to claim 1 is characterized in that described anhydrous low-carbon alcohol is one or more a mixture of methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol.
3, method according to claim 1, the mol ratio that it is characterized in that described presoma and anhydrous low-carbon alcohol is 1: 10～25, wherein, TiCl
4With Al (NO
3)
39H
2The mol ratio of O is 1: 2.
4, method according to claim 1, the temperature that it is characterized in that described drying treatment are 60～85 ℃, and the low temperature calcination system is to calcine 15～30min down at 400～500 ℃, and sintering temperature is to carry out at 1380～1450 ℃, insulation 1～2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100053150A CN100430321C (en) | 2006-01-12 | 2006-01-12 | Method for preparing modified aluminium titanate material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100053150A CN100430321C (en) | 2006-01-12 | 2006-01-12 | Method for preparing modified aluminium titanate material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1803629A true CN1803629A (en) | 2006-07-19 |
| CN100430321C CN100430321C (en) | 2008-11-05 |
Family
ID=36865808
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|---|---|---|---|
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|---|---|
| CN (1) | CN100430321C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100569697C (en) * | 2007-10-30 | 2009-12-16 | 景德镇陶瓷学院 | A kind of method that adopts sol-gel technology to prepare aluminium titanate film |
| CN101696030B (en) * | 2009-08-18 | 2011-04-06 | 景德镇陶瓷学院 | Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process |
| CN102424417A (en) * | 2011-09-02 | 2012-04-25 | 景德镇陶瓷学院 | Method for preparing stabilized aluminium titanate superfine powder by sol-gel technology under low temperature and product prepared therefrom |
| CN101423389B (en) * | 2008-11-26 | 2012-05-16 | 河北理工大学 | Method for preparing nano zircite combining aluminium titanate composite material |
| CN102701273A (en) * | 2012-05-22 | 2012-10-03 | 山东大学 | Preparation method of nano dysprosium titanate powder |
| CN111892083A (en) * | 2020-08-21 | 2020-11-06 | 景德镇陶瓷大学 | Preparation method of novel high-temperature-resistant stable aluminum titanate-based ceramic pigment and product prepared by preparation method |
| WO2023223269A1 (en) * | 2022-05-20 | 2023-11-23 | Universidad Libre | Synthesis of cahozrtio3 perovskite photocatalyst nanomaterial |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3096814B1 (en) * | 1999-11-08 | 2000-10-10 | 勉 福田 | Method for producing aluminum titanate sintered body |
| WO2004011386A1 (en) * | 2002-07-31 | 2004-02-05 | Corning Incorporated | Aluminum titanate-based ceramic article |
| EP1559696B1 (en) * | 2002-11-01 | 2016-11-16 | Ohcera Co., Ltd. | Aluminum magnesium titanate sintered product, method for producing it and its use |
| JP4766645B2 (en) * | 2003-02-18 | 2011-09-07 | 株式会社Ｌｉｘｉｌ | Damping member |
-
2006
- 2006-01-12 CN CNB2006100053150A patent/CN100430321C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100569697C (en) * | 2007-10-30 | 2009-12-16 | 景德镇陶瓷学院 | A kind of method that adopts sol-gel technology to prepare aluminium titanate film |
| CN101423389B (en) * | 2008-11-26 | 2012-05-16 | 河北理工大学 | Method for preparing nano zircite combining aluminium titanate composite material |
| CN101696030B (en) * | 2009-08-18 | 2011-04-06 | 景德镇陶瓷学院 | Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process |
| CN102424417A (en) * | 2011-09-02 | 2012-04-25 | 景德镇陶瓷学院 | Method for preparing stabilized aluminium titanate superfine powder by sol-gel technology under low temperature and product prepared therefrom |
| CN102701273A (en) * | 2012-05-22 | 2012-10-03 | 山东大学 | Preparation method of nano dysprosium titanate powder |
| CN111892083A (en) * | 2020-08-21 | 2020-11-06 | 景德镇陶瓷大学 | Preparation method of novel high-temperature-resistant stable aluminum titanate-based ceramic pigment and product prepared by preparation method |
| WO2023223269A1 (en) * | 2022-05-20 | 2023-11-23 | Universidad Libre | Synthesis of cahozrtio3 perovskite photocatalyst nanomaterial |
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| Publication number | Publication date |
|---|---|
| CN100430321C (en) | 2008-11-05 |
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