CN102557670A - Preparation method of aluminum oxide and titanium oxide compound nanometer powder body - Google Patents
Preparation method of aluminum oxide and titanium oxide compound nanometer powder body Download PDFInfo
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- CN102557670A CN102557670A CN2010106063913A CN201010606391A CN102557670A CN 102557670 A CN102557670 A CN 102557670A CN 2010106063913 A CN2010106063913 A CN 2010106063913A CN 201010606391 A CN201010606391 A CN 201010606391A CN 102557670 A CN102557670 A CN 102557670A
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Abstract
The invention discloses a preparation method of an aluminum oxide and titanium oxide compound nanometer powder body. The aluminum oxide and titanium oxide compound nanometer powder body prepared by the preparation method has a particle size of about 25-32nm, and the particle size is uniform, wherein the aluminum oxide is alpha phase, the titanium oxide is a rutile phase, and the calcination temperature is lower than the temperature of preparing the alpha aluminum oxide.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium oxide-titanium oxide composite nano powder, belong to the nanometer material science field.
Background technology
The aluminium oxide-titanium oxide nano-powder is with a wide range of applications at industrial circle, can be used to the excellent high-temperature wear resistant coating of processability, advanced ceramics material, support of the catalyst etc.Existing research shows that two kinds of powders mix evenly more, and its prepared material property is good more.The main method that preparation aluminium oxide-titanium oxide composite granule adopts at present is that two kinds of oxide powders are mixed through physical method, adopts simple hybrid system and high-energy ball milling method usually.These two kinds of methods all have limitation to a certain degree: the advantage of simple hybrid system is that output is big; But its shortcoming is resulting aluminium oxide-titanium oxide composite granule, and to mix degree poor; Do not reach nano level mixing requirement, be difficult to satisfy the requirement of preparation high-performance inorganic stupalith; Though and high-energy ball milling method can obtain uniform mixed oxide, but will consume lot of energy, and the product amount that once obtains is limited, is difficult to mass production.Just can fundamentally solve the existing problems of method for preparing aluminium oxide-titanium oxide composite nano powder with the direct borolon of the method for chemosynthesis-TiOx nano composite granule.
At present, the method for preparing oxide powder with chemical synthesis mainly contains the precipitator method, hydrothermal method, sol-gel method etc.Prepare alumina powder jointed, titanium alkoxide with aluminium-alcohol salt and prepare titanium oxide powder technology is fairly simple comparatively speaking, output is big, and aluminium-alcohol salt, titanium alkoxide can be dissolved in a kind of organic solvent, and form uniform solution.Therefore, the alkoxide hydrolysis in the sol-gel method is to prepare one of best method of aluminium oxide-titanium oxide composite nano powder.
The step that sol-gel method prepares nano-powder is: at first alkoxide is dissolved in the organic solvent; Adding deionized water again makes hydrolysis of alkoxide, condensation reaction form colloidal sol; Again along with evaporation of water changes gel into; Gel carries out the high-temperature calcination processing then and promptly obtains composite nano powder at low temperatures in the dry xerogel that obtains loosening.
Summary of the invention
The object of the present invention is to provide a kind of directly synthetic titanium oxide massfraction is the preparation method of 30% aluminium oxide-titanium oxide composite nano powder, and this method had overcome simple in the past hybrid system can not make aluminum oxide, two kinds of powders of titanium oxide realize that nano level mixes and high-energy ball milling method highly energy-consuming and low-producing shortcoming.
The present invention implements through following measure:
A kind of preparation method of aluminum oxide titanium oxide composite nano powder is characterized in that this method steps is:
A, aluminium-alcohol salt is dissolved in the alcoholic solvent, obtains the alcoholic solution of aluminium-alcohol salt;
B, the titanium alkoxide is dissolved in alcoholic solvent, obtains the alcoholic solution of titanium alkoxide;
C, the alcoholic solution of titanium alkoxide is joined in the alcoholic solution of aluminium-alcohol salt, vigorous stirring mixes two kinds of metal alkoxide solutions;
D, water or water and alcohol, water and alcohol and slow acid are added in the metal alkoxide solution in the stirring, make the slow gel of metal alkoxide solution;
E, vigorous stirring 12-24 hour, make colloid more even;
F, with colloid leave standstill, drying, obtain xerogel;
G, xerogel is levigate calcined 1-3 hour down at 900-1200 ℃;
H, the powder porphyrize after will calcining, the titanium oxide massfraction that contains that obtains particle size and be 25-32nm is 30% aluminium oxide-titanium oxide composite nano powder.
Aluminium-alcohol salt of the present invention is ASBD or aluminum isopropylate.
Titanium alkoxide of the present invention is titanium isopropylate or tetra-n-butyl titanate.
Alcoholic solvent that the present invention mentions or alcohol refer to one or more in ethanol, Virahol and the butanols.
Acid of the present invention is one or more in hydrochloric acid, acetic acid and the nitric acid.
The titanium oxide massfraction is 30% in the feasible composite granule that obtains at last of the add-on of titanium alkoxide of the present invention.
The aluminium oxide-titanium oxide composite nano powder particle diameter of preparation about 25-32nm, even particle size, wherein aluminum oxide is the α phase, titanium oxide is the rutile phase, and calcining temperature more generally to prepare the temperature of αYang Hualv low.
Embodiment
Embodiment 1:
ASBD is dissolved in the ethanol, and heated and stirred in 85 ℃ of water-baths makes ASBD fully dissolving in ethanol.Titanium isopropylate is dissolved in the ethanol, and the ethanolic soln with titanium isopropylate joins in the ethanolic soln of ASBD then, stirs 30 minutes, slowly adds the mixture of entry and absolute ethyl alcohol, makes ASBD and titanium isopropylate hydrolysis form gel.(in the entire reaction; Metal alkoxide (ASBD and titanium isopropylate) is 1: 25 with the mol ratio of absolute ethyl alcohol; The mol ratio of metal alkoxide and water is 1: 10, and the consumption of ASBD and titanium isopropylate makes that the massfraction of titanium oxide is 30% in the last resulting composite oxides).Vigorous stirring 24 hours makes the gel of generation more even.The gel of gained was left standstill 24 hours, and oven dry gets xerogel.Xerogel is levigate, to calcine 1 hour for 1100 ℃, acquisition titanium oxide massfraction is 30% aluminium oxide-titanium oxide composite nano powder.
Embodiment 2:
ASBD is dissolved in the Virahol vigorous stirring 20 minutes.Titanium isopropylate is dissolved in the Virahol, and the aqueous isopropanol with titanium isopropylate joins in the aqueous isopropanol of ASBD then, vigorous stirring 30 minutes.The mixture that slowly adds entry and Virahol makes ASBD and titanium isopropylate hydrolysis form gel.(in the entire reaction course; Metal alkoxide (ASBD and titanium isopropylate) is 1: 9 with the mol ratio of Virahol; The mole of metal alkoxide and water is 1: 3, and it is 30% that the consumption of ASBD and titanium isopropylate makes the massfraction of titanium oxide in the composite oxides that obtain at last).Vigorous stirring 24 hours makes the gel of generation more even.The gel of gained was left standstill 24 hours the dry xerogel that gets in baking oven.Xerogel is levigate, and 1000 ℃ of calcinings 2 hours, acquisition titanium oxide massfraction was 30% aluminium oxide-titanium oxide composite nano powder.
Embodiment 3:
Aluminum isopropylate is dissolved in the butanols vigorous stirring 20 minutes.Tetra-n-butyl titanate is dissolved in the butanols; Butanol solution with tetra-n-butyl titanate joins in the butanol solution of aluminum isopropylate then; Vigorous stirring 20 minutes slowly adds the mixture of entry, hydrochloric acid and butanols, makes aluminum isopropylate and tetra-n-butyl titanate hydrolysis form gel.(in the entire reaction course; Metal alkoxide (titanium isopropylate and tetra-n-butyl titanate) is 1: 10 with the mol ratio of butanols; The mol ratio of metal alkoxide and water is 1: 4; The mol ratio of metal alkoxide and hydrochloric acid is 1: 0.2, and it is 30% that the consumption of aluminum isopropylate and tetra-n-butyl titanate makes the massfraction of titanium oxide in the composite oxides that obtain at last).Vigorous stirring 24 hours makes the gel of generation more even.The gel of gained was left standstill 24 hours the dry xerogel that gets in baking oven.Xerogel is levigate, and 1200 ℃ of calcinings 2 hours, acquisition titanium oxide massfraction was 30% aluminium oxide-titanium oxide composite nano powder.
Claims (6)
1. the preparation method of an aluminum oxide titanium oxide composite nano powder is characterized in that this method steps is:
A, aluminium-alcohol salt is dissolved in the alcoholic solvent, obtains the alcoholic solution of aluminium-alcohol salt;
B, the titanium alkoxide is dissolved in alcoholic solvent, obtains the alcoholic solution of titanium alkoxide;
C, the alcoholic solution of titanium alkoxide is joined in the alcoholic solution of aluminium-alcohol salt, vigorous stirring mixes two kinds of metal alkoxide solutions;
D, water or water and alcohol, water and alcohol and slow acid are added in the metal alkoxide solution in the stirring, make the slow gel of metal alkoxide solution;
E, vigorous stirring 12-24 hour, make colloid more even;
F, with colloid leave standstill, drying, obtain xerogel;
G, xerogel is levigate calcined 1-3 hour down at 900-1200 ℃;
H, the powder porphyrize after will calcining, the titanium oxide massfraction that contains that obtains particle size and be 25-32nm is 30% aluminium oxide-titanium oxide composite nano powder.
2. the method for claim 1 is characterized in that aluminium-alcohol salt is ASBD or aluminum isopropylate.
3. the method for claim 1 is characterized in that the titanium alkoxide is titanium isopropylate or tetra-n-butyl titanate.
4. the method for claim 1 is characterized in that alcoholic solvent or alcohol refer to one or more in ethanol, Virahol and the butanols.
5. the method for claim 1 is characterized in that acid is one or more in hydrochloric acid, acetic acid and the nitric acid.
6. the method for claim 1, the add-on that it is characterized in that the titanium alkoxide make that the titanium oxide massfraction is 30% in the composite granule that obtains at last.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274435A (en) * | 2013-05-22 | 2013-09-04 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
| CN104096551A (en) * | 2013-04-08 | 2014-10-15 | 北京航空航天大学 | Aluminum-titanium oxide aerogel bead with high specific surface area and acid amount and preparation method thereof |
| CN105175025A (en) * | 2015-09-05 | 2015-12-23 | 苏州宏久航空防热材料科技有限公司 | Silicon carbide fiber surface alumina-titanium oxide composite coating preparation method |
| CN107417272A (en) * | 2017-06-20 | 2017-12-01 | 安徽省含山瓷业股份有限公司 | A kind of manufacture method of toughening modifying aluminum oxide domestic ceramics |
| CN116218580A (en) * | 2022-09-21 | 2023-06-06 | 湖南华擎润滑油有限责任公司 | Molybdenum-titanium additive and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104096551A (en) * | 2013-04-08 | 2014-10-15 | 北京航空航天大学 | Aluminum-titanium oxide aerogel bead with high specific surface area and acid amount and preparation method thereof |
| CN104096551B (en) * | 2013-04-08 | 2018-09-25 | 北京航空航天大学 | The tilalite gas gel small ball and preparation method thereof of high-specific surface area and acid amount |
| CN103274435A (en) * | 2013-05-22 | 2013-09-04 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
| CN103274435B (en) * | 2013-05-22 | 2015-01-07 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
| CN105175025A (en) * | 2015-09-05 | 2015-12-23 | 苏州宏久航空防热材料科技有限公司 | Silicon carbide fiber surface alumina-titanium oxide composite coating preparation method |
| CN107417272A (en) * | 2017-06-20 | 2017-12-01 | 安徽省含山瓷业股份有限公司 | A kind of manufacture method of toughening modifying aluminum oxide domestic ceramics |
| CN116218580A (en) * | 2022-09-21 | 2023-06-06 | 湖南华擎润滑油有限责任公司 | Molybdenum-titanium additive and preparation method and application thereof |
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Application publication date: 20120711 |