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Method for preparing aluminum titanate nano powder by non-hydrolytic sol-gel process

A technology of nano-powder and aluminum titanate, which is applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of coarsening, aluminum titanate powder agglomeration, and coarse powder particles, and achieve high synthesis rate, Agglomeration inhibition and good dispersibility

Inactive Publication Date: 2010-09-08
JINGDEZHEN CERAMIC INSTITUTE
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Problems solved by technology

The temperature of solid-phase synthesis of aluminum titanate is as high as 1500 °C, and the synthesized powder has coarse particles and low activity; when the precipitation method is used to synthesize aluminum titanate, it is difficult to synthesize aluminum titanate due to the large difference in the solubility product of aluminum and titanium precipitates. Achieve uniform precipitation, thereby affecting the synthesis rate of aluminum titanate powder; the traditional hydrolytic sol-gel synthesis of aluminum titanate has the advantages of good uniformity, high purity, and precise control of the stoichiometric ratio, but it is generally based on Alcoholates of aluminum and titanium are precursor raw materials, and the price of alkoxide is high, and the hydrolysis rate of different alkoxide precursors is different, which makes it difficult to achieve uniform mixing of components in the gel, and it is difficult to achieve low-temperature synthesis of aluminum titanate powder The target of the body, its synthesis temperature is generally higher than 1300 ℃
Since the temperature of the aluminum titanate synthesized by the hydrolytic sol-gel method is as high as 1300 ° C, the synthesized aluminum titanate particles are easy to agglomerate and coarsen, even if the dispersant is added, the purpose of preventing powder agglomeration cannot be achieved
ZL200610005316.5 discloses a method for synthesizing composite oxide powder by non-hydrolytic sol-gel method using alcohol as oxygen donor. Although the invention synthesizes aluminum titanate powder at a low temperature of 750°C, it does not solve the problem of titanium The difficult problem that aluminum acid powder is easy to agglomerate
On the one hand, if a dispersant is directly added to the precursor mixed solution like the traditional hydrolytic sol-gel method, the result is that the reactivity of the precursor is reduced, which affects the non-hydrolytic polycondensation reaction, resulting in low-temperature synthesis of titanic acid. aluminum doesn't work well
On the other hand, if no dispersant is added, the gelation reaction temperature of the non-hydrolytic sol-gel method is higher (generally above 110°C), which will easily cause the growth of colloidal particles and the agglomeration of colloidal particles. Lead to severe agglomeration and poor dispersion of the prepared aluminum titanate powder

Method used

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  • Method for preparing aluminum titanate nano powder by non-hydrolytic sol-gel process
  • Method for preparing aluminum titanate nano powder by non-hydrolytic sol-gel process
  • Method for preparing aluminum titanate nano powder by non-hydrolytic sol-gel process

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Effect test

Embodiment 1

[0031] Aluminum titanate sol was prepared according to the molar ratio of aluminum to titanium: 2:1, and 9.707g of anhydrous aluminum trichloride (analytical pure) was dissolved in 5.0ml of chloroform (chemically pure), sealed for use; 4.0ml of tetrachloromethane Titanium chloride (chemically pure) was added dropwise into 17.0 ml of n-butanol (chemically pure), and after sufficient magnetic stirring, a n-butanol solution of titanium tetrachloride was obtained. Then slowly add the n-butanol solution of titanium tetrachloride into the chloroform solution of anhydrous aluminum trichloride, and after magnetic stirring is sufficient, put the mixed solution in an oil bath at 80°C for 8 hours to form titanic acid. Aluminum sol. Dissolve 0.06g PEG1000 (analytical pure) in 5.0ml dichloromethane (chemically pure), add the dichloromethane solution of PEG1000 dropwise in aluminum titanate sol, carry out magnetic stirring, put into auxiliary pressure field reaction vessel, A wet gel was o...

Embodiment 2

[0033] In Example 1, 17.0ml of n-butanol (chemically pure) was changed to 11.0ml of ethanol (chemically pure), PEG1000 was changed to glycerin, and the precursor mixed solution was refluxed for 10 hours under 90°C oil bath heating condition to form aluminum titanate sol, and other The conditions remain unchanged, and aluminum titanate nanopowder with good dispersibility is obtained. The XRD analysis of product shows that the powder synthesized is aluminum titanate (see Figure 9 ); Figure 10 The TEM photos in the above show that the powder has good dispersion and the average particle size is less than 30nm.

Embodiment 3

[0035] Change PEG1000 in Example 1 to polyvinylpyrrolidone, change chloroform to carbon tetrachloride, change 17.0ml n-butanol (chemically pure) to 14.0ml isopropanol (chemically pure), and put aluminum titanate sol into auxiliary pressure After the field reaction container, the aluminum titanate wet gel was obtained by heating at 130° C. for 20 h, and the aluminum titanate nanopowder with good dispersibility was obtained under the same other conditions. The XRD analysis of product shows that the powder synthesized is aluminum titanate (see Figure 11 ); Figure 12 The TEM photos in the above show that the powder has good dispersion and the average particle size is less than 30nm.

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Abstract

The invention discloses a method for preparing an aluminum titanate nano powder by a non-hydrolytic sol-gel process, which comprises the following steps of: using anhydrous aluminum trichloride and titanium tetrachloride as precursors, using a low-carbon alcohol as an oxygen donor, uniformly mixing a low-carbon alcohol solution of the titanium tetrachloride and a chloroalkyl solution of the aluminum trichloride, then refluxing for 8-10 hours in an oil bath at 80-100 DEG C, adding a dispersant, stirring uniformly, loading in a pressure vessel, heating for 15-24 hours at 110-130 DEG C to form a wet gel, drying, grinding and calcining for 15-60 minutes at 750-800 DEG C to obtain the aluminum titanate nano powder with high synthetic ratio and good dispersivity.

Description

technical field [0001] The invention relates to the technical field of inorganic nano-powder preparation, in particular to a method for preparing aluminum titanate nano-powder by a non-hydrolytic sol-gel process. Background technique [0002] Aluminum titanate (Al 2 TiO 5 , referred to as AT) material has a high melting point (1860 ° C), low expansion (α < 1.5 × 10 -6 / °C), low thermal conductivity (1.5W / m K), good thermal shock resistance and strong corrosion resistance, are widely used in metals, steel, chemicals, glass, environmental protection, automobiles, industrial furnaces and other industries. At present, the main methods for preparing aluminum titanate powder include solid-phase method, co-precipitation method, hydrolytic sol-gel method and non-hydrolytic sol-gel method. The temperature of solid-phase synthesis of aluminum titanate is as high as 1500 °C, and the synthesized powder has coarse particles and low activity; when the precipitation method is used t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00B82B3/00
Inventor 江伟辉胡紫刘健敏朱庆霞谭训彦包镇红虞澎澎苗立锋
Owner JINGDEZHEN CERAMIC INSTITUTE
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