Method for synthesizing nano-scale oxide ceramic powder body

A nano-scale oxide and ceramic powder technology, which is applied in the field of ultra-fine nano-powder preparation, can solve the problems of high decomposition temperature, expensive equipment, and large particle size of nano-powder, and achieve high sintering activity, easier operation and control , The effect of lowering the decomposition temperature

Inactive Publication Date: 2011-03-30
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage of this method is that the process is simple and easy to control, but the equipment is expensive, the decomposition temperature is high, and the particle size of the nano-powder is large.

Method used

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  • Method for synthesizing nano-scale oxide ceramic powder body
  • Method for synthesizing nano-scale oxide ceramic powder body
  • Method for synthesizing nano-scale oxide ceramic powder body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of Sodium Bismuth Titanate (Bi 0.5 Na 0.5 TiO 3 ) Nano powder

[0033] Select tetrabutyl titanate (Ti(OC 4 H 9 ) 4 ), bismuth nitrate (Bi(NO 3 ) 3 ·5H 2 O), sodium nitrate (NaNO 3 ) Is a source of titanium, bismuth and sodium, and glycerol is used as a solvent.

[0034] 13.614g tetrabutyl titanate (Ti(OC 4 H 9 ) 4 ) After being diluted in 20mL of absolute ethanol, it is added dropwise to 40mL of glycerol, and stirred at room temperature to fully mix and dissolve. Weigh 9.7014g bismuth nitrate (Bi(NO 3 ) 3 ·5H 2 O), 1.6998g sodium nitrate (NaNO 3 ), adding to the above solution in sequence, heating to 40°C, and stirring vigorously at the same time to fully dissolve, and obtaining metal salt solution A. Weigh 21.6g of sugar and dissolve it into solution A, adjust the temperature of the solution to 60°C, and stir vigorously at the same time to fully dissolve the sugar. After obtaining a yellow viscous liquid, weigh 1.6008g of ammonium nitrate (NH 4 NO 3 )...

Embodiment 2

[0035] Example 2 Preparation of titanium dioxide nanopowder (organic solvent)

[0036] Tetrabutyl titanate was selected as the titanium source, and absolute ethanol was used as the solvent.

[0037] Dilute 17 g of tetrabutyl titanate in 40 mL of absolute ethanol at room temperature to obtain solution A, add 27 g of sugar to solution A, adjust the temperature to 60° C., stir vigorously to make the solution fully dissolved. After obtaining a yellow viscous liquid, weigh 2g of ammonium nitrate (NH 4 NO 3 ), stir to dissolve. The resulting solution was dried at 69°C for 4 hours to remove most of the solvent, and then transferred to a 190°C drying oven for 24 hours. The powder synthesis is carried out at 300℃, 500℃, 600℃, 700℃ and 900℃ respectively for 2-6 hours.

[0038] Such as image 3 , 4 As shown, XRD characterization shows that a pure anatase phase is formed at 300°C, a pure rutile phase is formed at 700°C, and two phases coexist at the two temperature points in the middle. XRD p...

Embodiment 3

[0039] Example 3 Preparation of titanium dioxide nanopowder (water)

[0040] Titanium tetrachloride stabilized with alcohols (TiCl 4 ) As the titanium source, deionized water is used as the solvent.

[0041] Dissolve 380 g of titanium tetrachloride in 400 mL of absolute ethanol to obtain 548 g of stable titanium tetrachloride solution. Weigh 2.73582 g of the above stable solution, and dissolve it in 10 mL of deionized water at room temperature to obtain solution A. Weigh 10.8g of sugar, add to liquid A and stir to dissolve. Weigh 1g of ammonium nitrate (NH 4 NO 3 ), stir to dissolve. The resulting solution was first dried at 105°C for 4 hours to remove most of the solvent, and then transferred to a drying oven at 190°C for 24 hours. Pre-fired at 300℃, 500℃, 700℃ and 900℃ for 6h for powder synthesis.

[0042] Such as Figure 5 , 6 As shown, the XRD structure analysis shows that a well-crystallized anatase phase can be obtained at 300°C and 500°C, a pure rutile phase is formed at 9...

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Abstract

The present invention belongs to the technology of preparing ultra-fine nano powder and in particular discloses a synthetic method of preparing nano oxide ceramic powder. In the method, sugar is added for pyrolysis. Under the atmospheric conditions, a metal ion source is dissolved in an appropriate solvent; sugar and foamer ammonium nitrate are added; the prepared solution is dried; and the prepared substance is pre-sintered at a lower temperature to synthesize the nano powder. The synthetic method requires no high-temperature sintering, inhibits the generation of agglomeration and excessive growth of grains, and can prepare the ceramic powder with the grain size of 10 to 90nm, uniform distribution of grains, high sintering activity, and uniform and stable ingredients. The synthetic method has universality for preparing various oxide nano powder, and can be used for preparing powder only by using the appropriate solvent to dissolve the metal ion source; and the prepared powder has higher chemical activity in wider application range.

Description

Technical field [0001] The invention belongs to the preparation technology of ultrafine nano powder, and particularly relates to a method for synthesizing nano-level oxide ceramic powder. Background technique [0002] Oxide ceramic powder is used as a raw material for preparing a variety of ceramics, and its purity and fineness have a direct impact on the performance and quality of ceramic components, especially electronic components. With the rapid development of electronic components in the direction of high integration, high precision, high reliability, multi-function and miniaturization, the industry has put forward higher requirements for the purity, particle size, molding and sintering characteristics of the powder. Therefore, the development of high-purity, ultra-fine ceramic powder with ideal particle morphology has broad application prospects and important strategic significance. [0003] The preparation methods of ceramic powder mainly include solid phase method, precipi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/626C04B35/01
Inventor 齐建全孙黎杜鹏王晓慧马振伟李龙土
Owner TSINGHUA UNIV
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