Method for low-temperature preparation of pure phase oxide material

An oxide and pure-phase technology, which is applied in the field of low-temperature preparation of pure-phase oxide materials, can solve the problems of lowering the synthesis temperature, limiting practical applications, and short reaction time, so as to reduce the synthesis reaction temperature, overcome uneven mixing and liquid phase The process is complex and the effect of reducing energy consumption

Active Publication Date: 2008-08-27
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology

Although the combustion method can effectively reduce the synthesis temperature, the reaction time is short, and it is easy to obtain powder materials with small particle sizes, but the samples obtained by this method are often not high in purity, and powder sintering is prone to occur.
Although the above methods have their own advantages, their practical application is limited due to their own defects.

Method used

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  • Method for low-temperature preparation of pure phase oxide material
  • Method for low-temperature preparation of pure phase oxide material
  • Method for low-temperature preparation of pure phase oxide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 0.045 moles (19.32 grams) of Zr(NO 3 ) 4 ·5H 2 O and 0.005 mol (1.91 g) In(NO3 ) 3 4.5H 2 O was dissolved in 100 ml of distilled water and stirred well, then slowly added 5.00 g of CaCO 3 , and stir until all the calcium carbonate is dissolved. Add 5ml of PEG200 (polyethylene glycol) to the above solution, and continue stirring until the solution turns into a gel. React the gel at 850°C for 2 hours to obtain a uniformly dispersed high-purity CaZr of about 60 nanometers 0.90 In 0.10 o 2.95 Powder. More than 99% dense ceramics can be obtained by sintering at 1350°C for 6 hours. Mechanical tests show that the bending resistance of ceramics reaches 283Mpa; the results of proton conductivity test show that the proton conductivity of grain boundaries in hydrogen-containing and water-containing atmospheres is 2.64×10 at 800°C. -3 S cm -1 , the bulk proton conductivity is 8.72×10 -4 S cm -1 The conductance of the grain boundary is greatly improved, and the conductan...

Embodiment 2

[0029] 0.05 moles (21.47 grams) of Zr(NO 3 ) 4 ·5H 2 O and 0.05 mol (19.1 g) In(NO 3 ) 3 4.5H 2 O was dissolved in 200 ml of distilled water and stirred well, then slowly added 22.53 g of BaC 2 o 4 , and stir until the barium oxalate is completely dissolved. Add 20ml of PEG400 (polyethylene glycol) to the above solution, and continue stirring until the solution turns into a gel. The gel was reacted at 700°C for 10 hours to obtain a uniformly dispersed 60nm white powder BaZr 0.50 In 0.50 o 2.75 . Ceramics with a density greater than 98% can be obtained by sintering at 1400°C for 5 hours. The proton conductivity test results show that the ceramics obtained by pressing and sintering the powder obtained by this method have good proton conductivity. At 800°C, the proton conductivity can reach 10 -3 order of magnitude.

Embodiment 3

[0031] 0.09 mol (39.08 g) Ce(NO 3 ) 3 ·6H 2 O and 0.01 mol (4.34 g) La(NO 3 ) 3 ·6H 2 O was dissolved in 200 ml of distilled water and stirred evenly, then slowly added 17.13 g of Ba(OH) 2 , and stir until the barium hydroxide is completely dissolved. Add 10ml of PVP (polyvinylpyrrolidone) to the above solution, and continue stirring until the solution turns into a gel. The gel was reacted at 850°C for 6 hours to obtain uniformly dispersed 80nm BaCe 0.90 ln 0.10 o 2.95 Powder. Under wet hydrogen, the conductivity can reach 10 at 1000°C -1 Magnitude.

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Abstract

The invention relates to a method for preparing pure phase oxide at low temperature, belonging to the material preparation technical field. The inventive method referrs the chemical formual of ABM<1-x>O3, (x=0.50-1.0), to dissolve the nitrates of cerium, zirconium, titanium or gallium into water, and slowly add the carbonate, oxalate, nitrate, acetate, basic hydroxide, hydroxide or oxide of calcium, barium, strontium, lead or lanthanide metal element into the solution to be dissolved completely, heats and mixes precursor solution in water bath or oil bath at 50-100DEG C, until the solution changes to gel, and reacts the gel at 1000DEG C for 2-10h, to obtain oxide materials of pure phase and high crystallinity. The method for preparing pure phase oxide at low temperature has simple process, easy operation, low cost, high product purity and easily accessible industrial production.

Description

technical field [0001] The invention relates to a method for preparing a pure-phase oxide material at low temperature, belonging to the field of material preparation. technical background [0002] With the global energy crisis and environmental pollution gradually intensified, countries all over the world are spending huge sums of money on the development of new energy materials. In 2005, China, the United States, Japan, South Korea, Russia and the European Union launched the largest international scientific cooperation project after the International Space Station - the ITER program (international heat). Huge sums of money are used for the development of new energy materials. In 2005, China, the United States, Japan, South Korea, Russia and the European Union launched the largest international scientific cooperation project after the International Space Station - the ITER program (International Thermonuclear Fusion Reactor Cooperation Program) began Implemented, once the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01C04B35/624C04B35/50C04B35/48C04B35/462
Inventor 温兆银韩金铎张敬超吴相伟林宾徐孝和顾中华
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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