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A kind of method for preparing yttrium zirconate by oxalic acid dihydrazide combustion method

A technology of oxalic acid dihydrazide and yttrium zirconate, which is applied in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve the problems of high temperature of reactants, large size of generated products, and uncontrollable particle size, etc., so as to promote Rapid formation, low synthesis temperature, and easy operation

Active Publication Date: 2018-06-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above methods, the disadvantage of the high-temperature solid-phase sintering method is that the synthesis temperature is high, the size of the generated product is large, the particle size cannot be controlled, and there is an impure phase due to uneven distribution of components, which has a stoichiometric loss; the simple sol-gel method The disadvantage is that the reaction temperature is higher and the reaction time is longer
The advantage of the hydrothermal method is that it overcomes the disadvantages of uneven distribution of components and stoichiometric loss. However, the requirements for equipment are higher and the reaction time is longer.

Method used

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  • A kind of method for preparing yttrium zirconate by oxalic acid dihydrazide combustion method
  • A kind of method for preparing yttrium zirconate by oxalic acid dihydrazide combustion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Weigh the analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2 Dissolve O in a beaker with deionized water to prepare a solution with a Y ion concentration of 0.1 mol / L, wherein the molar ratio of Y to Zr is 1:1.

[0027] 2) Using oxalic acid dihydrazide as complexing agent and combustion agent, adding 1 mol / L oxalic acid dihydrazide aqueous solution into the stirred solution by dropwise addition to obtain a mixed solution; wherein, oxalic acid dihydrazide and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 2:1.

[0028] 3) After stirring for 2 hours with a magnetic stirrer at a speed of 350 rpm, a stable mixed solution is obtained, and the stable mixed solution is placed in a constant temperature magnetic stirrer, and the temperature is controlled at 60 ° C. After 5 hours in a water bath, the excess water is evaporated to obtain a white color gel.

[0029] 4) Place the obtained white gel in a muffle furnace that has been preheated to 350° C., and react for ...

Embodiment 2

[0032] 1) The analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2Dissolve O in a beaker with deionized water to prepare a solution with a Y ion concentration of 0.2 mol / L, where the molar ratio of Y to Zr is 1:1.

[0033] 2) Using oxalic acid dihydrazide as complexing agent and combustion agent, adding 1 mol / L oxalic acid dihydrazide aqueous solution into the stirred solution by dropwise addition to obtain a mixed solution; wherein, oxalic acid dihydrazide and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 3:1.

[0034] 3) After stirring for 2 hours with a magnetic stirrer at a speed of 500 rpm, a stable mixed solution is obtained, and the stable mixed solution is placed in a constant temperature magnetic stirrer, and the temperature is controlled at 80°C. After 5 hours in a water bath, the excess water is evaporated to obtain a white color gel.

[0035] 4) Put the obtained white gel in a muffle furnace whose temperature has been preheated to 350° C., and react for ...

Embodiment 3

[0040] 1) The analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2 Dissolve O in a beaker with deionized water to prepare a solution with a concentration of 0.3 mol / L, wherein the molar ratio of Y to Zr is 1:1.

[0041] 2) Using oxalic acid dihydrazide as complexing agent and combustion agent, add 1.5mol / L oxalic acid dihydrazide aqueous solution into the stirred solution by dropwise addition to obtain a mixed solution; wherein, oxalic acid dihydrazide with Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 3:1.

[0042] 3) Stirring with a magnetic stirrer at a speed of 400 rpm for 3 hours to obtain a stable mixed solution, put the stable mixed solution into a constant temperature magnetic stirrer, control the temperature at 70°C, and evaporate the excess water after 4 hours in a water bath to obtain a white gel.

[0043] 4) Put the obtained white gel in a muffle furnace whose temperature has been preheated to 400° C., and react for 15 minutes to promote the combustion o...

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Abstract

The invention provides a method for preparing yttrium zirconate by using an oxalyl dihydrazide combustion process. The method comprises the following steps: adding Y(NO3)3.6H2O and ZrO(NO3)2.H2O into deionized water to prepare a solution and adding an aqueous oxalyl dihydrazide solution into the solution drop by drop so as to obtain a mixed solution; subjecting the mixed solution to stirring, then evaporating water and carrying out heating so as to obtain a fluffy block; and subjecting the fluffy block to heat treatment at 500 to 700 DEG C for 1 to 3 h so as to obtain yttrium zirconate. The method provided by the invention is simple in process, convenient and easy to operate and low in preparation cost. The method can promote low-temperature sintering of powder and is beneficial for synthesis of yttrium zirconate powder with high sintering activity. A reaction system is mild and controllable; a combustion product contains few impurities and is low in loss late; heat released in combustion of oxalyl dihydrazide in a short period of time can promote low-temperature rapid synthesis of yttrium zirconate; and the method has the advantages of energy conservation and environmental protection compared with a conventional high-temperature solid-phase method.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a method for preparing yttrium zirconate by an oxalic acid dihydrazide combustion method. Background technique [0002] In recent years, Re 2 Zr 2 o 7 (Re=rare earth element)-type ternary oxides have attracted great attention of researchers. This type of composite oxide is mainly pyrochlore-type structure (Fd3m space group) or defect fluorite-type structure (Fm3m space group). The pyrochlore-type structure will gradually transform into a defective fluorite-type structure with the decrease of the cation radius ratio. due to Y 3+ has a smaller size, so yttrium zirconate (Y 2 Zr 2 o 7 ) is a defect fluorite structure. [0003] As an important class of functional materials, rare earth zirconates have attracted great attention in their synthesis and properties due to their low thermal conductivity, high thermal expansion coefficient, high stability, and ability...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00
CPCC01G25/00C01P2002/72C01P2004/03C01P2006/80
Inventor 曹丽云罗艺佳黄剑锋吴建鹏冯亮亮李瑞梓
Owner SHAANXI UNIV OF SCI & TECH
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