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Method for preparing hydrated sodium-cobalt-oxygen superconducting material

A technology of hydrated sodium cobalt oxide and superconducting materials, which is applied in the usage of superconducting elements, superconducting devices, superconducting/high conducting conductors, etc. It can solve the problems of insufficient reaction between compounds, poor material performance, high reaction temperature, etc. Problems, to achieve the effect of shortening the production cycle, reducing costs, and simple process

Inactive Publication Date: 2008-07-30
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The weak point of existing preparation method is: Na 0.3 CoO 2 1.3H 2 O superconducting precursor NaxCoO 2 prepared by solid phase reaction
This kind of solid-phase reaction at high temperature, due to insufficient contact between solid compounds, makes the reaction between compounds insufficient, so that the chemical composition of the finished product is uncertain and cannot be controlled in advance, and its particles are coarse and poor in uniformity. , poor material properties
And the reaction temperature is high, the high temperature time is long, the energy consumption is large, and the production cost is high

Method used

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  • Method for preparing hydrated sodium-cobalt-oxygen superconducting material

Examples

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Embodiment 1

[0031] A method for preparing a hydrated sodium cobalt oxide superconducting material, the steps of which are precursor preparation, oxidation and doping, and hydration in sequence. The method of precursor preparation is:

[0032] Sodium cobaltoxide Na x COO 2 , x=0.7, the stoichiometric ratio of the mol ratio Na of middle sodium, cobalt Na:Co=0.7:1 weighs raw material sodium carbonate Na 2 CO 3 with cobalt oxalate CoC 2 o 4 ), the raw materials were dissolved in 28% ammonia water for reaction, and the reacted solution was sprayed into liquid nitrogen with a nebulizer, and placed in a vacuum desiccator for lyophilization and vacuum drying to obtain a mixed powder.

[0033]First raise the temperature of the mixed powder to 300°C, keep it warm for 0.5 hours, carry out preheating and decomposition, then raise the temperature to 600°C, keep it warm for 12 hours, and carry out thermal decomposition; finally raise the temperature to 800°C, keep it warm for 18 hours for sinterin...

Embodiment 2

[0037] This example is basically the same as Example 1, the difference is only:

[0038] According to the preparation material sodium cobalt oxide NaxCoO 2 , the stoichiometric ratio of x=0.5, that is, the molar ratio Na:Co=0.5:1 Weigh the raw material Na 2 CO 3 with CoC 2 o 4 . The resulting NaxCoO 2 The chemical formula of superconducting material precursor is Na 0.5 CoO 2 . Experiments have shown that the Na prepared in this example 0.3 CoO 2 1.3H 2 The superconducting transition temperature of O superconducting material is 3.0K.

[0039] Then put the mixed powder into the concentration of 0.1mol / L bromo-acetonitrile (CH 3 CN) solution, take it out after soaking for 1 day, rinse with acetonitrile, and then rinse with deionized water for oxidation and doping. , and finally place it in water vapor for 1 day for hydration, and the hydrated sodium cobalt oxide superconducting material Na 0.3 CoO 2 1.3H 2 O.

Embodiment 3

[0041] This example is basically the same as Example 1, the difference is only:

[0042] According to the preparation material sodium cobalt oxide NaxCoO 2 , the stoichiometric ratio of x=1.0, that is, the molar ratio Na:Co=1:1 Weigh the raw material Na 2 CO 3 with CoC 2 o 4 . The chemical formula of the prepared material precursor is NaCoO 2 . Experiments have shown that the Na prepared in this example 0.3 CoO 2 1.3H 2 The superconducting transition temperature of the O superconducting material is less than 2.0K.

[0043] Then put the mixed powder into the concentration of 2mol / L bromo-acetonitrile (CH 3 CN) solution, take it out after soaking for 7 days, rinse with acetonitrile, and then rinse with deionized water for oxidation and doping. Finally, after placing it in water vapor for 5 days for hydration, the hydrated sodium cobalt oxide superconducting material Na 0.3 CoO 2 1.3H 2 O.

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Abstract

The invention relates to a method for preparing hydration natrium-cobalt-oxygen superconducting materials, wherein, a method for preparing precursor comprises the following steps: according to a molar ratio of the natrium and cobalt in the natrium-cobalt-oxygen (NaxCoO2, x is more than or equal to 0.5 and is less than or equal to 1.0) that Na: Co is x:1, raw material sodium carbonate (Na2CO3) and cobalt oxalate (CoC2O4) are weighed; the raw material is dissolved in aqua ammonia of 25 to 35 percent to carry out reaction; the reacted liquor is sprayed in liquid nitrogen with a sprayer; then the liquid nitrogen is put into a vacuum dryer to carry out freezing vacuum drying to obtain mixed powder which is warmed up to 500 to 700 DEG C and the temperature is preserved for 1 to 20 hours to carry out thermal decomposition; the mixed powder is again warmed up to 700 to 900 DEG C and the temperature is preserved for 1 to 30 hours to carry out sintering; then the mixed powder is naturally cooled to room temperature; the sinter is taken out and is grinded into the powder. The product of the invention has the advantages of definite chemical component, easiness to be prior controlled, even granule, small granularity, good material performance, low preparation temperature, short period and low cost.

Description

technical field [0001] The invention relates to a preparation method of a superconducting material, in particular to a preparation method of a hydrated sodium cobalt oxide superconducting material. Background technique [0002] Sodium cobalt oxide (NaxCoO 2 0.5≤x≤1.0) materials have rich physical phenomena, there are mutual competition between charge and spin degrees of freedom, and a variety of complex phase diagrams such as long-range and short-range spin correlations, charge ordering, and superconductivity. A promising thermoelectric material and battery cathode material with superconductivity upon hydration. Especially sodium cobalt oxide (NaxCoO 2 ) The hydrated sodium cobalt oxide superconducting material Na formed after hydration 0.3 COO 2 1.3H 2 O has very good superconductivity, is an excellent superconducting material, and has a good application prospect. Existing synthetic Na 0.3 COO 2 1.3H 2 The method of O is a solid-state reaction method, including th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01C04B35/622C01G51/00H01B12/00
CPCY02E40/64Y02E40/60
Inventor 张勇赵勇伍志寰
Owner SOUTHWEST JIAOTONG UNIV
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