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Method for preparing high-stability gamma-phase nanometer lanthanum sulfide powder in low temperature

A high-stability, lanthanum sulfide technology, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve problems such as high cost, difficulty in obtaining pure γ-phase products, incomplete reaction, etc., achieve broad application prospects, shorten Heat preservation time and low cost effect

Inactive Publication Date: 2013-06-19
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to avoid the deficiencies of the prior art, the present invention proposes a method for preparing high-stability γ-phase nano-lanthanum sulfide powder at low temperature, which overcomes the high cost, incomplete reaction and difficulty in obtaining pure γ-phase products in the prior art lack of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The first step, the configuration of the reaction solution

[0030] At 25°C, 35.3 g of analytically pure LaCl 3 ·6H 2 O was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of lanthanum chloride; then 14.3 grams of analytically pure sodium N, N-dimethyldithiocarbamate (NaS 2 CNMe 2 ) was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of N,N-dimethyldithiocarbamate sodium; then 15.6 grams of 2,2'-bipyridyl was dissolved in absolute ethanol to prepare A saturated solution of 2,2'-bipyridine was obtained. The molar ratios of the solutes in the above solutions are respectively (LaCl 3 ·6H 2 O): (NaS 2 CNMe 2 ):(2,2'-bipy)=1:3:1. Then the saturated solution of lanthanum chloride and the saturated solution of N,N-dimethyl dithiocarbamate sodium were mixed, stirred with a magnetic stirrer until uniform, and then 2,2' -The bipyridyl saturated solution was added dropwise into the two saturated...

Embodiment 2

[0036] The first step, the configuration of the reaction solution

[0037] At 25°C, 17.7 g of analytically pure LaCl 3 ·6H 2 O was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of lanthanum chloride; then 7.2 grams of analytically pure sodium N,N-dimethyldithiocarbamate (NaS 2 CNMe 2 ) was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of N,N-dimethyldithiocarbamate sodium; then 7.8 grams of 2,2'-bipyridyl was dissolved in absolute ethanol to prepare A saturated solution of 2,2'-bipyridine was obtained. The molar ratios of the solutes in the above solutions are respectively (LaCl 3 ·6H 2 O): (NaS 2 CNMe 2 ):(2,2'-bipy)=1:3:1. Then mix the saturated solution of lanthanum chloride and the saturated solution of N,N-dimethyldithiocarbamate sodium, stir until uniform with a magnetic stirrer, and then mix the 2,2' -The bipyridine saturated solution was added dropwise into the two saturated solu...

Embodiment 3

[0043] The first step, the configuration of the reaction solution

[0044]At 25°C, 26.7 g of analytically pure LaCl 3 ·6H 2 O was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of lanthanum chloride; then 10.8 grams of analytically pure sodium N, N-dimethyldithiocarbamate (NaS 2 CNMe 2 ) was dissolved in absolute ethanol under stirring conditions to obtain a saturated solution of N,N-dimethyldithiocarbamate sodium; then 11.7 grams of 2,2'-bipyridyl was dissolved in absolute ethanol to prepare A saturated solution of 2,2'-bipyridine was obtained. The molar ratios of the solutes in the above solutions are respectively (LaCl 3 ·6H 2 O): (NaS 2 CNMe 2 ):(2,2'-bipy)=1:3:1. Then mix the saturated solution of lanthanum chloride and the saturated solution of N,N-dimethyldithiocarbamate sodium, stir until uniform with a magnetic stirrer, and then stir the 2,2' -The bipyridine saturated solution was added dropwise at a speed of 30 drops / m...

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Abstract

The invention relates to a method for preparing high-stability gamma-phase nanometer lanthanum sulfide powder in low temperature. The method includes the steps as follows: preparing solid-state compound (La (S2CNMe2)3(2,2 '-bipy)) with saturated solution of lanthanum chloride, saturated solution of N,N-Sodium dimethyldithiocarbamate and 2,2'-bipyridyl solution; preparing amorphous La2S3 powder ina closed microwave solvent thermal reaction kettle; and finally preparing the high-stability pure gamma-phase La2S3 powder in an atmosphere tube furnace. In the invention, the experimental temperature is lowered, the temperature keeping time is shortened and the strict requirements for anhydrous and anaerobic environment are eliminated. The gamma-phase La2S3 belongs to a stable phase when the temperature is higher than 1300 DEG C, therefore the lanthanum sulfide powder prepared by the method can be stably kept in a gamma-phase structure in the full temperature range. Simultaneously, the method is simple in technology, low in cost and suitable for preparing high-stability and high-purity gamma-phase lanthanum sulfide powder in large scales.

Description

technical field [0001] The invention relates to a method for preparing high-stability γ-phase nano-lanthanum sulfide powder at low temperature. The γ-phase lanthanum sulfide powder prepared by the method can still maintain a γ-phase structure at room temperature to 1300°C, and has a high Thermodynamic stability, suitable for providing raw materials for preparing cubic lanthanum sulfide polycrystalline materials by hot pressing sintering. Background technique [0002] There are three crystal phase structures in lanthanum sulfide compounds: α phase, β phase and γ phase, in which α-La 2 S 3 It belongs to the orthorhombic system and is a stable phase at room temperature; β-La 2 S 3 It is a tetragonal structure, and its thermodynamic stability ranges from 900°C to 1300°C; γ-La 2 S 3 Body-centered cubic structure (Th with metal holes 3 P 4 structure), which is a stable phase at temperatures above 1300 °C. In practical technical applications, γ-phase lanthanum sulfide has a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y40/00
Inventor 李焕勇付泽华罗发介万奇李培森
Owner NORTHWESTERN POLYTECHNICAL UNIV