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Method for preparing nano Co2(OH)3Cl gas sensitive material by ultrasonic-microwave hydrothermal method and application

A technology of microwave hydrothermal method and gas-sensitive materials, which is applied in nanotechnology, nanotechnology, material resistance, etc., can solve the problems of unsatisfactory nanomaterials and high energy consumption, and achieve uniform shape distribution, high reactivity, and shortened The effect of reaction time

Inactive Publication Date: 2015-04-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently preparing M 2 (OH) 3 X series materials are mainly traditional hydrothermal method, but the preparation time of this method is often tens or even dozens of hours, the energy consumption is very large, and the particle size of the product is in the micron level, which cannot meet the needs of preparing nanomaterials

Method used

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  • Method for preparing nano Co2(OH)3Cl gas sensitive material by ultrasonic-microwave hydrothermal method and application
  • Method for preparing nano Co2(OH)3Cl gas sensitive material by ultrasonic-microwave hydrothermal method and application
  • Method for preparing nano Co2(OH)3Cl gas sensitive material by ultrasonic-microwave hydrothermal method and application

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Experimental program
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Embodiment 1

[0033] 1. Preparation of nano-Co by ultrasonic-microwave hydrothermal method 2 (OH) 3 Cl gas sensitive material

[0034] 1) Analytical pure cobalt acetate tetrahydrate (Co(CH 3 COO) 2 4H 2 O) dissolved in deionized water to prepare Co 2+ The concentration is 1 μmol L -1 solution A; to solution A was added TiCl as a catalyst 3 hydrochloric acid solution, and then ultrasonically pretreated at 100W for 10min to obtain Co 2+ The concentration is 0.7μmol·L -1 Precursor B; among them, TiCl 3 The hydrochloric acid solution is composed of TiCl with a volume ratio of 1:1 3 and 6mol L -1 mixed with hydrochloric acid;

[0035] 2) Use analytically pure ammonia water to adjust the pH value of precursor B to 5.0, and then add it to the reaction kettle, the filling degree of the reaction kettle is less than 50%; react under microwave hydrothermal conditions, after the reaction is completed, the reaction kettle is obtained The reaction system was cooled to below 60°C, and then the...

Embodiment 2

[0041] 1. Preparation of nano-Co by ultrasonic-microwave hydrothermal method 2 (OH) 3 Cl gas sensitive material

[0042] 1) Analytical pure cobalt acetate tetrahydrate (Co(CH 3 COO) 2 4H 2 O) dissolved in deionized water to prepare Co 2+ The concentration is 10 μmol L -1 solution A, add TiCl as a catalyst to solution A 3 hydrochloric acid solution, and then ultrasonically pretreated at 200W for 10min to obtain Co 2+ The concentration is 7 μmol L -1 Precursor B; among them, TiCl 3 The hydrochloric acid solution is composed of TiCl with a volume ratio of 1:5 3 and 6mol L -1 mixed with hydrochloric acid;

[0043] 2) Use analytically pure ammonia water to adjust the pH value of precursor B to 8.0, and then add it to the reactor, and the filling degree of the reactor is less than 50%; react under microwave hydrothermal conditions, and after the reaction is completed, obtain The reaction system was cooled to below 60°C, and then the product in the reaction system in the ...

Embodiment 3

[0049] 1. Preparation of nano-Co by ultrasonic-microwave hydrothermal method 2 (OH) 3 Cl gas sensitive material

[0050] 1) Analytical pure cobalt acetate tetrahydrate (Co(CH 3 COO) 2 4H 2 O) dissolved in deionized water to prepare Co 2+ The concentration is 20μmol L -1 solution A, add TiCl as a catalyst to solution A 3 hydrochloric acid solution, and then ultrasonically pretreated at 50W for 20min to obtain Co 2+ The concentration is 15 μmol L -1 Precursor B; among them, TiCl 3 The hydrochloric acid solution is composed of TiCl with a volume ratio of 1:8 3 and 6mol L -1 mixed with hydrochloric acid;

[0051] 2) Use analytically pure ammonia water to adjust the pH value of precursor B to 10.0, and then add it to the reaction kettle, the filling degree of the reaction kettle is less than 50%; react under microwave hydrothermal conditions, after the reaction is completed, the reaction kettle is obtained The reaction system was cooled to below 60°C, and then the produ...

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Abstract

The invention discloses a method for preparing a nano Co2(OH)3Cl gas sensitive material by an ultrasonic-microwave hydrothermal method. The method comprises the following steps: dissolving cobalt acetate tetrahydrate into deionized water to prepare a solution A; adding A TiCl3 hydrochloric acid solution to the solution A, and then carrying out ultrasonic pretreatment to obtain a precursor B; adjusting the pH value of the precursor B to 3.0-11.0; adding to a reaction kettle, reacting under the microwave hydrothermal condition; after reaction is ended, centrifugally collecting a product in the reaction system obtained from the reaction kettle and washing, thereby obtaining the nano Co2(OH)3Cl gas sensitive material. The nano Co2(OH)3Cl gas sensitive material prepared by the method is applied to fabrication of a gas sensitive element, so that the method is simple in process, low in energy consumption and high in synthetic efficiency; and the prepared material is small in particle size and uniform in distribution, and can be applied to fabrication of the gas sensitive element.

Description

technical field [0001] The invention relates to a preparation method and application of a gas-sensitive material, in particular to an ultrasonic-microwave hydrothermal method for preparing nano-Co 2 (OH) 3 Methods and applications of Cl gas sensitive materials. Background technique [0002] Hydroxy transition metal halide M 2 (OH) 3 X (M=Mn, Fe, Co, Ni, Cu; X=Cl, Br, I) is a novel magnetic geometric frustration material (MGF_Magnetic Geometric Frustration) [Balents L.Spin liquids in frustrated magnets[J]. Nature, 2010, 464 (7286): 199-208]; Gardner J S, Gingras M J P, Greedan J E. Magnetic pyrochlore oxides [J]. Reviews of Modern Physics, 2010, 82 (1): 53]. It causes many unknown and novel quantum states, especially although it is composed of a single magnetic ion, there are spin order (such as ferromagnetic or antiferromagnetic order) and disorder (such as spin fluctuation or automagnetism) in the system at the same time. The phenomenon of spin glass state) has attract...

Claims

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Application Information

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IPC IPC(8): C01G51/08G01N27/12B82Y30/00
Inventor 卢靖王勇张亚宾黄剑锋曹丽云
Owner SHAANXI UNIV OF SCI & TECH
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