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Microemulsion-solvothermal technique of orthorhombic InOOH

An orthorhombic and solvothermal technology, which is applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of large equipment investment, high energy consumption, and demanding equipment requirements

Active Publication Date: 2013-08-14
河南圣玛斯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the precursor of hexagonal indium oxide, orthorhombic InOOH has a one-dimensional nanostructure, large specific surface area, and good stability. Previous literature reports that hexagonal indium oxide needs to be prepared under high temperature and high pressure, such as Prewitt et al. At 1000°C and 65 kbar, Atou et al. prepared hexagonal indium oxide at 15-25 GPa, which has relatively high energy consumption and relatively strict requirements for equipment, which requires a large investment in equipment.

Method used

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  • Microemulsion-solvothermal technique of orthorhombic InOOH
  • Microemulsion-solvothermal technique of orthorhombic InOOH
  • Microemulsion-solvothermal technique of orthorhombic InOOH

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1). Preparation of microemulsion

[0040] a. The microemulsion consists of 18ml n-hexane and 4ml n-pentanol, and 8ml octadec-cis-9-enoic acid is added to the beaker in turn under magnetic stirring, b. Then 2ml 0.5mol / l indium salt solution is added to the beaker In, dropwise add 3.0ml of sodium hydroxide solution whose mass percentage concentration is 15%, continue to stir for 15 minutes, adjust pH value to be 8, obtain emulsion;

[0041] (2). Solvothermal preparation of orthorhombic InOOH

[0042] a. Move the emulsion to a polytetrafluoroethylene container, then seal the tetrafluoroethylene container in a stainless steel autoclave, heat and react at 180°C for 20 hours, and then cool to room temperature,

[0043] b. The product is centrifuged and washed, and the precipitate is dried and ground to obtain one-dimensional orthorhombic InOOH.

Embodiment 2

[0045] (1). Preparation of microemulsion

[0046] a. The microemulsion consists of 20ml of n-hexane and 5ml of n-pentanol, and 9ml of octadec-cis-9-enoic acid was added to the beaker in turn under magnetic stirring, b. Then 1.5ml of 0.8mol / l indium salt solution was added In the beaker, add 2.5ml of sodium hydroxide solution with a mass percentage concentration of 17% dropwise, continue stirring for 15 minutes, and adjust the pH value to 9 to obtain an emulsion;

[0047] (2). Solvothermal preparation of orthorhombic InOOH

[0048] a. Move the emulsion to a polytetrafluoroethylene container, then seal the tetrafluoroethylene container in a stainless steel autoclave, heat and react at 190°C for 19 hours, and then cool to room temperature,

[0049] b. The product is centrifuged and washed, and the precipitate is dried and ground to obtain one-dimensional orthorhombic InOOH.

Embodiment 3

[0051] (1). Preparation of microemulsion

[0052] a. The microemulsion consists of 22ml of n-hexane and 6ml of n-pentanol, and 12ml of octadeca-cis-9-enoic acid is added to the beaker in turn under magnetic stirring, b. Then 1.2ml of 0.7mol / l indium salt solution is added In the beaker, add 2.0 ml of sodium hydroxide solution with a mass percentage concentration of 19% dropwise, continue stirring for 15 minutes, and adjust the pH value to 10 to obtain an emulsion;

[0053] (2). Solvothermal preparation of orthorhombic InOOH

[0054] a. Move the emulsion to a polytetrafluoroethylene container, then seal the tetrafluoroethylene container in a stainless steel autoclave, heat and react at 200 ° C for 18 hours, and then cool to room temperature,

[0055] b. The product is centrifuged and washed, and the precipitate is dried and ground to obtain one-dimensional orthorhombic InOOH.

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Abstract

The invention discloses a microemulsion-solvothermal technique of orthorhombic InOOH, which comprises the following steps: (1) preparation of microemulsion: a. sequentially adding microemulsion, mixture of n-hexane, n-pentanol or n-butanol, and surfactant into a beaker in a volume ratio of (18-22):(4-6):(8-12) under magnetic stirring conditions; b. adding 1-2ml of indium salt solution into the beaker, dropwisely adding 1.5-3ml of organic amine or inorganic alkali solution, continuing stirring for 12-18 minutes, and regulating the pH value to 8-11 to obtain an emulsion; and (2) preparation of orthorhombic InOOH by solvothermal technique: a. transferring the emulsion to a polytetrafluoroethylene vessel, closing the polytetrafluoroethylene vessel in a stainless steel high-pressure reaction kettle, heating to 180-220 DEG C to react for 18-20 hours, and cooling to room temperature; b. centrifuging the product, washing, drying the precipitate, and grinding to obtain the orthorhombic InOOH. The technique enhances the yield on the premise of lowering the optimum reaction temperature; and the prepared orthorhombic InOOH has excellent gas sensitivity.

Description

technical field [0001] The invention belongs to the field of preparation of orthorhombic InOOH, in particular to a method for preparing orthorhombic InOOH by a microemulsion-solvothermal process. Background technique [0002] Indium oxide is a special wide-bandgap oxide semiconductor with low resistance and high catalytic activity. It has been widely used in solar cells, flat panel displays, optical and optoelectronic devices, and gas sensors. The structure of cubic indium oxide can be imagined as an incomplete close-packed structure of oxygen ions. Indium ions form a face-centered cubic lattice. 3 / 4 of the tetrahedral gaps in the sub-lattice are occupied by oxygen ions, and 1 / 4 are empty. The defects are oxygen vacancies and interstitial indium ions. Under high pressure, the structure of indium oxide changes from cubic to hexagonal, and hexagonal indium oxide belongs to The space group contains 6 In2O3 molecules in its unit cell, and the crystal constants a=0.549 nm, c=0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00
Inventor 王晓华孙兰轩
Owner 河南圣玛斯科技有限公司
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