A delafossite-structured CuCoO2 crystal material and a low-temperature preparation method thereof

A technology of crystalline material and delafossite, applied in chemical instruments and methods, inorganic chemistry, cobalt compounds, etc., can solve the problems that have not been found so far, and achieve the effects of less environmental pollution, simple preparation process and wide range of sources

Active Publication Date: 2017-08-29
WUHAN UNIV OF TECH
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  • Summary
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  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the research reports on the synthesis of a series of copper-based delafossite materials by low-temperature hydrothermal method are mostly focused on CuAlO 2 , CuGaO 2 , CuCrO 2 and CuFeO 2 At present, there is no discovery of any copper iron ore structure CuCoO synthesized by low temperature hydrothermal method. 2 Materials Research Reports

Method used

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  • A delafossite-structured CuCoO2 crystal material and a low-temperature preparation method thereof
  • A delafossite-structured CuCoO2 crystal material and a low-temperature preparation method thereof
  • A delafossite-structured CuCoO2 crystal material and a low-temperature preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] At room temperature, according to Co 2+ : Cu 2+ Weigh Co(NO 3 ) 2 ·6H 2 O and Cu(NO 3 ) 2 ·3H 2 After adding O into pure water, Cu 2+ and Co 2+ The concentrations are 4.33-4.92Wt%, 5.17-5.87Wt%, respectively, stirred by a magnetic stirrer for 30-60 minutes; 2+ or contain Co 2+ 4 times the molar amount of NaOH of the compound, and continue to stir for 30-60 minutes until completely dissolved to form a hydrothermal reaction precursor and obtain a reaction precursor. The above-mentioned reaction precursor is transferred to a hydrothermal reactor (generally polytetrafluoroethylene), and the filling rate of the reaction solution (ie, the reaction precursor) is controlled to be about 70%. After sealing the kettle body, place it in a program temperature-controlled box for hydrothermal reaction, set the reaction temperature to 100°C, and the reaction time to 24-36 hours.

[0037] After the reaction, the kettle body was naturally cooled to room temperature, and the ke...

Embodiment 2

[0039] At room temperature according to Co 2+ : Cu 2+ Weigh Co(NO 3 ) 2 ·6H 2 O and Cu(NO 3 ) 2 ·3H 2 After adding O into pure water, Cu 2+ and Co 2+ The concentrations are 4.33-4.92Wt%, 5.17-5.87Wt%, respectively, stirred by a magnetic stirrer for 30-60 minutes, and after being completely dissolved, then add Cu-containing mineralizer 2+ or contain Co 2+ 5 times the molar amount of NaOH of the compound, and continue to stir for 30-60 minutes until completely dissolved to form a hydrothermal reaction precursor and obtain a reaction precursor. Transfer the above reaction precursor to a hydrothermal reactor (generally polytetrafluoroethylene), and control the filling rate of the reaction solution to about 70%. After sealing the kettle body, place it in a program temperature-controlled box for hydrothermal reaction, set the reaction temperature to 100°C, and the reaction time to be 12 to 36 hours.

[0040] After the reaction, the kettle body was naturally cooled to room...

Embodiment 3

[0042] At room temperature according to Co 2+ : Cu 2+ Weigh Co(NO 3 ) 2 ·6H 2 O and Cu(NO 3 ) 2 ·3H 2 After adding O into pure water, Cu 2+ and Co 2+ The concentrations are 4.33-4.92Wt%, 5.17-5.87Wt%, respectively, stirred by a magnetic stirrer for 30-60 minutes, and after being completely dissolved, then add Cu-containing mineralizer 2+ or contain Co 2+ 6 times the molar amount of the compound (NaOH), and continue to stir for 30 to 60 minutes until completely dissolved to form a hydrothermal reaction precursor and obtain a reaction precursor.

[0043] Transfer the above reaction precursor to a hydrothermal reactor (generally polytetrafluoroethylene), and control the filling rate of the reaction solution to about 70%. After sealing the kettle body, place it in a program temperature-controlled box for hydrothermal reaction, set the reaction temperature to 100-120°C, and the reaction time to 24 hours.

[0044] After the reaction, the kettle body was naturally cooled t...

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Abstract

The invention relates to the field of preparation of delafossite-structured crystal materials, particularly relates to preparation of a CuCoO2 crystal material at a low temperature by utilizing a hydrothermal process, and more particularly relates to a low-temperature preparation method of the delafossite-structured CuCoO2 crystal material. The method is characterized in that a low-temperature hydrothermal reaction is utilized, reaction precursor components, the reaction temperature and the filling coefficient of a filling liquid in a hydrothermal reactor are regulated, and after Co(NO3)<2>.6H2O and Cu(NO3)<2>.3H2O are reacted at 100-120 DEG C for 12-36 h, a reaction product is subjected to centrifugal cleaning treatment and drying to obtain the crystal material the particle size of which is 1-4 microns. The method when compared with other CuCoO2 crystal material preparing methods has advantages of an ultralow temperature, a high yield, a low cost and low pollution.

Description

technical field [0001] The invention relates to the field of synthesis and preparation of delafossite structure crystal materials, in particular to the synthesis and preparation of CuCoO at a relatively low temperature by hydrothermal method 2 crystal material. Background technique [0002] In 1997, Professor Kawazoe of Tokyo Institute of Technology reported for the first time in Nature that based on the theory of Chemical modulation of Valence band (CMVB) and using the technology of Pulse Laser Deposition (PLD) to prepare a material suitable for a large number of The delafossite structure with the existence and transport of many sub-holes (ABO 2 ) of intrinsic p-type transparent conductive CuAlO 2 Thin film, the conductivity of the film at room temperature is 0.95s / cm. This achievement has promoted the rapid development of p-type delafossite-structured transparent conductive oxide (TCO) materials, and has brought hope for the preparation of fully transparent p-n junction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00
CPCC01G51/40C01P2002/72C01P2004/03C01P2004/22C01P2004/61
Inventor 李宏杜子娟熊德华
Owner WUHAN UNIV OF TECH
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