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Low-temperature preparation method for CuFeO2 crystal material of delafossite structure

A technology of crystalline materials, delafossite, applied in the fields of nanotechnology, chemical instruments and methods, iron compounds, etc. for materials and surface science, which can solve the problem that the nanometer effect of photoelectrochemical properties has not been fully reflected, and the nanometer effect has not been reached. scale and other issues, to achieve the effect of easy control of process parameters, low price, and good experimental repeatability

Active Publication Date: 2014-09-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Given the currently reported CuFeO 2 The crystal size of the material is relatively large, far from reaching the nanoscale, so that the nano-effects of the photoelectrochemical properties related to the crystal structure, morphology, and size of the material have not been fully reflected

Method used

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  • Low-temperature preparation method for CuFeO2 crystal material of delafossite structure
  • Low-temperature preparation method for CuFeO2 crystal material of delafossite structure
  • Low-temperature preparation method for CuFeO2 crystal material of delafossite structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh Cu(NO 3 ) 2 and FeCl 2 Finally, add deionized water and stir it with a magnetic stirrer for about 10-15 minutes. After it is completely dissolved, add 4 times the molar amount of NaOH that acts as a mineralizer, and continue stirring for about 10-15 minutes until it is completely dissolved and forms water. Thermally reactive precursor. Transfer the above reaction precursor to a hydrothermal reaction kettle (generally polytetrafluoroethylene), and control the filling rate of the reaction liquid to about 65%. After sealing the kettle body, place it in a programmed temperature-controlled oven for hydrothermal reaction, set the reaction temperature to 160°C, and the reaction time to 12 to 48 hours.

[0031] After the reaction, the kettle body was naturally cooled to room temperature, and the kettle body was opened to take out the reaction product. Use deionized water, dilute NH 3 ·H 2 O, deionized water, absolute ethanol, etc., were centrifuged and washed severa...

Embodiment 2

[0033] Weigh Cu(NO 3 ) 2 and FeCl 2 Finally, add deionized water and stir it with a magnetic stirrer for about 10-15 minutes. After it is completely dissolved, add 6 times the molar amount of NaOH that acts as a mineralizer, and continue stirring for about 10-15 minutes until it is completely dissolved and forms water. Thermally reactive precursor.

[0034] The above-mentioned reaction precursor is transferred to a hydrothermal reaction kettle (generally polytetrafluoroethylene), and the filling rate of the reaction liquid is controlled to be about 65-75%. After sealing the kettle body, place it in a programmed temperature-controlled oven for hydrothermal reaction, set the reaction temperature to 160° C., and the reaction time to 36 hours.

[0035] After the reaction, the kettle body was naturally cooled to room temperature, and the kettle body was opened to take out the reaction product. Use deionized water, dilute NH 3 ·H 2 O, deionized water, absolute ethanol, etc., w...

Embodiment 3

[0037] Weigh Cu(NO 3 ) 2 and FeCl 2 Finally, add deionized water and stir with a magnetic stirrer for about 10 to 15 minutes. After it is completely dissolved, add 4 to 10 times the molar amount of NaOH that acts as a mineralizer, and continue stirring for about 10 to 15 minutes until it is completely dissolved. Formation of hydrothermal reaction precursors.

[0038] 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 programmed temperature-controlled oven for hydrothermal reaction, set the reaction temperature to 100°C, and the reaction time to 12 to 48 hours.

[0039] After the reaction, the kettle body was naturally cooled to room temperature, and the kettle body was opened to take out the reaction product. Use deionized water, dilute NH 3 ·H 2 O, deionized water, absolute ethanol, etc., were centrifuged and ...

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Abstract

The invention discloses a low-temperature preparation method for a CuFeO2 crystal material of a delafossite structure, in particular to a low-temperature hydrothermal synthesis method for rapidly preparing the CuFeO2 nanocrystalline material of the delafossite structure. The method comprises the steps that parameters including reaction precursor components, the reaction temperature and the filling rate of a reaction solution in a hydrothermal reaction kettle are regulated and controlled through a low-temperature hydrothermal reaction, reactants including Cu(NO3)2 and FeCl2 react for 12 hours to 48 hours at the temperature ranging from 100 DEG C to 160 DEG C, and then, after a reaction product is processed through centrifugal cleaning and dried, the nanoscale CuFeO2 crystal material is obtained. The low-temperature preparation method for the CuFeO2 crystal material of the delafossite structure is easy to operate, the technological parameters are easy to control, no pollution is caused, the yield is high, and the method can be widely used for photoelectricity functional devices such as transparent conducting oxide.

Description

technical field [0001] The invention relates to the field of synthesis and preparation of nanomaterials, in particular to the synthesis and preparation of nanoscale CuFeO at a relatively low temperature by hydrothermal method 2 crystal material. Background technique [0002] In 1946, Pabst reported for the first time that copper-iron ore (ABO 2 ) structure of CuFeO 2 material whose crystal structure is composed of two-dimensional close-packed Cu + and Fe 3+ o 6 Octahedrons are stacked alternately along the c-axis. CuFeO 2 Crystal is a typical ABO 2 The structural p-type semiconductor material has a forbidden band width of 1.5eV-2.0eV, and a unit cell parameter of a=b=0.3035nm, c=1.7162nm. At present, CuFeO can be prepared by high-temperature solid-state reaction or sol-gel method followed by high-temperature sintering. 2 materials such as Cu 2 O and Fe 2 o 3 CuFeO can be produced by solid phase reaction at high temperature of 900-1200 °C 2 crystal material. Not...

Claims

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Application Information

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IPC IPC(8): C01G49/00B82Y30/00
Inventor 熊德华赵修建李宏常海梅柳星星李夏雯齐永康
Owner WUHAN UNIV OF TECH
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