Method for quickly preparing single-phase delafossite structure CuFeO2 microcrystalline material

Abstract

The invention discloses a method for quickly preparing a single-phase delafossite structure CuFeO2 microcrystalline material. The method comprises the steps that Cu(NO3)<2>.3H2O and Fe(NO3)<3>.9H2O are added into deionized water according to the mole ratio of 1:1, magnetic stirring for dissolving is conducted, and thus a mixed solution is obtained; a NaOH solution is dropwise added into the mixedsolution drop by drop, and then ultrasonic stirring and magnetic stirring are conducted in sequence; n-propanal is added into the solution dropwise, and then magnetic stirring is continued till colloidal suspension is formed; and the colloidal suspension is added into a microwave digestion tank, the filling rate of the colloidal suspension is 10-35%, microwave heating is conducted after sealing, after reaction is completed, a reaction product is naturally cooled to the room temperature, the microwave digestion tank is opened to take the reaction product out, and the reaction product is washedand dried to obtain the single-phase delafossite structure CuFeO2 microcrystalline material. According to the method, the reaction time is extremely short, energy consumption is less, operation is easy, technological parameters are easy to control, pollution is avoided, the yield is high, grains are developed completely, particle size distribution is even, and the single-phase delafossite structure CuFeO2 microcrystalline material can be widely applied to the fields of photocatalysis, photovoltaics, transparent conductive oxide, ferroelectric and the like.

Description

technical field [0001] The invention relates to a method for rapidly preparing single-phase delafossite structure CuFeO 2 A method for a microcrystalline material belongs to the field of synthesis and preparation of metal oxide semiconductor materials. Background technique [0002] copper iron ore ABO 2 The delafossite-type material was first reported by Friedel in 1873, and the delafossite-type material CuFeO was first synthesized by Pabst in 1946. 2 . CuFeO 2 The crystal structure is composed of two-dimensional close-packed Cu + and Fe 3+ o 6 Octahedrons are stacked alternately along the c-axis. Due to different stacking methods, hexagonal 2H structures (stacked in the manner of ... ABABAB ...) and rhombic 3R structures (stacked in the manner of ... ABCABC ...) will be formed respectively. Under practical preparation conditions, rhombohedral 3R structures have relatively low formation energies and are therefore more common. CuFeO 2 Due to its unique crystal struct...

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Problems solved by technology

CuFeO 2 Usually by high-temperature solid-state reaction (>850°C, >12h), sol-gel method with high-temperature (>650°C, 10h) post-treatment, or hydrothermal synthesis (180°C, <24h), all of these preparations The methods all involve high temperature and long reaction time, and the energy consumption is high

In addition, in the preparation of CuFeO by the above method 2 In the process, it is usually inevitable to introduce point defects such as: 2H and 3R mixed phases, copper vacancies, interstitial oxygen, etc., as well as CuO, Cu 2 O, Fe 2 o 3 、CuFe 2 o 4 and other by-products, a fact that leads to very serious consequences: CuFeO provided in the literature 2 Basic physicochemical properties are often inaccurate and inconsistent, limiting the application and further development of this material in the field of photoelectric conversion

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