Quaternary sulfide semiconductor material, and preparation method and application thereof

Abstract

The invention discloses a quaternary sulfide semiconductor material, and a preparation method and application thereof. An alkali metal compound, metallic copper, binary solid solution solid solution and elemental sulfur are used as raw materials, hydrazine hydrate and polyethylene glycol are used as solvents, and a reaction is carried out in a baking oven with a temperature of 120 to 190 DEG C for 4 to 9 d so as to prepare the quaternary sulfide semiconductor material. The chemical composition of the quaternary sulfide semiconductor material is A<x>Cu<y>Sb<z>S<x+y+3z> / 2, wherein A is alkali metal atoms of a balanced anion skeleton, x represents the molar weight of the alkali metal atoms, y is the molar weight of transition metal atoms composing the skeleton and z is the molar weight of atoms composing the skeleton. The preparation method has the advantages of simple operation process, low cost of raw materials, mild reaction conditions, low synthesis temperatures, etc. Quaternary sulfide prepared by using the method has yield of 60 to 90%, a crystal grain size of 150 to 300 [mu]m and high chemical purity and can be used for preparing optical semiconductor devices.

Description

technical field [0001] The invention relates to a quaternary sulfide semiconductor material, a preparation method and application thereof, and belongs to the field of inorganic semiconductor materials. Background technique [0002] Infrared nonlinear optical materials can be made into optical devices such as second harmonic generators, frequency converters, and optical parametric oscillators. They have important and extensive applications in the fields of laser communication and military technology, and thus have attracted widespread attention. According to the difference of material application bands, nonlinear optical materials are mainly divided into three categories: ultraviolet light region, visible and near-infrared light region and mid-far infrared light region. Marketed nonlinear optical crystals are basically composed of inorganic materials, including KTiOPO 4 (KTP), β-BaB 2 o 4 (BBO), AgGaS 2 (AGS) etc. In recent years, multi-component chalcogenide materials h...

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Problems solved by technology

However, due to the disadvantages of high reaction temperature, many side reactions, complicated experimental operation, and high experimental cost, its wide application is limited.

[0005] 2) Medium-temperature co-solvent method: Introduce co-solvent in the high-temperature solid-phase method to reduce the crystal growth temperature, but the growth cycle is prolonged. Most fluxes have varying degrees of toxicity and cause harm to the human body and the environment when volatilized, and the prepared crystals The particles are small, there are by-products, and co-solvent needs to be removed, so it is not suitable for industrial production

Lei Xiaowu and others successfully prepared [dienH 2 ]Hg 2 Sb 2 S 6 (Lei Xiaowu et al., Journal of Jining University, 35,36(2014)), but because the organic group is included in the product, the thermal stability of the product is poor, and the yield is only 35%

Chen Zhen et al. successfully prepared CsSb by solvothermal method 2 (Se 2 ) 0.5 Se 3 (Chen Zhen et al., Acta Inorganic Chemistry, 22, 27 (2006)), but the preparation process needs to be filled with argon for protection, and then the tube is sealed. The whole experimental process is cumbersome and requires high conditions.

An Yonglin et al. (Inorganic Chemistry 53, 4856 (2014)) chose a mixed solution of 1,2-propanediamine and methanol water as a solvent, and reacted at 160 °C for 5 days to prepare Rb 2 Cu 2 Sb 2 S 5 Sulfide semiconductor materials, the experimental process involves sealing tube operation, the process is more complicated, and the product yield is low, only 36%

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