Quaternary sulfide semiconductor material, and preparation method and application thereof

A semiconductor and sulfide technology, which is applied in the field of quaternary sulfide semiconductor materials and its preparation, can solve the problems of cumbersome experimental process, high reaction temperature, and flux toxicity, etc., and achieve simple and convenient operation process, mild reaction conditions, and synthesis temperature low effect

Inactive Publication Date: 2015-08-26
ZHEJIANG UNIV
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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 o...

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  • Quaternary sulfide semiconductor material, and preparation method and application thereof
  • Quaternary sulfide semiconductor material, and preparation method and application thereof
  • Quaternary sulfide semiconductor material, and preparation method and application thereof

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preparation example Construction

[0025] The preparation method of the quaternary sulfide semiconductor material is as follows: use alkali metal compound, metal copper, binary solid solution antimony sulfide and elemental sulfur as raw materials, hydrazine hydrate and polyethylene glycol as solvent, and react 4- After 9 days, the quaternary sulfide semiconductor material was obtained.

[0026] The molar ratio of the alkali metal compound, metallic copper, binary solid solution antimony sulfide and elemental sulfur is 0.5-1.0:2.0-3.0:0.5-1.0:2.0-2.5; the molar ratio of hydrazine hydrate and polyethylene glycol is 1.0 -2.0: 2.5-3.0. The alkali metal compound is: alkali metal hydroxide, carbonate or chloride. The preparation method of the binary solid solution antimony sulfide is as follows: put Sb and S with a molar ratio of 2:3 into a quartz tube to seal the tube, then put the sealed quartz tube into a muffle furnace, and slowly raise the temperature to 560°C , and keep it warm for 8 hours, then naturally coo...

Embodiment 1

[0029] KCu 2 Sb 3 crystals. Weigh the initial raw material K 2 CO 3 0.5 mmol (0.069g), Cu 2.0 mmol (0.128g), Sb 2 S 3Put 0.5 mmol (0.170g) and S 2.0 mmol (0.064g) into a hydrothermal kettle, then add 1.0 mL of hydrazine hydrate and 2.5 mL of polyethylene glycol, and place the hydrothermal kettle at 120°C for 9 days. After the reaction was over, the hydrothermal kettle was opened, the product was taken out, and washed twice with distilled water and absolute ethanol respectively to obtain black blocky crystals with a yield of 80% and a grain size of 150-230 μm (see figure 1 ). According to single crystal X-ray diffraction analysis, the crystal composition formula is KCu 2 Sb 3 , belonging to the triclinic crystal system, the space group is P -1 (2), a=6.3857 ?, b=9.1361 ?, c=10.4672 ?, α=90.51°, β=91.32°, γ=91.49°, Z=4, V=610.26 ? 3 , and the crystal structure is shown in 7. EDX elemental analysis showed that the crystals only contained four elements: K, Cu, Sb, and S...

Embodiment 2

[0031] RbCuSb 2 S 4 crystals. Weigh the initial raw materials RbCl 1.0 mmol (0.121g), Cu 2.0 mmol (0.128g), Sb 2 S 3 Put 0.8mmol (0.170g) and S 2.0mmol (0.064g) into a hydrothermal kettle, then add hydrazine hydrate 1.6mL and polyethylene glycol 2.5mL, and place the hydrothermal kettle at 170°C for 7 days. The product was washed twice with distilled water and absolute ethanol respectively to obtain dark red rod-shaped crystals, the yield could reach 60%, and the grain size was 180-280 μm (see figure 2 ). According to single crystal X-ray diffraction analysis, the crystal composition formula is RbCuSb 2 S 4 , belongs to the monoclinic crystal system, the space group is C12 / c1, a=7.3272 ?, b=11.1628?, c=10.7849?, β=105.75°, Z=4, V=849.01 ? 3 , and the crystal structure is shown in 8. EDX elemental analysis showed that the crystals only contained four elements: Rb, Cu, Sb, and S, and the content ratio of each element was consistent with the results of single crystal diff...

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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...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B7/14C30B28/04H01L31/032
CPCC30B7/14C30B28/04C30B29/46H01L31/032
Inventor 刘毅沈亚英刘畅候佩佩洪樟连
Owner ZHEJIANG UNIV
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