CN102502790A - Method for preparing SnS powder through microwave hydrothermal-ultrasonic chemistry method - Google Patents

Abstract

A method for preparing SnS powder by microwave hydrothermal-ultrasonic chemistry, dissolving SnCl ₂ 2H ₂ O in absolute ethanol to obtain solution A; dissolving thioacetamide in deionized water to obtain solution B; adding Solution B forms precursor solution C; pour solution C into a hydrothermal reaction kettle, seal the hydrothermal reaction kettle, put it into a temperature-pressure dual-control microwave hydrothermal reaction instrument for hydrothermal reaction, and after the reaction, water The thermal reaction kettle is placed in a numerically controlled ultrasonic reactor for ultrasonic reaction, and then cooled to room temperature naturally; the reaction kettle is opened, the product is collected by centrifugation, and then dried in a vacuum drying oven to obtain the final product SnS powder. The invention adopts the microwave hydrothermal-ultrasonic chemical method to prepare SnS particles with good dispersibility, controllable shape, good repeatability, simple process equipment and short reaction cycle, so it has broad development prospects.

Description

Method for preparing SnS powder by microwave hydrothermal-sonic chemical method

technical field

The invention relates to a method for preparing SnS powder, in particular to a method for preparing SnS powder by a microwave hydrothermal-ultrasonic chemical method. the

Background technique

At present, among numerous solar cells, silicon solar cells occupy the main market due to its mature technology. Thin-film solar cells, because their cost is lower than that of silicon solar cells, will become the development direction of solar cells in the future. In recent years, orthorhombic tin sulfide (SnS) has been used as a new type of solar cell material. SnS is a semiconductor material with a layered orthorhombic crystal structure in groups IV to VI. Its optical direct band gap and indirect band gap are 1.3 to 1.5 eV and 1.0 to 1.1 eV, respectively, and it has a good spectral match with visible light in solar radiation. , with a photoelectric conversion efficiency of 25%, it is very suitable for use as a light-absorbing layer in solar cells, as well as near-infrared detectors and photovoltage devices for electroluminescent displays. In addition, the Sn and S elements that constitute SnS are abundant in the earth and non-toxic. Therefore, SnS, as a non-toxic and environmentally friendly new photoelectric conversion material with potential application prospects, has attracted extensive attention from researchers in recent years. the

At present, the methods for synthesizing novel SnS at home and abroad are: Zhu et al. SnS nanoflowers, the hydrothermal method requires a specific experimental setup and is not suitable for mass production; Reddy et al. Seed crystals synthesize SnS powder in the shape of an orthogonal box. The method has complicated steps and poor repeatability; Xu et al [Xu Y, Al-Salim N, Bumby CW, et al.J.Am.Chem.Soc., 131(2009 ) 15990-15991.] Synthesize SnS quantum dots in ethanolamine system, the raw material of this reaction system is expensive; Keigo Aso et al. Needle-shaped and disc-shaped SnS nanopowders were synthesized under high temperature conditions by using a mixed solvent method. The high temperature conditions of this method are relatively harsh; Li Yang et al. [Li Y, Xie H Q, Tu J P. 2009) 365-370.] SnS particles were prepared by methods such as high-energy ball milling, and the resulting product contained more impurities. Therefore, it is necessary to develop a method for preparing SnS powder suitable for industrial production, with simple preparation process, high product purity and short reaction cycle. the

Contents of the invention

The object of the present invention is to provide a kind of equipment simple, easy to operate, short preparation time,

A low-cost microwave hydrothermal-sonic chemical method for preparing SnS powder. the

In order to achieve the above object, the technical scheme adopted in the present invention is:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.001mol/L-0.01mol/L;

2) adding analytically pure thioacetamide (TAA) into deionized water to prepare a transparent solution B with an ^S2- concentration of 0.01mol/L to 0.1mol/L;

3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1: (1-10), forming precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, the filling degree is controlled at 30% to 80%; seal the hydrothermal reaction kettle, put it into the temperature-pressure dual-control microwave hydrothermal reaction instrument; select the temperature control mode for reaction , the hydrothermal temperature is controlled at 80°C-150°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 10-60min. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, and the power is controlled at 200-500W , the temperature is controlled at 50-80°C, the reaction time is controlled at 20-60 minutes, and naturally cooled to room temperature after the reaction;

5) Open the reaction kettle, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 40°C to 70°C to obtain the final product SnS powder. the

The invention adopts the microwave hydrothermal-ultrasonic chemical method to prepare SnS particles with good dispersion type, controllable appearance, good repeatability, simple process equipment and short reaction cycle, so it has broad development prospects. the

Description of drawings

Fig. 1 is the X-ray diffraction (XRD) collection of illustrative plates of the SnS powder prepared by the embodiment of the present invention 1;

Fig. 2 is a TEM photo of the SnS powder prepared in Example 1 of the present invention. the

Detailed ways

The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments. the

Example 1:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.005 mol/L;

2) adding analytically pure thioacetamide (TAA) to deionized water to prepare a transparent solution B whose S concentration is ^0.01mol /L;

3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1:2 to form precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, the filling degree is controlled at 50%; seal the hydrothermal reaction kettle, put it into the microwave hydrothermal reaction instrument with dual temperature and pressure control; select the temperature control mode for reaction, hydrothermal The temperature is controlled at 90°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 10 minutes. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, the power is controlled at 200W, the temperature is controlled at 60°C, and the reaction time is controlled at 30min, naturally cool to room temperature after the reaction finishes;

5) Open the reaction kettle, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 45° C. to obtain the final product SnS powder. the

The resulting SnS powder was analyzed with a Japanese Rigaku D/max2000PC X-ray diffractometer, and the 2θ was 26.009°, 30.473°, 31.531°, and 39.045° respectively along (120), (101), (111), (131 ) crystal plane growth, and the product is orthorhombic SnS of JCPDS No. 39-0354 (Fig. 1). The sample was observed with a JSM-6460 scanning electron microscope produced by JEOL (FIG. 2). It can be seen from the photo that the prepared SnS particles have a special morphology. the

Example 2:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.01 mol/L;

2) Adding analytically pure thioacetamide (TAA) to deionized water is prepared into a transparent solution B whose S ^{concentration} is 0.03mol/L;

3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1:1 to form precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, and the filling degree is controlled at 60%; seal the hydrothermal reaction kettle, and put it into a temperature-pressure dual-control microwave hydrothermal reaction instrument; select the temperature control mode for reaction, and the hydrothermal The temperature is controlled at 110°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 20 minutes. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, the power is controlled at 300W, the temperature is controlled at 60°C, and the reaction time is controlled at 25min, naturally cool to room temperature after the reaction finishes;

5) Open the reactor, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 40°C to obtain the final product SnS powder. the

Example 3:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.008 mol/L;

2) adding analytically pure thioacetamide (TAA) to deionized water to prepare a transparent solution B whose ^S concentration is 0.04mol/L;

3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1:5 to form precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, and the filling degree is controlled at 70%; seal the hydrothermal reaction kettle, and put it into a microwave hydrothermal reaction instrument with dual temperature and pressure control; select the temperature control mode for reaction, and the hydrothermal The temperature is controlled at 120°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 30 minutes. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, the power is controlled at 350W, the temperature is controlled at 70°C, and the reaction time is controlled at 40min, naturally cool to room temperature after the reaction finishes;

5) Open the reaction kettle, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 60° C. to obtain the final product SnS powder. the

Example 4:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.001 mol/L;

2) adding analytically pure thioacetamide (TAA) into deionized water to prepare a transparent solution B whose ^S concentration is 0.08mol/L;

3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1:8 to form precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, and the filling degree is controlled at 30%; seal the hydrothermal reaction kettle, and put it into a microwave hydrothermal reaction instrument with dual temperature and pressure control; select the temperature control mode for reaction, and the hydrothermal The temperature is controlled at 80°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 60 minutes. After the reaction, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, the power is controlled at 500W, the temperature is controlled at 50°C, and the reaction time is controlled at 60min, naturally cool to room temperature after the reaction finishes;

5) Open the reactor, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 50° C. to obtain the final product SnS powder. the

Embodiment 5:

1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.003 mol/L;

2) adding analytically pure thioacetamide (TAA) to deionized water to prepare a transparent solution B whose S concentration is ^0.1mol /L;

3) adding solution B to solution A, so that the molar ratio of Sn ²⁺ :S ^2- is 1:10, forming precursor solution C;

4) Pour solution C into the hydrothermal reaction kettle, the filling degree is controlled at 80%; seal the hydrothermal reaction kettle, put it into the temperature-pressure dual-control microwave hydrothermal reaction instrument; select the temperature control mode for reaction, hydrothermal The temperature is controlled at 150°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 50 minutes. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, the power is controlled at 400W, the temperature is controlled at 80°C, and the reaction time is controlled at 20min, naturally cool to room temperature after the reaction finishes;

5) Open the reaction kettle, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 70° C. to obtain the final product SnS powder. the

Claims (1)

1. The method for preparing SnS powder by microwave hydrothermal-ultrasonic chemical method is characterized in that: 1) Prepare analytically pure SnCl ₂ ·2H ₂ O with absolute ethanol to prepare a transparent solution A with a Sn ²⁺ concentration of 0.001mol/L-0.01mol/L; 2) adding analytically pure thioacetamide (TAA) into deionized water to prepare a transparent solution B with an ^S2- concentration of 0.01mol/L to 0.1mol/L; 3) adding solution B to solution A so that the molar ratio of Sn ²⁺ : S ^2- is 1: (1-10), forming precursor solution C; 4) Pour solution C into the hydrothermal reaction kettle, the filling degree is controlled at 30% to 80%; seal the hydrothermal reaction kettle, put it into the temperature-pressure dual-control microwave hydrothermal reaction instrument; select the temperature control mode for reaction , the hydrothermal temperature is controlled at 80°C-150°C, the pressure is less than 2.0MPa, and the reaction time is controlled at 10-60min. After the reaction is completed, the hydrothermal reactor is placed in a numerically controlled ultrasonic reactor, and the power is controlled at 200-500W. The temperature is controlled at 50-80°C, the reaction time is controlled at 20-60 minutes, and naturally cooled to room temperature after the reaction; 5) Open the reaction kettle, collect the product by centrifugation, wash with deionized water and isopropanol for 1 to 3 times, and then dry in a vacuum oven at 40°C to 70°C to obtain the final product SnS powder.

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