Method for preparing SmS thin film by solvothermal method

A solvothermal method, a thin-film technology, applied in chemical instruments and methods, solutions of liquid solvents at room temperature, and single crystal growth, etc., can solve the problems of difficult process control, expensive equipment, and high cost, improve the quality of the film, avoid Curl, good binding effect

Active Publication Date: 2012-04-11
JINGJIANG DKL COATING IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The equipment required for these methods to prepare SmS thin films is rela

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  • Method for preparing SmS thin film by solvothermal method
  • Method for preparing SmS thin film by solvothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Step 1: Introducing Ar gas into deionized water to remove O in water 2 ;

[0020] Step two: the analytically pure SmCl 3 ·6H 2 O is dissolved in deionized water with Ar gas and configured as SmCl with a concentration of 0.03mol / L 3 Solution, labeled A;

[0021] Analytical pure thioacetamide (H 3 CCSNH 2 ) was dissolved in absolute ethanol, and configured as a 0.2mol / L ethanol solution of thioacetamide, marked as B;

[0022] Step 3: Mix solutions A and B according to the volume ratio of 2:1 and stir evenly, adjust the pH value to 2.00 with 0.05mol / L HCl solution, and mark it as C;

[0023] Step 4: Pour solution C into the hydrothermal kettle, control the filling degree at 50%, put the cleaned substrate, seal the hydrothermal kettle, put it into the DHG-9075A electric vacuum drying oven, control the water The heat temperature is 120°C and the pressure is 20MPa for 48 hours;

[0024] Step 5: Cool down to room temperature naturally after the reaction, tur...

Embodiment 2

[0025] Example 2: Step 1: Introducing Ar gas into deionized water to remove O in water 2 ;

[0026] Step two: the analytically pure SmCl 3 ·6H 2 O is dissolved in deionized water fed with Ar gas to form SmCl with a concentration of 0.06mol / L 3 Solution, labeled A;

[0027] Analytical pure thioacetamide (H 3 CCSNH 2) is dissolved in absolute ethanol, and is configured into a 0.3mol / L ethanol solution of thioacetamide, marked as B;

[0028] Step 3: Mix and stir solutions A and B evenly according to the volume ratio of 1:6, adjust the pH value to 2.40 with 0.05mol / L HCl solution, and mark it as C;

[0029] Step 4: Pour solution C into the hydrothermal kettle, control the filling degree at 52%, put the cleaned substrate, seal the hydrothermal kettle, put it into the DHG-9075A electric vacuum drying oven, control the water The heat temperature is 150°C and the pressure is 10MPa for 30 hours;

[0030] Step 5: Cool down to room temperature naturally after the reaction, turn o...

Embodiment 3

[0031] Example 3: Step 1: Introducing Ar gas into deionized water to remove O in water 2 ;

[0032] Step two: the analytically pure SmCl 3 ·6H 2 O is dissolved in deionized water filled with Ar gas, and configured as SmCl with a concentration of 0.2mol / L 3 Solution, labeled A;

[0033] Analytical pure thioacetamide (H 3 CCSNH 2 ) was dissolved in absolute ethanol, and configured as a 0.03mol / L ethanol solution of thioacetamide, marked as B;

[0034] Step 3: Mix solutions A and B according to the volume ratio of 1:3 and stir evenly, adjust the pH value to 2.80 with 0.05mol / L HCl solution, and mark it as C;

[0035] Step 4: Pour solution C into the hydrothermal kettle, control the filling degree at 58%, put the cleaned substrate, seal the hydrothermal kettle, put it into the DHG-9075A electric vacuum drying oven, control the water The heat temperature is 130°C and the pressure is 15MPa for 40 hours;

[0036] Step 5: Cool down to room temperature naturally after the react...

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Abstract

The invention discloses a method for preparing a SmS thin film by a solvothermal method. The method comprises the following steps of: introducing Ar into de-ionized water to remove O2 from the water; dissolving analytic pure SmCl3 6H2O into the de-ionized water into which the Ar is introduced to prepare a solution A; dissolving analytic pure trioacetamide into absolute ethyl alcohol to prepare a solution B; uniformly mixing the solutions A and B, and regulating a pH value to obtain a solution C; and pouring the solution C into a hydrothermal reactor, arranging a substrate in the hydrothermal reactor, sealing the hydrothermal reactor, arranging the hydrothermal reactor in an electric vacuum drying oven for reaction, naturally cooling the hydrothermal reactor to room temperature, washing the substrate by using the absolute ethyl alcohol or isopropanol and drying the substrate to obtain the SmS optical thin film on the surface of the substrate. By the method, the reaction for the preparation of the SmS thin film is finished once in an organic or blended liquid phase without post crystallization thermal treatment, thereby overcoming the shortcomings of curling, seasoning cracking, grain enlargement, reaction between the thin film and the substrate or an atmosphere and the like which may be caused to the SmS thin film by a thermal treatment process; moreover, process equipment is simple, high voltage is easy to obtain, reaction temperature is low, and the obtained film has relatively higher purity and controllably grown grains.

Description

technical field [0001] The invention relates to a method for preparing a SmS thin film, in particular to a method for preparing an SmS thin film by a solvothermal method. Background technique [0002] SmS crystal is cubic structure, NaCl type crystal, black semiconductor at normal temperature and pressure, and its lattice parameter is 0.597nm. SmS transforms from semiconductor phase (S-SmS) to metal phase (M-SmS) at 6.5×10Pa, and reversibly transforms at (1.5~2.0)×10Pa. When the phase transition occurs, the lattice parameter of SmS changes from 0.597nm to 0.570nm, and the volume shrinks, but the NaCl type crystal structure is still maintained, and the color changes from blue-black to golden yellow. The transmission of S-SmS is green and the reflection is blue-black, while the transmission of M-SmS is blue and the reflection is golden yellow. M-SmS films can be transformed into S-SmS films by heat treatment at a certain temperature or laser initiation. These special struct...

Claims

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Application Information

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IPC IPC(8): C30B7/10C30B29/46C30B29/64
Inventor 殷立雄黄剑锋郝巍曹丽云吴建鹏侯艳超马小波
Owner JINGJIANG DKL COATING IND
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