Method for preparing hierarchical hexagonal flake cadmium sulfide crystals by microwave hydration heat

A microwave hydrothermal, hexagonal flake technology, applied in cadmium sulfide and other directions, can solve the problems of toxic raw materials, complex and harsh operating conditions, etc.

Inactive Publication Date: 2010-09-29
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional hydrothermal synthesis method has complex and harsh operating conditions, the raw materials used are toxic or inert gas protection is required during the synthesis process, and long-term reaction at high temperature and pressure or at low temperature is required.

Method used

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  • Method for preparing hierarchical hexagonal flake cadmium sulfide crystals by microwave hydration heat
  • Method for preparing hierarchical hexagonal flake cadmium sulfide crystals by microwave hydration heat

Examples

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Embodiment 1

[0010] Embodiment 1: 1) get the analytically pure cadmium acetate dihydrate (Cd(CH3COO) of 0.80g 2 2H 2 O) Place in a beaker, add 6mL of ethylenediamine monohydrate (C2H8N2·H) dropwise to the beaker 2 O) the resulting mixed substance is denoted as A; 2) adding deionized water to A, and constantly stirring, is configured into a transparent solution of 100mL, and the gained solution is denoted as B; 3) adding 3.00g of analytically pure thiourea to the B solution (molecular formula: NH2CSNH2), and keep stirring, the obtained solution is recorded as C; 4) adjust the pH value of solution C to 2.5, and the obtained solution is recorded as D; 5) pour solution D into the microwave hydrothermal reaction kettle, and control the filling The temperature is 65%; after sealing the hydrothermal reactor, put it into the microwave hydrothermal reactor; the hydrothermal temperature is controlled at 110 ° C, react for 3 minutes, and naturally cool to room temperature after the reaction; 6) Afte...

Embodiment 2

[0012] Embodiment 2: 1) get the analytically pure cadmium acetate dihydrate (Cd(CH COO) of 2.50g 2 2H 2 O) Place in a beaker, add 7mL of ethylenediamine monohydrate (C2H8N2·H) dropwise to the beaker 2 O) the resulting mixed substance is denoted as A; 2) adding deionized water to A, and constantly stirring, is configured into a transparent solution of 100mL, and the gained solution is denoted as B; 3) adding 4.00g analytically pure thiourea to the B solution (molecular formula: NH2CSNH2), and keep stirring, the obtained solution is recorded as C; 4) adjust the pH value of solution C to 4.0, and the obtained solution is recorded as D; 5) pour solution D into the microwave hydrothermal reaction kettle, and control the filling The temperature is 70%; after sealing the hydrothermal reactor, put it into the microwave hydrothermal reactor; the hydrothermal temperature is controlled at 100 °C, react for 10 minutes, and naturally cool to room temperature after the reaction; 6) After t...

Embodiment 3

[0013] Embodiment 3: 1) get the analytically pure cadmium acetate dihydrate (Cd(CH3COO) of 4.00g 2 2H 2 O) Place in a beaker, add 9 mL of ethylenediamine monohydrate (C2H8N2·H) dropwise to the beaker 2 0) the resulting mixed substance is denoted as A; 2) adding deionized water to A, and constantly stirring, is configured into a transparent solution of 100mL, and the gained solution is denoted as B; 3) adding 8.00g of analytically pure thiourea to the B solution (molecular formula: NH2CSNH2), and keep stirring, the obtained solution is recorded as C; 4) adjust the pH value of solution C to 6.0, and the obtained solution is recorded as D; 5) pour solution D into the microwave hydrothermal reaction kettle, and control the filling The temperature is 75%; after sealing the hydrothermal reactor, put it into the microwave hydrothermal reactor; the hydrothermal temperature is controlled at 150°C, react for 1min, and naturally cool to room temperature after the reaction; 6) After the ...

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Abstract

The invention discloses a method for preparing hierarchical hexagonal flake cadmium sulfide crystals by microwave hydration heat, which comprises the following steps of: mixing cadmium acetate dihydrate and ethylenediamine monohydrate to obtain A; adding deionized water into the A to obtain B; adding thiourea into the B solution to obtain C; adjusting the pH value of the C to between 2.0 and 7.0 to obtain D; pouring the D into a microwave hydrothermal reaction kettle, sealing the hydrothermal reaction kettle, then putting the hydrothermal reaction kettle into a microwave hydrothermal reaction instrument, and naturally cooling a reaction product to room temperature after the hydrothermal reaction is finished; and opening the microwave hydrothermal reaction kettle, centrifuging the reaction product and collecting a sample, washing the sample by using deionized water and acetone respectively, and then drying the sample to obtain the hexagonal flake cadmium sulfide crystals. The method prepares a cluster cadmium sulfide structure with a diameter of about 1 micron by combining a microwave method and a hydration heat method and adopting a simple microwave hydrothermal preparation process, and the cluster structure is assembled by the hexagonal flake cadmium sulfide crystals with the side length of about 100 nanometers and the thickness of about 20 to 50 nanometers.

Description

technical field [0001] The invention relates to a method for preparing cadmium sulfide crystals, in particular to a method for preparing graded hexagonal plate-shaped cadmium sulfide crystals by microwave hydrothermal heating. Background technique [0002] Cadmium sulfide (CdS) is an important typical direct-bandgap wide-bandgap semiconductor material in the II-VI group. The bandgap width of bulk CdS at room temperature is 2.42eV, and the nanoscale CdS particles have a larger bandgap width ( greater than 2.45eV). Because of its special optical and electrical properties, it has been widely used in photoluminescence, photocatalysis, photoelectric conversion, sensors, magnetic materials, biological detection and so on. As a very promising semiconductor material, cadmium sulfide has attracted worldwide research interest. So far, under special growth conditions, spherical, linear, rod, hierarchical, cluster and flower-shaped CdS have been successfully synthesized. The traditio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G11/02
Inventor 黄剑锋张钦峰胡宝云曹丽云吴建鹏熊信柏曾燮榕
Owner SHAANXI UNIV OF SCI & TECH
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