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Method and device for preparing thiourea zinc sulfate crystals

A technology of zinc sulfate and thiourea, which is applied in the field of growth and preparation of new nonlinear optical crystal materials, can solve the problems of large crystal size, unstable growth of zinc trithiourea sulfate crystals, quality defects, etc., and achieves regular crystal shape. , the effect of good transparency, crystal size and quality improvement

Pending Publication Date: 2022-02-08
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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Problems solved by technology

[0005] For the problems existing in the prior art, the purpose of this invention is to provide a kind of preparation method and device of thiourea zinc sulfate crystal, described preparation method can improve the transparency and transmittance of crystal, solve the problem of trithiourea zinc sulfate radical Due to problems such as unstable crystal growth and quality defects, the prepared crystal has a large size and good optical quality. After characterization tests, the light transmittance of the crystal reaches 76%, which is conducive to its use as a nonlinear optical material in laser devices. The application provides guarantee for the optical application of the crystal

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  • Method and device for preparing thiourea zinc sulfate crystals
  • Method and device for preparing thiourea zinc sulfate crystals

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preparation example Construction

[0027] In one embodiment of the present invention, a kind of preparation method of thiourea zinc sulfate crystal is provided, and described preparation method comprises the steps:

[0028] Preparation of growth solution: preset the saturation point temperature of the growth solution, calculate and weigh the thiourea zinc sulfate powder according to the temperature solubility curve of thiourea zinc sulfate, dissolve it in distilled water at a temperature higher than the saturation point, and obtain the crystal growth required growth solution, adjusting the pH value of the growth solution; then purifying the growth solution;

[0029] Prepare supersaturated thiourea zinc sulfate solution, and spontaneously crystallize to obtain small crystals as seed crystals for crystal growth through natural cooling evaporation method;

[0030] The seed crystal is fixed on the seed crystal rod, immersed in the growth solution, and the crystal is grown according to the theoretically calculated t...

Embodiment 1

[0050] A kind of thiourea zinc sulfate crystal growth device, described growth device comprises: growth bottle 6, is provided with seed crystal bar 4 in the growth bottle 6, and seed crystal bar is used for the growth of crystal; Described seed crystal bar 4 is connected with the growth bottle The upper crystal motor 1; the growth bottle is located in the water bath 10, and the water bath is used to maintain a constant temperature for the growth bottle.

[0051] The water bath 10 is provided with a water bath thermometer 3 , a thermal resistance 5 , a stirring device 7 and a heater 8 ; a silicone oil sealing device 2 is provided between the crystal turning motor 1 and the growth bottle 6 .

Embodiment 2

[0053] Adopt normal temperature aqueous solution method to grow and prepare thiourea zinc sulfate crystal:

[0054] (1) Synthetic thiourea zinc sulfate raw material: accurately calculate and weigh the high-purity zinc sulfate heptahydrate reagent and high-purity thiourea reagent according to the molar ratio of 1:3, dissolve them in a certain amount of distilled water respectively, mix them evenly, Complete reaction, spontaneous crystallization, filtration and drying to obtain raw materials. The raw material is recrystallized three times to reduce the impurity content in the raw material.

[0055] (2) Preparation of crystal growth solution: the preset temperature of the solution saturation point is 51°C, using an 800mL growth bottle, prepare a 600mL solution, calculate and weigh the raw materials according to the temperature solubility curve of thiourea zinc sulfate, and dissolve them in distilled water to obtain the growth solution required for crystal growth. Add 2mL of sul...

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Abstract

The invention relates to the technical field of growth and preparation of novel nonlinear optical crystal materials, in particular to a preparation method and device of thiourea zinc sulfate crystals. The preparation method comprises the following steps: preparing a growth solution: presetting the solution saturation point temperature to be 51 DEG C, calculating and weighing thiourea zinc sulfate powder according to a temperature solubility curve of thiourea zinc sulfate, dissolving the thiourea zinc sulfate powder in distilled water at a temperature higher than the saturation point temperature to obtain the growth solution required by crystal growth, and adjusting the pH value of the growth solution; then carrying out purification treatment on the growth solution; preparing a supersaturated thiourea zinc sulfate solution, and performing spontaneous crystallization through a natural cooling evaporation method to obtain small crystals as seed crystals for crystal growth; fixing the seed crystals on a seed crystal rod, immersing the seed crystal rod into the growth solution, performing crystal growth according to a theoretically calculated thiourea zinc sulfate crystal growth cooling curve, and obtaining the thiourea zinc sulfate crystals after growing for a period of time. The prepared crystals are relatively large in size and relatively good in optical quality.

Description

technical field [0001] The invention relates to the technical field of growth and preparation of novel nonlinear optical crystal materials, in particular to a method and device for preparing thiourea zinc sulfate crystals. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Zinc trithiourea sulfate is referred to as zinc thiourea sulfate ([Zn(CS(NH 2 ) 2 ) 3 SO 4 ]) As a kind of metal-organic complex nonlinear optical crystal is a kind of functional material with excellent performance, which has a large nonlinear optical coefficient, strong resistance to laser damage, wide transmission band, and small angle sensitivity And very good mechanical strength, the application po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/08C30B7/04C30B29/54G02F1/355
CPCC30B7/08C30B7/04C30B29/54G02F1/3551
Inventor 禹化健刘冰王旭平邱程程杨玉国
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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