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A kind of formate lica(cooh)3 single crystal optical material and preparation method thereof

A technology of optical materials and single crystal materials, applied in the growth of polycrystalline materials, chemical instruments and methods, single crystal growth, etc., can solve the problems of device application limitations, single crystal optical material preparation methods have not been reported, etc., to achieve easy operation, The effect of high product purity and strong process controllability

Active Publication Date: 2018-03-20
NINGXIANG XINYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the formate metal-organic framework materials synthesized by hydrothermal method are powder microcrystals and tiny single crystals, but their applications as devices are greatly limited, so how to better control the growth of their single crystals, It is of great significance to make the size of single crystal meet the requirements of easy fabrication of devices and broaden its industrial application
Currently, a formate LiCa(COOH) 3 Single crystal optical materials and their preparation methods have not been reported yet

Method used

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  • A kind of formate lica(cooh)3 single crystal optical material and preparation method thereof
  • A kind of formate lica(cooh)3 single crystal optical material and preparation method thereof
  • A kind of formate lica(cooh)3 single crystal optical material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve 2mmol calcium formate, 2mmol lithium formate, 5mL N,N-dimethylformamide (DMF) in 30mL of distilled water, stir to fully dissolve; wherein the molar ratio of calcium formate to lithium formate is 1:1, DMF and The volume ratio of distilled water is 1:6. Put the mixed solution into a reaction kettle, seal it, heat it to 105° C. for reaction, keep it warm for 60 hours, and then cool it naturally to room temperature. Take out the saturated supernatant liquid after reaction with a pipette and put it into the beaker cleaned in step (1), and then put the beaker into a constant temperature and humidity chamber; set a 30-stage cooling curve, and the temperature range is 30-21°C , each temperature difference is 0.3°C, each temperature interval is kept warm for 2 hours, and the humidity is 50%. The crystal particles at the bottom of the beaker were washed 3 times with absolute ethanol, and dried in vacuum at 60°C for 15 minutes to obtain colorless and transparent LiCa(COO...

Embodiment 2

[0030]As in Example 1, dissolve 2mmol of calcium formate, 2mmol of lithium formate, and 5mL of N,N-dimethylformamide (DMF) in 30mL of distilled water, and stir to fully dissolve it; wherein the molar ratio of calcium formate to lithium formate is 1 : 1, the volume ratio of DMF to distilled water is 1: 6. Put the mixed solution into a reaction kettle, seal it, heat it to 110° C. for reaction, keep it warm for 65 hours, and then cool it naturally to room temperature. Take out the saturated supernatant liquid after reaction with a pipette and put it into the beaker cleaned in step (1), then put the beaker into a constant temperature and humidity chamber; set a 30-stage cooling curve, the temperature range is 30-21°C , each temperature difference is 0.3°C, each temperature interval is kept warm for 1.5 hours, and the humidity is 55%. The crystal particles at the bottom of the beaker were washed 3 times with absolute ethanol, and dried in vacuum at 60°C for 15 minutes to obtain co...

Embodiment 3

[0032] As in Example 1, dissolve 2mmol of calcium formate, 2mmol of lithium formate, and 5mL of N,N-dimethylformamide (DMF) in 30mL of distilled water, and stir to fully dissolve it; wherein the molar ratio of calcium formate to lithium formate is 1 : 1, the volume ratio of DMF to distilled water is 1: 6. Put the mixed solution into a reaction kettle, seal it, heat it to 110° C. for reaction, keep it warm for 65 hours, and then cool it naturally to room temperature. Take out the saturated supernatant liquid after reaction with a pipette and put it into the beaker cleaned in step (1), then put the beaker into a constant temperature and humidity chamber; set a 30-stage cooling curve, the temperature range is 30-21°C , each temperature difference is 0.3°C, each temperature interval is kept warm for 2 hours, and the humidity is 60%. The crystal particles at the bottom of the beaker were washed three times with absolute ethanol, and dried in vacuum at 60°C for 15 minutes to obtain...

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Abstract

The invention discloses a formate LiCa(COOH)3 single-crystal optical material and a preparation method thereof. The optical material consists of LiCa(COOH)3 single crystals with sizes ranging from 4.0*4.0*1.5 mm<3> to 4.5*4.5*2.5 mm<3>. The LiCa(COOH)3 single crystals are colorless and transparent. The chemical formula of an LiCa(COOH)3 single crystal compound is LiCa(COOH)3. During preparation of the optical material, a used reagent is a commercial product, and tedious preparation is not required; large-size single crystals are obtained through combination of a hydrothermal method and a liquid phase method; the technology controllability is high, the operation is easy, and the prepared product is high in purity. The obtained lithium calcium formate single-crystal optical material is expected to be widely applied to novel metal-organic formwork semiconductors, optical communication and optical devices, and meanwhile, the preparation method of the LiCa(COOH)3 single crystals is simple and convenient.

Description

technical field [0001] The invention relates to a formate single crystal material and a preparation method thereof, in particular to a metal organic framework formate LiCa(COOH) 3 Single crystal optical material and its preparation method. technical background [0002] Metal-Organic Frameworks (MOFs) materials have attracted widespread attention due to their potential applications in catalysis, hydrogen storage, and optical components, and are currently a hot spot in the field of new functional materials research. Due to the advantages of flexible preparation, flexible skeleton, easy tailoring and easy formation of highly anisotropic and low lattice symmetry structures of organic compounds, people try to apply formate compounds to optical devices, hoping to design formate-based This class of new optical materials will greatly expand the exploration space of optical materials. [0003] In recent years, nonlinear optical devices have become a hot spot in the research field o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/54C30B7/14
CPCC30B7/14C30B29/54
Inventor 张香丽
Owner NINGXIANG XINYANG CHEM
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