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Synthesis of three-component fluoride ABF3 at low-temperature

A synthesis method and ternary compound technology, applied in the field of functional materials, can solve the problems of restricting the research of physical and chemical properties, restricting the comprehensive utilization of functional materials, etc., and achieve the effect of low corrosion and simple process

Inactive Publication Date: 2010-06-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, these methods are only suitable for the preparation of a small amount of complex fluorides, thus limiting the research on the physical and chemical properties of the large complex fluoride family, and also limiting the comprehensive utilization of this type of functional materials

Method used

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  • Synthesis of three-component fluoride ABF3 at low-temperature
  • Synthesis of three-component fluoride ABF3 at low-temperature
  • Synthesis of three-component fluoride ABF3 at low-temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: Weigh 0.02mol of KF·2H 2 O (1.883g) and 0.024mol of CaF 2 (1.874g) is mixed evenly and put into a 100ml flask, add 50ml ethylene glycol, add a few grains of zeolite, reflux at 156°C for 6 hours, let stand to cool, filter, and the obtained precipitate is washed with distilled water and absolute ethanol. Wash until the particles are dispersed and dry to obtain KCaF 3 crystals.

[0024] Adopt X'Pert Pro type X-ray diffractometer (Panalytical Company, USA) to carry out X-ray diffraction analysis to sample, such as figure 1 As shown, the position and relative intensity of the main diffraction front are consistent with the standard card diffraction data, which proves that the prepared sample has a stable perovskite structure, and the synthesized sample has uniform peak shape distribution, no miscellaneous peaks, and low noise, as Typical single-phase material. See Table 1 for specific data.

[0025] Table 1KCaF 3 XRD data

[0026]

[0027] The particle...

Embodiment 2

[0028] Embodiment 2: 0.012mol NH 4 F (0.4630g) and 0.004mol MnCl 2 4H 2 O (0.7916g), after mixing evenly, put it into a 100ml round bottom flask, add 30ml of n-hexane, add a few grains of zeolite, reflux at 216°C for 8 hours, let stand to cool, and filter under normal pressure. The resulting precipitate was washed with distilled water and absolute ethanol. Wash until the particles are dispersed and then dry to obtain NH 4 MnF 3 pink powder.

[0029] Adopt X'Pert Pro type X-ray diffractometer (Panalytical Company, USA) to carry out X-ray diffraction analysis to sample, such as image 3 As shown, it can be seen that the NH synthesized by the reflux method 4 MnF 3 The diffraction peak shape is good, there are no miscellaneous peaks, and the noise is low. It is a typical single-phase substance, which is consistent with the value of the standard card (PDF-#18-0114). to analyze, such as Figure 4 As shown, it can be seen that the NH synthesized by the reflux method 4 MnF ...

Embodiment 3

[0030] Embodiment 3: Weigh 0.02mol NaF (0.8397g) and 0.01mol Zn (NO 3 ) 2 ·6H 2 O (2.975g) was put into a 100ml retort, 50ml of dodecane was added, several zeolites were added, refluxed at 216°C for 4 hours, allowed to stand for cooling, and filtered under normal pressure. The resulting precipitate was washed with distilled water and absolute ethanol. Wash until the particles are dispersed and then dry to get NaZnF 3 crystals.

[0031] The samples were analyzed by X-ray diffraction using X'Pert Pro X-ray diffractometer (PANalytical Corporation, USA). Figure 5 ), it can be seen that NaZnF 3 The positions and relative intensities of all diffraction peaks in the spectrum are consistent with the standard diffraction data (PDF-#20-1182), and there are no other impurity peaks, indicating that the synthesized NaZnF 3 It belongs to the orthorhombic crystal system and has good crystallization; the phase is pure, and the product obtained is a single phase. The calculated unit ce...

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Abstract

The invention relates to a lower temperature synthesized method of the ternary composite fluoride ABF3. The steps include that: 1) the fluoride AF and BF2 solids are mixed and grinded sufficiently, and added to the solvent under room temperature; the solution is refluxed for 4-8 hours, cooled and deposited in room temperature; 2) the mixture solution is filtered in normal pressure, is washed by distilled water after the separation with the solvent, and then is washed to particles by less quantities of anhydrous alcohol so that the yield product is obtained after the dispersion and drying. Thelower temperature synthesized method has the advantages that the composite fluoride ABF3 is synthesized through the solvent reflux method; the process is simple; the synthesized method has small corrosion on the instrument devices and generates no HF gas; the lower temperature synthesized method can directly adopt the market sold commodities as the source material to synthesize the target yield product; the method is applicable to the synthesis of various composite fluorides; the synthesized products have single crystal structure.

Description

technical field [0001] The invention belongs to functional materials, in particular to ternary composite fluoride ABF 3 low-temperature synthesis method. Background technique [0002] Ternary compound fluoride ABF 3 It is a kind of functional material with special properties and has many excellent optical and electrical properties. The research and development of this kind of material has important theoretical significance and practical value for the development of new photoelectric functional materials. [0003] Fluoride comes in many forms, from the simplest AF n type to the more complex A m B n f p type. for AF n Type fluoride, so far, the best crystal growth method is the molten salt method, that is, the corresponding metal salt in the molten state is reacted with HF gas. For complex composite fluorides, the commonly used preparation methods include traditional high-temperature solid-phase method, molten salt method, hydrothermal and solvothermal synthesis method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B9/08
Inventor 杨秋华曲建强
Owner TIANJIN UNIV
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