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Preparation method of CaF2 hollow nanospheres

A nanomaterial, hollow sphere technology, applied in the direction of calcium/strontium/barium halide, calcium/strontium/barium fluoride, etc., can solve the problems of poor repeatability, uneven crystal size, short synthesis time, etc., to achieve uniform size , the appearance is consistent, the synthesis method is simple

Inactive Publication Date: 2019-05-10
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Currently, for CaF 2 The research on nanomaterial hollow spheres mainly includes the following reports: Literature (ACS Appl.Mater.Inter.2009,4,780-788) uses calcium chloride as the calcium source, sodium tungstate as the complexing agent, and sodium fluoride as the fluorine source. At room temperature, CaF was synthesized 2 Hollow spheres, and the formation mechanism of the hollow structure has been studied. However, the preparation process of this method takes too long and needs to be reacted for 5 days, and the obtained sample crystals are not uniform in size; literature (CrystEngComm, 2012, 14, 2630- 2634) using sodium dihydrogen phosphate as a complexing agent and 1-n-butyl-3-methylimidazolium tetrafluoroborate ionic liquid as a fluorine source, a microwave-assisted method was used to prepare CaF 2 Hollow spheres, but due to the short synthesis time and low temperature of this method, the synthesized CaF 2 The crystal size is not uniform; the literature (Chem.Eur.J.2010,16,5672-5680) uses calcium nitrate as the calcium source, trisodium citrate as the complexing agent, and sodium tetrafluoroborate as the fluorine source. Synthetic preparation of CaF with different sizes 2 Hollow spheres, and the introduction of rare earth elements into CaF 2 , making CaF 2 With stronger luminescent properties, but this method needs to strictly control the product of the reaction according to the pH of the solution, resulting in poor repeatability of the experiment

Method used

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  • Preparation method of CaF2 hollow nanospheres
  • Preparation method of CaF2 hollow nanospheres
  • Preparation method of CaF2 hollow nanospheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of mixed solution A: using F127 as surfactant, according to the molar ratio of F127 and deionized water of 0.0001, add 1.209g (g is gram, the same below) of F127 into 15ml of deionized water, stir magnetically at room temperature for 1h, and prepare Mixture A is obtained.

[0026] Preparation of mixed solution B: F127:Ca(NO 3 ) 2 :Na 3 C 6 h 5 o 7 :NaBF 4 :H 2 O=0.093:1:0.5:2:838, 0.236g Ca(NO 3 ) 2 4H 2 O, 0.147g Na 3 C 6 h 5 o 7 2H 2 O and 0.219 g NaBF 4 Add to the mixed solution A sequentially every five minutes, and magnetically stir at room temperature for five minutes to obtain the mixed solution B.

[0027] Transfer the mixed solution B to a 30mL stainless steel reactor lined with polytetrafluoroethylene, statically crystallize at a constant temperature of 180°C for 18h, cool to room temperature naturally, and then wash, centrifuge and dry with distilled water and absolute ethanol in sequence to obtain CaF 2 powder.

[0028] The synt...

Embodiment 2

[0032] Preparation of mixed solution A: Using F127 as surfactant, according to the molar ratio of F127 and deionized water of 0.0001, add 1.209g of F127 into 15ml of deionized water, and magnetically stir for 1 hour at room temperature to prepare mixed solution A.

[0033] Preparation of mixed solution B: F127:Ca(NO 3 ) 2 :Na 3 C 6 h 5 o 7 :NaBF 4 :H 2 O=0.093:1:0.5:2:838, 0.236g Ca(NO 3 ) 2 4H 2 O, 0.147g Na 3 C 6 h 5 o 7 2H 2 O and 0.219 g NaBF 4 Sequentially added to the mixed solution A every five minutes, and magnetically stirred at room temperature for five minutes to obtain the mixed solution B.

[0034]Transfer the mixed solution B to a 30mL stainless steel reactor lined with polytetrafluoroethylene, statically crystallize at a constant temperature of 150°C for 18h, cool to room temperature naturally, then wash, centrifuge and dry with distilled water and absolute ethanol in sequence to obtain CaF 2 powder.

[0035] XRD characterization results such as...

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Abstract

The invention relates to a preparation method of CaF2 hollow nanospheres. F127 is taken as surfactant, calcium nitrate tetrahydrate is taken as calcium source, sodium citrate dihydrate is taken as complexing agent, and sodium tetrafluoroborate is taken as fluorine source, and the CaF2 hollow nanospheres are synthesized by hydrothermal method. The synthesis method is simple, rapid and easy to repeat. The hollow spheres obtained are uniform in shape and size.

Description

technical field [0001] The invention relates to the field of inorganic material preparation technology, in particular to a CaF 2 A method for preparing nanomaterial hollow spheres. Background technique [0002] Solid inorganic fluorides are widely used in optics, electronics, semiconductors, and biology due to their characteristics of low phonon energy, high ion energy, high resistivity, and anion conductivity. Among them, nanoscale calcium fluoride (CaF 2 ) is an important fluoride, which has attracted extensive attention from researchers due to its excellent biocompatibility and excellent transmittance in the ultraviolet range. [0003] In recent years, hollow spheres assembled from nanomaterials have become a research hotspot due to their porous shell, low density, high surface-to-volume ratio, and low thermal expansion coefficient. Such materials can be used as drug release carriers, adsorbents, etc. , catalysts, sensors and photonic crystals, etc. Currently, for CaF...

Claims

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Application Information

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IPC IPC(8): C01F11/22
Inventor 朱伟东张璐璐杨宁严春浩许春慧陈德利王海赵晓亚王树华周黎旸
Owner ZHEJIANG NORMAL UNIVERSITY
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