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CaF2 nano material with high specific surface area and high thermal stability as well as preparation method and application thereof

A technology with high thermal stability and high specific surface area, used in chemical instruments and methods, separation methods, fluorine/hydrogen fluoride, etc.

Pending Publication Date: 2020-08-11
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, researchers have prepared CaF with different sizes and shapes by hydrothermal method. 2 Materials, for example, literature (Physica.B,2016,501,106-112) with Na 2 EDTA was used as a complexing agent, calcium nitrate was used as a calcium source, and ammonium fluoride was used as a fluorine source. Nanoparticle-shaped CaF 2 Materials; Literature (CrystEngComm, 2011, 13, 835-840) also adopts hydrothermal method, with Na 2 EDTA as complexing agent, with Ca(CH 3 COO) 2 As calcium source, take NaBF 4 As a fluorine source, CaF with multi-layered nanoflakes was prepared 2 materials; however, none of these reports have any 2 Research on thermal stability and water absorption performance of materials

Method used

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  • CaF2 nano material with high specific surface area and high thermal stability as well as preparation method and application thereof
  • CaF2 nano material with high specific surface area and high thermal stability as well as preparation method and application thereof
  • CaF2 nano material with high specific surface area and high thermal stability as well as preparation method and application thereof

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Embodiment 1

[0046] According to the molar ratio of each material, Ca(CH 3 COO) 2 :Na 2 EDTA:NaBF 4 :H 2 O=1:5:2:1676.6, the 1mmolCa (CH 3 COO) 2 Dissolve in 30mL distilled water, after stirring and dissolving, add 5mmol Na 2 EDTA·2H 2 O, magnetically stirred for 30min to obtain mixed solution A, then in mixed solution A, add 2mmol NaBF 4 At the same time, acetic acid was added dropwise to adjust the pH value of the solution to 3.9; the mixed solution B was obtained after magnetic stirring for 10 minutes, and the mixed solution B was transferred to a hydrothermal stainless steel reactor lined with polytetrafluoroethylene, and placed in a 433K oven for crystallization After 1 h; cool to room temperature, alternately centrifuge and wash with distilled water and absolute ethanol, repeat 3 times, and finally place the obtained sample in a 333K oven to dry overnight to obtain a white powdery solid. Heat treatment at 573K and vacuum condition for 7h to obtain the sample after heat treatm...

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Abstract

The invention relates to the field of adsorption separation, in particular to a CaF2 nano material with high specific surface area and high thermal stability as well as a preparation method and application thereof. The CaF2 nano material is a multilayer nanosheet flower-shaped CaF2 material synthesized by taking disodium ethylene diamine tetraacetate as a complexing agent, calcium acetate as a calcium source and sodium tetrafluoroborate as a fluorine source and adopting a hydrothermal method. According to the CaF2 nano-material provided by the invention, the pH value and crystallization time of the synthetic liquid are optimized, so that the morphology and size of the CaF2 nano-material are effectively controlled, and the highest thermal stability, the maximum specific surface area and theoptimal water absorption performance of the CaF2 nano-material are obtained. In addition, the CaF2 material prepared by the technical scheme of the invention can be used as a water absorbent to efficiently adsorb trace moisture in HF gas to prepare HF high-purity electronic special gas, and can be recycled after regeneration.

Description

technical field [0001] The invention relates to the field of adsorption separation, in particular to a high specific surface area and high thermal stability CaF 2 Nanomaterial and its preparation method and application in the preparation of HF high-purity electronic special gas by adsorbing trace moisture of HF gas. Background technique [0002] Corrosive electron gas HF is mainly used in the etching and surface cleaning of silicon wafers in the semiconductor industry, and is one of the key gases in the manufacture of micro-nano electronics. With the development of advanced manufacturing of micro-nano electronics industry towards high integration, large size, narrow line width, high uniformity and integrity, the requirements for the purity of HF electronic gas are getting higher and higher, especially for the control of impurity moisture. More stringent requirements, because impurity moisture will induce and accelerate the corrosion of HF gas on the materials it contacts, r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/04B01J20/28B01J20/30C01F11/22C01B7/19B01D53/26
CPCB01J20/046B01J20/28035B01J20/28014C01F11/22C01B7/197B01D53/261C01P2002/72C01P2004/03C01P2004/04C01P2004/30C01P2006/12B01J2220/4812B01J2220/4806
Inventor 朱伟东张璐璐许春慧王雪王宁伟陈德利赵晓亚王树华周黎旸
Owner ZHEJIANG NORMAL UNIVERSITY
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