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CaF2 material for absorbing trace water in HF gas and preparation method thereof

A technology of trace moisture and gas, applied in the field of CaF2 material and its preparation, can solve the problem of water absorption without thermal stability and other problems

Active Publication Date: 2019-07-23
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, researchers have prepared CaF with different sizes and shapes by a simple hydrothermal method. 2 Materials, for example, literature (Physica.B,2016,501, 106-112) with disodium edetate (Na 2 EDTA) as the complexing agent, calcium nitrate as the calcium source, and ammonium fluoride as the fluorine source, the nanoparticle CaF 2 Materials; Literature (CrystEngComm, 2011, 13, 835-840) also adopts hydrothermal method, with Na 2 EDTA was used as complexing agent, calcium acetate was used as calcium source, and sodium tetrafluoroborate was used as fluorine source to prepare CaF 2 materials; however, none of these reports have any 2 Material thermal stability and water absorption performance research

Method used

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  • CaF2 material for absorbing trace water in HF gas and preparation method thereof
  • CaF2 material for absorbing trace water in HF gas and preparation method thereof
  • CaF2 material for absorbing trace water in HF gas and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take Na 3 C 6 h 5 o 7 2H 2 O is a complexing agent, Ca(CH 3 COO) 2 For calcium source, NaBF 4 is the source of fluorine, according to the molar ratio of each material is Ca(CH 3 COO) 2 :Na 3 C 6 h 5 o 7 :NaBF 4 :H 2 O=1:5:2:1676.6, with 1mmol Ca(CH 3 COO) 2 Dissolve in 30mL distilled water, after stirring and dissolving, add 5mmol Na 3 C 6 h 5 o 7 2H 2 O, magnetically stirred for 10min to form a mixed solution A, and then added 2mmol NaBF in the mixed solution A 4 At the same time, add ammonia water dropwise to adjust the pH value of the solution to 10; magnetically stir for 60 minutes to obtain the mixed solution B, transfer the mixed solution B to a polytetrafluoroethylene-lined hydrothermal stainless steel reactor, and place it in an oven with a temperature setting of 433K Medium crystallization for 1 h; cooled to room temperature, alternately centrifuged and washed with distilled water and absolute ethanol, repeated 3 times, and finally the obta...

Embodiment 2

[0043] Take by weighing the nano flower shape CaF that embodiment 1 makes 2 0.5 g of the sample is packed into Hastelloy (Inconel) sample tubes whose length, outer diameter, and inner diameter are 10 cm, 0.635 cm, and 0.465 cm, respectively. High purity N 2 (purity>7N), at N 2 The flow rate is 20ml(STP)min -1 and CaF at a temperature of 573K 2 The samples were pretreated for 10 h. After the pretreatment, when the temperature of the sample tube drops to 298K, the water content is 10ppm, and the total flow rate is 8ml (STP)min -1 HF gas through CaF 2 Adsorption bed, the total experimental pressure is 105kPa, and UnisearchRB110-MPCO-H 2 The O moisture meter detects the moisture content in the HF gas stream after passing through the adsorption bed.

[0044] The results show that when the water content is 10ppm and the total flow rate is 8ml(STP)min -1 HF gas through CaF 2 After the adsorption bed layer, its moisture content is reduced to 100ppb and below, when HF gas cont...

Embodiment 3

[0046] First, according to the same steps as in Example 2, the water content is 10ppm, and the total flow rate is 8ml (STP)min -1 HF gas through CaF 2 adsorption bed. When moisture is in CaF 2 After the adsorption bed is saturated, switch the HF feed to high-purity N 2 (purity>7N), at N 2 The flow rate is 20ml(STP)min -1 and CaF at a temperature of 473K 2 The adsorbent is pretreated for 3 hours to realize the regeneration of the adsorbent. After the pretreatment, when the temperature of the sample tube drops to 298K, the water content is 10ppm, and the total flow rate is 8ml (STP)min. -1 HF gas through CaF 2 Adsorption bed, the total pressure of the experiment is 105kPa, while using Unisearch RB110-MPCO-H 2 The O moisture meter detects the moisture content in the HF gas stream after passing through the adsorption bed.

[0047] The results show that when the water content is 10ppm and the total flow rate is 8ml(STP)min -1 HF gas passes through regenerated CaF 2 Afte...

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Abstract

The invention relates to a CaF2 material for absorbing trace water in HF gas and a preparation method thereof. The CaF2 material is synthesized by taking Na3C6H5O7.2H2O as a complexing agent, Ca(CH3COO)2 as a calcium source and NaBF4 as a fluorine source through a hydrothermal method; the mol ratio of the Ca(CH3COO)2 to the Na3C6H5O7.2H2O to the NaBF4 is 1 to 5 to 2. The CaF2 material prepared bythe method has good thermal stability, has excellent water absorption performance under ultralow water vapor pressure and can be used for effectively absorbing the trace water in the HF gas to prepareHF high-purity electronic gas.

Description

technical field [0001] The invention relates to the field of adsorption separation, in particular to a CaF 2 Materials and their preparation methods. 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, resulting in the release of secondary pollutants such as corrosion products and material impurities, reducing the purity of HF gas and causing downstream product defects...

Claims

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Application Information

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IPC IPC(8): B01J20/04B01J20/28B01J20/30B01D53/28
CPCB01J20/046B01J20/28011B01J20/30B01D53/28B01D53/261B01D2256/26B01D2257/80
Inventor 朱伟东杨宁张璐璐许春慧王雪王宁伟陈德利赵晓亚王树华
Owner ZHEJIANG NORMAL UNIVERSITY
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