CN112158807A - Water removing and oxygen removing method for fluoride melt material - Google Patents
Water removing and oxygen removing method for fluoride melt material Download PDFInfo
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- CN112158807A CN112158807A CN202010979157.9A CN202010979157A CN112158807A CN 112158807 A CN112158807 A CN 112158807A CN 202010979157 A CN202010979157 A CN 202010979157A CN 112158807 A CN112158807 A CN 112158807A
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- Prior art keywords
- fluoride
- water
- oxygen
- gas
- electromagnetic induction
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/08—Fluorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A method for deeply removing water and oxygen from a fluoride melt material is characterized in that water, hydroxyl and oxide in the melt are deeply removed by combining active fluorine plasma with electromagnetic induction heating and eddy disturbance. The method can realize the preparation of the fluoride melt material with the water content less than or equal to 50ppb and the oxygen content less than 10ppm, has the characteristics of good water and oxygen removing effect, high efficiency and simple and convenient operation, and can realize the deep water and oxygen removal of different types of fluoride melt materials.
Description
The technical field is as follows:
the invention relates to the technical field of water and oxygen removal, and particularly relates to a water and oxygen removal method for a fluoride melt material.
Background art:
fluoride materials have important applications in both military and civilian applications due to low phonon energy and excellent performance. For example: low refractive index materials such as hafnium fluoride and magnesium fluoride are widely used in various fields as important film materials; the fluoride molten salt material is used as a reactor coolant and plays an important role in a nuclear power station; the fluoride glass fiber is an important component of future photoelectric countermeasure, automatic driving, medical treatment, high-power medium infrared fiber laser and the like due to excellent medium infrared performance. Therefore, high quality fluoride materials have been one of the major targets for development in various countries.
In fluoride materials, water oxygen content is one of the core indicators for evaluating fluoride materials. Too high a water oxygen content can seriously affect the use of the fluoride material. One specific example can illustrate the importance of the oxygen content of water: theoretical loss of the ZBLAN glass fiber is 10-3dB/km, but the loss of the fluoride optical fiber is four orders of magnitude lower than the theoretical loss directly due to the excessive water oxygen content in the fluoride raw material and the glass melt, and the practical application of the fluoride optical fiber is seriously influenced. In conclusion, the deep removal of water and oxygen in the fluoride melt material is significant and urgent.
The invention content is as follows:
in order to solve the problems, the invention aims to provide a method for removing water and oxygen by using a fluoride melt material, thereby improving the quality of the fluoride material.
In order to achieve the above purpose, the water removing and oxygen removing method of the invention comprises the following steps: CF is prepared by4、SF6、NF3HF or F2The gas forms active fluorine plasma through a plasma gun, then contacts with a fluoride material melt generated by electromagnetic induction heating in a surface spraying or bubbling mode, and simultaneously realizes eddy current disturbance of the melt through an electromagnetic induction coil to achieve full contact of the active fluorine plasma and the melt, thereby realizing deep removal of water and oxygen in the fluoride material melt.
Further, the fluoride melt material has a great removal of water and hydroxyl group content, and the content is less than or equal to 10 ppb.
Further, the fluoride melt material was largely depleted of oxygen, with a level of < 10ppm (test limit for oxygen in solid material at 10 ppm).
The invention has the technical effects that:
compared with the existing water removal oxygen, the invention can realize that the water and hydroxyl in the fluoride material reach 50ppb and the oxygen content is less than 10 ppm.
The prior fluoride material has great application limit due to the over high water oxygen content, especially in the middle infrared field. The method for removing water and oxygen from the fluoride melt material can realize that the water content of the fluoride material is less than or equal to 50ppb and the oxygen content is less than 10 ppm. Can meet the application requirement of fluoride materials.
Description of the drawings:
FIG. 1 is a schematic diagram of a water-removing and oxygen-removing method for a fluoride melt material according to the present invention
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1:
first, a fluoride material was placed in a glassy carbon crucible and placed in an induction coil having a frequency of 5 kHz. After the fluoride material is melted, SF is added6The gas is sprayed on the surface of the molten liquid through active fluorine plasma formed by a plasma gun at the flow rate of 12mL/min, and the flowing time is 28 min. The melt was then quickly cast onto a 150 ℃ stainless steel template and allowed to cool to room temperature. The fired fluoride samples were cut and polished to produce sheets for subsequent testing.
The remaining example parameters are as follows:
Claims (5)
1. a method for removing water and oxygen from a fluoride melt material is characterized in that the water and oxygen removal of the fluoride melt material is realized by the combination of active fluorine plasma, electromagnetic induction heating and electromagnetic induction eddy disturbance. Wherein the time for introducing the active fluorine plasma into the melt is 5-360 min, and the induction frequency of the electromagnetic induction coil is 2-20 kHz.
2. The electromagnetic induction heating and eddy current disturbance of fluoride melt material as claimed in claim 1 is realized by electromagnetic induction coil in a glove box of fluoride material in a glassy carbon crucible, wherein the water content in the glove box is 0.1ppm, and the oxygen content in the glove box is 0.1 ppm.
3. The reactive fluorine plasma of claim 1 is generated from a fluoride reactive gas by a plasma gun.
4. The fluoride reactive gas of claim 3 comprising carbon tetrafluoride (CF)4) Gas, sulfur hexafluoride (SF)6) Gas, nitrogen trifluoride (NF)3) Gas, Hydrogen Fluoride (HF) gas and elemental fluorine (F)2) A gas.
5. The flow rate of the fluoride reactive gas introduced into the plasma gun according to claim 4 is 10L/min to 2000 mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010979157.9A CN112158807A (en) | 2020-09-17 | 2020-09-17 | Water removing and oxygen removing method for fluoride melt material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010979157.9A CN112158807A (en) | 2020-09-17 | 2020-09-17 | Water removing and oxygen removing method for fluoride melt material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112158807A true CN112158807A (en) | 2021-01-01 |
Family
ID=73859064
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010979157.9A Pending CN112158807A (en) | 2020-09-17 | 2020-09-17 | Water removing and oxygen removing method for fluoride melt material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112158807A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3816600A (en) * | 1970-09-25 | 1974-06-11 | Philips Corp | Method of manufacturing metal fluorides and metal fluoride mixtures which do not comprise oxygen |
| GB1453822A (en) * | 1973-02-09 | 1976-10-27 | Asea Ab | Method for the inductive heating of metallic melts |
| JPS63215523A (en) * | 1987-03-04 | 1988-09-08 | Sumitomo Electric Ind Ltd | Production of fluoride glass |
| US20050263064A1 (en) * | 2004-05-28 | 2005-12-01 | Bellman Robert A | Dehydroxylation and purification of calcium fluoride materials using a halogen containing plasma |
| JP2013249235A (en) * | 2012-06-01 | 2013-12-12 | Mitsubishi Chemicals Corp | Method for producing fluoride salts, and fluoride salts, and method for producing silicon using the fluoride salts |
| CN104138668A (en) * | 2014-07-16 | 2014-11-12 | 中国科学院上海应用物理研究所 | Electromagnetic type fused salt evaporating method |
-
2020
- 2020-09-17 CN CN202010979157.9A patent/CN112158807A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3816600A (en) * | 1970-09-25 | 1974-06-11 | Philips Corp | Method of manufacturing metal fluorides and metal fluoride mixtures which do not comprise oxygen |
| GB1453822A (en) * | 1973-02-09 | 1976-10-27 | Asea Ab | Method for the inductive heating of metallic melts |
| JPS63215523A (en) * | 1987-03-04 | 1988-09-08 | Sumitomo Electric Ind Ltd | Production of fluoride glass |
| US20050263064A1 (en) * | 2004-05-28 | 2005-12-01 | Bellman Robert A | Dehydroxylation and purification of calcium fluoride materials using a halogen containing plasma |
| JP2013249235A (en) * | 2012-06-01 | 2013-12-12 | Mitsubishi Chemicals Corp | Method for producing fluoride salts, and fluoride salts, and method for producing silicon using the fluoride salts |
| CN104138668A (en) * | 2014-07-16 | 2014-11-12 | 中国科学院上海应用物理研究所 | Electromagnetic type fused salt evaporating method |
Non-Patent Citations (1)
| Title |
|---|
| 胡伯平: "《稀土永磁材料 下》", 30 January 2017, 冶金工业出版社 * |
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Application publication date: 20210101 |
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