CN115650590B - Containing YF 3 Crystal phase fluoride microcrystalline glass and preparation method thereof - Google Patents
Containing YF 3 Crystal phase fluoride microcrystalline glass and preparation method thereof Download PDFInfo
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- CN115650590B CN115650590B CN202211173350.9A CN202211173350A CN115650590B CN 115650590 B CN115650590 B CN 115650590B CN 202211173350 A CN202211173350 A CN 202211173350A CN 115650590 B CN115650590 B CN 115650590B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
YF-containing material 3 Fluoride microcrystalline glass with crystalline phase and preparation method thereof, and the fluoride microcrystalline glass comprises InF as a component 3 ‑BaF 2 ‑‑SrF 2 ‑YF 3 -NaF. The concrete composition is as follows: inF (Inf) 3 :35‑40mol％；BaF 2 ‑SrF 2 :35‑40mol％；YF 3 15-20mol%; naF 8-10mol%. The material is YF 3 Microcrystalline glass is formed by uniformly distributing microcrystals in a fluoride glass matrix. Said YF-containing 3 The fluoride microcrystalline glass with the crystalline phase can realize the full-wave band transmission from visible light to middle infrared. The invention adopts a strong quenching method, is prepared in one step, and has simple and safe preparation flow without subsequent heat treatment.
Description
Technical Field
The invention relates to material preparation, in particular to a material containing YF 3 Fluoride microcrystalline glass with crystalline phase and its preparation process.
Background
Fluoride glass ceramics are materials composed of pure fluoride materials that contain crystalline and glassy phases, unlike the conventionally mentioned oxyfluoride, fluorophosphorus and other systems of glass ceramics. The latter is a material in which fluoride crystals are precipitated by heat treatment in a fluoroxy or non-fluorine glass system, which increases phonon energy of the fluoride crystals and the refractive index matching of the glass phase and the crystal phase is low, resulting in poor visible and infrared transmittance. The perfluorinated glass ceramic can keep the low phonon energy of fluoride, keeps the characteristics of excellent mid-infrared transmission and fluorescence performance, and has great application potential in the mid-infrared technical field.
However, because the fluoride glass system lacks a traditional network forming body, the fluoride microcrystalline glass prepared by using a traditional heat treatment method cannot controllably separate out a specific single crystal phase, so that the preparation material of the fluoride microcrystalline glass has no specific application value and development prospect, which hinders the wide application and development of the fluoride microcrystalline glass. In patent CN110194594a, a method for preparing fluoride glass ceramics is disclosed, which does not need heat treatment, but the obtained fluoride glass ceramics contains two crystal phases instead of a single crystal phase, and the existence of multiple crystal phases will seriously affect the transmittance of the glass ceramics, which also hinders the practical application of the glass ceramics. The preparation of fluoride microcrystalline glass containing a single crystal phase is a key technology, and the design and preparation methods of the components are therefore quite challenging to optimize.
Disclosure of Invention
The invention aims to prepare the single YF-containing material by a simple, safe, efficient and easily-controlled method without subsequent heat treatment by using the preferable component proportion 3 Microcrystalline perfluorinated glass ceramics. The microcrystalline glass has single crystalline phase and is transparent from visible light to middle infrared all wave bands.
The technical scheme of the invention is as follows:
containing a single YF 3 The fluoride microcrystalline glass of the crystalline phase is characterized by comprising the following components in percentage by mole:
InF 3 :35-40mol％
BaF 2 -SrF 2 :35-40mol％
YF 3 :15-20mol％
NaF:8-10mol％
YF-containing material 3 The preparation method of the fluoride microcrystalline glass with the crystalline phase is characterized by comprising the following steps:
<1>preparation of raw materials: containing YF as described above 3 Weighing the components of the fluoride microcrystalline glass with crystalline phase in mole percent;
<2> melting: placing the mixture into a platinum crucible in a glove box filled with nitrogen, and placing the crucible into a furnace with the furnace temperature of 860-900 ℃ for melting for 60-90 minutes to obtain molten liquid;
<3>and (3) forming: the melt was cast between two flat molds and the upper and lower surfaces of the melt were ensured to be in full contact with the two molds, the mold preheating temperature being 270±5 ℃. After curing, the YF-containing material with uniform thickness is obtained 3 Transparent thin plate fluoride microcrystalline glass with crystalline phase.
Compared with the prior art, the invention has the following technical effects:
the invention adopts a strong quenching method to prepare the fluorine-containing single YF in one step by designing the components of a fluoride system 3 Compared with the prior art, the fluoride microcrystalline glass with the crystalline phase can obtain fluoride microcrystalline glass with single crystalline phase, and the obtained material is transparent from visible light to mid-infrared full wave band. In addition, the preparation steps are simple and the operation is convenient.
Drawings
FIG. 1 is a YF-containing sample of the present invention 3 XRD diffraction pattern of fluoride glass ceramics in crystalline phase.
FIG. 2 is a YF-containing image of the present invention 3 Transmission spectrum of fluoride glass ceramics in crystalline phase.
Detailed Description
The invention is further illustrated in the following examples and figures, which should not be taken to limit the scope of the invention.
Example 1
Preparation of raw materials: the mol percent is as follows: 40InF 3 -20BaF 2 -15SrF 2 -15YF 3 -10NaF weigh 20g of batch.
Melting: placing the mixture into a platinum crucible in a glove box filled with nitrogen, and placing the crucible into a furnace with the furnace temperature of 860 ℃ for melting for 90 minutes to obtain molten liquid;
quenching and forming: the melt was cast between two flat molds and the upper and lower surfaces of the melt were ensured to be in full contact with the two molds, the mold preheating temperature being 270±5 ℃. After curing, the YF-containing material with uniform thickness is obtained 3 Transparent thin plate fluoride microcrystalline glass with crystalline phase.
Example 2
Preparation of raw materials: 40InF in mole percent 3 -20BaF 2 -13SrF 2 -15YF 3 8NaF weigh 20g of batch.
Melting: placing the mixture into a platinum crucible in a glove box filled with nitrogen, and melting for 80 minutes at the furnace temperature of 870 ℃ to obtain a melt;
quenching and forming: casting the melt between two flat molds and ensuring the meltThe upper and lower surfaces are fully contacted with two dies, and the preheating temperature of the dies is 270+/-5 ℃. After curing, the YF-containing material with uniform thickness is obtained 3 Transparent thin plate fluoride microcrystalline glass with crystalline phase.
Example 3
Preparation of raw materials: 35InF in mole percent 3 -15BaF 2 -20SrF 2 -20YF 3 -10NaF weigh 20g of batch.
Melting: placing the mixture into a platinum crucible in a glove box filled with nitrogen, and melting for 60 minutes at the furnace temperature of 900 ℃ to obtain a melt;
quenching and forming: the melt was cast between two flat molds and the upper and lower surfaces of the melt were ensured to be in full contact with the two molds, the mold preheating temperature being 270±5 ℃. After curing, the YF-containing material with uniform thickness is obtained 3 Transparent thin plate fluoride microcrystalline glass with crystalline phase.
The remaining examples of parameters are shown in the following table:
FIG. 1 is a YF-containing sample of the present invention 3 XRD diffraction diagram of fluoride microcrystalline glass with crystalline phase, YF can be seen in the diagram 3 The characteristic diffraction peak of (2) shows that the crystal phase in the microcrystalline glass is YF 3 。
FIG. 2 is a YF-containing image of the present invention 3 The transmission spectrum of the fluoride glass ceramics in the crystalline phase can be seen to be transparent in the full band from visible (0.5 μm) to mid-infrared (9.5 μm).
Claims (2)
1. Containing a single YF 3 The fluoride microcrystalline glass of the crystalline phase is characterized by comprising the following components in percentage by mole:
InF 3 :35-40mol％；
BaF 2 and SrF 2 :35-40mol％；
YF 3 :15-20mol％；
NaF:8-10mol％。
2. Containing a single YF 3 The preparation method of the fluoride microcrystalline glass with the crystalline phase is characterized by comprising the following steps:
<1>preparation of raw materials: the process of claim 1 wherein the composition comprises a single YF 3 Weighing the components of the fluoride microcrystalline glass with crystalline phase in mole percent;
<2> melting: placing the mixture into a platinum crucible in a glove box filled with nitrogen, and placing the crucible into a furnace with the furnace temperature of 860-900 ℃ for melting for 60-90 minutes to obtain molten liquid;
<3>quenching and forming: casting the melt between two flat plates, ensuring that the upper and lower surfaces of the melt are fully contacted with the two dies, preheating the dies at 270+/-5 ℃, and solidifying to obtain the single YF-containing material with uniform thickness 3 Thin fluoride glass ceramics with crystalline phases.
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| CN202211173350.9A CN115650590B (en) | 2022-09-26 | 2022-09-26 | Containing YF 3 Crystal phase fluoride microcrystalline glass and preparation method thereof |
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| CN115650590B true CN115650590B (en) | 2023-09-01 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087884A (en) * | 1992-09-21 | 1994-06-15 | 康宁股份有限公司 | Contain rare earth addition, stable cadmium halide glasses |
| CN1927752A (en) * | 2006-09-27 | 2007-03-14 | 中国科学院上海光学精密机械研究所 | Infrared-transmitting fluorozirconate microcrystalline glass and preparation method thereof |
| CN110194594A (en) * | 2019-05-29 | 2019-09-03 | 中国科学院上海光学精密机械研究所 | Fluorine indium glass ceramics and preparation method thereof containing erbium ion-doped strontium fluoride and yttrium fluoride mixed crystal |
| CN111925117A (en) * | 2020-06-05 | 2020-11-13 | 哈尔滨工程大学 | Ho3+Doped ZBYA fluoride glasses |
| CN114835403A (en) * | 2022-03-25 | 2022-08-02 | 哈尔滨工程大学 | Zinc fluoride-aluminum fluoride based microcrystalline glass and preparation method thereof |
-
2022
- 2022-09-26 CN CN202211173350.9A patent/CN115650590B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087884A (en) * | 1992-09-21 | 1994-06-15 | 康宁股份有限公司 | Contain rare earth addition, stable cadmium halide glasses |
| CN1927752A (en) * | 2006-09-27 | 2007-03-14 | 中国科学院上海光学精密机械研究所 | Infrared-transmitting fluorozirconate microcrystalline glass and preparation method thereof |
| CN110194594A (en) * | 2019-05-29 | 2019-09-03 | 中国科学院上海光学精密机械研究所 | Fluorine indium glass ceramics and preparation method thereof containing erbium ion-doped strontium fluoride and yttrium fluoride mixed crystal |
| CN111925117A (en) * | 2020-06-05 | 2020-11-13 | 哈尔滨工程大学 | Ho3+Doped ZBYA fluoride glasses |
| CN114835403A (en) * | 2022-03-25 | 2022-08-02 | 哈尔滨工程大学 | Zinc fluoride-aluminum fluoride based microcrystalline glass and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Composition adjustments in fuoroindate glasses;Ahmed Boutarfaia等;Journal of Materials chemistry;第937-939页 * |
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