CN112777940A - Fluorine indium acid salt glass with wide infrared transmission wave band and preparation method thereof - Google Patents
Fluorine indium acid salt glass with wide infrared transmission wave band and preparation method thereof Download PDFInfo
- Publication number
- CN112777940A CN112777940A CN202110110692.5A CN202110110692A CN112777940A CN 112777940 A CN112777940 A CN 112777940A CN 202110110692 A CN202110110692 A CN 202110110692A CN 112777940 A CN112777940 A CN 112777940A
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- Prior art keywords
- glass
- infrared transmission
- wide infrared
- fluoroindate
- transmission band
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- 239000011521 glass Substances 0.000 title claims abstract description 42
- 230000005540 biological transmission Effects 0.000 title claims abstract description 33
- 239000002253 acid Substances 0.000 title claims description 3
- 238000002360 preparation method Methods 0.000 title abstract description 9
- KMUCDTMYYQBVMN-UHFFFAOYSA-N [F].[In] Chemical compound [F].[In] KMUCDTMYYQBVMN-UHFFFAOYSA-N 0.000 title description 3
- 150000003839 salts Chemical class 0.000 title description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 6
- BHHYHSUAOQUXJK-UHFFFAOYSA-L Zinc fluoride Inorganic materials F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 6
- 239000011737 fluorine Substances 0.000 claims abstract description 6
- 229910021620 Indium(III) fluoride Inorganic materials 0.000 claims abstract description 4
- 229910002319 LaF3 Inorganic materials 0.000 claims abstract description 4
- 229910007998 ZrF4 Inorganic materials 0.000 claims abstract description 3
- JNLSTWIBJFIVHZ-UHFFFAOYSA-K trifluoroindigane Chemical compound F[In](F)F JNLSTWIBJFIVHZ-UHFFFAOYSA-K 0.000 claims abstract description 3
- XGDBOJRURXXJBF-UHFFFAOYSA-M fluoroindium Chemical compound [In]F XGDBOJRURXXJBF-UHFFFAOYSA-M 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000005368 silicate glass Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910001369 Brass Inorganic materials 0.000 claims description 5
- 239000010951 brass Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000006060 molten glass Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000002887 superconductor Substances 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 12
- 238000007496 glass forming Methods 0.000 abstract description 6
- 239000013307 optical fiber Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 4
- 239000005383 fluoride glass Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910005270 GaF3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/041—Non-oxide glass compositions
- C03C13/042—Fluoride glass compositions
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a fluorine indate glass with wide infrared transmission wave band and a preparation method thereof, belonging to the technical field of glass, wherein the glass comprises the following components in percentage by weight: InF3：25～35mol％、BaF2‑SrF2‑ZnF2：55～65mol％、GaF3‑LaF3：6～10mol％、ZrF42 to 5 mol%. The wide infrared transmission waveband fluoroindate glass has good glass forming performance, the thermal stability criterion delta T of the glass is more than or equal to 80 ℃, the middle infrared transmittance is high, the transmittance T of the transmission waveband is more than or equal to 90 percent (the sample thickness is 7mm) at 3.2-6 mu m, and the wide infrared transmission waveband, the transmission cut-off wavelength is 8.3 mu m (the sample thickness is 7mm, the cut-off transmittance is 50 percent), so the wide infrared transmission waveband is an ideal matrix material for a middle infrared optical fiber.
Description
Technical Field
The invention relates to the technical field of glass, in particular to fluoroindate glass with a wide infrared transmission waveband and a preparation method thereof.
Background
The fluoroindium silicate glass is InF3Conventional fluoride glasses, which are the main forming components, have been reported since 1980In the past, the wide attention of the scientific field is gained. The glass has a wider transmission waveband (5 mu m) than the zirconium fluoride glass, can break through the limitation of 4 mu m cutoff of optical fiber transmission of the zirconium fluoride glass, can meet the application requirement of a future longer waveband, and has lower phonon energy (509 cm)-1) The material provides a lower phonon energy environment for rare earth ions, and is a core candidate material of a new generation of intermediate infrared transmission media and lasers.
However, the fluoroindium silicate glass has poor glass forming performance and is easy to crystallize, so that severe preparation conditions are required, and large-size fluoroindium glass with uniform performance is not easy to obtain in air, which limits the practical application range thereof.
Therefore, improvement of the glass forming properties of the fluoroindate glass is a critical issue, which needs to be started from the composition optimization of the fluoroindate glass, and a stable fluoroindate glass composition is the basis for the preparation of high quality fluoroindium glass. The component of the fluorine indium glass base is InF3-BaF2-SrF2-ZnF2On the basis of which the composition adjustment is carried out. Currently, there is no fixed and stable fluoroindate glass component system.
Disclosure of Invention
The invention mainly solves the technical problems of easy crystallization, easy volatilization and difficult uniform preparation under the air condition of the existing fluoroindate glass, and provides fluoroindate glass with wide infrared transmission band and good glass forming performance.
The technical scheme of the invention is realized as follows:
the invention provides a fluorine indate glass with wide infrared transmission wave band, which comprises the following components in percentage by weight: InF3：25～35mol％、BaF2-SrF2-ZnF2：55～65mol％、GaF3-LaF3：6～10mol％、ZrF4:2～5mol％。
As a further improvement of the invention, saidBaF2The content range is 18-20 mol%.
As a further improvement of the invention, the SrF2The content range is 20-25 mol%.
As a further development of the invention, the ZnF2The content range is 18-20 mol%.
As a further improvement of the invention, the GaF3The content range is 5-7 mol%.
As a further improvement of the invention, the LaF3The content range is 2-3 mol%.
As a further development of the invention, the superconductor transition temperature (T) of the glassc) Glass transition temperature (T)g)≥80℃。
The invention further provides a preparation method of the wide infrared transmission waveband fluorine indate glass, which is characterized by comprising the following steps:
(1) weighing the batch materials according to the proportion of each component, and fully mixing;
(2) under the protection of inert gas, putting the mixed batch into a platinum crucible, and melting for 1-1.5 h in a melting furnace at 850-900 ℃;
(3) pouring the molten glass onto a brass template preheated to 250-270 ℃, and cooling to obtain the blocky fluoroindium silicate glass.
As a further improvement of the invention, the inert gas is nitrogen.
As a further development of the invention, the temperature of the brass die plate is 260 ℃.
The invention has the following beneficial effects: the wide infrared transmission waveband fluoroindate glass has good glass forming performance, the thermal stability criterion delta T of the glass is more than or equal to 80 ℃, the middle infrared transmittance is high, the transmittance T of the transmission waveband is more than or equal to 90 percent (the sample thickness is 7mm) at 3.2-6 mu m, and the wide infrared transmission waveband, the transmission cut-off wavelength is 8.3 mu m (the sample thickness is 7mm, the cut-off transmittance is 50 percent), so the wide infrared transmission waveband is an ideal matrix material for a middle infrared optical fiber.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a graph of the differential thermal profile of a wide infrared transmission band fluoroindate glass prepared in example 3 of the present invention;
FIG. 2 is a graph showing the infrared transmittance of a wide infrared transmittance band fluoroindate glass prepared in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The glass compositions of 6 specific examples of the invention and 3 comparative examples are listed in table 1 below:
TABLE 1
The preparation method comprises the following steps:
(1) weighing the batch materials according to the proportion of each component, and fully mixing;
(2) under the protection of nitrogen gas, putting the mixed batch into a platinum crucible, and melting for 1.5h in a melting furnace at 870 ℃;
(3) and pouring the molten glass onto a brass template preheated to 260 ℃, and cooling to obtain the blocky fluoroindium silicate glass.
Test example 1
The performance of the fluoroindium silicate glasses prepared in examples 1 to 6 of the present invention and comparative examples 1 to 3 was measured, and the results are shown in Table 2.
The test method comprises the following steps: the characteristic temperature value of the glass sample is measured by a TG-DTA thermogravimetric analyzer, and the transmittance is measured by a Fourier transform infrared spectrometer.
TABLE 2
Compared with the prior art, the prepared fluorine indate glass with wide infrared transmission wave band has good glass forming performance, the criterion of glass thermal stability Delta T is more than or equal to 80 ℃, the middle infrared transmittance is high, the transmittance T of the transmission wave band at 3.2-6 mu m is more than or equal to 90% (the thickness of a sample is 7mm), and the transmission cut-off wavelength of the wide infrared transmission wave band is 8.3 mu m (the thickness of the sample is 7mm, and the cut-off transmittance is 50%), so that the fluorine indate glass is an ideal matrix material for the middle infrared optical fiber.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The wide infrared transmission waveband fluorine indate glass is characterized by comprising the following components in percentage by weight: InF3：25～35mol％、BaF2-SrF2-ZnF2：55～65mol％、GaF3-LaF3：6～10mol％、ZrF4:2～5mol％。
2. The wide infrared transmission band fluoroindate glass of claim 1, wherein the BaF is2The content range is 18-20 mol%.
3. The wide infrared transmission band fluoroindate glass of claim 1, wherein the SrF is2The content range is 20-25 mol%.
4. The wide infrared transmission band fluoroindium acid of claim 1Salt glass, characterized in that the ZnF2The content range is 18-20 mol%.
5. The wide infrared transmission band fluoroindate glass of claim 1, wherein the GaF is a glass of the type3The content range is 5-7 mol%.
6. The wide infrared transmission band fluoroindate glass of claim 1, wherein the LaF is selected from the group consisting of3The content range is 2-3 mol%.
7. The wide infrared transmission band fluoroindate glass of any one of claims 1 to 6, wherein Δ T ═ glass has a superconductor transition temperature (T ═ glass)c) Glass transition temperature (T)g)≥80℃。
8. A method for preparing the wide infrared transmission band fluoroindate glass according to any one of claims 1 to 7, comprising the steps of:
(1) weighing the batch materials according to the proportion of each component, and fully mixing;
(2) under the protection of inert gas, putting the mixed batch into a platinum crucible, and melting for 1-1.5 h in a melting furnace at 850-900 ℃;
(3) pouring the molten glass onto a brass template preheated to 250-270 ℃, and cooling to obtain the blocky fluoroindium silicate glass.
9. The method of claim 8, wherein the inert gas is nitrogen.
10. The method of manufacturing according to claim 8, wherein the temperature of the brass die plate is 260 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110110692.5A CN112777940A (en) | 2021-01-27 | 2021-01-27 | Fluorine indium acid salt glass with wide infrared transmission wave band and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110110692.5A CN112777940A (en) | 2021-01-27 | 2021-01-27 | Fluorine indium acid salt glass with wide infrared transmission wave band and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112777940A true CN112777940A (en) | 2021-05-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110110692.5A Pending CN112777940A (en) | 2021-01-27 | 2021-01-27 | Fluorine indium acid salt glass with wide infrared transmission wave band and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN112777940A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155549A (en) * | 1984-01-25 | 1985-08-15 | Nippon Sheet Glass Co Ltd | Fluoride glass for transmitting infrared ray |
| EP0234581A2 (en) * | 1986-02-28 | 1987-09-02 | Hoya Corporation | Fluoride glass and use thereof |
| JPS62256740A (en) * | 1986-04-30 | 1987-11-09 | Hoya Corp | Fluoride glass |
| CN1375471A (en) * | 2002-03-22 | 2002-10-23 | 中国科学院上海光学精密机械研究所 | Infrared transmitting germanate glass containing fluoride |
| CN112010557A (en) * | 2020-09-09 | 2020-12-01 | 哈尔滨工程大学 | Transparent glass with middle infrared 3.5 mu m luminescence characteristic and preparation method thereof |
-
2021
- 2021-01-27 CN CN202110110692.5A patent/CN112777940A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155549A (en) * | 1984-01-25 | 1985-08-15 | Nippon Sheet Glass Co Ltd | Fluoride glass for transmitting infrared ray |
| EP0234581A2 (en) * | 1986-02-28 | 1987-09-02 | Hoya Corporation | Fluoride glass and use thereof |
| US4761387A (en) * | 1986-02-28 | 1988-08-02 | Hoya Corporation | Fluoride glass |
| JPS62256740A (en) * | 1986-04-30 | 1987-11-09 | Hoya Corp | Fluoride glass |
| CN1375471A (en) * | 2002-03-22 | 2002-10-23 | 中国科学院上海光学精密机械研究所 | Infrared transmitting germanate glass containing fluoride |
| CN112010557A (en) * | 2020-09-09 | 2020-12-01 | 哈尔滨工程大学 | Transparent glass with middle infrared 3.5 mu m luminescence characteristic and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 董大奎 等: "InF3-ZnF2-BaF2-SrF2-RFn系统玻璃性质研究", 《玻璃》 * |
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Application publication date: 20210511 |
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| RJ01 | Rejection of invention patent application after publication |