CN114507011A - Bismuth germanate glass with high near-infrared band transmittance and preparation method thereof - Google Patents
Bismuth germanate glass with high near-infrared band transmittance and preparation method thereof Download PDFInfo
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- CN114507011A CN114507011A CN202210055374.8A CN202210055374A CN114507011A CN 114507011 A CN114507011 A CN 114507011A CN 202210055374 A CN202210055374 A CN 202210055374A CN 114507011 A CN114507011 A CN 114507011A
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- glass
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- bismuth germanate
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- 239000011521 glass Substances 0.000 title claims abstract description 47
- 238000002834 transmittance Methods 0.000 title claims abstract description 16
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 11
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 8
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract 2
- 238000000227 grinding Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 229910001018 Cast iron Inorganic materials 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 239000000156 glass melt Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 239000005347 annealed glass Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- -1 rare earth ions Chemical class 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
Images
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
- C03C4/00—Compositions for glass with special properties
- C03C4/10—Compositions for glass with special properties for infrared transmitting glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses bismuth germanate glass with high transmittance in a near-infrared band and a preparation method thereof. The glass component comprises the following raw materials in percentage by mole: GeO2:40~60%、Bi2O3:25~45%、Ga2O3:5~15%、Na2CO310 to 15 percent. The glass is prepared by a melting quenching method. The glass provided by the invention is simple in preparation method, good in rare earth ion doped luminescent property and high in transmittance in a wave band of 700 nm-2700 nmHigh, the highest transmittance is over 80 percent. The glass is suitable for being applied to a rare earth ion doped matrix material capable of emitting light in a near infrared band.
Description
Technical Field
The invention relates to the technical field of rare earth luminescent materials, in particular to bismuth germanate glass with high transmittance in near-infrared band and a preparation method thereof.
Background
The near infrared light is an electromagnetic wave band covering 780-2526 nm, and due to the specific wavelength range of the near infrared light, the near infrared light has unique characteristics: low absorption rate, high penetrability and high heat effect. Based on the excellent characteristics of near infrared, the near infrared technology has been developed into a new optical technology field at home and abroad, and plays a very important role in a plurality of fields such as material analysis, fluorescent marking, optical fiber communication, medical detection, infrared camouflage, military reconnaissance, petrochemical industry, nonlinear optical materials and the like.
The research on near-infrared luminescent ions is mainly focused on Nd3+、Er3+Plasma of rare earth ions due to Er3+Ion(s)4I13/2→4I15/2The transition emission of near-infrared light of 1.54 μm has many unique advantages, and various near-infrared fluorescent materials and laser materials doped with erbium are widely researched and applied. At present, the requirements on the aspects of luminous efficiency, luminous intensity, material stability and the like of the near-infrared luminescent material are gradually increased, and a proper matrix is searched for further improving Er3+The near infrared luminescence of the rare earth ions has very important significance.
The bismuth germanate glass has lower phonon energy, excellent physicochemical stability and higher transmission performance in a near infrared band, and the characteristics are Er3+The realization of the plasma in the near infrared high-efficiency luminescence provides guarantee.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide bismuth germanate glass with high transmittance in a near-infrared band and a preparation method thereof. The bismuth germanate glass with high near-infrared band transmittance is prepared from the following raw materials in percentage by mole: GeO2: 40~60%、Bi2O3: 25~45%、Ga2O3: 5~15%、Na2CO3: 10~15%。
The preparation method of the bismuth germanate glass with high near-infrared band transmittance comprises the following steps:
1) preparing materials: weighing raw materials with corresponding mass according to the mol percentage of the glass composition by using a Ge-containing compound and/or salt, a Bi-containing compound and/or salt, a Ga-containing compound and/or salt and a Na-containing compound and salt, and grinding and uniformly mixing in a mortar;
2) melting: pouring the glass raw materials which are ground and mixed uniformly into a crucible, putting the crucible into a silicon carbide rod electric furnace, and melting the glass raw materials in an air atmosphere at the melting temperature of 1000-1200 ℃ for 30-60 minutes;
3) molding: pouring the glass melt into a cast iron mold preheated to 350-450 ℃;
4) annealing: putting the formed glass into a muffle furnace for annealing at the temperature of 350-450 DEG CoAnd C, annealing for 2-4 hours. Then, a power supply of the muffle furnace is closed and cooled to room temperature along with the furnace;
5) polishing: and cutting, grinding and polishing the annealed glass to obtain a glass sample.
The bismuth germanate glass with high near-infrared band transmittance has the advantages of high near-infrared band transmittance, simple preparation process and low phonon energy, and can be used as a near-infrared band substrate luminescent material.
Drawings
FIG. 1 shows a transmission spectrum of a bismuth germanate glass provided in example 1 of the present invention.
Detailed Description
The present invention is further described below.
Example 1:
according to the composition: 40GeO2-40Bi2O3-10Ga2O3-10Na2CO3(mol%) the GeO required was weighed so that the total mass was 20 g2、Bi2O3、Ga2O3、Na2CO3And (3) putting the powder raw materials into an agate mortar, fully grinding and uniformly mixing. Pouring the uniformly mixed glass raw materials into a crucible, covering a mullite cover, and placing the crucible at 1100 DEGoMelting in a C silicon carbide rod electric furnace for 40 minutes, and then quickly pouring the glass melt into a preheating pipe 350oC in the cast iron die, after the glass is formed, the glass is transferred into 380oAnd C, annealing for 2 hours in a muffle furnace, and naturally cooling to room temperature to obtain initial glass. After annealingAnd cutting, grinding and polishing the glass to obtain a glass sample.
In this example, a transmittance chart of bismuth germanate glass having a high transmittance in a near-infrared band is shown in fig. 1.
Example 2:
according to the composition: 40GeO2-40Bi2O3-8Ga2O3-12Na2CO3(mol%) the GeO required was weighed so that the total mass was 20 g2、Bi2O3、Ga2O3、Na2CO3And (3) putting the powder raw materials into an agate mortar, fully grinding and uniformly mixing. Pouring the uniformly mixed glass raw materials into a crucible, covering the crucible with a mullite cover, and placing the crucible at 1100 DEG CoMelting for 40 minutes in a C silicon carbide rod electric furnace, and then quickly pouring the glass melt into a preheating 360℃ furnaceoC in the cast iron die, the glass is turned to 370 after being formedoAnd C, annealing for 3 hours in a muffle furnace, and naturally cooling to room temperature to obtain initial glass. And cutting, grinding and polishing the annealed glass to obtain a glass sample.
Example 3:
according to the composition: 50GeO2-30Bi2O3-12Ga2O3-8Na2CO3(mol%) the GeO required was weighed so that the total mass was 20 g2、Bi2O3、Ga2O3、Na2CO3And (3) putting the powder raw materials into an agate mortar, fully grinding and uniformly mixing. Pouring the uniformly mixed glass raw materials into a crucible, covering the crucible with a mullite cover, and placing 1050oMelting in a C silicon carbide rod electric furnace for 40 minutes, and then quickly pouring the glass melt into a preheating pipe 350oC in the cast iron die, the glass is turned to 370 after being formedoAnd C, annealing for 4 hours in a muffle furnace, and naturally cooling to room temperature to obtain initial glass. And cutting, grinding and polishing the annealed glass to obtain a glass sample.
Example 4:
according to the composition: 52GeO2-25Bi2O3-10Ga2O3-13Na2CO3（mol%）Weighing GeO with total mass of 20 g2、Bi2O3、Ga2O3、Na2CO3And (3) putting the powder raw materials into an agate mortar, fully grinding and uniformly mixing. Pouring the uniformly mixed glass raw materials into a crucible, covering the crucible with a mullite cover, and placing the crucible at 1000 DEGoMelting in a C silicon carbide rod electric furnace for 40 minutes, and then quickly pouring the glass melt into a preheating pipe 350oC, in the cast iron die, the glass is turned to 360 degrees after being formedoAnd C, annealing for 2 hours in a muffle furnace, and naturally cooling to room temperature to obtain initial glass. And cutting, grinding and polishing the annealed glass to obtain a glass sample.
The above-described embodiments are intended to illustrate rather than to limit the invention, and any modifications and variations of the present invention are within the spirit of the invention and the scope of the appended claims.
Claims (3)
1. The bismuth germanate glass with high near-infrared band transmittance is characterized by comprising the following components in percentage by mole:
GeO2: 40~60%；
Bi2O3: 25~45%；
Ga2O3: 5~15%；
Na2CO3: 8~15%。
2. the bismuth germanate glass with high near-infrared band transmittance according to claim 1, wherein the glass comprises the following components in percentage by mole:
GeO2: 40~52%；
Bi2O3: 25~40%；
Ga2O3: 8~12%；
Na2CO3: 10~13%。
3. a method for preparing bismuth germanate glass with high near-infrared band transmittance according to claim 1 or 2, which is characterized by comprising the following steps:
1) preparing materials: weighing raw materials with corresponding mass according to the mol percentage of the selected glass composition by using a Ge-containing compound and/or salt, a Bi-containing compound and/or salt, a Ga-containing compound and/or salt and a Na-containing compound and/or salt, and grinding and uniformly mixing in a mortar;
2) melting: pouring the glass raw material which is ground and mixed uniformly into a crucible, putting the crucible into a silicon carbide rod electric furnace, and melting the glass raw material in an air atmosphere at the melting temperature of 1000-1200 DEG CoC, melting time is 30-60 minutes;
3) molding: pouring the glass melt into a preheating furnace for 350-450oC, in the cast iron die;
4) annealing: putting the formed glass into a muffle furnace for annealing at the temperature of 350-450 DEG CoC, annealing for 2-4 hours, and then closing a power supply of the muffle furnace to cool to room temperature along with the furnace;
5) polishing: and cutting, grinding and polishing the annealed glass to obtain a glass sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210055374.8A CN114507011A (en) | 2022-01-18 | 2022-01-18 | Bismuth germanate glass with high near-infrared band transmittance and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210055374.8A CN114507011A (en) | 2022-01-18 | 2022-01-18 | Bismuth germanate glass with high near-infrared band transmittance and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674690A (en) * | 2012-05-31 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | 3 mu m rare earth ion doped bismuth-germinate laser glass and preparation method thereof |
| CN103030274A (en) * | 2013-01-17 | 2013-04-10 | 中国科学院上海光学精密机械研究所 | Intermediate infrared 2.7 mum luminous erbium ion-doped gallium germanium bismuthate glass |
| CN108585482A (en) * | 2018-05-08 | 2018-09-28 | 上海应用技术大学 | A kind of white light LEDs fluorescent glass piece and preparation method thereof |
-
2022
- 2022-01-18 CN CN202210055374.8A patent/CN114507011A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674690A (en) * | 2012-05-31 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | 3 mu m rare earth ion doped bismuth-germinate laser glass and preparation method thereof |
| CN103030274A (en) * | 2013-01-17 | 2013-04-10 | 中国科学院上海光学精密机械研究所 | Intermediate infrared 2.7 mum luminous erbium ion-doped gallium germanium bismuthate glass |
| CN108585482A (en) * | 2018-05-08 | 2018-09-28 | 上海应用技术大学 | A kind of white light LEDs fluorescent glass piece and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| QIUHUA NIE等: "Upconversion and fluorescence spectral studies of Er3+/Yb3+-codoped Bi2Q3–GeO2–Ga2O3–Na2O glasses", 《SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY》 * |
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Application publication date: 20220517 |