CN112707641A - Edge-covered glass for neodymium-doped phosphate laser glass integrated edge covering and preparation method thereof - Google Patents
Edge-covered glass for neodymium-doped phosphate laser glass integrated edge covering and preparation method thereof Download PDFInfo
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- CN112707641A CN112707641A CN202110135700.1A CN202110135700A CN112707641A CN 112707641 A CN112707641 A CN 112707641A CN 202110135700 A CN202110135700 A CN 202110135700A CN 112707641 A CN112707641 A CN 112707641A
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- 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
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
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- 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
- C03B5/225—Refining
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- 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
- C03B5/235—Heating the glass
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Abstract
A bordure glass for neodymium-doped phosphate laser glass integrated bordure and a preparation method thereof are disclosed, wherein the bordure glass comprises the following components in molar ratio formula P2O5:58‑62mol％、Al2O3：8‑12mol％、K2O：12‑16mol％、Na2O：4‑6mol％、BaO：8‑12mol％、La2O3: 1-2 mol% Cu in edge glass for absorbing spontaneous amplified emission (ASE) and suppressing Parasitic Oscillation (PO)2+Is added in the form of CuO, and the content is 1 percent of the total weight of the formula. Expansion curve and T of the edge-wrapped glass and the N31 type neodymium-doped phosphate laser glassgAnd TfClose or even equal, thereby reducing or even eliminating the residual stress caused by the factor and leading the bonding strength of the integrated edge covering to be higher, and simultaneously adjusting the edge coveringThe refractive index of the glass is close to or equal to that of the neodymium-doped phosphate laser glass so as to reduce residual reflection caused by the difference of the refractive indexes; the N31 type neodymium-doped phosphate laser glass after the integrated hard edge covering can meet the engineering application and has practical significance, and meets the engineering application requirements of a high-power solid laser system.
Description
Technical Field
The invention relates to laser glass, in particular to edge-covered glass for integrated edge covering of neodymium-doped phosphate laser glass and a preparation method thereof.
Background
The high-power solid laser system mainly adopts the sheet-shaped neodymium-doped phosphate laser glass as a gain medium, but Amplified Spontaneous Emission (ASE) and Parasitic Oscillation (PO) can be generated in the sheet-shaped neodymium-doped phosphate laser glass, and the energy storage efficiency and the laser output capability of the system are influenced. At present, the main method for inhibiting ASE and PO is to edge cover the neodymium-doped phosphate laser glass, i.e. the side edge of the sheet neodymium-doped phosphate laser glass perpendicular to the optical path direction is provided with a medium for absorbing ASE and PO. The sheet neodymium-doped phosphate laser glass is generally rectangular sheet or oval sheet, and the rectangular sheet is generally bound by adopting a polymer bonding and binding technology[1：Howard T.Powell,Michael o.Riley,Charles R.Wolfe,et al.Composite polymer glass edge for laser disks[P].U.S.English,4849036,July 18,1989；2：T.Meng,J.Tang,J.Hu et al.Edge cladding technology to suppress the amplified stimulated emission(ASE)of the laser disks[P],Chinese Patent ZL201010273819.7,October 27,2013]The problem that the neodymium-doped phosphate laser glass with the organic polymer edge covering cannot bear thermal shock under a high-power working condition and cannot work in a cooling medium under the high-power condition exists. The oval sheet is generally coated and sintered to cover the edges[3：Hisayoshi Toratani,Hidakamachi.Edge-cladding glass of disc laser glass:us4217382[p].1980-08-12；4：Alexander J.Marker.Cladding glass ceramic for use in high powered lasers:us 5718979[p].1998-02-17；5：S E Stokowski,S M Yarema,I F Stowers.Edge Cladding,Laser Program Annual Report 1980,Vol(1):p214-217]However, the coating and edge covering technology is mainly applied to the N21 type neodymium-doped phosphate laser glass elliptical sheet, and the coating and sintering edge covering surface has a large amount of bubbles, defects and carbides, so that the residual reflection is increased (about 0.1 multiplied by 10)-2～25×10-2Range) and influence the ability to inhibit ASE and PO. For the new generation of N31 type Nd doped phosphate laser glass, its TgT at 450 ℃ to N21gThe temperature of 550 ℃ is about 100 ℃, the corresponding sintering temperature needs to be reduced, so that the coated edge-wrapping glass powder has incomplete sintering and the risk of stress cracking, the refractive index of N31 is lower than that of N21, the refractive index of the edge-wrapping glass powder is also correspondingly reduced to match the refractive index, and the problem of low melting point and low refractive index is difficult to take into account is solved, so that only the N31 type neodymium-doped phosphate laser glass elliptical sheet can be integrally wrapped based on the method, namely the side surface of the neodymium-doped phosphate laser glass is polished and is subjected to T-shaped surface treatmentgAnd (3) preserving heat near the temperature, then pouring and welding the molten edge-covered glass melt on the side surface of the laser neodymium glass, and then annealing and cooling. At present, no wrapping glass specially applied to N31 type neodymium-doped phosphate laser glass integrated wrapping exists, and the expansion curve and T of wrapping glass of a polymer wrapping technology and a coating sintering wrapping technology and N31 type neodymium-doped phosphate laser glassg、TfAnd the refractive indexes are not matched, so that the edge-coated glass suitable for the integrated edge coating needs to be developed according to the characteristics of the N31 type neodymium-doped phosphate laser glass.
Disclosure of Invention
In order to reduce residual stress and residual reflection after the integrated edge covering of the N31 type neodymium-doped phosphate laser glass, the invention provides edge covering glass for the integrated edge covering of the neodymium-doped phosphate laser glass and a preparation method thereof, wherein the expansion curve and T of the edge covering glass and the N31 neodymium-doped phosphate laser glass are the samegAnd TfThe refractive index of the edge glass is adjusted to be similar or equal to that of the neodymium-doped phosphate laser glass so as to reduce residual reflection caused by the difference of the refractive indexes; the N31 type neodymium-doped phosphate laser glass after hard edge covering can meet the engineering application and has practical significance, and meets the engineering application requirements of a high-power solid laser system.
The specific technical solution of the invention is as follows:
the utility model provides a glass that bordures that is used for high power neodymium-doped phosphate laser glass's integration to bordure, its characterized in that this glass that bordures mole percentage composition as follows:
P2O5：58-62mol％、
Al2O3：8-12mol％、
K2O：12-16mol％、
Na2O：4-6mol％、
BaO：8-12mol％、
La2O3：1-2mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation method of the edge-coated glass comprises the following steps:
1) the following introductions with a purity of more than 99.99% are used as raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO. And weighing the introduced substances as raw materials according to the molar ratio of the glass components, and uniformly mixing to form a mixture.
2) And transferring the mixture into a platinum crucible, placing the crucible into a 1200-1300 ℃ silicon carbide melting furnace for melting and stirring for 0.5-1.5 hours to obtain glass liquid.
3) And covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 0.5-1.5 hours.
4) After stopping introducing oxygen, clarifying the glass liquid for 3-4 hours at 1200 ℃.
5) Pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
The invention has the following technical effects:
the invention relates to edge-covered glass developed by aiming at the integrated edge covering of N31 type neodymium-doped phosphate laser glass, which can reduce the residual stress of an interface and reduce the residual reflection after the integrated edge covering. The invention relates to a formula of N31 type neodymium-doped phosphate laser neodymium glass, which comprises the following components: (58-62) P2O5-(8-12)Al2O3-(12-16)K2O-(8-12)BaO-(1-2)Re2O3(molar ratio, Re)2O3Rare earth oxide) as a base for the edge-coated glass by addition of Na2O, while adding Re2O3Is set to La2O3And adjusting the expansion curve and T by adding CuO and adjusting the component proportiongAnd TfThe expansion curve, T, of the glass was adjusted to that of N31 Nd-doped phosphate laser glassgAnd TfThe refractive index of the edge glass can be adjusted to be similar to or equal to that of the neodymium-doped phosphate laser glass so as to reduce residual reflection caused by the difference of the refractive indexes; the N31 type neodymium-doped phosphate laser glass after hard edge covering can meet the engineering application and has practical significance, and meets the engineering application requirements of a high-power solid laser system.
Drawings
FIGS. 1-5 are sequential stress birefringence measurements of samples after the overclad glasses of examples 1-5 were applied to an integrated overclad.
FIGS. 6 to 10 are graphs showing the temperature expansion curves and T of the edge-coated glasses of examples 1 to 5 in this orderg、Tf
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the scope of the present invention should not be limited thereto.
Example 1:
the coated glass of example 1 consists of the following mole percentages:
P2O5：58mol％、
Al2O3：8mol％、
K2O：16mol％、
Na2O：4mol％、
BaO：12mol％、
La2O3：2mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation steps of the edge-wrapped glass are as follows:
1) adopting an introduction substance with the purity of more than 99.99 percent as a raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO. Weighing the introduced substances as raw materials according to the molar ratio of the glass components in the example 1, and uniformly mixing to form a mixture;
2) transferring the mixture into a platinum crucible, putting the crucible into a 1200 ℃ silicon carbide melting furnace for melting and stirring for 0.5 hour to obtain glass liquid;
3) covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 0.5 hour;
4) after stopping introducing oxygen, clarifying the molten glass for 3 hours at 1200 ℃;
5) pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour. FIG. 1 shows the stress birefringence of example 1, and FIG. 6 shows the expansion curve of the edge glass of example 1.
Example 2:
the edge-coated glass example 2 consists of the following mole percentages:
P2O5：59mol％、
Al2O3：10mol％、
K2O：13mol％、
Na2O：6mol％、
BaO：10mol％、
La2O3：2mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation steps of the edge-wrapped glass are as follows:
1) adopting an introduction substance with the purity of more than 99.99 percent as a raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO, weighing the introduced substances as raw materials according to the molar ratio of the glass components in the embodiment 2, and uniformly mixing to form a mixture;
2) transferring the mixture into a platinum crucible, putting the crucible into a silicon carbide melting furnace at 1250 ℃, melting and stirring for 1 hour to obtain glass liquid;
3) covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 1 hour;
4) after stopping introducing oxygen, clarifying the molten glass for 3 hours at 1200 ℃;
5) pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
FIG. 2 stress birefringence for example 2, FIG. 7 expansion curve for example 2. edge glass.
Example 3:
the coated glass of example 3 consists of the following mole percentages:
P2O5：60mol％、
Al2O3：9mol％、
K2O：14mol％、
Na2O：5mol％、
BaO：11mol％、
La2O3：1mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation steps of the edge-wrapped glass are as follows:
1) adopting an introduction substance with the purity of more than 99.99 percent as a raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO. Weighing the introduced substances as raw materials according to the molar ratio of the glass components in the embodiment 3, and uniformly mixing to form a mixture;
2) transferring the mixture into a platinum crucible, putting the crucible into a 1300 ℃ silicon carbide melting furnace for melting and stirring for 1.5 hours to obtain glass liquid;
3) covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 1.5 hours;
4) after stopping introducing oxygen, clarifying the molten glass at 1200 ℃ for 4 hours;
5) pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
FIG. 3 stress birefringence for example 3, FIG. 8 expansion curve for example 3 clad glass.
Example 4:
the edge-coated glass of example 4 consists of the following mole percentages:
P2O5：61mol％、
Al2O3：12mol％、
K2O：12mol％、
Na2O：6mol％、
BaO：8mol％、
La2O3：1mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation steps of the edge-wrapped glass are as follows:
1) adopting an introduction substance with the purity of more than 99.99 percent as a raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO. According to the molar ratio of the glass components in the example 4, the introduced substances are weighed and taken as raw materials to be uniformly mixed to form a mixture.
2) And transferring the mixture into a platinum crucible, putting the crucible into a 1200 ℃ silicon carbide melting furnace to melt and stir for 0.5 hour to obtain glass liquid.
3) And covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 0.5 hour.
4) After the oxygen supply was stopped, the glass was clarified at 1200 ℃ for 3 hours.
5) Pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
FIG. 4 stress birefringence for example 4, FIG. 9 expansion curve for example 4, edge glass.
Example 5
The coated glass of example 5 consists of the following mole percentages:
P2O5：62mol％、
Al2O3：11mol％、
K2O：12mol％、
Na2O：4mol％、
BaO：9mol％、
La2O3：2mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
The preparation steps of the edge-wrapped glass are as follows:
1) by purity ofMore than 99.99% of the introduced substance is used as raw material P2O5、Al(H2PO4)3、KPO3、NaPO3、Ba(H2PO4)2、La2O3And CuO. The glass components of example 5 were weighed and mixed uniformly to form a mixture.
2) And transferring the mixture into a platinum crucible, putting the crucible into a 1300 ℃ silicon carbide melting furnace for melting and stirring for 1.5 hours to obtain glass liquid.
3) And covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 1.5 hours.
4) After the oxygen supply was stopped, the glass was clarified at 1200 ℃ for 4 hours.
5) Pouring the molten glass onto a preheated iron plate for shaping, then quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
FIG. 5 stress birefringence for example 5, FIG. 10 expansion curve for example 5. bordure glass.
Table 1 shows the refractive index values of the edge-coated glasses of examples 1 to 5.
Table 2 shows the residual reflectance values of the samples after the edge-coated glasses of examples 1 to 5 were applied to the integrated edge coating.
Table 3 shows clear aperture stress birefringence measurements of samples after the edge-coated glasses of examples 1 to 5 were applied to the integrated edge coating. The neodymium-doped phosphate laser glass had a thickness of 5.0cm and a stress birefringence value of the test value divided by the thickness in FIGS. 1-6.
Claims (2)
1. An integrated edge-coated glass for high-power neodymium-doped phosphate laser glass is characterized by comprising the following components in percentage by mol:
P2O5：58-62mol％、
Al2O3：8-12mol％、
K2O：12-16mol％、
Na2O：4-6mol％、
BaO：8-12mol％、
La2O3：1-2mol％，
CuO is added in an additional mode, and the weight of CuO is 1 percent of the total weight of the preparation.
2. The method of making an integrally overclad glass for a neodymium-doped phosphate laser glass according to claim 1, characterised in that the method of making comprises the steps of:
1) the following introductions with a purity of more than 99.99% are used as raw material P2O5、Al(H2PO4)3、KPO3、
NaPO3、Ba(H2PO4)2、La2O3And CuO, weighing the introduced substances as raw materials according to the molar ratio of the glass components in claim 1, and uniformly mixing to form a mixture;
2) transferring the mixture into a platinum crucible, placing the crucible into a 1200-1300 ℃ silicon carbide melting furnace for melting and stirring for 0.5-1.5 hours to obtain glass liquid;
3) covering the platinum crucible with a cover, and introducing oxygen into the glass liquid to remove water for 0.5-1.5 hours;
4) after stopping introducing oxygen, clarifying the molten glass for 3-4 hours at 1200 ℃;
5) pouring the molten glass onto a preheated iron plate for shaping, quickly transferring the molten glass into a muffle furnace at the temperature of 460 ℃, preserving the heat for 3 to 4 hours, and then cooling the molten glass to the room temperature at the speed of 6 ℃/hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185145A (en) * | 2021-04-28 | 2021-07-30 | 中国建筑材料科学研究总院有限公司 | Laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and preparation method and application thereof |
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| US4217382A (en) * | 1978-06-20 | 1980-08-12 | Hoya Corporation | Edge-cladding glass of disc laser glass |
| US4229220A (en) * | 1977-08-31 | 1980-10-21 | Hoya Corporation | Edge-coating glass for laser disks |
| CN202384295U (en) * | 2011-11-22 | 2012-08-15 | 中国建筑材料科学研究总院 | Micro-channel plate with high gain and low noise |
| CN105293902A (en) * | 2015-11-19 | 2016-02-03 | 中国建筑材料科学研究总院 | Edge-cladding glass, optical fiber image transmitting element and their preparation methods |
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2021
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| US4229220A (en) * | 1977-08-31 | 1980-10-21 | Hoya Corporation | Edge-coating glass for laser disks |
| US4217382A (en) * | 1978-06-20 | 1980-08-12 | Hoya Corporation | Edge-cladding glass of disc laser glass |
| CN202384295U (en) * | 2011-11-22 | 2012-08-15 | 中国建筑材料科学研究总院 | Micro-channel plate with high gain and low noise |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185145A (en) * | 2021-04-28 | 2021-07-30 | 中国建筑材料科学研究总院有限公司 | Laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and preparation method and application thereof |
| CN113185145B (en) * | 2021-04-28 | 2022-05-17 | 中国建筑材料科学研究总院有限公司 | Laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation and its preparation method and application |
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