CN101870555B - Method for preparing high erbium-doped barium-contained phosphate laser glass - Google Patents

Method for preparing high erbium-doped barium-contained phosphate laser glass Download PDF

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CN101870555B
CN101870555B CN2010101984508A CN201010198450A CN101870555B CN 101870555 B CN101870555 B CN 101870555B CN 2010101984508 A CN2010101984508 A CN 2010101984508A CN 201010198450 A CN201010198450 A CN 201010198450A CN 101870555 B CN101870555 B CN 101870555B
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glass
erbium
doped barium
phosphate laser
laser glass
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CN101870555A (en
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郭宏伟
贺祯
古先文
王彦青
盖言成
张鲲鹏
李文福
董琦
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for preparing high erbium-doped barium-contained phosphate laser glass, which comprises the following steps of: after uniformly mixing P2O5, BaO, Al2O3 and Er2O3, placing the mixture into a corundum crucible and melting to form glass liquid; then shifting the melted glass liquid together with the corundum crucible into a furnace at 400 DEG C for insulating for 8-20 hours; and finally cooling to room temperature at the rate of 0.1-0.5 DEG C/minute to obtain the high erbium-doped barium-contained phosphate laser glass. The invention for preparing the high erbium-doped barium-contained phosphate laser glass with a high-temperature melting method has simple operation process of preparation process, low melting temperature, low cost, energy saving, environmental protection and adaption to industrialized production. The high rare earth erbium-doped barium-contained phosphate laser glass obtained according to the preparation method of the invention has favorable chemical stability and heat stability, high rare earth dosage, simple melting process, easy clarification of glass and high glass uniformity and is suitable for industrialized production.

Description

The preparation method of high erbium-doped barium-contained phosphate laser glass
Technical field
The present invention relates to a kind of preparation method of phosphate laser glass, particularly a kind of preparation method of high erbium-doped barium-contained phosphate laser glass.
Background technology
Laser glass is widely used in aspects such as industry, natural science, medical science, military affairs.Be used for laser boring, welding, cutting, range finding etc. at industrial circle; The natural science field is used for the research of raman scattering spectra, Brillouin scatter etc.; Medical field is used for the treatment of tetter, tumor resection etc.; Military field is used for aspects such as guidance, navigation and inertial confinement.Phosphate glass has the narrowest effective line width in all oxide glasses, and coefficient of expansion height, thermostability and chemical stability are better, is considered to have most in the following laser glass kind of researching value.
Rare earth element reaches purposes widely because of its particular performances, extremely especially material expert's concern of various countries scientist, the opticglass of doping with rare-earth ions is easy to preparation, good optical character is arranged, bigger emission cross section and high quantum yield, especially for the performance of improving optical function glass and the new optical function of exploitation glass, rare earth has become indispensable important source material.Rare earth ion doped various functional glass just are being subjected to fully paying attention to and using in the fields such as optical communication, lasing safety and 3 nonlinear opticses.People such as Mc Pherson (Mc Pherson.Laser Absorbing FilterGlass[P] .U.S.Patent:5413971,1971) developed the rare earth opticglass that can protect 0.53m and 1.06m wavelength laser. and Nanjing University of Technology (Lu Chunhua. the preparation of high-performance laser safety glass and performance thereof [D], Nanjing: Nanjing University of Technology, 2002) developed laser safety glass with high visible light transmissivity and high optical density (OD).The host glass of above-mentioned materials all is borosilicate glasses.At present, research only limits to the research of low-dosage RE phosphate glass for phosphate laser glass, and the kind of rare earth doped material is less, and the glass of adaptation is formed single.And report very few both at home and abroad about the research of high volume RE phosphate laser glass.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation method of high erbium-doped barium-contained phosphate laser glass is provided.According to the baric phosphate laser glass that preparation method of the present invention obtains, the rare earth volume is big, and melting technology is simple, and glass is easy to clarification, and glass uniformity coefficient height is suitable for suitability for industrialized production.
For achieving the above object, the technical solution used in the present invention is: 1) at first, and by mole% with 50～65% P 2O 5, 25～30% BaO, 3～4% Al 2O 3With 1～20% Er 2O 3Mix; 2) secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1250～1350 ℃ with 20 ℃/minute heating rates and found the formation glass metal, under glass melting temperature, be incubated 3～8 hours, found in the process and adopted the corundum stirring rod to stir 1 minute every 1 hour; 3) then, the glass metal that melts is moved into together with corundum crucible in 400 ℃ the stove and be incubated 8～20 hours; 4) last, be cooled to room temperature with 0.1～0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.
P of the present invention 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide.
The present invention is to Fe in the raw material that mixes 2O 3Content must be less than 0.001% of mixture quality percentage.
The present invention prepares high erbium-doped barium-contained phosphate laser glass by the method for high-temperature fusion, and preparation technology's operating process is simple, and glass melting temperature is low, and is with low cost, and energy-conserving and environment-protective are suitable for suitability for industrialized production.According to high volume rare earth erbium baric phosphate laser glass chemical stability and the good thermal stability that preparation method of the present invention obtains, rare earth volume height, melting technology is simple, and glass is easy to clarification, and glass uniformity coefficient height is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 1 preparation, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 2 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 2 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 3 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 3 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 4 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 4 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 5 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 5 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 6 is the light transmittance curve figure of the high erbium-doped barium-contained phosphate laser glass of embodiment 6 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1: at first, and by mole% with 65% P 2O 5, 30% BaO, 4% Al 2O 3With 1% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1250 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 3 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 8 hours; At last, be cooled to room temperature with 0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.。The density of measuring sample by Archimedes's method is 3.25g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 1.
Embodiment 2: at first, and by mole% with 63% P 2O 5, 29% BaO, 3% Al 2O 3With 5% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1280 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 5 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 10 hours; At last, be cooled to room temperature with 0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.The density of measuring sample by Archimedes's method is 3.31g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 2.
Embodiment 3: at first, and by mole% with 62% P 2O 5, 27% BaO, 3% Al 2O 3With 8% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1300 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 6 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 12 hours; At last, be cooled to room temperature with 0.3 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.The density of measuring sample by Archimedes's method is 3.39g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 3.
Embodiment 4: at first, and by mole% with 59% P 2O 5, 26% BaO, 3% Al 2O 3With 12% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1350 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 6 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 12 hours; At last, be cooled to room temperature with 0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.The density of measuring sample by Archimedes's method is 3.52g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 4.
Embodiment 5: at first, and by mole% with 56% P 2O 5, 26% BaO, 3% Al 2O 3With 15% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1350 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 7 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 15 hours; At last, be cooled to room temperature with 0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.The density of measuring sample by Archimedes's method is 3.69g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 5.
Embodiment 6: at first, and by mole% with 54% P 2O 5, 25% BaO, 3% Al 2O 3With 18% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1350 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 8 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 16 hours; At last, be cooled to room temperature with 0.5 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.The density of measuring sample by Archimedes's method is 3.91g/cm 3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 6.
Embodiment 7: at first, and by mole% with 50% P 2O 5, 26% BaO, 4% Al 2O 3With 20% Er 2O 3Mix, wherein, P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP), BaO is introduced by analytically pure brium carbonate, Al 2O 3Introduced Er by analytically pure aluminium hydroxide 2O 3Introduced by analytically pure erbium oxide; Secondly, adopt the alumina silicate fibre parcel 900 ℃ of lower this raw material that mixes are added, and in the corundum crucible with cover, be warming up to 1320 ℃ with 20 ℃/minute heating rates and found the formation glass metal, insulation is 4 hours under glass melting temperature, founds in the process and adopts the corundum stirring rod to stir 1 minute every 1 hour; Then, the glass metal that melts is moved in 400 ℃ the stove insulation together with corundum crucible 20 hours; At last, be cooled to room temperature with 0.1 ℃/minute speed, namely get high erbium-doped barium-contained phosphate laser glass.
The present invention prepares high volume rare earth erbium baric phosphate laser glass by the method for the broken crucible of high-temperature fusion, and preparation technology's operating process is simple, and glass melting temperature is low, and is with low cost, and energy-conserving and environment-protective are suitable for suitability for industrialized production.The high volume rare earth erbium baric phosphate laser glass chemical stability and the good thermal stability that obtain according to preparation method of the present invention, the rare earth volume is big, melting technology is simple, glass is easy to clarification, glass uniformity coefficient height, be suitable for suitability for industrialized production, have considerable economic and social benefit, application prospect is very wide.

Claims (5)

1. the preparation method of high erbium-doped barium-contained phosphate laser glass is characterized in that:
1) at first, by mole% with 50～65% P 2O 5, 25～30% BaO, 3～4% Al 2O 3With 1～20% Er 2O 3Mix;
2) secondly, down this raw material that mixes is added employing aluminum silicate fiber parcel at 900 ℃, and in the corundum crucible with cover, be warming up to 1250～1350 ℃ with 20 ℃/minute temperature rise rates and found the formation glass metal, under glass melting temperature, be incubated 3～8 hours, found in the process and adopted the corundum stirring rod to stir 1 minute every 1 hour;
3) then, the glass metal that melts is moved into together with corundum crucible in 400 ℃ the stove and be incubated 8～20 hours;
4) last, be cooled to room temperature with 0.1～0.5 ℃/minute speed, promptly get high erbium-doped barium-contained phosphate laser glass.
2. the preparation method of high erbium-doped barium-contained phosphate laser glass according to claim 1 is characterized in that: said P 2O 5Introduced by analytically pure ammonium dihydrogen phosphate (ADP).
3. the preparation method of high erbium-doped barium-contained phosphate laser glass according to claim 1, it is characterized in that: said BaO is introduced by analytically pure barium carbonate.
4. the preparation method of high erbium-doped barium-contained phosphate laser glass according to claim 1 is characterized in that: said Al 2O 3Introduced by analytically pure aluminium hydroxide.
5. the preparation method of high erbium-doped barium-contained phosphate laser glass according to claim 1 is characterized in that: said Er 2O 3Introduced by analytically pure erbium oxide.
CN2010101984508A 2010-06-11 2010-06-11 Method for preparing high erbium-doped barium-contained phosphate laser glass Expired - Fee Related CN101870555B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180670A (en) * 1996-04-17 1998-05-06 康宁股份有限公司 Rare earth doped oxyhalide laser glass
EP0867985A1 (en) * 1997-03-27 1998-09-30 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Erbium-doped planar waveguide
CN1594160A (en) * 2004-04-15 2005-03-16 中国科学院上海光学精密机械研究所 Low-refractive-index high-concentration Er-doped3+Fluorophosphate glass and preparation method thereof
CN1765796A (en) * 2005-08-24 2006-05-03 中国科学院上海光学精密机械研究所 Low-refractive-index erbium-doped fluorophosphate glass and preparation method thereof
CN101481213A (en) * 2009-02-25 2009-07-15 中国科学院上海光学精密机械研究所 2 mu m high-phosphorus-content fluorophosphate laser glass and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6853659B2 (en) * 2002-08-28 2005-02-08 Schott Glass Technologies, Inc. Laser system utilizing highly doped laser glass
US7608551B2 (en) * 2005-07-05 2009-10-27 Margaryan Alfred A Bismuth containing fluorophosphate glass and method for making thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180670A (en) * 1996-04-17 1998-05-06 康宁股份有限公司 Rare earth doped oxyhalide laser glass
EP0867985A1 (en) * 1997-03-27 1998-09-30 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Erbium-doped planar waveguide
CN1594160A (en) * 2004-04-15 2005-03-16 中国科学院上海光学精密机械研究所 Low-refractive-index high-concentration Er-doped3+Fluorophosphate glass and preparation method thereof
CN1765796A (en) * 2005-08-24 2006-05-03 中国科学院上海光学精密机械研究所 Low-refractive-index erbium-doped fluorophosphate glass and preparation method thereof
CN101481213A (en) * 2009-02-25 2009-07-15 中国科学院上海光学精密机械研究所 2 mu m high-phosphorus-content fluorophosphate laser glass and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Shibin Jiang,etl.Er3＋ doped phosphate glasses and lasers.《Journal of Non-Crystalline Solids》.1998,143-148. *
杨钢锋,等.碱土金属氧化物对掺铒磷酸盐玻璃光谱性质的影响.《硅酸盐学报》.2004,第32卷(第8期),954-958. *

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