CN103030299B - P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof - Google Patents

P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof Download PDF

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CN103030299B
CN103030299B CN201210550109.3A CN201210550109A CN103030299B CN 103030299 B CN103030299 B CN 103030299B CN 201210550109 A CN201210550109 A CN 201210550109A CN 103030299 B CN103030299 B CN 103030299B
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glass
ceramic
bao
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CN103030299A (en
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张永明
于磊
马晶
曹启华
宋国轶
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Abstract

P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof, relates to a kind of glass-ceramic and preparation method thereof, and its Mole percent consists of P 2o 5: 40-70, BaO:12-25, Na 2o:3-18, K 2o:3-18, Y 2o 3: 6-25, Eu 2o 3: 1-6, weigh each raw material, the glass metal melted is poured on preheated stainless steel mould, then put into retort furnace and within 1-2 hours, anneal in glass transformation temperature Tg place's insulation; According to the thermal analysis experiment data obtaining glass sample, glass is put into resistance furnace and carry out micritization thermal treatment, namely obtaining pure phase is YPO 4glass-ceramic sample.The glass-ceramic of preparation is translucent shape, and the physicochemical property that to have that solubilize rare earth ions degree is high, rare earth ion spectrum property is wherein good, nonlinear factor is little etc. excellent, are applicable to the fields such as fiber amplifier.

Description

P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof
Technical field
The present invention relates to a kind of glass-ceramic and preparation method thereof, particularly relate to a kind of P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof.
Background technology
Rare earth ion doped glass ceramic material, owing to having homogeneous transparent, moulding process is simple, the superior over-all properties such as physical strength is high, thermal expansivity is adjustable, good thermal shock, resistance to chemical attack, thermal stability are good, it is novel excellent material, for this reason, exploitation physical and chemical performance is stablized with the glass ceramic material of good luminous performance significant, is widely used in the fields such as microelectronics, biomedicine, science and techniques of defence, building decoration as structured material and functional materials.
In recent years, phosphate glass is high and a series of good characteristic such as rare earth ion spectrum property is wherein excellent, nonlinear factor is little because its phonon energy is moderate, to solubilize rare earth ions degree, make phosphoric acid salt become a kind of important laser host material, and obtain investigation and application widely.20 century 70s start to study phosphate laser glass, up to now, rare earth doped phosphate glass passes through drawing process, and make phosphoric acid salt Active Optical Fiber, be widely used in the fields such as ultrashort pulse laser, optical communication amplifier, laser fusion, laser weapon, laser ranging.
In research to different substrates material, as everyone knows, YPO 4effective substrate material, as doping Eu 3+ion and Tb 3+ion, its lanthanide orthophosphate as stable substrate material, always by investigation and application widely.Lanthanide orthophosphate has two kinds of crystalline structure: oblique system monazite structure and tetragonal system zircon structure.Wherein YPO 4for tetragonal system zircon structure, and EuPO 4for oblique system monazite structure.
Fiber amplifier is the key part in dense wave division multipurpose (DWDM) system, which replaces the trunking of Traditional photovoltaic light, achieves the high gain of optical signal, low noise amplification.In recent years, along with the develop rapidly of computer network and other data transmission service, long-distance optical fiber transmission increases day by day to the demand improving dense wavelength division multiplexing system transmission capacity, and people get more and more to the utilization of fiber bandwidth.The initial stage nineties successfully have developed erbium-doped fiber amplifier (EDFA), has broken fiber-optic communications traffic distance by the restriction of fibre loss, has made all optical communication distance extend to several thousand kilometers, therefore realized long distance, jumbo optical communication.At present, achieve the transmission of remote optical-fibre communications both at home and abroad, but, also need after power loss, to carry out amplifying supplementary a kind of laser amplifier to do further further investigation in transmitting procedure to flashlight.
Summary of the invention
The object of the present invention is to provide a kind of P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof.The method technique is simple, and the glass-ceramic of preparation has excellent physicochemical property, can realize the power loss of supplementary fiber-optic communication signals in transmitting procedure, realize long distance, the optical communication of heavy body.
The object of the invention is to be achieved through the following technical solutions:
P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic, this ceramic Mole percent consists of:
P 2O 5：40—70；
BaO：12—25；
Na 2O： 3—18；
K 2O：3—18；
Y 2O 3：6—25；
Eu 2O 3：1—6。
P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic preparation method, method described in it comprises following process: P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3be founding of glass: by the formula P of following molar percentage 2o 5: 40-70, BaO:12-25, Na 2o:3-18, K 2o:3-18, Y 2o 3: 6-25, Eu 2o 3: 1-6, wherein P 2o 5, BaO, Na 2o and K 2o is respectively with NH 4h 2pO 4analytical pure, BaCO 3analytical pure, Na 2cO 3analytical pure and K 2cO 3analytical pure form is introduced, weigh each raw material, pour in platinum crucible after raw material is mixed and melt, temperature of fusion is 1300-1600 DEG C, be incubated 0.5-2 hours, the glass metal melted is poured on preheated stainless steel mould, then puts into retort furnace and within 1-2 hours, anneal in glass transformation temperature Tg place's insulation, close after retort furnace naturally cools to room temperature and take out; P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3the preparation of series vitro-ceramic: according to the thermal analysis experiment data obtaining glass sample, glass is put into resistance furnace and carry out micritization thermal treatment, thermal treatment temp is 600-1400 DEG C, and soaking time is 1-20 hours, powered-down takes out after cooling to room temperature with the furnace, and namely obtaining pure phase is YPO 4glass-ceramic sample.
Advantage of the present invention and effect are:
The present invention adopts P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3system, obtaining principal crystalline phase is YPO 4glass-ceramic; production cost is low; technique is simple; can accomplish scale production; there are simple, the high launching efficiency of moulding process, high heat conductance, life-span length, the high excellent physicochemical property of solubilize rare earth ions degree; the power loss of supplementary fiber-optic communication signals in transmitting procedure can be realized, thus realize long distance, the optical communication of heavy body.
Accompanying drawing explanation
Fig. 1 is P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3x-ray diffraction (XRD) figure of the glass-ceramic of system after 1300 DEG C of thermal treatment 1h.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1: raw material is weighed according to molar content shared by component each in host glass, is respectively: P 2o 5: 45, BaO:24, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 700 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining principal crystalline phase is Y (PO 3) 3be NaPO with paracrystalline phase 3, Ba (PO 3) 2, Y 2o 3glass-ceramic.
Embodiment 2: raw material is weighed according to molar content shared by component each in host glass, is respectively: P 2o 5: 45, BaO:24, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 1000 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining principal crystalline phase is Y (PO 3) 3be YPO with paracrystalline phase 4, Ba (PO 3) 2, Y 2o 3glass-ceramic.
Embodiment 3: raw material is weighed according to molar content shared by component each in host glass, is respectively: P 2o 5: 45, BaO:24, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 1300 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining principal crystalline phase is Y (PO 3) 3be YPO with paracrystalline phase 4glass-ceramic.
Embodiment 4: raw material is weighed according to molar content shared by component each in host glass, is respectively: P 2o 5: 53, BaO:16, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 1000 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining principal crystalline phase is YPO 4be Y (PO with paracrystalline phase 3) 3glass-ceramic.
Embodiment 5: raw material is weighed according to molar content shared by component each in host glass, is respectively: P 2o 5: 53, BaO:16, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 1300 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining pure phase is YPO 4glass-ceramic.

Claims (1)

1.P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic preparation method, is characterized in that, described method comprises following process: weighed according to molar content shared by component each in host glass by raw material, be respectively: P 2o 5: 53, BaO:16, Na 2o:7.5, K 2o:8.5, Y 2o 3: 14.55, Eu 2o 3: 0.45, after 30g raw material Homogeneous phase mixing good for precise, pour in platinum crucible and melt, temperature of fusion is 1510 DEG C, is incubated after 0.5 hour, is poured on by the glass metal of fusing on preheated stainless steel mould, then put into retort furnace to anneal, annealing temperature is 600 DEG C, is heat-treated by the glass obtained, and thermal treatment temp is 1300 DEG C, temperature rise rate is 10 DEG C/min, soaking time is 1 hour, and powered-down takes out after cooling to room temperature with the furnace, and obtaining pure phase is YPO 4glass-ceramic.
CN201210550109.3A 2012-12-18 2012-12-18 P 2o 5-BaO-Na 2o-K 2o-Y 2o 3-Eu 2o 3series vitro-ceramic and preparation method thereof Expired - Fee Related CN103030299B (en)

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CN103288350B (en) * 2013-05-17 2015-05-27 沈阳化工大学 P2O5-BaO-K2O-NaF-Eu<3+>:GGG systemic glass ceramic and preparation method thereof
CN103265177A (en) * 2013-05-17 2013-08-28 沈阳化工大学 P2O5-BaO-Na2O-K2O-Gd2O3-Eu2O3 glass ceramic and preparation method thereof
CN112723737B (en) * 2021-02-05 2022-01-25 太原科技大学 Low-dielectric phosphorus glass and preparation method and application thereof

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US4075120A (en) * 1975-05-14 1978-02-21 Kogre, Inc. Laser phosphate glass compositions
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US6853659B2 (en) * 2002-08-28 2005-02-08 Schott Glass Technologies, Inc. Laser system utilizing highly doped laser glass
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US4075120A (en) * 1975-05-14 1978-02-21 Kogre, Inc. Laser phosphate glass compositions
CN1583627A (en) * 2004-06-01 2005-02-23 中国科学院上海光学精密机械研究所 Manufacturing method for phosphate glass optical waveguide
CN101117271A (en) * 2007-07-25 2008-02-06 中国科学院上海光学精密机械研究所 Ytterbium-bismuth co-doped phosphonate based optical glass and method for making same

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