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Rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and preparation method thereof

A technology of oxyfluorogermanate and glass-ceramic, applied in the field of glass-ceramic and its preparation, can solve the problems of limited glass-forming ability, environmentally harmful transparent oxy-fluorogermanate glass-ceramic, poor chemical stability, and the like, Achieve the effect of improving luminous intensity and excellent physical and chemical properties

Inactive Publication Date: 2010-06-09
苏州恒仓红外光学材料研发中心有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: The purpose of the present invention is to provide a transparent oxyfluorogermanic acid doped with rare earth ions in order to overcome the environmental hazards, limited glass-forming ability and poor chemical stability of the current transparent oxyfluorogermanate glass-ceramics Salt glass-ceramic and its preparation method

Method used

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  • Rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and preparation method thereof
  • Rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and preparation method thereof
  • Rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: Weigh 50g of raw materials, and weigh the raw materials according to the molar percentages of each component in the matrix glass, and the molar percentages of each component in the matrix glass are: 48%GeO 2 , 17% Al 2 o 3 , 3% Ga 2 o 3 , 32%CaF 2 , the raw materials are the corresponding oxides, carbonates and fluorides of analytical purity and above. Mix the weighed 50g of raw materials evenly, place them in a platinum crucible, cover the surface, heat and melt in a silicon carbide rod circuit at 1300-1350°C, keep the temperature for 1.5h, and pour the molten material on a preheated stainless steel template , then enter the muffle furnace for annealing, the annealing temperature is 550°C, keep warm for 2 hours and then cool down with the furnace to obtain colorless transparent glass.

[0016] Differential thermal analysis (DTA) test is carried out on the matrix glass, and the transition temperature T of the glass is g is 578°C, the first crystalliz...

Embodiment 2

[0017] Embodiment 2: Weigh 50g of raw material, and weigh the raw material according to the molar percentage of each component in the matrix glass, and the molar percentage of each component in the matrix glass is respectively: 48%GeO 2 , 17% Al 2 o 3 , 3% Ga 2 o 3 , 2% LiF, 28% CaF 2 , 2% ErF 3 , wherein the raw materials are the corresponding oxides, carbonates and fluorides of analytical purity and above. Mix 50g of the weighed raw materials evenly, place them in a platinum crucible, cover the surface, heat and melt in a silicon carbide rod circuit at 1350-1380°C, keep it warm for 1.5 hours, and pour it on a preheated stainless steel template, then Enter the muffle furnace for annealing. The annealing temperature is 530°C, and after 2 hours of heat preservation, it is cooled with the furnace to obtain pink transparent glass.

[0018] Differential thermal analysis (DTA) shows the transition temperature T of the matrix glass g is 572°C, the first crystallization peak ...

Embodiment 3

[0019] Example 3: The preparation method of the matrix glass in this example is basically the same as in Example 1, the difference is the components of the matrix glass, and the molar percentage of each component in the matrix glass in this example is: 38 %GeO 2 , 10% Al 2 o 3 , 5% Ga 2 o 3 , 1% LiF, 2% NaF, 40% CaF 2 , 4% PrF 3 , and then melted according to the method in Example 1, a light brown transparent matrix glass sample can be obtained.

[0020] According to the results of the differential thermal test, the heat treatment temperature for microcrystallization is selected to be 610-630° C., and the holding time is 64 hours to obtain a transparent glass-ceramic sample. Under the excitation of 1016nm Ti:Sapphire laser, the fluorescence of 1300nm was observed in the glass-ceramic sample, but no signal was observed in the matrix glass.

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Abstract

The invention discloses a rare earth iron-doped transparent oxygen fluorine germanate microcrystalline glass and a preparation method thereof. The transparent microcrystalline glass comprises the following components by mole percentage: 38-60 percent of GeO2, 4-26 percent of Al2O3, 0-8 percent of Ga2O3, 15-40 percent of CaF2, 0-12 percent of MF, 0-6 percent of ErF3, 0-8 percent of YbF3 and 0-4 percent of PrF3, wherein M is one or more of Li+, Na+ and K+. The preparation method comprises the steps of pouring by melting method to obtain matrix glass and carrying out special thermal treatment on the matrix glass to obtain the microcrystalline glass containing CaF2 crystalline phase in nanometer level. The transparent oxygen fluorine germinate microcrystalline glass is environment-friendly, has stable physicochemical property and does not contain toxic Pb element, and has high transparency from visible area to near-infrared and intermediate infrared areas and excellent active optics property. The invention can be used in the field of optical communication, display, storage, and the like.

Description

technical field [0001] The invention relates to a glass-ceramic and a preparation method thereof, in particular to a rare-earth ion-doped transparent oxyfluorgermanate glass-ceramic and a preparation method thereof. Background technique [0002] Rare earth ion-doped transparent oxyfluoride glass-ceramics is a new type of active optical material developed in recent years. It has broad application prospects in optical fiber communication, lasers and three-dimensional display, so it has aroused great interest of scientific researchers. . In this type of glass-ceramic, the fluoride crystal grain size precipitated by heat treatment is nanoscale and uniformly distributed inside the mother glass, which ensures the visible transparency of the glass; rare earth ions are selectively enriched in lower In the fluoride crystal phase of phonon energy, the probability of non-radiative transition is reduced, and the quantum efficiency and emission efficiency are greatly increased. This co...

Claims

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Application Information

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IPC IPC(8): C03C10/16
Inventor 唐彬薛天峰李家成
Owner 苏州恒仓红外光学材料研发中心有限责任公司
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