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Yb3+ doped oxyfluoride transparent glass-ceramic material and preparation method thereof

A technology of glass-ceramics and oxyfluoride, which is applied in the field of glass-ceramics materials and their preparation, can solve the problems of high raw material purity requirements, harsh preparation conditions, difficult material performance tailoring, etc., and achieve excellent physical properties and chemical stability, The preparation method is simple and the production cost is low

Inactive Publication Date: 2011-12-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, crystalline materials have problems such as harsh preparation conditions, difficulty in obtaining large-sized products, narrow composition range, great influence by impurities, and difficulty in "tailoring" and optimizing material properties through composition and process control, and their development is limited to a certain extent; Transparent ceramic materials have problems such as high requirements for raw material purity, high requirements for preparation equipment, difficult removal of pores, and large influence of impurities. The method of microcrystallizing the basic glass to prepare transparent glass-ceramic materials is expected to overcome the problems of crystal materials and transparency. The above-mentioned main problems in the development and research of ceramic materials

Method used

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  • Yb3+ doped oxyfluoride transparent glass-ceramic material and preparation method thereof
  • Yb3+ doped oxyfluoride transparent glass-ceramic material and preparation method thereof
  • Yb3+ doped oxyfluoride transparent glass-ceramic material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1、2、3

[0016] Table 1 shows the glass chemical composition of 7 specific examples.

[0017] Embodiment 1,2,3 is taken by the chemical composition in table 1

[0018] Specific steps are as follows:

[0019] Step 1: Melting of glass, according to the chemical composition in Table 1, convert it into the weight of corresponding raw materials. Accurately weigh the weight of the corresponding raw materials for each composition, and make batches by ball milling and mixing evenly. Put the batch material into a quartz crucible or a platinum crucible, raise the temperature to 1400°C at a rate of 5-10°C / min in a silicon-molybdenum rod resistance furnace, and keep it warm for 1.5h to prepare a uniform glass solution. Quickly pour the glass melt into a stainless steel mold that has been preheated at 560°C, and quickly move it to the muffle furnace that has been heated to the preheating temperature, anneal at 530°C for 1.5h, and then close the muffle furnace The furnace is cooled to room temper...

Embodiment 4、5、6、7

[0022] Step 1: Melting of glass, according to the chemical composition in Table 1, convert it into the weight of corresponding raw materials. Accurately weigh the weight of the corresponding raw materials for each composition, and make batches by ball milling and mixing evenly. Put the batch material into a quartz crucible or a platinum crucible, raise the temperature to 1420°C in a silicon-molybdenum rod resistance furnace at a heating rate of 5-10°C / min, and keep it for 1.5h to prepare a uniform glass solution. Quickly pour the glass melt into a stainless steel mold that has been preheated at 560°C, and quickly move it to the muffle furnace that has been heated to the preheating temperature, anneal at 530°C for 1.5h, and then close the muffle furnace The furnace is cooled to room temperature to obtain a colorless, transparent, uniform, and bubble-free bulk base glass.

[0023] Step 2: According to the characteristic temperature value obtained by the DSC test of the basic gl...

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Abstract

A Yb3+-doped oxyfluoride transparent glass-ceramic material and its preparation method. The molar percentage composition range of the basic glass of the present invention is: SiO2: 42.0-52.0%, Al2O3: 18.0-27.0%, CaF2: 14.0-21.0% , NaF: 9.0-11.0%, Na2O: 4.5-5.5%, Yb2O3: 0.5-7.0%. The preparation method is as follows: ball mill the raw materials and mix them uniformly to obtain batch materials; place them in a crucible, heat them to 1390-1450°C for 1-3 hours, heat-preserve and melt them for 1-3 hours, cast them, and anneal them at 520-540°C for 1-2 hours. The base glass is heat-treated near its first crystallization peak temperature point (Tx) to obtain glass-ceramics. The crystal phase of the glass-ceramic material includes CaF2 and Ca0.8Yb0.2F2.2 crystal phase formed by part of Yb3+ ions entering the CaF2 lattice. It is a laser dielectric material with excellent spectral performance. Its comprehensive properties are as follows: the absorption cross section is 2.68pm2, the stimulated emission cross section is 5.51pm2, the fluorescence lifetime is 1.32ms, the saturation pump intensity (Isat) is 5.77, and the minimum pump intensity (Imin) is 0.60.

Description

technical field [0001] The invention relates to a glass-ceramic material and a preparation method thereof, in particular to a novel laser medium with excellent performance Yb 3+ Doped oxyfluoride transparent glass-ceramic material. Background technique [0002] New functional crystal materials and transparent ceramic materials are considered to be a new generation of materials that are of great significance to national security and the sustainable development of the national economy. The development of key high-tech, which can be widely used in the traditional transparent material industry, is an important frontier direction of research and application in the current material field. However, crystalline materials have problems such as harsh preparation conditions, difficulty in obtaining large-sized products, narrow composition range, great influence by impurities, and difficulty in "tailoring" and optimizing material properties through composition and process control, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C10/16
Inventor 卢安贤罗志伟陈媛媛朱立刚李婧韩立国
Owner CENT SOUTH UNIV
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