Infrared transparent fluozirconate microcrystalline glass and preparation method thereof

A fluorozirconate, glass-ceramic technology, used in glass manufacturing equipment, glass furnace equipment, manufacturing tools, etc., can solve the problem of not making great progress, low chemical stability and mechanical properties of fluoride glass, hindering optical applications and other problems, to achieve the effect of good transmittance, good mechanical properties and good anti-devitrification properties

Inactive Publication Date: 2007-03-14
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the low chemical stability and mechanical properties of fluoride glasses hinder their optical applications
As we all know, the mechanical strength and thermal performance of the glass can be improved by heat treatment and microcrystallization of fluoride glass to make it evenly crystallized. A lot of research has been done on the crystallization of fluoride glass at home and abroad, and some progress has been made, but in How to control the crystallization process of fluoride glass, so as to obtain fluoride glass-ceramics with good infrared transmission performance and uniform crystal phase in the glass, especially fluorozirconate glass-ceramics has not made great progress.
In China, there is no report on fluorozirconate glass-ceramic

Method used

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  • Infrared transparent fluozirconate microcrystalline glass and preparation method thereof
  • Infrared transparent fluozirconate microcrystalline glass and preparation method thereof

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Experimental program
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Effect test

Embodiment 1 and 2

[0026] Embodiments 1 and 2 are only different in glass formula composition, but the glass melting process is the same. The specific process from glass melting to heat treatment microcrystallization is as follows:

[0027] (1) Melting of fluorozirconate glass: Weigh the raw materials according to the glass formula in Table 1, mix the powdered raw materials evenly, put them in a platinum crucible and melt them in a silicon carbide rod electric furnace at 1000-1050 °C, completely After being melted and clarified for 15-20 minutes, the molten glass is poured on a preheated graphite mold, and then the glass is quickly moved into a muffle furnace heated to 310°C for annealing. The annealing process is: keep warm at 310°C for 3 to 4 hours, then drop to 200°C at a rate of 3°C / hour, and finally drop to room temperature at a rate of 5°C / hour, and take out the glass sample after complete cooling.

[0028] (2) Preparation method of fluorozirconate glass-ceramics: According to glass therm...

Embodiment

[0029] Examples: 3, 4 and 5:

[0030] Concrete preparation process is as follows:

[0031] The first step: carry out batching according to the glass component of embodiment 3,4 and 5 described in table 1; The process is essentially the same, with a slight increase in the temperature at which the glass is melted and the temperature at which the glass is annealed.

[0032] Second step: the preparation process of embodiment 3, 4 and 5 fluoride glass-ceramics is basically the same as that of embodiment 1 and 2, that is, according to the glass thermal analysis (DTA) data, the glass sample made is changed from room temperature to 10 °C / min rate of heating above T g After nucleation at a temperature above 20°C for 4 to 5 hours, heat to the first crystallization peak temperature at a rate of 0.5°C / min (T x ) in the vicinity of crystallization for 30 to 50 minutes, and finally cooled to room temperature at a rate of 1° C. / min and then taken out to obtain transparent fluorozirconate ...

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Abstract

The present invention is infrared transmitting fluorozirconate microcrystal glass and its preparation process, and features that LaF3 is added into ZrF4-BaF2-YF3-AlF3 fluoride glass components to form the fluorozirconate microcrystal glass in the molar composition of: ZrF4 50-55 mol%, BaF2 15-33 mol%, YF3 10-22 mol%, AlF3 3-7 mol%, and LaF3 2-8 mol%. The preparation process includes the first smelting process to prepare fluorozirconate glass and the subsequent precise heat treatment to microcrystallize the base glass into infrared transmitting fluorozirconate microcrystal glass. The preparation process is simple, and the prepared fluorozirconate microcrystal glass has excellent resistance to transparency loss and higher mechanical performance than fluoride glass. The fluorozirconate microcrystal glass is suitable for use as the optical window material in medium infrared band.

Description

technical field [0001] The present invention relates to fluorozirconate glass-ceramics, especially a kind of infrared-transmitting fluoro-zirconate glass-ceramics and its preparation method. Compared with fluoride glass, its mechanical strength is greatly enhanced. Background technique [0002] In the past few decades, a great deal of research has been done on how to form uniform submicroscale crystal phases in silica-based glasses. Compared with traditional glass, glass-ceramic has excellent thermal and mechanical properties, such as low thermal expansion coefficient and high elastic modulus, especially when the crystallite phase size in glass-ceramic is smaller than a certain wave band, it has a high Through the characteristics, the thermal and mechanical properties of the glass are greatly improved. [0003] Fluoride glass has a small refractive index, low phonon energy, and good infrared transmission performance in the range of 0.2-7 μm, making fluoride glass a popular...

Claims

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Application Information

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IPC IPC(8): C03C10/02C03C3/32C03B5/235C03B32/02
CPCC03C4/10C03C3/325
Inventor 赖杨琼张军杰于春雷吴家禄
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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