Preparation method for glass and glass film both containing rare-earth-ion-doped lutetium chloride microcrystalline

A glass film, rare earth ion technology, applied in glass manufacturing equipment, glass molding, manufacturing tools, etc., can solve problems such as device development limitations, achieve the effect of overcoming incomplete uniformity, preventing decomposition and volatilization, and promoting densification

Inactive Publication Date: 2016-02-03
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually thin film and fibrous materials are the most suitable raw materials for making such devices, so the current form of scintillation materials will have great restrictions on the development of future devices

Method used

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  • Preparation method for glass and glass film both containing rare-earth-ion-doped lutetium chloride microcrystalline
  • Preparation method for glass and glass film both containing rare-earth-ion-doped lutetium chloride microcrystalline
  • Preparation method for glass and glass film both containing rare-earth-ion-doped lutetium chloride microcrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The preparation method of glass and glass thin film containing rare earth ion-doped lutetium chloride crystallite comprises the following steps:

[0041] (1), the preparation raw materials are composed by mole percent: ethyl orthosilicate: 65mol%, aluminum sec-butoxide: 24mol%, lutetium chloride: 10mol%, cerium chloride: 1mol%, and the total amount is weighed to be 20 Each preparation raw material of the analytical purity of gram, stand-by;

[0042] (2), according to the following molar ratio: the sum of tetraethyl orthosilicate and aluminum sec-butoxide: dehydrated alcohol: distilled water=1: 2.5: 2, weigh corresponding dehydrated alcohol and distilled water respectively, and set aside;

[0043] (3), hydrolysis of aluminum sec-butoxide: take 1 / 3rd of the dehydrated alcohol weighed in the step (2), dissolve all the aluminum sec-butoxide weighed in the step (1), add ice rapidly Acetic acid, the volume ratio of aluminum sec-butoxide and glacial acetic acid is 1: 1, and c...

Embodiment 2

[0054] Basically the same as Example 1, the difference is that in step (1), the raw materials are prepared in the following molar percentages: tetraethyl orthosilicate: 70mol%, aluminum sec-butoxide: 10mol%, lutetium chloride: 15mol%, chlorine Europium chloride: 5mol%, each preparation raw material that takes by weighing total amount is 20 grams, stand-by; In step (8), solution E is coated on the clean quartz glass substrate by dip-coating, The pulling speed of the quartz glass substrate in the gel solution is controlled at 1 mm / s, and it is pulled 5 times, and the interval between each pulling is 15 minutes to obtain a glass film; in step (10), put it in the furnace The glass film or glass is kept at 100°C for 2 hours to remove residual water and ethanol, and then heated to 360°C and held for 40 minutes to remove residual organic matter. The heating rate for glass is 15°C per hour. The cooling rate is 20°C per hour, the heating rate of the glass film is 50°C per hour, and the...

Embodiment 3

[0057] Basically the same as Example 1, the difference is that in step (1), the raw materials are prepared in the following molar percentages: tetraethyl orthosilicate: 67mol%, aluminum sec-butoxide: 18mol%, lutetium chloride: 13mol%, chlorine Terbium: 2mol%, take by weighing a total amount of 20 grams of analytically pure ethyl orthosilicate, aluminum sec-butoxide, lutetium chloride and terbium chloride raw materials, stand-by; in step (8), the pulling speed Controlled at 0.6 mm / s, according to the specific thickness requirements, the pulling can be repeated 3 times, and the interval between each pulling is 15 minutes, and the coated film is dried at room temperature for 4 hours to obtain a glass film; in step (10) In the process, put the glass film or glass in the furnace at 100°C for 1.5 hours to remove residual water and ethanol, then raise the temperature to 360°C and hold for 30 minutes to remove residual organic matter, the heating rate for glass 12°C per hour, the cool...

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Abstract

The invention discloses a sol-gel preparation method for glass and a glass film both containing rare-earth-ion-doped lutetium chloride microcrystalline. The technical scheme is characterized in that the preparation raw materials comprise, in percent by mole, 65-70 mol% of ethyl orthosilicate, 10-24 mol% of aluminium tri-sec-butoxide, 10-15 mol% of lutetium chloride, and 1-5 mol% of a rare-earth chloride, wherein the rare-earth chloride is one of cerium chloride, europium chloride and terbium chloride. The advantages comprise that the sol-gel technology is a low-temperature wet-chemical-process glass preparation technology, the glass and the glass film are obtained through hydrolysis of a precursor raw material and a polymerization chemical reaction process, the film material can be prepared under a certain liquid viscosity condition, and the low-temperature synthesis condition is capable of effectively preventing the chloride raw material from being decomposed and volatilized; and because of volatilization and decomposition of the solvent, certain micropores are generated in the glass and film prepared through the sol-gel method, and the micropores provide good environment for generation of nanometer chloride microcrystalline, and thus crystallized-particle nonuniformity and glass devitrification caused by incomplete uniformity of melt-glass chemical compositions and crystallization processing temperature are overcome to a certain degree.

Description

technical field [0001] The invention relates to a preparation technology of glass and glass film containing crystallite, in particular to a preparation method of glass containing rare earth ion doped lutetium chloride microcrystal and glass film used as a scintillation material. Background technique [0002] Scintillation material is a photofunctional material that can emit visible light under the excitation of high-energy rays (such as x-rays, γ-rays) or other radioactive particles, and can be widely used in nuclear medicine diagnosis, security inspection, anti-terrorism, high-energy physics and geological exploration and other fields. In recent years, with the rapid development of fields such as medical imaging and security inspection, there is a large demand for new scintillation materials with high performance. Excellent scintillation materials mainly have the following properties: high luminous efficiency, high material density, fast fluorescence decay, good radiation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16C03C4/12C03B19/12C03C17/02
Inventor 王成夏海平冯治刚江东升张健何仕楠盛启国汤庆阳
Owner NINGBO UNIV
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