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Preparation method of glass film containing cerium ion doped lanthanum bromide microcrystals

A rare earth ion and glass thin film technology is applied in the field of rare earth ion-doped lanthanum iodide microcrystal glass thin film and its sol-gel method preparation, which can solve problems such as device development limitations, and achieve the goal of overcoming incomplete uniformity, The effect of promoting densification and high transmittance

Inactive Publication Date: 2016-04-06
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 of glass film containing cerium ion doped lanthanum bromide microcrystals
  • Preparation method of glass film containing cerium ion doped lanthanum bromide microcrystals
  • Preparation method of glass film containing cerium ion doped lanthanum bromide microcrystals

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Experimental program
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Effect test

Embodiment 1

[0039] The preparation method of the glass film containing rare earth ion-doped lanthanum iodide microcrystals comprises the following specific steps:

[0040] (1), the preparation raw materials are composed by mole percent: ethyl orthosilicate: 65mol%, tri-n-butyl borate: 24mol%, lanthanum iodide: 10mol%, cerium iodide: 1mol%, the total amount taken is 20 grams of analytically pure raw materials for each preparation;

[0041] (2), the hydrolysis of tri-n-butyl borate: the tri-n-butyl borate weighed in step (1) is dissolved in dehydrated alcohol, and the mol ratio of dehydrated alcohol and tri-n-butyl borate is 3: 1, fast Add glacial acetic acid, the volume ratio of tri-n-butyl borate and glacial acetic acid is 1:1, and carry out strong magnetic stirring, gradually drop distilled water, the molar ratio of distilled water and tri-n-butyl borate is 1:1, and carry out hydrolysis at room temperature React for 1 hour to make solution A;

[0042] (3), the hydrolysis of ethyl ortho...

Embodiment 2

[0051] It is basically the same as Example 1, except that the raw materials are prepared in step (1) according to the following mole percentages: ethyl orthosilicate: 70mol%, tri-n-butyl borate: 10mol%, lanthanum iodide: 15mol% , europium iodide: 5mol%, each preparation raw material of analytical purity is weighed respectively; In step (7), the pulling speed of glass substrate in gel solution is controlled at 1 millimeter / second, and pulling 5 times, every time The pulling interval is 15 minutes; in step (8), the temperature is raised to 100°C at a rate of 50°C per hour, and the temperature is kept for 1 hour to remove residual water and ethanol, and then the furnace is heated to 340°C at a rate of 50°C per hour. ℃, keep warm for 20 minutes, to remove the residual organic matter in the film; step (9), with the rate of 60 ℃ per hour, gradually heat up the furnace to 580 ℃, and react at this temperature for 2 hours, the reaction treatment ends, and Slowly cool the tubular resist...

Embodiment 3

[0054] It is basically the same as Example 1, except that in the step (1), the raw materials are prepared according to the following mole percentages: ethyl orthosilicate: 67mol%, tri-n-butyl borate: 18mol%, lanthanum iodide: 13mol% , terbium iodide: 2mol%, each preparation raw material of analytical purity is taken respectively; In step (7), the pulling speed of glass substrate in gel solution is controlled at 0.6 mm / s, repeats pulling 3 times, each The second pulling interval is 15 minutes; in the step (8), the temperature is raised to 100°C at a rate of 40°C per hour, and it is incubated for 1 hour to remove residual water and ethanol, and then the furnace is heated up to 340°C, heat preservation for 20 minutes, to remove residual organic matter in the film; in step (9), gradually raise the temperature of the furnace to 570°C at a rate of 55°C per hour, and react at this temperature for 3 hours, and the reaction process ends, and Slowly cool the tubular resistance furnace t...

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Abstract

The invention discloses a sol-gel preparation method of a glass film containing cerium ion doped lanthanum bromide microcrystals. The glass film is characterized by comprising the starting materials of 65-70mol% of TEOS, 10-24 mol% of tri-n-butyl borate, 10-15mol% of lanthanum iodide and 1-5mol% of rare earth iodide, wherein the rare earth iodide is one of cerium iodide, europium iodide and terbium iodide. The invention has the following advantages: the sol-gel method is a low temperature wet chemical glass preparation technology; glass is obtained by hydrolysis and polymeric chemical reaction process of precursor materials, so the glass can be made into a film material under certain liquid viscosity; low-temperature synthesis conditions effectively prevent decomposition and volatilization of iodide raw materials; the glass prepared by the sol-gel method, due to volatilization and decomposition of the solvent, can generate certain micropores in the material, and the micropores provide a good environment for generating the nano iodide microcrystals, so as to overcome non-uniformity of crystallization particles and glass devitrification due to the chemical composition of glass melting and incompletely uniform crystallization treatment temperature.

Description

technical field [0001] The invention relates to a glass-ceramic film doped with a rare earth ion, in particular to a glass film containing a rare earth ion doped lanthanum iodide microcrystal used as a scintillation material and a preparation method thereof by a sol-gel method. 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 r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16
CPCC03C4/12C03C10/16C03C2203/20C03C2203/52
Inventor 江东升夏海平冯治刚王成张健何仕楠盛启国汤庆阳
Owner NINGBO UNIV
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