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Preparation method of anhydrous lanthanum bromide

An aqueous lanthanum bromide and ammonium bromide technology, applied in the field of preparation of anhydrous lanthanum bromide, can solve the problems of restricting the development of lanthanum bromide scintillation crystals, demanding content control, difficult process control and the like, and achieving an easy preparation process. Control, low production cost, low cost effect

Active Publication Date: 2015-03-18
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the strong hydrolysis of anhydrous lanthanum bromide at high temperature, its preparation process has extremely strict requirements on the control of oxygen and water vapor content in the surrounding environment, resulting in the current production process of high-purity anhydrous lanthanum bromide is complicated, the process control is difficult, and the product cost is very high. High, restricting the development of lanthanum bromide scintillation crystals

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  • Preparation method of anhydrous lanthanum bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 6.52g of lanthanum oxide and 23.5g of ammonium bromide were mixed uniformly and then added to the corundum crucible. The mixture was first held at 400°C for 2.0 hours and then at 550°C for 1.0 hour. In this way, anhydrous lanthanum bromide is obtained. In this embodiment, the mass ratio of ammonium bromide and lanthanum oxide is 3.60:1, the mixture of lanthanum oxide and ammonium bromide is the covering, and the covering thickness is 7 mm.

[0063] According to the above measurement method, the obtained anhydrous lanthanum bromide was characterized, and the results are as follows:

[0064] Perform XRD phase analysis on the sample composition, the composition is anhydrous LaBr 3 , See attached figure 1 .

[0065] The precipitate after the sample was dissolved in water was titrated, and the purity of the anhydrous lanthanum bromide was determined to be 99.58%.

[0066] The moisture content in the sample is determined, and the moisture content in the sample is 0.08%.

Embodiment 2

[0068] 3.26g lanthanum oxide and 11.75g ​​ammonium bromide were mixed uniformly and then added to the corundum crucible. Then, 10 mm thick aluminum oxide was coated on the mixture of lanthanum oxide and ammonium bromide. The mixture was first held at 350°C for 2.0 hours and then at 550°C for 1.0 hour. In this way, the upper layer of alumina with obvious stratification and the lower layer of anhydrous lanthanum bromide are obtained. In this embodiment, the mass ratio of ammonium bromide and lanthanum oxide is 3.60:1, aluminum oxide is the covering, and the covering thickness is 10 mm.

[0069] According to the above measurement method, the obtained anhydrous lanthanum bromide was characterized, and the results are as follows:

[0070] Perform XRD phase analysis on the sample composition, the composition is anhydrous LaBr 3 .

[0071] The precipitate after the sample was dissolved in water was titrated, and the purity of anhydrous lanthanum bromide was determined to be 99.60%.

[007...

Embodiment 3

[0074] 13.04g lanthanum oxide and 47.00g ammonium bromide were mixed uniformly and then added to the corundum crucible. Then, 13mm thick aluminum oxide was coated on the mixture of lanthanum oxide and ammonium bromide. The mixture was first held at 400°C for 2.5 hours and then at 600°C for 1.0 hour. In this way, the upper layer of alumina with obvious stratification and the lower layer of anhydrous lanthanum bromide are obtained. In this embodiment, the mass ratio of ammonium bromide and lanthanum oxide is 3.60:1, alumina is the covering, and the covering thickness is 13 mm.

[0075] According to the above measurement method, the obtained anhydrous lanthanum bromide was characterized, and the results are as follows:

[0076] Perform XRD phase analysis on the sample composition, the composition is anhydrous LaBr 3 .

[0077] The precipitate after the sample was dissolved in water was titrated, and the purity of anhydrous lanthanum bromide was determined to be 99.69%.

[0078] The mo...

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Abstract

The invention discloses a preparation method of anhydrous lanthanum bromide, which comprises the following steps: (1) well mixing ammonium bromide with lanthana; (2) heating the mixture obtained in step (1) in closed environment with a certain leakproofness to obtain anhydrous lanthanum bromide. The method of the invention is easily available in raw materials, and low in cost; the preparation process is simple, short in flow, easy to control, high in product yield, and low in production cost; the prepared anhydrous lanthanum bromide is high in purity, and has a purity of up to 99.5%; and the preparation method can be used for preparation of lanthanum bromide scintillation crystals, and has very good industrial and commercial prospects.

Description

Technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to a preparation method of anhydrous lanthanum bromide. Background technique [0002] Take Ce 3+ Ion activated lanthanum bromide crystals (LaBr 3 :Ce 3+ ) Is a new type of inorganic scintillation crystal developed in recent years. Compared with similar crystals, this crystal has the advantages of higher light yield, better energy resolution, faster decay time, and less nonlinear response. Compared with traditional NaI(TI) crystals, it has the advantages of Ce 3+ Ion-activated lanthanum bromide crystals have many excellent properties and have viable prospects for industrialization and commercialization. They are expected to fully replace traditional NaI (TI) crystals, and thus can be used in medical instruments, high-energy physics experimental research, oil well exploration and safety inspections. It is widely used. [0003] The preparation of anhydrous lanthanu...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01F17/10C01F17/253
Inventor 卢旭晨张志敏
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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