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Lead difluoride base material with Eu<2+> characteristic luminescence and preparation method thereof

A base material and matrix technology, applied in the field of inorganic fluorescent materials and scintillation materials, can solve the problems of not meeting the technical indicators of dual readout materials, slow decay time, etc., and achieve the effect of wide application range and simple process

Inactive Publication Date: 2015-02-11
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology

Mao et al. (IEEE Transactions on Nuclear Science, 57(6)(2010), 3841-3845) have done up to 116 rare earth ions doped PbF 2 The samples were studied and found that although these samples can emit visible light, their decay time is too slow, all on the order of milliseconds, such as PbF doped with trivalent Eu 2 The decay time of the sample is 8.5ms, which cannot meet the technical indicators of dual readout materials

Method used

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  • Lead difluoride base material with Eu&lt;2+&gt; characteristic luminescence and preparation method thereof
  • Lead difluoride base material with Eu&lt;2+&gt; characteristic luminescence and preparation method thereof
  • Lead difluoride base material with Eu&lt;2+&gt; characteristic luminescence and preparation method thereof

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preparation example Construction

[0034] The present invention has Eu 2+ Characteristically luminescent PbF 2 The preparation method of base powder material comprises:

[0035] (1) with CaF 2 as the matrix, EuF 2 or EuF 3 As a dopant, it is mixed and ground according to the stoichiometric ratio and then heat-treated at 800-900°C under the protection of an inert gas to obtain a co-dopant (Ca 1-y Eu y ) F 2 ;as well as

[0036] (2) with PbF 2 as matrix, with (Ca 1-y Eu y ) F 2 As a co-dopant, after mixing and grinding according to the stoichiometric ratio, the Eu 2+ Characteristically luminescent PbF 2 base material.

[0037] Specifically, as an example, the present invention may include the following steps.

[0038] First with EuF 2 or EuF 3 as a dopant, with CaF 2 The matrix is ​​mixed and ground according to the required stoichiometric ratio, and kept in a heating device such as a box furnace under an inert atmosphere at 800-900°C for 1-2 hours to prepare (Ca 1-y Eu y )F 2 Intermediate pow...

Embodiment 1

[0044] in CaF 2 、EuF 2 As raw materials, Ca 0.995 Eu 0.005 f 2 (700), Ca 0.995 Eu 0.005 f 2 (800), Ca 0.995 Eu 0.005 f 2 (900), Ca 0.995 Eu 0.005 f 2 (1000) series samples.

[0045] in CaF 2 、EuF 2 As raw material, fixed CaF 2 with EuF 2 The molar ratio is 0.995:0.005, the raw materials are mixed and ground, and they are heat treated in a box furnace at 700, 800, 900, 1000°C for 1 to 2 hours under the protection of Ar gas atmosphere, and then cooled with the furnace to prepare Ca 0.995 Eu 0.005 f 2 (700), Ca 0.995 Eu 0.005 f 2 (800), Ca 0.995 Eu 0.005 f 2 (900), Ca 0.995 Eu 0.005 f 2 (1000) series samples.

[0046] As shown in Fig. 1(a), the sample Ca 0.995 Eu 0.005 f 2 (700) is mainly derived from Eu at 613nm under the excitation of 393nm wavelength light 3+ of 5 D. 0 → 7 f 2 The luminescence of the transition, under the excitation of light with a wavelength of 336nm, has a relatively weak source at 422nm from Eu 2+ 4f 6 5d 1 →4f 7 Tran...

Embodiment 2

[0049] in CaF 2 、EuF 3 As raw materials, Ca 0.995 Eu 0.005 f 2 (800-EuF 3 ), Ca 0.995 Eu 0.005 f 2 (900-EuF 3 ) samples, the main study is to use EuF 3 Can Eu be obtained as a raw material 2+ glowing.

[0050] in CaF 2 、EuF 3 As raw material, fixed CaF 2 with EuF 3 The molar ratio of the compound is 0.995:0.005, the raw materials are mixed and ground, and the heat treatment is carried out in a box furnace at 800 and 900 ° C for 1 to 2 hours under the protection of Ar gas atmosphere, and then cooled with the furnace to prepare Ca 0.995 Eu 0.005 f 2 (800-EuF 3 ), Ca 0.995 Eu 0.005 f 2 (900-EuF 3 )sample.

[0051] Such as Figure 2(a) , 2(b) As shown, due to the principle of charge compensation, the sample Ca 0.995 Eu 0.005 f 2 (800-EuF 3 ) and Ca 0.995 Eu 0.005 f 2 (900-EuF 3 ) are mainly derived from Eu at 422nm under the excitation of 336nm wavelength 2+ 4f 6 5d 1 →4f 7 The luminescent band of the transition also has the source of Eu at 592 ...

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Abstract

The invention relates to a lead difluoride base material with Eu<2+> characteristic luminescence and a preparation method thereof. The chemical structure general formula of the base material is Pb1-x (Ca1-yEuy)xF2, wherein y is not less than 0.005 and not greater than 0.05 and x is not less than 0.05. The base material is prepared through codoping thermal treatment by taking PbF2 as a matrix and Ca1-yEuy as a codoping agent, wherein the codoping agent is prepared through thermal treatment with the temperature of 800-900 DEG C by taking CaF2 as a matrix and EuF2 or EuF3 as a doping agent. In the base material disclosed by the invention, Eu mainly exists in a form of Eu<2+> so that Eu<2+> characteristic luminescence (5d-4f transition) with a band spectrum and high attenuation speed is combined with an excellent Cherenkov luminophor (PbF2) with high density and relatively low price. Therefore, the lead difluoride base material with Eu<2+> characteristic luminescence can be applied to research of a PbF2-based double readable material (crystal / glass / ceramic) and has an important practical value in the research and application field of high energy physics.

Description

technical field [0001] The invention relates to a luminescent material, in particular to a divalent europium ion (Eu 2+ ) characteristically luminescent PbF 2 The base powder material and its preparation method belong to the technical field of inorganic fluorescent materials and scintillation materials. Background technique [0002] High-density scintillation materials are the core materials in high-energy particle physics experiment detectors. Most scintillation materials have good energy resolution for incident electrons or photons, and for other high-energy particles with large e / h ratios (such as hadrons) Therefore, it is a scientific and technological challenge to develop scintillation materials that can simultaneously detect electrons, photons and higher energy particles. [0003] With the continuous exploration of the origin of matter, there is an urgent need for a dual readout material (DREAM) that can simultaneously read out scintillation light (visible light band...

Claims

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Application Information

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IPC IPC(8): C09K11/85
Inventor 周真真刘茜刘光辉魏钦华
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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