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Preparation method and use of phosphate radical cadmium germanate blue fluorescence crystal material

A crystal material and crystallization technology, which is applied in the field of new transition metal germanium phosphate crystal material and its synthesis, can solve the problems of few reports on fluorescence properties, no reports on preparation methods and related work, and difficulty in preparing pure phases of compounds, etc. Achieve the effect of simple method, mild condition and good thermal stability

Active Publication Date: 2017-05-31
JIANGNAN UNIV
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  • Application Information

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Problems solved by technology

However, the preparation of related materials reported in the literature is mostly high-temperature solid-phase synthesis, and the pure phase of the compound is difficult to prepare, and the research on the fluorescence properties is rarely reported.
[0003] This application prepares a transition metal germanium phosphate crystal material with a new structure, introduces transition metal Cd into the germanium phosphate system, and obtains a new anhydrous cadmium germanium phosphate compound Cd 7 Ge(PO 4 ) 6 , the preparation method is mild and convenient, and the preparation method and related work have not been reported

Method used

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  • Preparation method and use of phosphate radical cadmium germanate blue fluorescence crystal material
  • Preparation method and use of phosphate radical cadmium germanate blue fluorescence crystal material
  • Preparation method and use of phosphate radical cadmium germanate blue fluorescence crystal material

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Embodiment 1

[0029] Example 1 sample preparation

[0030] Using triethylamine, 1,2-propylene glycol, and water as solvents, mix the cadmium source, germanium source, and phosphorus source in a certain proportion to obtain the initial gel mixture, and seal the initial gel mixture in a 15mL polytetrafluoroethylene liner put into a box-type resistance furnace, crystallize at the crystallization temperature for a period of time, filter, wash, and dry to obtain a colorless block of Cd 7 Ge(PO 4 ) 6 crystal sample. Table 1 shows the relationship between the types and ratios of raw materials in the initial gel mixture, crystallization temperature, crystallization time, and sample numbers.

[0031] Table 1 Relationship between sample synthesis conditions and sample numbers

[0032]

[0033]

Embodiment 2

[0034] The crystal structure analysis of embodiment 2 sample

[0035] The structures of samples 1# to 10# were analyzed by single crystal X-ray diffraction and powder X-ray diffraction.

[0036] The single crystal X-ray diffraction was carried out on a D8VENTURE X-ray single crystal diffractometer of Bruker AXS Company in Germany. The crystal size is 0.15×0.09×0.04mm 3 ; The data collection temperature is 293K, and the diffraction light source is Mo-Kα ray monochromated by graphite The scanning method is ω-2θ; the data is processed by the Multi-Scan method for absorption correction. Structural analysis was completed using the SHELXTL-97 program package; the position of the heavy atom was determined by the direct method, and the coordinates of the remaining atoms were obtained by the difference Fourier synthesis method; 2 The full-matrix least-squares method was used to refine all atomic coordinates and anisotropic thermal parameters.

[0037] Powder X-ray diffraction wa...

Embodiment 3

[0045] Embodiment 3 thermogravimetric analysis experiment and result

[0046] The thermogravimetric analysis experiment of sample 1# is specifically as follows: Weigh 5-10mg sample 1#, adopt 1100SF type thermogravimetric analyzer, in 50cm 3 .min -1 N 2 Under the protection of airflow, measure its thermal stability, the temperature range is 50-800°C (10°C / min), so as to obtain the thermogravimetric pattern of the sample. The result is as image 3 shown.

[0047] The test results showed that the compound Cd 7 Ge(PO 4 ) 6 The crystals have very good thermal stability and can be heated up to 800 °C without significant mass loss.

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Abstract

The invention discloses a novel crystal material, a preparation method and an application thereof. The chemical formula of the crystal material is Cd7Ge (PO4) 6, the crystal material belongs to a trigonal system, the space group is R-3, the cell parameter is as shown in the specification, wherein alpha=beta=90 degrees, gamma=120 degrees, and Z=3. The crystal material exhibits better blue fluorescence emission performance, and the strongest emission peak is at 440nm (the optimal excitation wavelength is 363nm). In addition, the crystal material is prepared from a relatively mild solvothermal preparation method, thereby having very good thermal stability. The crystal material has extensive potential application prospects in industrial and residential lighting, light emitting diodes, field emission displays and other fields.

Description

technical field [0001] The application relates to a novel transition metal germanium phosphate crystal material and a synthesis method thereof. Background technique [0002] Fluorescent materials have become a research hotspot due to their wide application in industrial and residential lighting, light-emitting diodes, field emission displays and other fields. Germanium phosphate is doped with transition metals (Zn, Cd, etc.) or rare earth ions (Eu 3+ , Tb 3+ etc.), with the characteristics of milder preparation conditions, higher chemical stability, high-brightness doped luminescence, unique structure diversity, and lower thermal quenching phenomenon, it becomes the first choice for exploring new luminescent material substrates. , has been used as a base material in recent years and has also been studied in optics. However, the preparation of related materials reported in the literature is mostly high-temperature solid-phase synthesis, and it is difficult to prepare the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/32C30B7/14C30B7/10
CPCC30B7/10C30B7/14C30B29/32
Inventor 宋俊玲崔建秋
Owner JIANGNAN UNIV
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