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A kind of preparation method of polycrystalline photoluminescence zinc tungstate film

A technology of luminescence and zinc tungstate, applied in the direction of vacuum evaporation plating, metal material coating process, coating, etc., can solve the problems of difficult to realize large-area film preparation, complex process parameters, complex preparation process, etc., and achieve excellent Photoluminescence performance, process parameters are easy to control, and the effect of simple process

Active Publication Date: 2019-06-28
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In 1998, M. Bonanni et al. in Germany (M. Bonanni, et al, Chem. Mater. 1998, 10, 304-310) ZnWO was prepared from the heterogeneous colloidal complex of zinc acetate and tungsten hexaformate 4 Thin film, this kind of film can emit strong blue light, but its preparation process is complicated, involving the pre-dehydration treatment of metal-organic compounds at different temperatures and the subsequent sol-gel process, and the prepared film is not ideally bonded to the substrate
In 2003, Japanese Hideki Hayashi et al. (Hideki Hayashi, et al, Appl. Phys. Lett. 2003, 82: 1365) prepared ZnO-WO by pulse deposition method 3 Binary composite thin films have obtained luminescent thin films based on zinc tungstate, but it is difficult to achieve large-area thin films by this preparation method
In 2012 Ukraine A. M. Dubovik et al (A. M. Dubovik, et al, J. Phys. & Astronmy, 2012, 1(1): 56) Using ion beam sputtering ZnWO 4 Single crystal prepared ZnWO 4 thin film, which emits blue-green light under X-ray irradiation, but its sputtering target ZnWO 4 The cost of single crystal is too expensive, and it is easy to form non-stoichiometric ZnWO in the sputtering process 4
In recent years, people have used sodium tungstate, ammonium tungstate, zinc nitrate, zinc acetate, etc. as raw materials to prepare polycrystalline ZnWO on glass substrates by sol-gel method and hydrothermal method. 4 Luminescent film, found that the film can emit light of 470-490nm under the excitation of 270-300nm light, but this method is easy to introduce impurities during the preparation process, the process parameters are complicated, and the low annealing temperature (<500°C) is also It will lead to low crystallinity of the film, affect the luminous performance, and the bonding force between the coating layer and the substrate is weak

Method used

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  • A kind of preparation method of polycrystalline photoluminescence zinc tungstate film
  • A kind of preparation method of polycrystalline photoluminescence zinc tungstate film
  • A kind of preparation method of polycrystalline photoluminescence zinc tungstate film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for preparing a polycrystalline photoluminescent zinc tungstate film, comprising the steps of:

[0041] (a) Preparation of tungsten oxide thin film layer:

[0042] (a1) Ultrasonic clean the quartz substrate with acetone, alcohol and deionized water successively, and use N 2 Blow dry, then dry the cleaned quartz substrate for 30min;

[0043] (a2) placing a metal tungsten target in a magnetron sputtering chamber, the purity of the metal tungsten target being 99.99%;

[0044] (a3) Put the clean quartz substrate in step (a1) into the magnetron sputtering chamber with a metal tungsten target, and evacuate to -4 Pa;

[0045] (a4) Introduce argon and oxygen into the above-mentioned magnetron sputtering chamber, adjust the volume flow ratio of argon and oxygen to 20:15, and the pressure of the magnetron sputtering chamber to 4Pa;

[0046] (a5) Turn on the magnetron sputtering power supply, adjust the sputtering power to 80W, start pre-sputtering for 3~10 minutes, an...

Embodiment 2

[0057] The experimental method is the same as in Example 1, other conditions remain unchanged, and the sputtering deposition time in step (a6) is set as a variable, which is 10min and 15min respectively, and the results are as follows figure 1 shown.

[0058] From figure 1 It can be seen that the annealing conditions for the fixed deposition ZnO layer are: the annealing temperature is 750°C, the holding time is 30min, and the heating rate is 3°C / min. 3 When the deposition time is 15min, under the same test conditions, the peak value of the emission spectrum of the obtained sample increases significantly when excited by light at about 285nm, which is WO 3 Deposit 2.5 times the sample for 10 min.

Embodiment 3

[0060] The experimental method is the same as that in Example 1, and other conditions remain unchanged. In step (b3), the volume flow ratio of argon and oxygen is adjusted to be variable, which are 20:0, 20:3, 20:6 and 20:10 respectively. The results are as follows figure 2 shown.

[0061] From figure 2 It can be seen that the fixed deposited WO 3 The annealing conditions are as follows: the annealing temperature is 750°C, the holding time is 30min, the heating rate is 3°C / min, when the volume flow ratio of argon and oxygen is 20:6, under the same test conditions, use The intensity of the emission spectrum of the obtained sample is the strongest when the light excitation is around 285nm, but when the volume flow ratio of argon and oxygen is 20:10, the luminous intensity of the obtained sample is significantly reduced, even lower than that of the sample obtained by oxygen-free sputtering The luminous intensity indicates that the oxygen content should not be too high during ...

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Abstract

The invention discloses a preparation method for a polycrystalline photo-induced luminous zinc tungstate film. The preparation method adopts a magnetron sputtering method for preparing, and comprisesthe following steps of: (a) preparing a tungsten oxide film layer; (b) preparing a zinc oxide film layer on the basis of the step (a); (c) preparing a tungsten oxide film on the basis of step (b), andrepeating operations in step (a); and (d) annealing a WO3 / ZnO / WO3 multi-layer film prepared in the step (d) in air, and naturally cooling to obtain a final sample. The preparation method adopts metaltungsten and zinc oxide ceramic as a target material, is low in cost, is environmentally friendly, and can be used for large-scale production; and the prepared polycrystalline photo-induced luminouszinc tungstate film is combined with a substrate to have excellent photoluminescence performance and relatively good transparency (greater than 70%).

Description

technical field [0001] The invention relates to the technical field of coating, in particular to a method for preparing a polycrystalline photoluminescence zinc tungstate film. technical background [0002] Luminescent materials have been widely used in various fields of the national economy and people's daily life, and are indispensable materials in optoelectronic devices such as lighting, displays, energy-saving lamps, and radiation detectors. Among them, based on tungstate ion (WO 4 2- ) zinc tungstate (ZnWO 4 ) crystal is an excellent scintillation crystal, under the excitation of ultraviolet light, ZnWO 4 Crystals can emit strong blue-green light, and have the advantages of stable chemical properties, strong resistance to radiation and strong light damage, and have good application prospects in exciting crystals and ionizing radiation detectors. At the same time, with the continuous improvement of the miniaturization, integration, energy saving and performance requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/08C23C14/35C23C14/58
CPCC23C14/083C23C14/086C23C14/352C23C14/5806C23C14/5846
Inventor 张锋袁春林颜陈晨汤起云胡冬冬张宜林
Owner CHONGQING UNIV OF TECH
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