Method for preparing niobium pentaoxide membrane

A niobium pentoxide and thin film technology, applied in the field of thin film preparation, can solve the problems of high equipment requirements, complex process, unstable niobium alkoxide and inorganic salt, etc. Effect

Inactive Publication Date: 2009-11-04
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods also have many defects. The film prepared by oxidation method is directly deposited on the surface of niobium metal electrode, which is only suitable for the research of related phenomena and mechanisms; the film prepared by electron beam evaporation method has obvious columnar structure. The aggregation density of the film layer is reduced, the refractive index is not high, and the optical properties of the scattered layer drift greatly after moisture absorption; when the sol-gel method is prepared, the precursor niobium alkoxide and inorganic salt suitable for the preparation of the niobium pentoxide film are very unstable. This makes the process control extremely difficult, and the prepared niobium pentoxide film not only has poor firmness, but also has a low refractive index; while the reactive sputtering method must coordinate many factors such as the gas composition and pressure in the sputtering chamber, in order to obtain the desired thin film, which requires high equipment requirements and complicated processes

Method used

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  • Method for preparing niobium pentaoxide membrane
  • Method for preparing niobium pentaoxide membrane
  • Method for preparing niobium pentaoxide membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a, take niobium pentoxide 39.8721g and potassium carbonate 6.9105g respectively, put into agate mortar and fully grind evenly;

[0028] b. Put the ground mixture in a muffle furnace to react at 600° C. for 6 hours.

[0029] c. Take out 1 g of calcined material, add 1 L of 1 mol / L hydrochloric acid and stir for 24 hours, after filtering, add hydrochloric acid in the same proportion, stir for the same time and filter, repeat 4 times.

[0030] d. The filter cake filtered in step c is fully washed with deionized water, and put into an oven at 60° C. for 6 hours.

[0031] e. Take out 1 g of the dried powder and add it to 100 ml of 0.5 mol / l tetra-n-butylammonium hydroxide solution, stir for 72 hours, and then centrifuge for 10 minutes in a high-speed centrifuge at 10,000 r / min to obtain niobium pentoxide nanosheet sol.

[0032] f. Take a 30×10×1.5mm quartz plate, wash it ultrasonically with detergent, acetone and deionized water in sequence, and dry it with pure nitrogen fo...

Embodiment 2

[0035] a. Weigh 79.7442 g of niobium pentoxide and 13.8210 g of potassium carbonate, respectively, put them into an agate mortar and grind them evenly.

[0036] b. Put the ground mixture in a muffle furnace to react at 800° C. for 12 hours.

[0037] c. Take out 1 g of calcined material, add 1 L of 1 mol / L hydrochloric acid and stir for 24 hours, after filtering, add hydrochloric acid in the same proportion, stir for the same time and filter, repeat 4 times.

[0038] d. The filter cake filtered in step c is fully washed with deionized water, and put into an oven at 80° C. for 8 hours.

[0039] e. Take out 1 g of the dried powder and add it to 100 ml of 0.5 mol / l tetra-n-butylammonium hydroxide solution, stir for 72 hours, and then centrifuge for 15 minutes under a high-speed centrifuge at 10,000 r / min to obtain niobium pentoxide nanosheet sol.

[0040] f. Take a 30×10×1.5mm quartz plate, wash it ultrasonically with detergent, acetone and deionized water in sequence, and dry it...

Embodiment 3

[0043] a. Weigh 79.7442 g of niobium pentoxide and 13.8210 g of potassium carbonate, respectively, put them into an agate mortar and grind them evenly.

[0044] b. Put the ground mixture in a muffle furnace to react at 1000° C. for 8 hours.

[0045] c. Take out 1 g of the calcined material, add 1L of 1mol / L hydrochloric acid and stir for 12 hours, after filtering, add hydrochloric acid in the same proportion, stir for the same time and filter, repeat 4 times.

[0046] d. The filter cake filtered in step c is fully washed with deionized water, and put into an oven at 100° C. for 12 hours.

[0047] e. Take out 1 g of the dried powder and add it to 100 ml of 0.5 mol / l tetra-n-butylammonium hydroxide solution, stir for 72 hours, and then centrifuge for 20 minutes in a high-speed centrifuge at 10,000 r / min to obtain niobium pentoxide nanosheet sol.

[0048] f. Take a 30×10×1.5mm quartz plate and clean it ultrasonically with detergent, acetone and deionized water in sequence, and d...

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Abstract

The invention discloses a method for preparing a niobium pentaoxide membrane. The method comprises the following steps: mixing niobium pentaoxide and potassium carbonate in a molar ratio of 3:1; after calcination, adding the calcinated materials into hydrochloric acid, stirring and filtering the mixed solution, adding hydrochloric acid in the same ratio into the mixed solution, stirring and filtering the mixed solution, and repeating four times; washing filter cakes by deionized water, drying the filter cakes, adding a 0.5mol/l tetrabutylammonium hydroxide solution into the filter cakes, stirring the mixture, and obtaining niobium pentaoxide nano flake sol under high-speed centrifugation; and preparing a 2.5g/l polyethyleneimine solution, immersing a clean quartz plate into the polyethyleneimine solution for soaking, taking the quartz plate out, washing the quartz plate by the deionized water, blowing the quartz plate to dryness, immersing the quartz plate into niobium pentaoxide sol for soaking, taking the quartz plate out, washing the quartz plate by the deionized water, blowing the quartz plate to dryness by pure nitrogen to obtain a layer of the niobium pentaoxide membrane, and repeating the process to prepare different layers of the niobium pentaoxide membrane. The method has the advantages of simple operation, low cost and suitability for industrial production.

Description

technical field [0001] The invention relates to the preparation of a thin film, specifically a method for preparing a niobium pentoxide thin film by using niobium pentoxide as a niobium source, tetramethylammonium hydroxide as an intercalation agent, and a quartz plate as a substrate. Background technique [0002] Niobium pentoxide thin film has excellent optical properties, and its optical waveguide loss is small, so it has been widely used in waveguide devices. It can be used as a protective film for ultraviolet sensitive materials by using its strong ultraviolet absorption ability Silicon oxide and the like can prepare thin films with different refractive indices. Niobium pentoxide thin film is also an electrochromic material with excellent performance. Some studies believe that the electrochromic performance of niobium pentoxide film is comparable to that of tungsten oxide, which has been extensively researched and applied to a certain extent; some researchers also beli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/34
Inventor 李强褚晶张娜夏金峰李彩霞宋杰
Owner EAST CHINA NORMAL UNIV
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