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Process for preparing potassium columbate K4Nb6O17 film

A technology of k4nb6o17 and potassium niobate, applied in the production of hydrogen and other directions, can solve the problems of long preparation time and high preparation cost

Inactive Publication Date: 2006-06-28
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, niobate thin films, such as LiNbO 3 , KNbO 3 etc., mostly use niobium alkoxide as raw material: In this method, in order to avoid the hydrolysis of niobium alkoxide and the precipitation of niobium oxide precipitation, the hydrolysis rate of niobium alkoxide sol must be strictly controlled every time a film is prepared, and an appropriate amount of niobium alkoxide sol must be added. water, control the appropriate acidity, the whole process requires precise control, long preparation time, and high preparation cost

Method used

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  • Process for preparing potassium columbate K4Nb6O17 film
  • Process for preparing potassium columbate K4Nb6O17 film
  • Process for preparing potassium columbate K4Nb6O17 film

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Experimental program
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Effect test

Embodiment 1

[0014] Molar ratio Nb 2 O 5 :Citric acid=1∶10, respectively measure hydrated niobium oxide and citric acid, add them to the ethylene glycol monomethyl ether solvent, and then add Nb 2 O 5 Peroxygen water of 2% of moles. The above-mentioned mixed system was refluxed for 4 hours at a temperature range of 80° C. to form a transparent niobium-containing solution. The acetic acid solution of potassium acetate (KAc) is added to the niobium-containing solution at a molar ratio of K:Nb=4.1:6, and heated to 80°C and stirred and mixed for 30 minutes to form a transparent and uniform potassium niobate sol The precursor liquid, the concentration of the precursor liquid is 0.10M. Before film formation, the precursor solution was filtered to remove the sediment and then aged for 24 hours under sealed conditions. The precursor solution was spin-coated into a film, the spinning speed was 3000 rpm, and the time was 45 seconds, and then dried at a temperature of 100°C, pretreated at a temperature o...

Embodiment 2

[0016] Molar ratio Nb 2 O 5 :Citric acid=1:20, respectively measure the hydrated niobium oxide and citric acid, add them to the ethylene glycol monomethyl ether solvent, and then add Nb 2 O 5 Peroxygen water of 3% of moles. The above-mentioned mixed system was refluxed for 4 hours at a temperature range of 90° C. to form a transparent niobium-containing solution. Add the acetic acid solution of potassium acetate (KAc) to the niobium-containing solution at a molar ratio of K:Nb=4.2:6. Heat to 70°C and stir and mix for 30 minutes to form a transparent and uniform potassium niobate sol The precursor fluid, the concentration of the precursor fluid is 0.15M. Before film formation, the precursor solution was filtered to remove the sediment and then aged for 36 hours under sealed conditions. The precursor liquid was spin-coated into a film, the spinning speed was 3500 rpm, the time was 40s, and then it was dried at a temperature of 100°C, and pretreated at a temperature of 400°C for 10 m...

Embodiment 3

[0018] Molar ratio Nb 2 O 5 :Citric acid=1:20, respectively measure the hydrated niobium oxide and citric acid, add them to the ethylene glycol monomethyl ether solvent, and then add Nb 2 O 5 Peroxygen water of 1% of moles. The above-mentioned mixed system was refluxed for 8 hours at a temperature range of 70° C. to form a transparent niobium-containing solution. Add the acetic acid solution of potassium acetate (KAc) to the niobium-containing solution at a molar ratio of K:Nb=4.2:6. Heat to 70°C and stir and mix for 30 minutes to form a transparent and uniform potassium niobate sol The precursor fluid, the concentration of the precursor fluid is 0.15M. Before film formation, the precursor solution was filtered to remove the sediment and then aged for 36 hours under sealed conditions. The precursor liquid was spin-coated into a film, the spinning speed was 3500 rpm, the time was 40s, and then it was dried at a temperature of 110°C, and pretreated at a temperature of 400°C for 15 m...

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Abstract

The invention relates to functional ceramic field. The process includes the following steps: according Nb2O5: citric acid=1:10-20 adding to ethylene glycol single methyl ether, adding peroxy water channeling back for 4-8 hours at 70-90 degree centigrade to make niobium contained solution, potassium acetate dissolving in acetic acid solution to form potassium contained solution, mixing the two solutions according to K: Nb=4.0-4.2:6, mixing for 30-45 minutes at 70-90 degree centigrade to form precursor liquid, aging for 24-48 hours, spin coating to form film and the spinning speed is 3000-4000 round / min for 30-45s, drying, pre-treating for 10-15 minutes at 350-400 degree centigrade, repeating for 3-4 times, the film that has 80-100nm thickness would be gained. Then, heating to 600-700 degree centigrade at the speed of 10-15 degree centigrade, anneals 10-15 minutes. The invention has good tropism structure and has good poto-catalysis water decomposition hydrogen making capability.

Description

Technical field [0001] The present invention relates to a kind of potassium niobate (K 4 Nb 6 O 17 , KN) functional ceramic film, its main content includes the use of hydrated niobium oxide to prepare potassium niobate film sol precursor, spin-coating film formation and film heat treatment to prepare KN functional ceramic film, which belongs to a special film in the field of new energy materials. Background technique [0002] Potassium Niobate (K 4 Nb 6 O 17 ), is an oxide with a special layered structure, has good characteristics of hydrogen production by solar semiconductor photocatalytic reaction, and has important applications in energy and fuel cells. In order to facilitate the finalization of the hydrogen production equipment, the oxide used for photocatalysis needs to be fixed on a specific support. The film preparation method can effectively solve this problem. Currently, K used for photocatalytic hydrogen production 4 Nb 6 O 17 There is no patent report on the preparatio...

Claims

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Application Information

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IPC IPC(8): C04B35/495C01B3/02C04B35/622
Inventor 朱满康钟涛侯育冬唐剑兰汪浩王波严辉
Owner BEIJING UNIV OF TECH