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Process for preparing potassium columbate K4Nb6O17 film

A k4nb6o17, potassium niobate technology, applied in chemical instruments and methods, catalyst activation/preparation, niobium compounds, etc., can solve the problems of long preparation time and high preparation cost

Inactive Publication Date: 2007-04-25
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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] By molar ratio Nb 2 o 5 : citric acid=1:10 measure niobium oxide hydrate and citric acid respectively, join in ethylene glycol monomethyl ether solvent, then add Nb 2 o 5 Molecular 2% peroxide water. The above mixed system was refluxed at a temperature range of 80° C. for 4 hours to form a transparent niobium-containing solution. Add the acetic acid solution of potassium acetate (KAc) into the niobium-containing solution according to the molar ratio K:Nb=4.1:6, heat to 80°C and stir and mix for 30 minutes to form a transparent and uniform potassium niobate sol Precursor solution, the concentration of the precursor solution is 0.10M. Before film formation, the precursor solution was filtered to remove sediment and aged for 24 hours under sealed conditions. The precursor solution was spin-coated to form a film, the spinning speed was 3000 rpm, the time was 45s, and then dried at a temperature of 100°C, and pretreated at a temperature of 400°C for 10 minutes, after 4 ...

Embodiment 2

[0016] By molar ratio Nb 2 o 5 : citric acid=1:20 Measure niobium oxide hydrate and citric acid respectively, join in ethylene glycol monomethyl ether solvent, add Nb 2 o 5 Molecular 3% peroxide water. The above mixed system was refluxed at a temperature range of 90° C. for 4 hours to form a transparent niobium-containing solution. Add the acetic acid solution of potassium acetate (KAc) into the niobium-containing solution according to the molar ratio 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 Precursor solution, the concentration of the precursor solution is 0.15M. Before film formation, the precursor solution was filtered to remove precipitates and aged for 36 hours under sealed conditions. The precursor solution was spin-coated to form a film, the spinning speed was 3500 rpm, the time was 40s, and then dried at a temperature of 100°C, and pretreated at a temperature of 400°C for 10 minutes, after 4 t...

Embodiment 3

[0018] By molar ratio Nb 2 o 5 : citric acid=1:20 Measure niobium oxide hydrate and citric acid respectively, join in ethylene glycol monomethyl ether solvent, add Nb 2 o 5 Molecular 1% peroxide water. The above mixed system was refluxed at a temperature range of 70° C. for 8 hours to form a transparent niobium-containing solution. Add the acetic acid solution of potassium acetate (KAc) into the niobium-containing solution according to the molar ratio 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 Precursor solution, the concentration of the precursor solution is 0.15M. Before film formation, the precursor solution was filtered to remove precipitates and aged for 36 hours under sealed conditions. The precursor solution was spin-coated to form a film at a speed of 3500 rpm for 40s, then dried at a temperature of 110°C, and pretreated at a temperature of 400°C for 15 minutes, after 4 times of film formation-d...

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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 invention relates to a kind of potassium niobate (K 4 Nb 6 o 17 , KN) functional ceramic thin film, the main contents of which include preparing KN functional ceramic thin film by using hydrated niobium oxide to prepare sol precursor solution of potassium niobate thin film, spin coating film formation and thin film heat treatment, etc., which belongs to a special thin film in the field of new energy materials. Background technique [0002] Potassium niobate (K 4 N b 6O 17 ), is an oxide with a special layered structure, which has good properties of solar semiconductor photocatalytic reaction for hydrogen production, and has important applications in energy and fuel cells. In order to facilitate the finalization of hydrogen production equipment, it is necessary to fix the oxide used for photocatalysis on a specific support, and the thin film preparation method can effectively solve this problem. Currently, K for photocatalytic hydrogen product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/20B01J37/04C04B35/495C01G33/00C01B3/02
Inventor 朱满康钟涛侯育冬唐剑兰汪浩王波严辉
Owner BEIJING UNIV OF TECH