CN102443833A - Nb2O5 nano-grade porous membrane and preparation method thereof - Google Patents

Nb2O5 nano-grade porous membrane and preparation method thereof Download PDF

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CN102443833A
CN102443833A CN2011103965900A CN201110396590A CN102443833A CN 102443833 A CN102443833 A CN 102443833A CN 2011103965900 A CN2011103965900 A CN 2011103965900A CN 201110396590 A CN201110396590 A CN 201110396590A CN 102443833 A CN102443833 A CN 102443833A
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nano
porous
film
porous films
matrix
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李广忠
汤慧萍
张文彦
李纲
康新婷
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Northwest Institute for Non Ferrous Metal Research
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Northwest Institute for Non Ferrous Metal Research
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Abstract

The invention discloses a Nb2O5 nano-grade porous membrane which is a self-sustaining Nb2O5 nano-grade porous membrane with a specific surface area no less than 15m<2>/g, or a Nb2O5 nano-grade porous membrane attached on a Nb substrate, wherein the specific surface area of the membrane is no less than 15m<2>/g. Also, the invention discloses a preparation method of the Nb2O5 nano-grade porous membrane. The preparation method provided by the invention is simple, and operations are convenient and reasonably designed. The prepared Nb2O5 nano-grade porous membrane has excellent optical properties such as low optical waveguide loss and high ultraviolet absorbing capacity. Therefore, the membrane can be used in protective membranes of waveguide devices and ultraviolet-sensitive materials. Meanwhile, the membrane can be used in fields of gas sensors, catalysts, and dye-sensitized solar cells.

Description

A kind of Nb 2O 5Nano-porous films and preparation method thereof
Technical field
The invention belongs to the mould material preparing technical field, be specifically related to a kind of Nb 2O 5Nano-porous films and preparation method thereof.
Background technology
Along with science and technology development, niobium oxides is more and more wider in the application in fields such as metallurgy, electronics, glass, has promoted China Nb effectively 2O 5Increasing rapidly of throughput.Nb 2O 5Film has excellent optical property, and its optical waveguide loss is little, in waveguide property device, has obtained bigger application; It has stronger uv-absorbing ability simultaneously, can be used as the protective membrane of ultraviolet sensitivity material, with SiO 2Can prepare film Deng mixing with different refractivity.Nb in recent years 2O 5Film has also caused investigator's interest as a kind of electrochromic material of excellent property.
Preparation Nb 2O 5The method of film is a lot, is used to prepare Nb at first 2O 5The method of film is a thermal oxidation method, comprises that and then modern crafts such as magnetically controlled DC sputtering, radio-frequency sputtering, chemical vapour deposition, electrochemistry anodic oxidation, electrochemical deposition, sol-gel method and pulsed laser deposition successively are used for Nb 2O 5The preparation of film, the Nb of these method preparations 2O 5Film all have preferably lithium ion embed extraction performance, its discoloration and preparation method and technology have substantial connection.
Electrochemistry anodic oxidation is the high-new manufacturing technology of a kind of inorganic materials, uses the material character of this method preparation and evenly and easily controls, and need not expensive equipment; Temperature of reaction is low, and purity is high, and process is simple to operation; Cost is low, and preparation is easy to film forming during film, and processing parameters such as composition that can be through regulating electrolytic solution, oxidizing temperature are controlled the microtexture of film easily; Can on the matrix of random shape, obtain nano-porous films, be easy to realize continuous batch production, be suitable for industrial production; Therefore have realistic meaning, received and paid attention to widely and use.
Yet, adopt electrochemistry anodic oxidation to prepare Nb 2O 5The report of nano-porous films seldom and adopts this method at H 2SO 4Can't obtain unsupported Nb in the electrolytic solution of+HF 2O 5Nano-porous films, the thickness of film is less than 0.5 μ m simultaneously.Therefore, seriously limited Nb 2O 5The research of nano-porous films and application.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art, and a kind of excellent optical property that has is provided, and the optical waveguide loss is little, and the Nb of stronger uv-absorbing ability is arranged 2O 5Nano-porous films.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of Nb 2O 5Nano-porous films is characterized in that, said Nb 2O 5Nano-porous films is that specific surface area is not less than 15m 2The unsupported Nb of/g 2O 5Nano-porous films is perhaps for to be not less than 15m attached to the specific surface area on the Nb matrix 2The Nb of/g 2O 5Nano-porous films.
Above-mentioned a kind of Nb 2O 5Nano-porous films, said attached to the Nb on the Nb matrix 2O 5The thickness of nano-porous films is 0.05 μ m～150 μ m, said unsupported Nb 2O 5The thickness of nano-porous films is 0.5 μ m～150 μ m.
Above-mentioned a kind of Nb 2O 5Nano-porous films, said Nb 2O 5The aperture of nano-porous films is not less than 5nm, and pitch of holes is not less than 3nm.
The present invention also provides a kind of Nb 2O 5The preparation method of nano-porous films is characterized in that, this method may further comprise the steps:
Step 1, with thickness be the Nb sheet of 50 μ m～300 μ m with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, with anhydrous organic reagent and ydrogen peroxide 50 or water according to 95～99: 1～5 volume ratio uniform mixing makes mixed solvent, fluorochemical is added in the mixed solvent to stir then, obtains the electrolytic solution that fluorinion concentration is 0.2mol/L～2mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode; As negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 5V～30V; Oxidizing temperature is 10 ℃～40 ℃, and oxidization time is 0.5h～28h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with placing retort furnace to carry out anneal attached to the porous-film on the Nb matrix described in the step 4, obtain attached to the Nb on the Nb matrix 2O 5Nano-porous films; Perhaps, the Nb matrix is separated with porous-film, obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain unsupported Nb adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4 2O 5Nano-porous films.
Anhydrous organic reagent described in the above-mentioned steps two is one or more in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Fluorochemical described in the above-mentioned steps two is HF or NH 4F.
The system of anneal is described in the above-mentioned steps five: 300 ℃～1400 ℃ of annealing temperatures, soaking time 0.5h～6h.
The present invention compared with prior art has the following advantages:
1, preparation method of the present invention is simple, and is easy and simple to handle and reasonable in design.
2, adopt the inventive method can prepare the Nb that thickness is 0.05 μ m～150 μ m 2O 5Nano-porous films, the Nb of preparation 2O 5The nano-porous films specific surface area is not less than 15m 2/ g, the aperture is not less than 5nm, and pitch of holes is not less than 3nm.
3, adopt the Nb of the inventive method preparation 2O 5Nano-porous films has excellent optical property; Its optical waveguide loss is little, and stronger uv-absorbing ability is arranged, and can be widely used in the protective membrane of waveguide property device and ultraviolet sensitivity material; Simultaneously can also be applied to fields such as gas sensor, catalyzer and dye sensitization solar battery.
Through embodiment, technical scheme of the present invention is done further to describe in detail below.
Embodiment
Embodiment 1
Step 1, be that to be machined into area be 80cm for the Nb sheet of 300 μ m with thickness 2Rectangular pieces, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, USP Kosher and ydrogen peroxide 50 are made mixed solvent according to 98: 2 volume ratio uniform mixing, HF is added in the mixed solvent stir then, obtain the electrolytic solution that fluorinion concentration is 0.5mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 9V, oxidizing temperature is 20 ℃, oxidization time is 2h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4; The Nb matrix is separated with porous-film; Obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain specific surface area and be not less than 15m 2/ g, thickness are 0.5 μ m, and the aperture is not less than 5nm, and pitch of holes is not less than the unsupported Nb of 3nm 2O 5Nano-porous films; The system of said anneal is: 500 ℃ of annealing temperatures, soaking time 2h.
Embodiment 2
Present embodiment is identical with embodiment 1, and wherein difference is: used anhydrous organic reagent is terepthaloyl moietie, methyl alcohol, methane amide or methyl-sulphoxide, perhaps is at least two kinds in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Embodiment 3
Step 1, be that to be machined into area be 20cm for the Nb sheet of 100 μ m with thickness 2Disk, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, terepthaloyl moietie and water are made mixed solvent according to 98: 2 volume ratio uniform mixing, HF is added in the mixed solvent stir then, obtain the electrolytic solution that fluorinion concentration is 1mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 19V, oxidizing temperature is 28 ℃, oxidization time is 5h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4; The Nb matrix is separated with porous-film; Obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain specific surface area and be not less than 15m 2/ g, thickness are 50 μ m, and the aperture is not less than 5nm, and pitch of holes is not less than the unsupported Nb of 3nm 2O 5Nano-porous films; The system of said anneal is: 700 ℃ of annealing temperatures, soaking time 1h.
Embodiment 4
Present embodiment is identical with embodiment 3, and wherein difference is: used anhydrous organic reagent is USP Kosher, methyl alcohol, methane amide or methyl-sulphoxide, perhaps is at least two kinds in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Embodiment 5
Step 1, be that to be machined into area be 1cm for the Nb sheet of 50 μ m with thickness 2Disk, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, methyl alcohol and water are made mixed solvent according to 99: 1 volume ratio uniform mixing, HF is added in the mixed solvent stir then, obtain the electrolytic solution that fluorinion concentration is 0.2mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 5V, oxidizing temperature is 20 ℃, oxidization time is 0.5h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with placing retort furnace to carry out anneal attached to the porous-film on the Nb matrix described in the step 4, obtain specific surface area and be not less than 15m 2/ g, thickness are 0.05 μ m, and the aperture is not less than 5nm, pitch of holes be not less than 3nm attached to the Nb on the Nb matrix 2O 5Nano-porous films; The system of said anneal is: 300 ℃ of annealing temperatures, soaking time 6h.
Embodiment 6
Present embodiment is identical with embodiment 5, and wherein difference is: used anhydrous organic reagent is terepthaloyl moietie, USP Kosher, methane amide or methyl-sulphoxide, perhaps is at least two kinds in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Embodiment 7
Step 1, be that to be machined into area be 80cm for the Nb sheet of 100 μ m with thickness 2Rectangular pieces, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, methane amide and water are made mixed solvent according to 95: 5 volume ratio uniform mixing, then with NH 4Stir in the F adding mixed solvent, obtain the electrolytic solution that fluorinion concentration is 2mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 30V, oxidizing temperature is 10 ℃, oxidization time is 10h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with placing retort furnace to carry out anneal attached to the porous-film on the Nb matrix described in the step 4, obtain specific surface area and be not less than 15m 2/ g, thickness are 100 μ m, and the aperture is not less than 5nm, pitch of holes be not less than 3nm attached to the Nb on the Nb matrix 2O 5Nano-porous films; The system of said anneal is: 300 ℃ of annealing temperatures, soaking time 6h.
Embodiment 8
Present embodiment is identical with embodiment 7, and wherein difference is: used anhydrous organic reagent is terepthaloyl moietie, USP Kosher, methyl alcohol or methyl-sulphoxide, perhaps is at least two kinds in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Embodiment 9
Step 1, be that to be machined into area be 50cm for the Nb sheet of 300 μ m with thickness 2Rectangular pieces, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, methyl-sulphoxide and water are made mixed solvent according to 95: 5 volume ratio uniform mixing, HF is added in the mixed solvent stir then, obtain the electrolytic solution that fluorinion concentration is 0.7mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 20V, oxidizing temperature is 40 ℃, oxidization time is 28h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4; The Nb matrix is separated with porous-film; Obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain specific surface area and be not less than 15m 2/ g, thickness are 150 μ m, and the aperture is not less than 5nm, pitch of holes be not less than 3nm attached to the Nb on the Nb matrix 2O 5Nano-porous films; The system of said anneal is: 1400 ℃ of annealing temperatures, soaking time 0.5h.
Embodiment 10
Present embodiment is identical with embodiment 9, and wherein difference is: used anhydrous organic reagent is terepthaloyl moietie, USP Kosher, methyl alcohol or methane amide, perhaps is at least two kinds in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
Embodiment 11
Step 1, be that to be machined into area be 60cm for the Nb sheet of 300 μ m with thickness 2Disk, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, terepthaloyl moietie, USP Kosher and water are made mixed solvent according to 40: 57: 3 volume ratio uniform mixing, then with NH 4Stir in the F adding mixed solvent, obtain the electrolytic solution that fluorinion concentration is 1.2mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 20V, oxidizing temperature is 10 ℃, oxidization time is 28h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with placing retort furnace to carry out anneal attached to the porous-film on the Nb matrix described in the step 4, obtain specific surface area and be not less than 15m 2/ g, thickness are 150 μ m, and the aperture is not less than 5nm, pitch of holes be not less than 3nm attached to the Nb on the Nb matrix 2O 5Nano-porous films; The system of said anneal is: 1000 ℃ of annealing temperatures, soaking time 3h.
Embodiment 12
Present embodiment is identical with embodiment 11; Wherein difference is: used anhydrous organic reagent is a kind of in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide or more than three kinds; Perhaps being two kinds in USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide, perhaps is the mixture of a kind of and terepthaloyl moietie in methyl alcohol, methane amide or the methyl-sulphoxide.
Embodiment 13
Step 1, be that to be machined into area be 50cm for the Nb sheet of 50 μ m with thickness 2Disk, the Nb sheet after then will processing is with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, with USP Kosher, methyl alcohol, methane amide and water according to 20: 35: 42: 3 volume ratio uniform mixing makes mixed solvent, HF is added in the mixed solvent to stir then, obtains the electrolytic solution that fluorinion concentration is 0.4mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode, as negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 20V, oxidizing temperature is 40 ℃, oxidization time is 10h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4; The Nb matrix is separated with porous-film; Obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain specific surface area and be not less than 15m 2/ g, thickness are 100 μ m, and the aperture is not less than 5nm, pitch of holes be not less than 3nm attached to the Nb on the Nb matrix 2O 5Nano-porous films; The system of said anneal is: 800 ℃ of annealing temperatures, soaking time 5h.
Embodiment 14
Present embodiment is identical with embodiment 13; Wherein difference is: used anhydrous organic reagent be in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide a kind of, two kinds, four kinds or five kinds; Perhaps be three kinds in terepthaloyl moietie, methyl alcohol, methane amide and the methyl-sulphoxide; Perhaps being two kinds and the mixture of USP Kosher in terepthaloyl moietie, methyl alcohol and the methyl-sulphoxide, perhaps is terepthaloyl moietie, USP Kosher and methane amide, perhaps is methyl-sulphoxide, USP Kosher and methane amide.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every according to inventing technical spirit to any simple modification, change and equivalent structure variation that above embodiment did, all still belong in the protection domain of technical scheme of the present invention.

Claims (7)

1. Nb 2O 5Nano-porous films is characterized in that, said Nb 2O 5Nano-porous films is that specific surface area is not less than 15m 2The unsupported Nb of/g 2O 5Nano-porous films is perhaps for to be not less than 15m attached to the specific surface area on the Nb matrix 2The Nb of/g 2O 5Nano-porous films.
2. a kind of Nb according to claim 1 2O 5Nano-porous films is characterized in that, and is said attached to the Nb on the Nb matrix 2O 5The thickness of nano-porous films is 0.05 μ m～150 μ m, said unsupported Nb 2O 5The thickness of nano-porous films is 0.5 μ m～150 μ m.
3. a kind of Nb according to claim 1 2O 5Nano-porous films is characterized in that, said Nb 2O 5The aperture of nano-porous films is not less than 5nm, and pitch of holes is not less than 3nm.
4. one kind prepares like claim 1,2 or 3 said Nb 2O 5The method of nano-porous films is characterized in that, this method may further comprise the steps:
Step 1, with thickness be the Nb sheet of 50 μ m～300 μ m with carborundum paper polishing light, the Nb sheet after will polishing then cleans up, and dries for use;
Step 2, with anhydrous organic reagent and ydrogen peroxide 50 or water according to 95～99: 1～5 volume ratio uniform mixing makes mixed solvent, fluorochemical is added in the mixed solvent to stir then, obtains the electrolytic solution that fluorinion concentration is 0.2mol/L～2mol/L;
Step 3, with in the step 1 oven dry after the Nb sheet place electrolytic solution described in the step 2 as anode; As negative electrode, utilize direct supply antianode Nb sheet to carry out anodic oxidation with platinum electrode, oxidation voltage is 5V～30V; Oxidizing temperature is 10 ℃～40 ℃, and oxidization time is 0.5h～28h;
Step 4, the Nb sheet behind electrolytic oxidation in the step 3 is taken out and uses washed with de-ionized water, after the drying, obtain attached to the porous-film on the Nb matrix;
Step 5, with placing retort furnace to carry out anneal attached to the porous-film on the Nb matrix described in the step 4, obtain attached to the Nb on the Nb matrix 2O 5Nano-porous films; Perhaps, the Nb matrix is separated with porous-film, obtain unsupported porous-film, place retort furnace to carry out anneal unsupported porous-film then, obtain unsupported Nb adopting mechanical means to peel off attached to the porous-film on the Nb matrix described in the step 4 2O 5Nano-porous films.
5. method according to claim 4 is characterized in that, anhydrous organic reagent described in the step 2 is one or more in terepthaloyl moietie, USP Kosher, methyl alcohol, methane amide and the methyl-sulphoxide.
6. method according to claim 4 is characterized in that, fluorochemical described in the step 2 is HF or NH 4F.
7. method according to claim 4 is characterized in that, the system of anneal described in the step 5 is: 300 ℃～1400 ℃ of annealing temperatures, soaking time 0.5h～6h.
CN2011103965900A 2011-12-04 2011-12-04 Nb2O5 nano-grade porous membrane and preparation method thereof Pending CN102443833A (en)

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CN103855386A (en) * 2014-03-21 2014-06-11 西北有色金属研究院 Fe-doped Nb2Ox nano porous material with oxygen deficiency structure and application
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CN111217392B (en) * 2018-11-27 2021-09-14 中国科学院大连化学物理研究所 Niobium oxide nano mesh material and preparation method thereof
CN109652838A (en) * 2018-12-27 2019-04-19 浙江工业大学 A kind of method of titanium-niobium alloy surface anodization coloring
CN109652838B (en) * 2018-12-27 2021-05-18 浙江工业大学 Titanium-niobium alloy surface anodic oxidation coloring method
CN112831818A (en) * 2021-02-05 2021-05-25 成都印钞有限公司 Tantalum, niobium and precious metal composite multicolor coin and stamp manufacturing method and multicolor coin and stamp

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Application publication date: 20120509