CN106469645B - A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material - Google Patents
A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material Download PDFInfo
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Abstract
本发明公开了一种有机超晶格锐钛型钛化氧化钨薄膜红外光敏材料的制备方法，其步骤如下：步骤1，制备钨镀膜液；步骤2，得到二氧化钛镀膜液；步骤3，制备改性液；步骤4，将基底材料浸泡至钨镀膜液中，搅拌均匀后，在烘箱内烘干，得到钨膜；步骤5，将钨膜浸泡至二氧化钛镀膜液中，然后快速冷却，形成纳米二氧化钛前驱薄膜；步骤6，将步骤5中的薄膜基底材料进行高温烧结，形成纳米二氧化钛‑氧化钨薄膜；步骤7，将步骤6的薄膜浸泡至步骤3中乙醇水溶液中，多次微沸蒸煮，捞出后，快速固化；步骤8，步骤7中的薄膜材料退火处理得到产品。本发明制备方法简单，解决了钛化和氧化钨薄膜材料的平整度和均匀性低、缺陷大、粗糙度高等问题。The invention discloses a preparation method of an organic superlattice anatase titanium oxide tungsten oxide thin film infrared photosensitive material. The steps are as follows: step 1, preparing a tungsten coating solution; step 2, obtaining a titanium dioxide coating solution; step 4, soak the base material in the tungsten coating solution, stir evenly, and dry it in an oven to obtain a tungsten film; step 5, soak the tungsten film into the titanium dioxide coating solution, and then rapidly cool it to form nano-titanium dioxide Precursor film; step 6, sintering the film base material in step 5 at high temperature to form a nano-titanium dioxide-tungsten oxide film; step 7, immersing the film in step 6 in the ethanol aqueous solution in step 3, boiling for several times, and removing After extraction, rapid curing; step 8, annealing of the thin film material in step 7 to obtain a product. The preparation method of the invention is simple, and solves the problems of low flatness and uniformity, large defects and high roughness of titaniumized and tungsten oxide thin film materials.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of organic superlattices anatase titanium dioxide titanizing tungsten oxide film is infrared
The preparation method of light-sensitive material.
Background technique
In optoelectronic applications field, three-dimensional flower-shaped nano structural material is excellent with respect to for one-dimensional nano line and two-dimensional nano piece
Gesture is fairly obvious, and high specific surface area is conducive to the absorption of photon, in interpenetrating network be conducive to photoproduction current-carrying
Son transports.Two during the last ten years, and people have been successfully prepared many semiconductor flower-like nanometers crystalline substances by nanotechnology, such as aoxidizes
Iron nanometer snowflake, zinc-oxide nano lilac, vulcanized lead nanometer Flos Albiziae, TiOx nano camellia, cupric oxide nano tree peony, sulphur
Change copper nanometer rose, nanometer nickel sulfide flower, cobalt sulfide nano flower etc..But in the application of nano photoelectric device, three-dimensional flower-shaped nanometer
Structural material is still faced with light induced electron and the high problem of hole-recombination probability.Recent study discovery, super-lattice nanostructure
With the quantum confined effect that people wish eagerly, distinctive superlattices modulated structure is equivalent to heterojunction boundary, can be effectively
Improve photo-generate electron-hole pair yield and separative efficiency, therefore super-lattice nanostructure be known as " open research in nanotechnology and
The new page of application ".Yang study group is prepared for by mixed pulses laser ablation-chemical vapor deposition (PLA-CVD) technology
Si/SiGe superlattices, GaAs/GaP superlattices have been made also by similar method in Lieber study group, and Samuelson is ground
Study carefully group and InAs/InP superlattices are then obtained by chemical beam epitaxy technology CBE.The common feature of these methods is all to pass through gas
Body-liquid-solid growth process (VLS) realizes equiblibrium mass distribution of the foreign atom in lattice, and this method is needed in reactant gas
Multiple checker reactant under conditions of change, complex process equipment, operation require stringent and a large amount of energy consumptions, are difficult to realize industry
Metaplasia produces.
Summary of the invention
The object of the present invention is to provide a kind of systems of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material
Preparation Method, preparation method of the present invention is simple, and flatness and the uniformity for solving titanizing and tungsten oxide film material be low, defect
Greatly, the problems such as roughness is high.
A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material, its step are as follows:
Step 1, ammonium tungstate, tungsten chloride are put into alkaline solution, nanometer foaming agent is added, form tungsten coating liquid；
Step 2, tetrabutyl titanate, stabilizer, lysate, acidulant and bleeding agent are put into stirred tank, are stirred evenly
TiO 2 coating film liquid can be obtained；
Step 3, using inorganic modifier and organic metal modifying agent as material, it is dipped to ethanol water, is modified
Liquid；
Step 4, base material is dipped in tungsten coating liquid, after mixing evenly, in drying in oven, obtains tungsten film；
Step 5, tungsten film is dipped in TiO 2 coating film liquid, is then quickly cooled down, form nanometer titanium dioxide titanium precursor
Film；
Step 6, the film base material in step 5 is subjected to high temperature sintering, it is thin forms nano-titanium dioxide-tungsten oxide
Film；
Step 7, the film of step 6 is dipped in step 3 in ethanol water, heating for multiple times boiling, after pulling out, quickly
Solidification；
Step 8, the thin-film material in step 7 makes annealing treatment to obtain product.
Formula in the step 1 is ammonium tungstate 6-10 parts, 1-3 parts of tungsten chloride, 30-50 parts of alkaline solution, nanometer foam
2-4 parts of agent；The alkaline solution uses sodium hydroxide solution or potassium hydroxide solution, and the nanometer foaming agent uses nano-sized carbon
Sour hydrogen sodium.
Formula in the step 2 is tetrabutyl titanate 11-15 parts, 3-5 parts of stabilizer, 40-60 parts of lysate, acidulant
0.3-1.0 parts, 2-3 parts of bleeding agent；The stabilizer uses acetic acid acetone, and the lysate uses ethyl acetate or isopropanol,
The acidulant uses fatty alcohol polyoxyethylene ether using one of acetic acid, hydrochloric acid or sulfuric acid, bleeding agent.
Formula in the step 3 is inorganic modifier 1-3 parts, 3-5 parts of organic metal modifying agent, ethanol water 20-
25 parts, ethanol content is 50-70% in the ethanol water；The inorganic modifier uses silica or silicon carbide, described
Organic metal modifying agent uses acrylic tin or isopropyl alcohol radical nickel.
Soaking time in the step 4 is 11-20min, and the baking oven drying temperature is 90-110 DEG C, and drying time is
20-40min。
Rapid cooling in the step 5 uses air-cooled technology, and the flow velocity of the rapid cooling is 5-15mL/min.
High temperature sintering temperature in the step 6 is 250-320 DEG C, sintering time 2-4h.
Soaking time in the step 7 is 12-18min, and heating temperature is 100-120 DEG C, and the heating times are 2-
10 times.
Annealing in the step 8 is that 120-400 DEG C is heated under 20-35MPa pressure.
Compared with prior art, the invention has the following advantages:
1, preparation method of the present invention is simple, and flatness and the uniformity for solving titanizing and tungsten oxide film material are low, scarce
Fall into the problems such as big, roughness is high.
2, the present invention is deposited in titanic oxide material surface using by modifying agent heating, fills up defect problem, can be significantly
Photoelectric conductivity.
3, the present invention is uniformly mixed using uniformly mixed modification, organic-inorganic, can be greatly reduced defect, substantially reduced
Roughness, film layer is more uniform, planarization is splendid.
Specific embodiment
The present invention is described further below with reference to embodiment:
Embodiment 1
A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material, its step are as follows:
Step 1, ammonium tungstate, tungsten chloride are put into alkaline solution, nanometer foaming agent is added, form tungsten coating liquid；
Step 2, tetrabutyl titanate, stabilizer, lysate, acidulant and bleeding agent are put into stirred tank, are stirred evenly
TiO 2 coating film liquid can be obtained；
Step 3, using inorganic modifier and organic metal modifying agent as material, it is dipped to ethanol water, is modified
Liquid；
Step 4, base material is dipped in tungsten coating liquid, after mixing evenly, in drying in oven, obtains tungsten film；
Step 5, tungsten film is dipped in TiO 2 coating film liquid, is then quickly cooled down, form nanometer titanium dioxide titanium precursor
Film；.
Soaking time in the step 4 is 11min, and the baking oven drying temperature is 90 DEG C, drying time 200min.
Rapid cooling in the step 5 uses air-cooled technology, and the flow velocity of the rapid cooling is 5mL/min.
High temperature sintering temperature in the step 6 is 250 DEG C, sintering time 2h.
Soaking time in the step 7 is 12min, and heating temperature is 100 DEG C, and the heating times are 2 times.
Annealing in the step 8 is that 120 DEG C are heated under 20MPa pressure.
Embodiment 2
A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material, its step are as follows:
Step 1, ammonium tungstate, tungsten chloride are put into alkaline solution, nanometer foaming agent is added, form tungsten coating liquid；
Step 2, tetrabutyl titanate, stabilizer, lysate, acidulant and bleeding agent are put into stirred tank, are stirred evenly
TiO 2 coating film liquid can be obtained；
Step 3, using inorganic modifier and organic metal modifying agent as material, it is dipped to ethanol water, is modified
Liquid；
Step 4, base material is dipped in tungsten coating liquid, after mixing evenly, in drying in oven, obtains tungsten film；
Step 5, tungsten film is dipped in TiO 2 coating film liquid, is then quickly cooled down, form nanometer titanium dioxide titanium precursor
Film；
Step 6, the film base material in step 5 is subjected to high temperature sintering, it is thin forms nano-titanium dioxide-tungsten oxide
Film；
Step 7, the film of step 6 is dipped in step 3 in ethanol water, heating for multiple times boiling, after pulling out, quickly
Solidification；
Step 8, the thin-film material in step 7 makes annealing treatment to obtain product.
Formula in the step 1 is 10 parts of ammonium tungstate, 3 parts of tungsten chloride, 4 parts of 50 part, nanometer foaming agent of alkaline solution；Institute
Alkaline solution is stated using potassium hydroxide solution, the nanometer foaming agent uses nano-calcium carbonate hydrogen sodium.
Formula in the step 2 is 15 parts of tetrabutyl titanate, 5 parts of stabilizer, 60 parts of lysate, 1.0 parts of acidulant, seeps
Saturating 3 parts of agent；The stabilizer uses acetic acid acetone, and the lysate uses isopropanol, and the acidulant uses hydrochloric acid, bleeding agent
Using fatty alcohol polyoxyethylene ether.
Formula in the step 3 is 3 parts of inorganic modifier, 5 parts of organic metal modifying agent, 25 parts of ethanol water, institute
Stating ethanol content in ethanol water is 70%；The inorganic modifier uses silicon carbide, and the organic metal modifying agent uses
Isopropyl alcohol radical nickel.
Soaking time in the step 4 is 20min, and the baking oven drying temperature is 110 DEG C, drying time 40min.
Rapid cooling in the step 5 uses air-cooled technology, and the flow velocity of the rapid cooling is 15mL/min.
High temperature sintering temperature in the step 6 is 320 DEG C, sintering time 4h.
Soaking time in the step 7 is 18min, and heating temperature is 120 DEG C, and the heating times are 10 times.
Annealing in the step 8 is that 400 DEG C are heated under 35MPa pressure.
Embodiment 3
A kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material, its step are as follows:
Step 1, ammonium tungstate, tungsten chloride are put into alkaline solution, nanometer foaming agent is added, form tungsten coating liquid；
Step 2, tetrabutyl titanate, stabilizer, lysate, acidulant and bleeding agent are put into stirred tank, are stirred evenly
TiO 2 coating film liquid can be obtained；
Step 3, using inorganic modifier and organic metal modifying agent as material, it is dipped to ethanol water, is modified
Liquid；
Step 4, base material is dipped in tungsten coating liquid, after mixing evenly, in drying in oven, obtains tungsten film；
Step 5, tungsten film is dipped in TiO 2 coating film liquid, is then quickly cooled down, form nanometer titanium dioxide titanium precursor
Film；
Step 6, the film base material in step 5 is subjected to high temperature sintering, it is thin forms nano-titanium dioxide-tungsten oxide
Film；
Step 7, the film of step 6 is dipped in step 3 in ethanol water, heating for multiple times boiling, after pulling out, quickly
Solidification；
Step 8, the thin-film material in step 7 makes annealing treatment to obtain product.
Formula in the step 1 is 8 parts of ammonium tungstate, 2 parts of tungsten chloride, 4 parts of 45 part, nanometer foaming agent of alkaline solution；Institute
Alkaline solution is stated using sodium hydroxide solution, the nanometer foaming agent uses nano-calcium carbonate hydrogen sodium.
Formula in the step 2 is 13 parts of tetrabutyl titanate, 4 parts of stabilizer, 55 parts of lysate, 0.9 part of acidulant, seeps
Saturating 3 parts of agent；The stabilizer uses acetic acid acetone, and the lysate uses isopropanol, and the acidulant uses sulfuric acid, bleeding agent
Using fatty alcohol polyoxyethylene ether.
Formula in the step 3 is 2 parts of inorganic modifier, 4 parts of organic metal modifying agent, 24 parts of ethanol water, institute
Stating ethanol content in ethanol water is 60%；The inorganic modifier uses silica, and the organic metal modifying agent uses
Acrylic tin.
Soaking time in the step 4 is 15min, and the baking oven drying temperature is 100 DEG C, drying time 35min.
Rapid cooling in the step 5 uses air-cooled technology, and the flow velocity of the rapid cooling is 5-15mL/min.
High temperature sintering temperature in the step 6 is 290 DEG C, sintering time 4h.
Soaking time in the step 7 is 16min, and heating temperature is 110 DEG C, and the heating times are 8 times.
Annealing in the step 8 is that 320 DEG C are heated under 28MPa pressure.
The foregoing is merely one embodiment of the invention, are not intended to limit the present invention, all to use equivalent substitution or equivalent transformation
Mode technical solution obtained, fall within the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material, its step are as follows:
Step 1, ammonium tungstate, tungsten chloride are put into alkaline solution, nanometer foaming agent is added, form tungsten coating liquid；
Step 2, tetrabutyl titanate, stabilizer, lysate, acidulant and bleeding agent are put into stirred tank, are stirred evenly
Obtain TiO 2 coating film liquid；
Step 3, using inorganic modifier and organic metal modifying agent as material, it is dipped to ethanol water, obtains modification liquid；
Step 4, base material is dipped in tungsten coating liquid, after mixing evenly, in drying in oven, obtains tungsten film；
Step 5, tungsten film is dipped in TiO 2 coating film liquid, is then quickly cooled down, form nano-titanium dioxide precursor thin film；
Step 6, the film base material in step 5 is subjected to high temperature sintering, forms nano-titanium dioxide-tungsten oxide film；
Step 7, the film of step 6 is dipped in step 3 in ethanol water, heating for multiple times boiling, it is quickly solid after pulling out
Change；
Step 8, the thin-film material in step 7 makes annealing treatment to obtain product；
Formula in the step 2 is tetrabutyl titanate 11-15 parts, 3-5 parts of stabilizer, 40-60 parts of lysate, acidulant 0.3-
1.0 parts, 2-3 parts of bleeding agent；The stabilizer uses acetic acid acetone, and the lysate uses ethyl acetate or isopropanol, described
Acidulant uses fatty alcohol polyoxyethylene ether using one of acetic acid, hydrochloric acid or sulfuric acid, bleeding agent；
Soaking time in the step 7 is 12-18min, and the temperature of boiling is 100-120 DEG C, and number is 2-10 times.
2. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the formula in the step 1 is ammonium tungstate 6-10 parts, 1-3 parts of tungsten chloride, alkaline solution 30-50
Part, 2-4 parts of nanometer foaming agent；The alkaline solution uses sodium hydroxide solution or potassium hydroxide solution, the nanometer foaming
Agent uses nano-calcium carbonate hydrogen sodium.
3. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the formula in the step 3 is inorganic modifier 1-3 parts, 3-5 parts of organic metal modifying agent, ethyl alcohol
20-25 parts of aqueous solution, ethanol content is 50-70% in the ethanol water；The inorganic modifier uses silica or carbon
SiClx, the organic metal modifying agent use acrylic tin or isopropyl alcohol radical nickel.
4. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the soaking time in the step 4 is 11-20min, and the baking oven drying temperature is 90-110 DEG C,
Drying time is 20-40min.
5. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the rapid cooling in the step 5 uses air-cooled technology, and the flow velocity of the rapid cooling is 5-
15mL/min。
6. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the high temperature sintering temperature in the step 6 is 250-320 DEG C, sintering time 2-4h.
7. a kind of system of organic superlattices anatase titanium dioxide titanizing tungsten oxide film infra-red sensitive material according to claim 1
Preparation Method, which is characterized in that the annealing in the step 8 is that 120-400 DEG C is heated under 20-35MPa pressure.
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| CN101757907A (en) * | 2008-12-26 | 2010-06-30 | 晶锐瓷业（北京）有限公司 | Titanium dioxide powder containing tungsten for preparing honeycomb SCR DeNOx catalyst and preparation method thereof |
| CN103646989A (en) * | 2013-11-27 | 2014-03-19 | 华东师范大学 | Preparation method of a p-n type Cu2O/TiO2 nanowire array composite film |
| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
| CN105789352A (en) * | 2016-03-24 | 2016-07-20 | 上海交通大学 | Tungsten trioxide/titanium dioxide nano heterojunction thin film and preparation and application thereof |
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| CN101757907A (en) * | 2008-12-26 | 2010-06-30 | 晶锐瓷业（北京）有限公司 | Titanium dioxide powder containing tungsten for preparing honeycomb SCR DeNOx catalyst and preparation method thereof |
| CN103646989A (en) * | 2013-11-27 | 2014-03-19 | 华东师范大学 | Preparation method of a p-n type Cu2O/TiO2 nanowire array composite film |
| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
| CN105789352A (en) * | 2016-03-24 | 2016-07-20 | 上海交通大学 | Tungsten trioxide/titanium dioxide nano heterojunction thin film and preparation and application thereof |
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