CN109046402A - A kind of BiOBr/TiO2The preparation method of composite photoelectric film material - Google Patents
A kind of BiOBr/TiO2The preparation method of composite photoelectric film material Download PDFInfo
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- CN109046402A CN109046402A CN201810779369.5A CN201810779369A CN109046402A CN 109046402 A CN109046402 A CN 109046402A CN 201810779369 A CN201810779369 A CN 201810779369A CN 109046402 A CN109046402 A CN 109046402A
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- 239000000463 material Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010409 thin film Substances 0.000 claims abstract description 30
- 239000010408 film Substances 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000020477 pH reduction Effects 0.000 claims abstract description 7
- 229960003431 cetrimonium Drugs 0.000 claims abstract description 6
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000005622 photoelectricity Effects 0.000 description 3
- 206010070834 Sensitisation Diseases 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Hybrid Cells (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of BiOBr/TiO2The preparation method of composite photoelectric film material is that titanium source hydro-thermal reaction in hydrochloric acid solution prepares TiO using butyl titanate2Nano-stick array thin film, by TiO2Nano-stick array thin film acidification in sulfuric acid solution；Polyvinylpyrrolidone and bismuth nitrate are dispersed in ethylene glycol solution, cetrimonium bronmide is added and are uniformly mixed, is transferred to the TiO of acidification in autoclave simultaneously2Nano-stick array thin film is put into autoclave, and in 160 DEG C of reaction 30min, cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains BiOBr/TiO after the reaction was completed2Composite photoelectric film material.BiOBr/TiO produced by the present invention2The catalyst that composite photoelectric film material is reacted as optical electro-chemistry can significantly improve the capture ability to incident light, improve service life and transmission and the separative efficiency of photo-generated carrier, and then improve photoelectric conversion efficiency.
Description
Technical field
The invention belongs to the synthesis technical fields of composite photoelectric film material, and in particular to a kind of BiOBr/TiO2Complex light
The preparation method of conductive film material.
Background technique
TiO2It is widely applied due to the features such as its physicochemical properties is stable, source material is from a wealth of sources, environmental-friendly
Photocatalysis, photoelectrocatalysis catalyst.But TiO2Band gap be 3.4eV, the ultraviolet light in sunlight can only be absorbed, and ultraviolet
Light only accounts for the 5% of sunlight, and most visible light and infrared light cannot utilize.In order to improve TiO2Nano-stick array thin film pair
The capture ability of incident light is usually repaired using element doping, narrow gap semiconductor sensitization, dye sensitization and plasma resonance metal
The methods of decorations.In photronic research, the photocell activity for the diode structure being made of N-shaped and P-type semiconductor is significantly high
In single semiconductor form, because the structure is conducive to separation of charge.Therefore in order to further promote electron hole mobility, press down
Back reaction processed improves the separative efficiency of photo-generated carrier, and the photocatalytic activity for improving photochemical catalyst passes through p-n junction composite construction
Design can effectively improve photocatalytic activity, be the effective way for designing high efficiency photocatalyst.
BiOBr is a kind of novel p-type semiconductor material, has unique electronic structure, good optical property and catalysis
Performance.The band gap width of BiOBr is ~ 2.7eV, has good absorption in visible region, and have the characteristics that it is less toxic, cheap,
It has a good application prospect in field of photovoltaic materials.BiOBr/TiO2Photo-generated carrier can be improved in composite photoelectric film material
Separative efficiency, to improve the photocatalytic activity of catalyst, however the still not no relevant report of this aspect at present.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple, quickly and the BiOBr/TiO that is easy to commercially produce2
The preparation method of composite photoelectric film material, composite photoelectric film material made from this method can significantly improve the photoelectricity of device
Transfer efficiency.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of BiOBr/TiO2Composite photoelectric film material
The preparation method of material, it is characterised in that specific steps are as follows:
Step S1: by deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is stirred
It is even to obtain clear solution A, solution A is transferred in autoclave to while being put into a piece of electro-conductive glass, in 150 DEG C of reaction 20h,
Cooled to room temperature after the reaction was completed, clean, dry after obtain TiO2Nano-stick array thin film；
Step S2: the TiO that step S1 is obtained2Nano-stick array thin film is put into the sulfuric acid solution that molar concentration is 1mol/L,
It takes out after the completion of 60 DEG C of immersion treatment 2h, processing and is rinsed with deionized water and remove what extra sulfuric acid solution was acidified
TiO2Nano-stick array thin film；
Step S3: 0.1 ~ 0.5g polyvinylpyrrolidone and 0.7 ~ 4.2g bismuth nitrate are dispersed in 10mL ethylene glycol solution
In, it adds 1.6 ~ 8.2g cetrimonium bronmide and is uniformly mixed to obtain solution B, solution B is transferred to high pressure
Simultaneously by the TiO of the obtained acidification of step S2 in reaction kettle2Nano-stick array thin film is put into autoclave, anti-in 160 DEG C
30min is answered, after the reaction was completed cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains
BiOBr/TiO2Composite photoelectric film material.
Compared with the prior art, the invention has the following beneficial effects:
1, BiOBr/TiO produced by the present invention2The catalyst that composite photoelectric film material is reacted as optical electro-chemistry, can be significant
The service life for improving photo-generated carrier to the capture ability of incident light and transmission and separative efficiency are improved, and then improves photoelectricity and turns
Change efficiency；
2, BiOBr/TiO produced by the present invention2Composite photoelectric film material is synthesized using liquid phase method, and preparation process is simple, cost
Cheap and energy consumption is lower.
Detailed description of the invention
A is that TiO is made in embodiment 1 in Fig. 12The scanning electron microscope (SEM) photograph of nano-stick array thin film, b is made for embodiment 2 in Fig. 1
BiOBr/TiO2The scanning electron microscope (SEM) photograph of composite photoelectric film material；
Fig. 2 is that TiO is made in Examples 1 and 22Nano-stick array thin film and BiOBr/TiO2The photoelectricity of composite photoelectric film material
Stream-voltage curve, as the result is shown BiOBr/TiO2Composite photoelectric film material is compared to TiO2Nano-stick array thin film, photoelectric current
Density significantly improves；
Fig. 3 is that TiO is made in Examples 1 and 22Nano-stick array thin film and BiOBr/TiO2The electrochemistry of composite photoelectric film material
Impedance Bode schemes, as the result is shown BiOBr/TiO2Composite photoelectric film material is compared to TiO2Nano-stick array thin film, resistance are significant
It reduces, illustrates BiOBr/TiO2Composite photoelectric film material be conducive to the transmission of photogenerated charge with separate.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
By deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is uniformly mixed to obtain
Solution A is transferred in autoclave while being put into a piece of electro-conductive glass (FTO) by clear solution A, in 150 DEG C of reaction 20h,
Cooled to room temperature after the reaction was completed, clean, dry after obtain TiO2Nano-stick array thin film.
Embodiment 2
Step S1: by deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is stirred
It is even to obtain clear solution A, solution A is transferred in autoclave while being put into a piece of electro-conductive glass (FTO), it is anti-in 150 DEG C
Answer 20h, after the reaction was completed cooled to room temperature, clean, dry after obtain TiO2Nano-stick array thin film；
Step S2: the TiO that step S1 is obtained2Nano-stick array thin film is put into the sulfuric acid solution that molar concentration is 1mol/L,
It takes out after the completion of 60 DEG C of immersion treatment 2h, processing and is rinsed with deionized water and remove what extra sulfuric acid solution was acidified
TiO2Nano-stick array thin film；
Step S3: 0.1g polyvinylpyrrolidone and 0.7g bismuth nitrate are dispersed in 10mL ethylene glycol solution, added
1.6g cetrimonium bronmide simultaneously is uniformly mixed to obtain solution B, and solution B is transferred in autoclave while being incited somebody to action
The TiO for the acidification that step S2 is obtained2Nano-stick array thin film is put into autoclave, in 160 DEG C of reaction 30min, has been reacted
At rear cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains BiOBr/TiO2Complex light
Conductive film material.
Embodiment 3
Step S1: by deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is stirred
It is even to obtain clear solution A, solution A is transferred in autoclave while being put into a piece of electro-conductive glass (FTO), it is anti-in 150 DEG C
Answer 20h, after the reaction was completed cooled to room temperature, clean, dry after obtain TiO2Nano-stick array thin film；
Step S2: the TiO that step S1 is obtained2Nano-stick array thin film is put into the sulfuric acid solution that molar concentration is 1mol/L,
It takes out after the completion of 60 DEG C of immersion treatment 2h, processing and is rinsed with deionized water and remove what extra sulfuric acid solution was acidified
TiO2Nano-stick array thin film；
Step S3: 0.2g polyvinylpyrrolidone and 1.4g bismuth nitrate are dispersed in 10mL ethylene glycol solution, added
3.2g cetrimonium bronmide simultaneously is uniformly mixed to obtain solution B, and solution B is transferred in autoclave while being incited somebody to action
The TiO for the acidification that step S2 is obtained2Nano-stick array thin film is put into autoclave, in 160 DEG C of reaction 30min, has been reacted
At rear cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains BiOBr/TiO2Complex light
Conductive film material.
Embodiment 4
Step S1: by deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is stirred
It is even to obtain clear solution A, solution A is transferred in autoclave while being put into a piece of electro-conductive glass (FTO), it is anti-in 150 DEG C
Answer 20h, after the reaction was completed cooled to room temperature, clean, dry after obtain TiO2Nano-stick array thin film；
Step S2: the TiO that step S1 is obtained2Nano-stick array thin film is put into the sulfuric acid solution that molar concentration is 1mol/L,
It takes out after the completion of 60 DEG C of immersion treatment 2h, processing and is rinsed with deionized water and remove what extra sulfuric acid solution was acidified
TiO2Nano-stick array thin film；
Step S3: 0.5g polyvinylpyrrolidone and 4.2g bismuth nitrate are dispersed in 10mL ethylene glycol solution, added
8.2g cetrimonium bronmide simultaneously is uniformly mixed to obtain solution B, and solution B is transferred in autoclave while being incited somebody to action
The TiO for the acidification that step S2 is obtained2Nano-stick array thin film is put into autoclave, in 160 DEG C of reaction 30min, has been reacted
At rear cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains BiOBr/TiO2Complex light
Conductive film material.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (1)
1. a kind of BiOBr/TiO2The preparation method of composite photoelectric film material, it is characterised in that specific steps are as follows:
Step S1: by deionized water and commercially available concentrated hydrochloric acid in equal volume than butyl titanate is added after mixing and is stirred
It is even to obtain clear solution A, solution A is transferred in autoclave to while being put into a piece of electro-conductive glass, in 150 DEG C of reaction 20h,
Cooled to room temperature after the reaction was completed, clean, dry after obtain TiO2Nano-stick array thin film；
Step S2: the TiO that step S1 is obtained2Nano-stick array thin film is put into the sulfuric acid solution that molar concentration is 1mol/L, in
60 DEG C of immersion treatment 2h take out after the completion of processing and rinse the TiO for removing extra sulfuric acid solution and being acidified with deionized water2
Nano-stick array thin film；
Step S3: 0.1 ~ 0.5g polyvinylpyrrolidone and 0.7 ~ 4.2g bismuth nitrate are dispersed in 10mL ethylene glycol solution
In, it adds 1.6 ~ 8.2g cetrimonium bronmide and is uniformly mixed to obtain solution B, solution B is transferred to high pressure
Simultaneously by the TiO of the obtained acidification of step S2 in reaction kettle2Nano-stick array thin film is put into autoclave, anti-in 160 DEG C
30min is answered, after the reaction was completed cooled to room temperature, takes out sample and cleaned respectively with water, ethyl alcohol, then naturally dry obtains
BiOBr/TiO2Composite photoelectric film material.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113970583A (en) * | 2021-10-25 | 2022-01-25 | 齐齐哈尔大学 | Preparation and use methods of photoelectrochemical aptamer sensor for detecting kanamycin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752332A (en) * | 2014-01-22 | 2014-04-30 | 玉林师范学院 | Dried persimmon-shaped visible-light-driven photocatalyst BiOBr and preparation method thereof |
| CN103908972A (en) * | 2013-12-19 | 2014-07-09 | 嘉兴学院 | Recyclable BiOX/TiO2 composite photocatalyst and preparation method thereof |
| CN106540673A (en) * | 2016-09-20 | 2017-03-29 | 河南师范大学 | A kind of three-dimensional TiO2The synthetic method of/ZnO heterojunction array |
-
2018
- 2018-07-16 CN CN201810779369.5A patent/CN109046402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908972A (en) * | 2013-12-19 | 2014-07-09 | 嘉兴学院 | Recyclable BiOX/TiO2 composite photocatalyst and preparation method thereof |
| CN103752332A (en) * | 2014-01-22 | 2014-04-30 | 玉林师范学院 | Dried persimmon-shaped visible-light-driven photocatalyst BiOBr and preparation method thereof |
| CN106540673A (en) * | 2016-09-20 | 2017-03-29 | 河南师范大学 | A kind of three-dimensional TiO2The synthetic method of/ZnO heterojunction array |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113970583A (en) * | 2021-10-25 | 2022-01-25 | 齐齐哈尔大学 | Preparation and use methods of photoelectrochemical aptamer sensor for detecting kanamycin |
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Application publication date: 20181221 |