CN106512985B - A kind of ZnO/WO3The synthetic method of heterojunction array - Google Patents
A kind of ZnO/WO3The synthetic method of heterojunction array Download PDFInfo
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002073 nanorod Substances 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004246 zinc acetate Substances 0.000 claims abstract description 11
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 5
- 229940043237 diethanolamine Drugs 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- -1 alkene imines Chemical class 0.000 claims 1
- 229920002873 Polyethylenimine Polymers 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000011787 zinc oxide Substances 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000007704 transition Effects 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B01J35/39—
Abstract
The invention discloses a kind of ZnO/WO3The synthetic method of heterojunction array, specific steps are as follows: (1) ZnO crystal seed is grown in FTO substrate；(2) FTO for covering ZnO crystal seed is put into the container of the mixed aqueous solution equipped with zinc acetate, polyethyleneimine and urotropine, and oil bath heating reacts to obtain the FTO that growth has ZnO nano-rod array；(3) FTO that growth has ZnO nano-rod array is placed in the hydrothermal reaction kettle of the alcohol-water mixed solution equipped with ammonium paratungstate, concentrated hydrochloric acid solution and hydrogen peroxide, ZnO/WO is made in hydro-thermal reaction3Heterojunction array.Synthetic method craft of the invention is simple, environmental-friendly, is conducive to be mass produced.
Description
Technical field
The invention belongs to the synthesis technical fields of composite nano materials, and in particular to a kind of ZnO/WO3Heterojunction array
Synthetic method.
Background technique
Energy and environmental problem is the important bottleneck of current limitation society and development in science and technology, therefore exploitation is received based on semiconductor
The new energy materials of rice material cause the extensive concern of researcher.Such as TiO2、WO3, ZnO and SnO2Etc. a variety of semiconductor materials
For the photoelectric conversions electronic device such as solar battery, photoelectrocatalysis, the conversion of solar energy to electrical and chemical energy is realized, it is right
In solving, traditional fossil energy is insufficient and environmental problem has far-reaching theory and practice meaning.
ZnO is cheap, and raw material sources are extensive, electron mobility with higher, is widely used in photocatalytic degradation dirt
Contaminate the multiple fields such as object, photolysis water hydrogen and solar battery.But ZnO is wide band gap semiconducter, it can only be using in sunlight
Ultraviolet portion, and ultraviolet light only accounts for the 3%-4% of solar spectrum, significantly limits ZnO to the utilization efficiency of sunlight.For
ZnO is improved to the capture rate of sunlight, generally use element doping, quantum dot sensitized, plasma metal-modified and with it is narrow
Gap semiconductor is compounded to form the methods of heterogeneous section.WO3Band gap be 2.4eV, with ZnO it is compound after can widen to sunlight
Response range, and WO3II type semiconductor can be formed with ZnO, and light induced electron is from WO3Conduction band transitions to ZnO2Conduction band,
Photohole stays in valence band, is conducive to the separation of photogenerated charge, for improving ZnO/WO3Photocatalysis and PhotoelectrocatalytiPerformance Performance have
Vital meaning.
The patent of Publication No. CN103071482A discloses a kind of utilization ball-milling method preparation ZnO/WO3The method of powder,
ZnO/WO made from this method3Powder photocatalytic activity increases compared with ZnO, but ZnO/WO3Powder is as optoelectronic pole
When due to a large amount of crystal boundaries presence, cause the combined efficiency of photogenerated charge to improve, as optical electro-chemistry decompose water optoelectronic pole when
Performance will receive influence.And ZnO/WO3In heterojunction array, one-dimensional ZnO nano-rod array is conducive to the transmission of photogenerated charge,
WO3Hetero-junctions can be improved to the capture rate of incident light and improve injection efficiency of the light induced electron to ZnO, improve ZnO/WO3
The photoelectric catalytically active of heterojunction array.Therefore, heterojunction structure nano material ZnO/WO is designed3Light can be improved as light anode
Anode is to the utilization efficiency of incident light and the separative efficiency of photo-generate electron-hole, photocatalysis efficiency with higher.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of easy and impregnated using crystal seed and two step hydro-thermal process
ZnO/WO3The synthetic method of heterojunction array.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of ZnO/WO3The synthesis of heterojunction array
Method, it is characterised in that specific steps are as follows:
(1) 6.585g zinc acetate stirring to solution is added in 100mL ethyl alcohol to clarify, add 3mL diethanol amine after
It is continuous to stir to get precursor solution, electro-conductive glass is immersed in precursor solution, takes out and naturally dry obtains covering ZnO crystalline substance
The electro-conductive glass of kind；
(2) electro-conductive glass for the covering ZnO crystal seed that step (1) obtains is placed in equipped with 0.5488g zinc acetate, 0.0517g
In the container of polyethyleneimine, 0.3505g urotropine and 100mL deionized water, in 80-110 DEG C of oil bath heating 1-
10h, cooled to room temperature, naturally dry after taking out sample clean completely, obtaining growth in 500 DEG C of annealing 2h has ZnO nano
The electro-conductive glass of stick array；
(3) 0.25g ammonium paratungstate is added in 25mL alcohol-water mixed solution, 0.5mL mass concentration, which is then added, is
The hydrogen peroxide that 37% hydrochloric acid solution and 0.5mL mass concentration is 30%, is poured into hydrothermal reaction kettle, after mixing evenly by step
(2) growth obtained has the electro-conductive glass of ZnO nano-rod array to be placed in above-mentioned hydrothermal reaction kettle, in 160 DEG C of hydro-thermal reaction 1-
4h, cooled to room temperature, naturally dry after taking out sample clean completely obtain ZnO/WO in 400 DEG C of calcining 2h3Hetero-junctions battle array
Column.
Further preferably, the volume ratio of ethyl alcohol and water is 1/2-2 in alcohol-water mixed solution described in step (3).
The present invention is impregnated using crystal seed and two one-step hydrothermals have synthesized ZnO/WO3Heterojunction array, WO3With relative narrower
Band gap, the capture range to sunlight, ZnO and WO can be widened3Can also play synergistic effect, improve electron-hole
Pair separative efficiency, and then improve the efficiency of photochemical catalyzing, and the synthetic method craft is simple, environmental-friendly, favorably
In large-scale production.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope picture of ZnO nano-rod array made from the embodiment of the present invention 1；
Fig. 2 is ZnO/WO made from the embodiment of the present invention 13The field emission scanning electron microscope picture of heterojunction array.
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
(1) 6.585g zinc acetate is added in 100mL ethanol solution and stirs 2h, added 3mL diethanol amine and continue to stir
2h is mixed, precursor solution is obtained, electro-conductive glass (FTO) is immersed in 30min in precursor solution, obtains covering ZnO crystal seed
FTO；
(2) 0.5488g zinc acetate and 0.0517g polyethyleneimine are added in 100mL deionized water and are stirred in ice bath
30min is mixed, 0.3505g urotropine is then added and continues to stir 30min, the covering ZnO for finally obtaining step (1)
The FTO of crystal seed is placed in above-mentioned solution, in 80 DEG C of oil bath heating 10h, cooled to room temperature, take out sample clean it is clean after from
It so dries, is subsequently placed in Muffle furnace the 2h that anneals in 500 DEG C and obtains the FTO that growth has ZnO nano-rod array；
(3) 0.25g ammonium paratungstate is added in the acetic acid and water mixed solution that 25mL volume ratio is 1:1, stirs 10min,
Then the concentrated hydrochloric acid solution that 0.5mL mass concentration is 37% is added, continues to stir 1h, adding 0.5mL mass concentration is 30%
Hydrogen peroxide continues to stir 1h, forms uniform mixed solution, the growth that step (2) is obtained has the FTO of ZnO nano-rod array
It is placed in the hydrothermal reaction kettle of 50mL, is then transferred to above-mentioned mixed solution in hydrothermal reaction kettle in 160 DEG C of hydro-thermal reaction 1h, most
Obtained ZnO/WO eventually3Heterojunction array.
Fig. 1 is the field emission scanning electron microscope picture for the ZnO nano-rod array that the present embodiment first step hydro-thermal reaction obtains, from
It can be seen that the top of ZnO nanorod shows hexagon in figure, illustrate that ZnO has hexagonal structure.Fig. 2 is the ZnO/ of preparation
WO3The field emission scanning electron microscope picture of heterojunction array, the as seen from the figure WO of sheet3It is grown on ZnO nanorod and forms hetero-junctions
Structure.
Embodiment 2
(1) 6.585g zinc acetate is added in 100mL ethanol solution and stirs 2h, added 3mL diethanol amine and continue to stir
2h is mixed, precursor solution is obtained, FTO is immersed in 30min in precursor solution, obtains the FTO with ZnO crystal seed；
(2) 0.5488g zinc acetate and 0.0517g polyethyleneimine are added in 100mL deionized water and are stirred in ice bath
30min is mixed, 0.3505g urotropine is then added and continues to stir 30min, finally there is ZnO by what step (1) obtained
The FTO of crystal seed is placed in above-mentioned solution in 95 DEG C of oil bath heating 5h, cooled to room temperature, and it is clean rear natural to take out sample clean
It dries, is subsequently placed in Muffle furnace and obtains the FTO that growth has ZnO nano-rod array in 500 DEG C of calcining 2h；
(3) 0.25g ammonium paratungstate is added in the acetic acid and water mixed solution that 25mL volume ratio is 1:2, stirs 10min,
Then the concentrated hydrochloric acid solution that 0.5mL mass concentration is 37% is added, continues to stir 1h, adding 0.5mL mass concentration is 30%
Hydrogen peroxide continues to stir 1h, forms uniform mixed solution, the growth that step (2) is obtained has the FTO of ZnO nano-rod array
It is placed in the hydrothermal reaction kettle of 50mL, is then transferred to above-mentioned mixed solution in hydrothermal reaction kettle in 160 DEG C of hydro-thermal reaction 4h, most
Obtained ZnO/WO eventually3Heterojunction array.
Embodiment 3
(1) 6.585g zinc acetate is added in 100mL ethanol solution and stirs 2h, added 3mL diethanol amine and continue to stir
2h is mixed, precursor solution is obtained, FTO is immersed in 30min in precursor solution, obtains the FTO with ZnO crystal seed；
(2) 0.5488g zinc acetate and 0.0517g polyethyleneimine are added in 100mL deionized water and are stirred in ice bath
30min is mixed, 0.3505g urotropine is then added and continues to stir 30min, finally there is ZnO by what step (1) obtained
The FTO of crystal seed is placed in above-mentioned solution in 110 DEG C of oil bath heating 1h, cooled to room temperature, after taking out sample clean completely certainly
It so dries, is subsequently placed in Muffle furnace and obtains the FTO that growth has ZnO nano-rod array in 500 DEG C of calcining 2h；
(3) 0.25g ammonium paratungstate is added in the acetic acid and water mixed solution that 25mL volume ratio is 2:1, stirring
Then the concentrated hydrochloric acid solution that 0.5mL mass concentration is 37% is added in 10min, continue to stir 1h, adding 0.5mL mass concentration is
30% hydrogen peroxide continues to stir 1h, forms uniform mixed solution, the growth that step (2) obtains is had ZnO nano-rod array
FTO be placed in the hydrothermal reaction kettle of 50mL, then above-mentioned mixed solution is transferred in hydrothermal reaction kettle in 160 DEG C of hydro-thermal reactions
ZnO/WO is finally made in 2h3Heterojunction array.
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 (2)
1. a kind of ZnO/WO3The synthetic method of heterojunction array, it is characterised in that specific steps are as follows:
(1) 6.585g zinc acetate is added to stirring to solution in 100mL ethyl alcohol to clarify, adds 3mL diethanol amine and continues to stir
It mixes to obtain precursor solution, electro-conductive glass is immersed in precursor solution, take out and naturally dry obtains covering ZnO crystal seed
Electro-conductive glass；
(2) electro-conductive glass for the covering ZnO crystal seed that step (1) obtains is placed in equipped with 0.5488g zinc acetate, the poly- second of 0.0517g
In the container of alkene imines, 0.3505g urotropine and 100mL deionized water, in 80-110 DEG C of oil bath heating 1-10h,
Cooled to room temperature, naturally dry after taking out sample clean completely, obtaining growth in 500 DEG C of annealing 2h has ZnO nanorod battle array
The electro-conductive glass of column；
(3) 0.25g ammonium paratungstate is added in 25mL alcohol-water mixed solution, it is 37% that 0.5mL mass concentration, which is then added,
Hydrochloric acid solution and 0.5mL mass concentration be 30% hydrogen peroxide, pour into hydrothermal reaction kettle after mixing evenly, by step (2)
To the growth electro-conductive glass that has ZnO nano-rod array be placed in above-mentioned hydrothermal reaction kettle, in 160 DEG C of hydro-thermal reaction 1-4h, from
It is so cooled to room temperature, naturally dry after taking out sample clean completely obtains ZnO/WO in 400 DEG C of calcining 2h3Heterojunction array.
2. ZnO/WO according to claim 13The synthetic method of heterojunction array, it is characterised in that: described in step (3)
The volume ratio of ethyl alcohol and water is 1/2-2 in alcohol-water mixed solution.
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| CN108187660A (en) * | 2018-01-22 | 2018-06-22 | 新疆大学 | A kind of method that liquid phase prepares witch culture zinc oxide nanosphere |
| CN109030578A (en) * | 2018-07-30 | 2018-12-18 | 清华大学 | A kind of NO based on the nano heterogeneous junction structure of CdTe/ZnO2The preparation method of gas sensor |
| CN110354863A (en) * | 2019-06-28 | 2019-10-22 | 广东工业大学 | A kind of tungstic acid/di-iron trioxide composite photo-catalyst and its preparation method and application |
| CN110776020B (en) * | 2019-11-20 | 2022-01-21 | 江苏师范大学 | NiMnO of stick equipment3Method for synthesizing nanoflower |
| CN111293304A (en) * | 2020-02-19 | 2020-06-16 | 湖北大学 | Carbon fiber-zinc oxide nanorod composite material and preparation method and application thereof |
| CN113652104B (en) * | 2021-09-03 | 2022-03-01 | 华东理工大学 | Heterojunction type metal anti-corrosion pigment |
| CN114700093B (en) * | 2022-05-10 | 2023-06-23 | 北方民族大学 | Photocatalytic material for degrading tetracycline in wastewater and preparation method thereof |
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| CN105347387A (en) * | 2015-12-01 | 2016-02-24 | 安徽大学 | Preparation method for Au-Ag co-modified N-doped ZnO nanorods and application of ZnO nanorods to hydrogen production through photo-electrochemical hydrolysis |
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| CN105347387A (en) * | 2015-12-01 | 2016-02-24 | 安徽大学 | Preparation method for Au-Ag co-modified N-doped ZnO nanorods and application of ZnO nanorods to hydrogen production through photo-electrochemical hydrolysis |
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