CN108014784A - A kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film and preparation method thereof - Google Patents
A kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film and preparation method thereof Download PDFInfo
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- CN108014784A CN108014784A CN201711066450.0A CN201711066450A CN108014784A CN 108014784 A CN108014784 A CN 108014784A CN 201711066450 A CN201711066450 A CN 201711066450A CN 108014784 A CN108014784 A CN 108014784A
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- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 38
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 23
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000004544 sputter deposition Methods 0.000 claims abstract description 9
- 238000005530 etching Methods 0.000 claims abstract description 4
- 238000003384 imaging method Methods 0.000 claims abstract description 4
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 4
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 4
- 238000000137 annealing Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 42
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000002061 nanopillar Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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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
- 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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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The present invention provides a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film and preparation method thereof, including substrate layer, porous ZnO film layer, metal nanoparticle, using ZnO on substrate layer vacuum thermal evaporation layer of ZnO film, then the heating anneal in chamber type electric resistance furnace, and the spin coating photoresist on the ZnO film for obtain crystalline state, exposure imaging, obtain the pattern for the hole for needing to etch, then the ZnO film of acetum etching crystalline state, obtain porous ZnO film layer, and one layer of metallic film is sputtered on it, so as to obtain metal nanoparticle；The present invention is applied widely, preparation process is simple, manufacturing cost is low, by the photocatalytic degradation efficiency on the surface of ZnO film and hole splash-proofing sputtering metal nano-particle, being conducive to improve ZnO film；The area of catalysis is added additionally by hole, and empty controlled shape is strong, further increases the catalytic efficiency of ZnO film.
Description
Technical field
The present invention relates to a kind of photocatalytic degradation thin film technique field, especially a kind of metal nanoparticle enhancing is porous
ZnO photocatalytic degradation films and preparation method thereof.
Background technology
With the raising that people live, the demand of color is also continuously improved in people, and then dyestuff is meeting us to face
While the demand of color, serious problem of environmental pollution is also brought；
Nanometer photocatalyst film technology is a kind of green technology of new and effective degradation of organic substances waste water.Wherein, half
The major advantage of conductor nanometer photocatalyst film technology is：Oxidability is strong, treatment effeciency is high, energy consumption is relatively low, reaction condition
Gently, non-secondary pollution, most of toxic organic compound exhaustive oxidations that is difficult to or cannot degrade can at normal temperatures decomposed, be easy to
It is applied in industrial organic waste water processing.In numerous semiconductor light-catalysts, the anatase structured TiO of tetragonal crystal system2With
The ZnO of hexagonal crystal system wurtzite structure, and WO3All it is more satisfactory semiconductor light-catalyst material Deng semi-conducting material,
They have fast catalytic activity height, reaction rate, the degraded non-selectivity to organic matter and the spy that can be allowed to exhaustive oxidation decomposition
Point, thus have a good application prospect in degradation of organic substances waste water.
In order to improve the catalytic efficiency of ZnO semi-conducting materials, the prior art usually utilizes the catalysis of nanometer technology enhancing ZnO
Efficiency, for example, nano-pillar ZnO, nano wire ZnO, Nanoparticle Modified ZnO film etc..In addition, also some investigators utilize
It is micro-/to receive organic ball and electrochemical plating method prepares porous ZnO film.However, there are complex process, controllability by nano-pillar/line ZnO
The shortcomings of poor, and there is the shortcomings of pollution, controllability is poor in electrochemical plating, and it is relatively inefficient.Thus, it is necessary to develop one
Kind controllability is good, technique is simple, the preparation method of high catalytic efficiency ZnO.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of metal nanoparticle with good photocatalytic degradation
Strengthen porous ZnO photocatalytic degradation film and preparation method thereof.
The technical scheme is that：A kind of metal nanoparticle strengthens porous ZnO photocatalytic degradation film, including substrate
Layer, porous ZnO film layer, metal nanoparticle, grow porous ZnO film layer, in porous ZnO film on the substrate layer
Clad metal nano particle in layer surface.
Further, the thickness of the porous ZnO film layer is 100-3500nm.
Further, a diameter of 2-20nm of the metal nanoparticle.
Further, the metal that splash-proofing sputtering metal nano-particle uses is any one in Ag, Pt, Ni, Fe.
The present invention also provides a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film preparation method, specifically
Comprise the following steps：
S1), hot evaporation electric current be 100-200A, vacuum be 1~9 × 10-4Under conditions of Pa, it is more than using purity
99.99% ZnO vacuum thermal evaporation layer of ZnO films on the substrate layer cleaned up, the then 300- in chamber type electric resistance furnace
700 DEG C of annealing 30-120min, obtain the ZnO film of crystalline state；
S2), the spin coating photoresist on crystalline state ZnO film, exposure imaging, acquisition need the pattern of the hole etched, so
The acetum etching crystalline state ZnO film 0.5-20min of 0.05-1mL is used afterwards, obtains the porous of regularly arranged crystalline state
ZnO film layer；
S3 one layer of metallic film), is sputtered on the porous ZnO film layer of crystalline state using sputter, wherein, sputtering current
For 8-20mA, vacuum 1~9 × 10-2Pa, then in a vacuum furnace 600-900 DEG C annealing 30-120s so that in the more of crystalline state
Metal nanoparticle is obtained on the surface of hole ZnO film layer and the wall of hole.
In above-mentioned technical proposal, step S2) in, the thickness of the porous ZnO film layer is 100-3500nm.
In above-mentioned technical proposal, step S2) in, the hole shape of the porous crystalline state ZnO film layer can be square hole, length
Any one or a few in square hole, round hole or polygonal hole.
In above-mentioned technical proposal, step S3) in, a diameter of 2-20nm of the metal nanoparticle.
In above-mentioned technical proposal, step S3) in, the splash-proofing sputtering metal that the metallic film uses is in Ag, Pt, Ni, Fe
Any one.
Beneficial effects of the present invention are：It is applied widely, preparation process is simple, manufacturing cost is low, by ZnO film
Surface and hole splash-proofing sputtering metal nano-particle, are conducive to improve the photocatalytic degradation efficiency of ZnO film；Increase additionally by hole
The area of catalysis, and empty controlled shape is strong, further increases the catalytic efficiency of ZnO film.
Brief description of the drawings
Fig. 1 is the structure diagram of porous ZnO photocatalytic degradation film prepared by the embodiment of the present invention.
In figure, 1- substrate layers, 2- porous ZnO film layers, 3- metal nanoparticles.
Embodiment
The embodiment of the present invention is described further below in conjunction with the accompanying drawings：
As shown in Figure 1, a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film, including it is substrate layer 1, porous
ZnO film layer 2, metal nanoparticle 3, grow the porous ZnO film layer that a layer thickness is 1500nm on the substrate layer 1
2, the metal nanoparticle 3 of a diameter of 10nm, the metallic nanoparticle are evenly distributed with 2 surface of porous ZnO film layer
Son 3, the metal nanoparticle can be Ag nanoparticle layers, Ni nanoparticle layers, Fe nanoparticle layers, be preferably that Pt receives
Rice corpuscles.
A kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film, comprises the following steps：
S1), hot evaporation electric current be 130A, vacuum be 5 × 10-4Under conditions of Pa, using purity more than 99.99%
The ZnO film that ZnO vacuum thermal evaporation a layer thickness on the substrate layer 1 cleaned up is 1500nm, then in chamber type electric resistance furnace
Middle 300-700 DEG C of annealing 30-120min, obtains the ZnO film of crystalline state；
S2), the spin coating photoresist on the ZnO film of crystalline state, exposure imaging, acquisition need the pattern of the hole etched,
Then the ZnO film 5min of the acetum etching crystalline state of 0.5mL is used, obtains the porous ZnO of regularly arranged crystalline state
Film layer 2；
S3 sputter), is used to sputter Pt films of a layer thickness for 10nm on the porous ZnO film layer 2 of crystalline state, its
In, sputtering current 10mA, vacuum 8 × 10-2Pa, then in a vacuum furnace 800 DEG C annealing 30s so that in the porous of crystalline state
Pt nano-particles are obtained on the surface of ZnO film layer 2 and the wall of hole.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this
On the premise of spirit and scope, various changes and modifications of the present invention are possible, these changes and improvements both fall within requirement and protect
In the scope of the invention of shield.
Claims (9)
1. a kind of metal nanoparticle strengthens porous ZnO photocatalytic degradation film, it is characterised in that：Including substrate layer, porous ZnO
Film layer, metal nanoparticle, porous ZnO film layer is grown on the substrate layer, is wrapped in porous ZnO film layer surface
It is covered with metal nanoparticle.
2. a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 1, its feature exist
In：The thickness of the porous ZnO film layer is 100-3500nm.
3. a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 1, its feature exist
In：A diameter of 2-20nm of the metal nanoparticle.
4. a kind of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 1, its feature exist
In：The metal that splash-proofing sputtering metal nano-particle uses is any one in Ag, Pt, Ni, Fe.
5. a kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 1,
It is characterised in that it includes following steps：
S1), hot evaporation electric current be 100-200A, vacuum be 1~9 × 10-4Under conditions of Pa, it is more than 99.99% using purity
ZnO on the substrate layer cleaned up vacuum thermal evaporation layer of ZnO film, then in chamber type electric resistance furnace 300-700 DEG C move back
Fiery 30-120min, obtains the ZnO film of crystalline state；
S2), the spin coating photoresist on crystalline state ZnO film, exposure imaging, obtains the pattern for the hole for needing to etch, then adopts
With the acetum etching crystalline state ZnO film 0.5-20min of 0.05-1mL, the porous ZnO of regularly arranged crystalline state is obtained
Film layer；
S3 one layer of metallic film), is sputtered on the porous ZnO film layer of crystalline state using sputter, wherein, sputtering current 8-
20mA, vacuum 1~9 × 10-2Pa, then in a vacuum furnace 600-900 DEG C annealing 30-120s so that in the porous ZnO of crystalline state
Metal nanoparticle is obtained on the surface of film layer and the wall of hole.
6. a kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 5,
It is characterized in that：Step S2) in, the thickness of the porous ZnO film layer is 100-3500nm.
7. a kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 5,
It is characterized in that：Step S2) in, the hole shape of the porous crystalline state ZnO film layer can be square hole, slot, circle
Any one or a few in hole or polygonal hole.
8. a kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 5,
It is characterized in that：Step S3) in, a diameter of 2-20nm of the metal nanoparticle.
9. a kind of preparation method of metal nanoparticle enhancing porous ZnO photocatalytic degradation film according to claim 5,
It is characterized in that：Step S3) in, the splash-proofing sputtering metal that the metallic film uses is any one in Ag, Pt, Ni, Fe.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956714A (en) * | 2018-06-29 | 2018-12-07 | 五邑大学 | ZnO/Si Nano/micron column array sensitive material and preparation method thereof and sensor |
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| CN1400674A (en) * | 2002-08-05 | 2003-03-05 | 浙江大学 | Preparation method of zinc oxide UV photodetector prototype device |
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| US20150182950A1 (en) * | 2013-12-31 | 2015-07-02 | Industrial Technology Research Institute | Photocatalytic film structure |
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2017
- 2017-11-02 CN CN201711066450.0A patent/CN108014784A/en active Pending
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| CN1400674A (en) * | 2002-08-05 | 2003-03-05 | 浙江大学 | Preparation method of zinc oxide UV photodetector prototype device |
| CN102476823A (en) * | 2010-11-23 | 2012-05-30 | 国家纳米科学中心 | Zinc oxide micro-nano array and preparation method thereof |
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Application publication date: 20180511 |