CN110252297A - A kind of gold nano grain-zinc-oxide nano cap array and preparation method thereof - Google Patents
A kind of gold nano grain-zinc-oxide nano cap array and preparation method thereof Download PDFInfo
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- CN110252297A CN110252297A CN201910556142.9A CN201910556142A CN110252297A CN 110252297 A CN110252297 A CN 110252297A CN 201910556142 A CN201910556142 A CN 201910556142A CN 110252297 A CN110252297 A CN 110252297A
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- zinc
- polystyrene microsphere
- oxide nano
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 229960001296 zinc oxide Drugs 0.000 title claims abstract description 91
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 91
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 67
- 239000010931 gold Substances 0.000 title claims abstract description 67
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000004793 Polystyrene Substances 0.000 claims abstract description 105
- 229920002223 polystyrene Polymers 0.000 claims abstract description 105
- 239000004005 microsphere Substances 0.000 claims abstract description 99
- 239000000758 substrate Substances 0.000 claims abstract description 62
- 239000002356 single layer Substances 0.000 claims abstract description 48
- 238000004544 sputter deposition Methods 0.000 claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 28
- 239000011701 zinc Substances 0.000 claims abstract description 28
- 239000010410 layer Substances 0.000 claims abstract description 26
- 238000000137 annealing Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011806 microball Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 71
- 239000011521 glass Substances 0.000 claims description 41
- 239000008367 deionised water Substances 0.000 claims description 39
- 229910021641 deionized water Inorganic materials 0.000 claims description 39
- 235000019441 ethanol Nutrition 0.000 claims description 32
- 239000000725 suspension Substances 0.000 claims description 27
- 238000002242 deionisation method Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000005477 sputtering target Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000013077 target material Substances 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- 238000001338 self-assembly Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 239000006228 supernatant Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 231100001261 hazardous Toxicity 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000003491 array Methods 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 20
- 239000011805 ball Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229920006389 polyphenyl polymer Polymers 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 241000549556 Nanos Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
-
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- B01J35/33—
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/347—Ionic or cathodic spraying; Electric discharge
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of gold nano grain-zinc-oxide nano cap arrays and preparation method thereof, using gas-liquid interface self-assembling technique in one strata phenylethylene micro ball of substrate upper berth, then one layer of zinc film is deposited on surface, it is very uniform that ingredient has been made after annealing in substrate, the orderly zinc-oxide nano cap array of queueing discipline, one layer of orderly aligned single layer polystyrene microsphere is covered in zinc-oxide nano cap array surface later, gold nano grain array has been made in zinc-oxide nano cap array surface using ion sputtering deposition method and thermal anneal process technology as template again, to obtain extremely uniform gold nano grain-zinc-oxide nano cap array.This composite construction can give full play to zinc-oxide nano cap to the absorption property and unique electronic transmission performance of specific hazardous organic molecule, the photocatalysis performance of the gold nano grain of zinc oxide surface is greatlyd improve, to greatly improve the light degradation property to hazardous organic molecule.
Description
Technical field
The present invention relates to hazardous organic molecule degradation technique field more particularly to a kind of gold nano grain-zinc-oxide nanos
Cap array and preparation method thereof.
Background technique
With the progress of science and technology and the raising of human living standard, the various non-renewable moneys such as coal, petroleum, natural gas
The demand in source is increasing, but these resources, during utilization, not only utilization efficiency is not high, but also unavoidably produces
Some wastes；Some pairs of life entities nocuousness are usually contained in these wastes and are not easy the organic molecule of natural degradation, thus
It is highly desirable to carry out degradation removing to these harmful organic molecules.
Currently, easily technology is to utilize noble metal nano particles (such as Pt, Au, Ag) under light irradiation for a kind of more environmental protection
Realize the light degradation of hazardous organic molecule, but for some organic point of nocuousness that do not adsorbed substantially with noble metal nano particles
Son, pure noble metal nano particles can not play preferable catalytic performance, improve the degradation rate of hazardous organic molecule.
Summary of the invention
For above-mentioned shortcoming in the prior art, the present invention provides a kind of gold nano grain-zinc-oxide nano caps
Array and preparation method thereof can give full play to zinc-oxide nano cap to specific molecular absorption property and unique electronic transporting
Can, greatly improve light degradation property of the gold nano grain to specific hazardous organic molecule of zinc oxide surface.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of gold nano grain-zinc-oxide nano cap array, comprising the following steps:
Step A, single layer polystyrene microsphere array is prepared in substrate using gas-liquid interface self-assembly method；
Step B, using the single layer polystyrene microsphere array as template, and using magnetron sputtering deposition method in the template table
Face deposits one layer of zinc film, then makes annealing treatment to the template for being deposited with zinc film, so that zinc-oxide nano cap array be made；
Step C, single layer polystyrene microsphere is made on the deionized water water surface, then uses and is loaded with zinc-oxide nano cap battle array
The substrate of column picks up single layer polystyrene microsphere from the deionized water water surface, is covered with single layer polystyrene microsphere to be made
Zinc-oxide nano cap array；
Step D, using the zinc-oxide nano cap array for being covered with single layer polystyrene microsphere as template, and ion is used
Sputtering method deposits one layer of golden film in the template surface, then makes annealing treatment to the template for being deposited with golden film, to make
Obtain gold nano grain-zinc-oxide nano cap array.
Preferably, single layer polystyrene microsphere array is prepared in substrate with gas-liquid interface self-assembly method includes following step
It is rapid:
Step A1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain table
The hydrophilic substrate of glass in face；Then deionized water is drawn with liquid-transfering gun, be then injected into the substrate of glass of surface hydrophilic, thus
Obtained surface is covered with the substrate of glass of deionization moisture film；
Step A2, taking polystyrene bulb diameter is the polystyrene microsphere suspension of 1000nm, and micro- according to polystyrene
Ball suspension: polystyrene microsphere suspension is mixed with ethyl alcohol, then carries out the ultrasound of 40min by ethyl alcohol=1.5:1 volume ratio
Oscillation treatment, so that finely dispersed polystyrene microsphere ethanol solution be made；
Step A3, the polystyrene microsphere ethanol solution is injected into the glass that the surface is covered with deionization moisture film
In substrate, and surfactant is added, is then transferred on the water surface of deionized water, to be made on the deionized water water surface single
Strata phenylethylene micro ball；
Step A4, single layer polystyrene microsphere is picked up from the deionized water water surface with substrate, to be made in substrate single
Strata phenylethylene micro ball array.
Preferably, it is described on the deionized water water surface be made single layer polystyrene microsphere the following steps are included:
Step C1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain table
The hydrophilic substrate of glass in face；Then deionized water is drawn with liquid-transfering gun, be then injected into the substrate of glass of surface hydrophilic, thus
Obtained surface is covered with the substrate of glass of deionization moisture film；
Step C2, taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 150nm, and micro- according to polystyrene
Ball suspension: polystyrene microsphere suspension is mixed with ethyl alcohol, then carries out the ultrasound of 40min by ethyl alcohol=1:1.5 volume ratio
Oscillation treatment, so that finely dispersed polystyrene microsphere ethanol solution be made；
Step C3, the polystyrene microsphere ethyl alcohol dilution is injected into the glass that the surface is covered with deionization moisture film
In glass substrate, and surfactant is added, is then transferred on the water surface of deionized water, to be made on the deionized water water surface
Single layer polystyrene microsphere.
Preferably, it includes: by the template that the use magnetron sputtering deposition method, which deposits one layer of zinc film in the template surface,
It is put into magnetic control sputtering device, selects zinc target as sputtering target material, setting vacuum degree is 30mtor, sputtering current 30mA, sputtering
Time is 6min, to deposit one layer of zinc film in the template surface.
Preferably, it includes: to be put into the template for being deposited with zinc film that the described pair of template for being deposited with zinc film, which carries out annealing,
In the crucible of Muffle furnace, setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, anneals naturally
Afterwards to get arrive zinc-oxide nano cap array.
Preferably, it includes: by the template that the use ion sputtering deposition method, which deposits one layer of golden film in the template surface,
It is put into ion sputtering instrument, selects gold target as sputtering target material, setting vacuum degree is 0.1mbar, sputtering current 30mA, sputtering
Time is 45~90s, to deposit one layer of golden film in the template surface.
Preferably, it includes: to be put into the template for being deposited with golden film that the described pair of template for being deposited with golden film, which carries out annealing,
In the crucible of Muffle furnace, setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, anneals naturally
Afterwards to get arrive gold nano grain-zinc-oxide nano cap array.
A kind of gold nano grain-zinc-oxide nano cap array, using above-mentioned gold nano grain-zinc-oxide nano cap array
Preparation method be prepared.
As seen from the above technical solution provided by the invention, gold nano grain-zinc oxide nano provided by the present invention
Rice cap array preparation method first with gas-liquid interface self-assembling technique in one strata phenylethylene micro ball of substrate upper berth, then in table
Face deposits one layer of zinc film, and the zinc-oxide nano that ingredient is very uniform, queueing discipline is orderly has been made in substrate after annealing
Cap array covers one layer of orderly aligned single layer polystyrene microsphere in zinc-oxide nano cap array surface later, then with this
Gold nano grain has been made in zinc-oxide nano cap array surface using ion sputtering deposition method and annealing technology for template
Array, to obtain extremely uniform gold nano grain-zinc-oxide nano cap array；This composite construction can give full play to
Zinc-oxide nano cap greatlys improve zinc oxide table to the absorption property and unique electronic transmission performance of specific hazardous organic molecule
The photocatalysis performance of the gold nano grain in face, to greatly improve the light degradation property to hazardous organic molecule.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 provides gold nano grain-zinc-oxide nano cap array scanning electron microscope by the embodiment of the present invention 1 and shines
Piece.
Fig. 2 is the flow diagram of gold nano grain-zinc-oxide nano cap array preparation method in the embodiment of the present invention.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
Gold nano grain provided by the present invention-zinc-oxide nano cap array and preparation method thereof is retouched in detail below
It states.The content being not described in detail in the embodiment of the present invention belongs to the prior art well known to professional and technical personnel in the field.
As shown in Fig. 2, a kind of gold nano grain-zinc-oxide nano cap array, preparation method may include steps of:
Step A, single layer polystyrene microsphere array is prepared (such as Fig. 2 a institute in substrate using gas-liquid interface self-assembly method
Show), and the diameter of polystyrene microsphere is at least 1000nm, and the diameter dimension of each polystyrene microsphere is consistent, such as: it is every
The diameter dimension of a polystyrene microsphere is 1000nm entirely, and the diameter dimension of each polystyrene microsphere is 2000nm etc. entirely.
Step B, using the single layer polystyrene microsphere array as template, and using magnetron sputtering deposition method in the template table
Face deposits one layer of zinc film (as shown in Figure 2 b), then makes annealing treatment to the template for being deposited with zinc film, to remove single layer polyphenyl
Ethylene microballoon, so that uniform component, orderly aligned zinc-oxide nano cap array (as shown in Figure 2 c) be made.
Step C, single layer polystyrene microsphere is made on the deionized water water surface, and the diameter of polystyrene microsphere is
The diameter dimension of 150~600nm, each polystyrene microsphere are consistent；Then using the substrate for being loaded with zinc-oxide nano cap array
Single layer polystyrene microsphere is picked up from the deionized water water surface, so that the zinc oxide nano for being covered with single layer polystyrene microsphere be made
Rice cap array (as shown in Figure 2 d).
Step D, using the zinc-oxide nano cap array for being covered with single layer polystyrene microsphere as template, and ion is used
Sputtering method deposits one layer of golden film (as shown in Figure 2 e) in the template surface, then anneals to the template for being deposited with golden film
Processing to remove single layer polystyrene microsphere, and forms gold nano grain in zinc oxide surface, so that extremely uniform gold be made
Nano particle-zinc-oxide nano cap array (as shown in figure 2f).
Specifically, each step of the gold nano grain-zinc-oxide nano cap array preparation method may include following scheme:
(1) in step, described that single layer polystyrene microsphere array packet is prepared in substrate with gas-liquid interface self-assembly method
Include following steps (by taking polystyrene microsphere diameter is 1000nm as an example):
Step A1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain table
The hydrophilic substrate of glass in face；Deionized water is drawn with liquid-transfering gun, is then injected into the substrate of glass of surface hydrophilic, to be made
Surface is covered with the substrate of glass of deionization moisture film.
Step A2, taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 1000nm, and according to polystyrene
Microsphere suspension liquid: ethyl alcohol=1.5:1 volume ratio mixes polystyrene microsphere suspension with ethyl alcohol, then carries out the super of 40min
Sound oscillation processing, so that finely dispersed polystyrene microsphere ethyl alcohol dilution be made.The polystyrene microsphere suspension
It can be using the polystyrene microsphere ball suspension bought by commercial means.
Step A3, the polystyrene microsphere ethanol solution is injected into the glass that the surface is covered with deionization moisture film
In substrate, surfactant is added in the beaker equipped with deionized water, is then transferred on the deionized water water surface, thus going
Single layer polystyrene microsphere is made on the ionized water water surface.
Step A4, single layer polystyrene microsphere is picked up from the deionized water water surface with substrate, to be made in substrate single
Strata phenylethylene micro ball array.
(2) in stepb, it includes: by institute that the use magnetron sputtering deposition method, which deposits one layer of zinc film in the template surface,
It states template to be put into magnetic control sputtering device, selects zinc target as sputtering target material, setting vacuum degree is 30mtor, and sputtering current is
30mA, sputtering time 6min, to deposit one layer of zinc film in the template surface.
(3) in stepb, it includes: that will be deposited with the template of zinc film that the described pair of template for being deposited with zinc film, which carries out heat treatment,
It is put into the crucible of Muffle furnace, setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, natural
After annealing, that is, single layer polystyrene microsphere is removed, forms zinc-oxide nano cap array.
(4) in step C, it is described on the deionized water water surface be made single layer polystyrene microsphere include the following steps (with
For polystyrene microsphere diameter is 150nm):
Step C1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain table
The hydrophilic substrate of glass in face；Deionized water is drawn with liquid-transfering gun, is then injected into the substrate of glass of surface hydrophilic, to be made
Surface is covered with the substrate of glass of deionization moisture film.
Step C2, taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 150nm, and micro- according to polystyrene
Ball suspension: polystyrene microsphere suspension is mixed with ethyl alcohol, then carries out the ultrasound of 40min by ethyl alcohol=1:1.5 volume ratio
Oscillation treatment, so that finely dispersed polystyrene microsphere ethanol solution be made.The polystyrene microsphere suspension can be with
Using the polystyrene microsphere suspension bought by commercial means.
Step C3, the polystyrene microsphere ethanol solution is injected into the glass that the surface is covered with deionization moisture film
In substrate, and surfactant is added in the beaker equipped with deionized water, is then transferred on the deionized water water surface, thus
Single layer polystyrene microsphere is made on the deionized water water surface.
(5) in step D, it includes: by institute that the use ion sputtering deposition method, which deposits one layer of golden film in the template surface,
It states template to be put into ion sputtering instrument, selects gold target as sputtering target material, setting vacuum degree is 0.1mbar, and sputtering current is
30mA, sputtering time are 45~90s, to deposit one layer of golden film in the template surface.
(6) in step D, it includes: that will be deposited with the template of golden film that the described pair of template for being deposited with golden film, which carries out heat treatment,
It is put into the crucible of Muffle furnace, setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, natural
After annealing, that is, removal single layer polystyrene microsphere is completed, gold nano grain-zinc-oxide nano cap array is obtained.
Further, compared with prior art, gold nano grain provided by the present invention-zinc-oxide nano cap array system
Preparation Method has at least the following advantages:
(1) in gold nano grain provided by the present invention-zinc-oxide nano cap array preparation method, gas-liquid is used first
Interface self-assembly method, magnetron sputtering deposition method and thermal anneal process technology be made in substrate ingredient it is very uniform, arrangement rule
Then orderly zinc-oxide nano cap array；There is this zinc-oxide nano cap array unique electronic transmission performance and surface to cut
Performance and biggish specific surface area can give full play to some harmful organic molecules of specific adsorption.
(2) in gold nano grain provided by the present invention-zinc-oxide nano cap array preparation method, in zinc-oxide nano
Cap array surface covers one layer of orderly aligned single layer polystyrene microsphere, then uses ion sputtering deposition as template
One layer of gold nano grain has been made in zinc-oxide nano cap array surface in method and thermal anneal process technology, to obtain extremely
Even gold nano grain-zinc-oxide nano cap array；This composite construction can give full play to zinc-oxide nano cap to be had to specific
The absorption property and unique electronic transmission performance of evil organic molecule, the light for greatling improve the gold nano grain of zinc oxide surface are urged
Change performance, to greatly improve the light degradation property to hazardous organic molecule.
(3) in gold nano grain provided by the present invention-zinc-oxide nano cap array preparation method, polystyrene microsphere
Diameter and golden film the sputtering sedimentation time determine zinc-oxide nano cap surface gold nano grain number and size, thus
Realize gold nano grain number and size it is controllable, this facilitate adjust material surface SPR (surface phasmon is total
Vibration), and then it is capable of all kinds of optical properties (such as photocatalysis, light absorption and reflection) of controlled material.
To sum up, the embodiment of the present invention can give full play to zinc-oxide nano cap to specific molecular absorption property and uniqueness
Electronic transmission performance greatlys improve light degradation property of the gold nano grain to specific hazardous organic molecule of zinc oxide surface.
In order to more clearly from show technical solution provided by the present invention and generated technical effect, below with tool
Gold nano grain provided by the present invention-zinc-oxide nano cap array and preparation method thereof is described in detail in body embodiment.
Embodiment 1
A kind of gold nano grain-zinc-oxide nano cap array, preparation method may include steps of:
Step a, clean substrate of glass is placed in UV ozone cleaning machine and irradiates 30min, to obtain surface parent
The substrate of glass of water；Deionized water is drawn with liquid-transfering gun, is then injected into the substrate of glass of surface hydrophilic, so that surface be made
It is covered with the substrate of glass of deionization moisture film.Taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 1000nm, and
According to polystyrene microsphere suspension: ethyl alcohol=1.5:1 volume ratio mixes polystyrene microsphere suspension with ethyl alcohol, then
The sonic oscillation processing for carrying out 40min, so that finely dispersed polystyrene microsphere ethyl alcohol dilution be made.By the polyphenyl second
Alkene microballoon ethyl alcohol dilution is injected into the surface and is covered in the substrate of glass of deionization moisture film, and deionized water is being housed
Surfactant is added in beaker, then polystyrene microsphere is transferred on the deionized water water surface in beaker, thus going
Single layer polystyrene microsphere is made on the ionized water water surface.It is micro- that single layer polystyrene is picked up from the deionized water water surface with silicon wafer substrate
Ball, so that single layer polystyrene microsphere array be made in substrate.
Step b, using the single layer polystyrene microsphere array as template, and the template is put into magnetic control sputtering device,
Select zinc target as sputtering target material, setting vacuum degree is 30mtor, sputtering current 30mA, sputtering time 6min, thus
The template surface deposits one layer of zinc film.The template that surface is deposited with zinc film is put into the crucible of Muffle furnace, setting heating speed
Rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, after annealing naturally, uniform component can be obtained, be arranged with
The zinc-oxide nano cap array that sequence obtains.
Step c, clean substrate of glass is placed in UV ozone cleaning machine and irradiates 30min, to obtain surface parent
The substrate of glass of water；Deionized water is drawn with liquid-transfering gun, is then injected into the substrate of glass of surface hydrophilic, so that surface be made
It is covered with the substrate of glass of deionization moisture film.Taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 150nm, and is pressed
According to polystyrene microsphere suspension: ethyl alcohol=1:1.5 volume ratio mixes polystyrene microsphere suspension with ethyl alcohol, then into
The sonic oscillation of row 40min is handled, so that finely dispersed polystyrene microsphere ethyl alcohol dilution be made.By the polystyrene
Microballoon ethanol solution is injected into the surface and is covered in the substrate of glass of deionization moisture film, and surfactant is added, then
It is transferred on the water surface of deionized water, so that single layer polystyrene microsphere be made on the deionized water water surface.It is aoxidized using being loaded with
The substrate of zinc nanometer cap array picks up single layer polystyrene microsphere from the deionized water water surface, is covered with single layer polyphenyl to be made
The zinc-oxide nano cap array of ethylene microballoon
Step d, using the zinc-oxide nano cap array for being covered with single layer polystyrene microsphere as template, by the template
It is put into ion sputtering instrument, selects gold target as sputtering target material, setting vacuum degree is 0.1mbar, sputtering current 30mA, sputtering
Time is 45~90s, to deposit one layer of golden film in the template surface.The template for being deposited with golden film is put into the earthenware of Muffle furnace
In crucible, setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, after annealing naturally, to obtain
Gold nano grain-zinc-oxide nano cap array.
Specifically, using scanning electron microscope to gold nano grain-zinc-oxide nano obtained by the embodiment of the present invention 1
Cap array is observed, to obtain electron scanning micrograph as shown in Figure 1.Fig. 1 a is that the embodiment of the present invention 1 is made
Gold nano grain-zinc-oxide nano cap array the top view obtained；Fig. 1 b is gold nano obtained by the embodiment of the present invention 1
The oblique view of grain-zinc-oxide nano cap array；Fig. 1 c be the embodiment of the present invention 1 step d in use sputtering time made for 45s
Gold nano grain-zinc-oxide nano cap array the electron scanning micrograph obtained；The step of Fig. 1 d is the embodiment of the present invention 1
Use sputtering time for gold nano grain obtained by 60s-zinc-oxide nano cap array electron scanning micrograph in d；
Fig. 1 e be the embodiment of the present invention 1 step d in use sputtering time for gold nano grain obtained by 75s-zinc-oxide nano cap
The electron scanning micrograph of array；Fig. 1 f be the embodiment of the present invention 1 step d in use sputtering time for obtained by 90s
Gold nano grain-zinc-oxide nano cap array electron scanning micrograph.As seen from Figure 1: the embodiment of the present invention 1
Obtained gold nano grain-zinc-oxide nano cap array is extremely orderly gold nano grain-zinc-oxide nano cap array, and
And the sputtering sedimentation time of golden film determines the size of the gold nano grain of zinc-oxide nano cap surface, when the sputtering sedimentation of golden film
Between it is longer, the size of the gold nano grain of zinc-oxide nano cap surface is bigger.
To sum up, the embodiment of the present invention can give full play to zinc-oxide nano cap to specific molecular absorption property and uniqueness
Electronic transmission performance greatlys improve light degradation property of the gold nano grain to specific hazardous organic molecule of zinc oxide surface.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (8)
1. a kind of gold nano grain-zinc-oxide nano cap array preparation method, which comprises the following steps:
Step A, single layer polystyrene microsphere array is prepared in substrate using gas-liquid interface self-assembly method；
Step B, using the single layer polystyrene microsphere array as template, and it is heavy in the template surface using magnetron sputtering deposition method
One layer of zinc film of product, then makes annealing treatment the template for being deposited with zinc film, so that zinc-oxide nano cap array be made；
Step C, single layer polystyrene microsphere is made on the deionized water water surface, then uses and is loaded with zinc-oxide nano cap array
Substrate picks up single layer polystyrene microsphere from the deionized water water surface, so that the oxidation for being covered with single layer polystyrene microsphere be made
Zinc nanometer cap array；
Step D, using the zinc-oxide nano cap array for being covered with single layer polystyrene microsphere as template, and ion sputtering is used
Sedimentation deposits one layer of golden film in the template surface, then makes annealing treatment to the template for being deposited with golden film, so that gold be made
Nano particle-zinc-oxide nano cap array.
2. gold nano grain according to claim 1-zinc-oxide nano cap array preparation method, which is characterized in that institute
State single layer polystyrene microsphere array is prepared in substrate with gas-liquid interface self-assembly method the following steps are included:
Step A1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain surface parent
The substrate of glass of water；Then deionized water is drawn with liquid-transfering gun, be then injected into the substrate of glass of surface hydrophilic, to be made
Surface is covered with the substrate of glass of deionization moisture film；
Step A2, taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 1000nm, and according to polystyrene microsphere
Suspension: ethyl alcohol=1.5:1 volume ratio mixes polystyrene microsphere suspension with ethyl alcohol, then carries out the ultrasound vibration of 40min
Processing is swung, so that finely dispersed polystyrene microsphere ethanol solution be made；
Step A3, the polystyrene microsphere ethanol solution is injected into the substrate of glass that the surface is covered with deionization moisture film
On, and surfactant is added, it is then transferred on the water surface of deionized water, so that it is poly- that single layer is made on the deionized water water surface
Phenylethylene micro ball；
Step A4, single layer polystyrene microsphere is picked up from the deionized water water surface with substrate, so that it is poly- that single layer is made in substrate
Phenylethylene micro ball array.
3. gold nano grain according to claim 1 or 2-zinc-oxide nano cap array preparation method, which is characterized in that
It is described on the deionized water water surface be made single layer polystyrene microsphere the following steps are included:
Step C1, clean substrate of glass is placed in 10~40min of irradiation in UV ozone cleaning machine, to obtain surface parent
The substrate of glass of water；Then deionized water is drawn with liquid-transfering gun, be then injected into the substrate of glass of surface hydrophilic, to be made
Surface is covered with the substrate of glass of deionization moisture film；
Step C2, taking polystyrene microsphere diameter is the polystyrene microsphere suspension of 150nm, and outstanding according to polystyrene microsphere
Supernatant liquid: polystyrene microsphere suspension is mixed with ethyl alcohol, then carries out the sonic oscillation of 40min by ethyl alcohol=1:1.5 volume ratio
Processing, so that finely dispersed polystyrene microsphere ethanol solution be made；
Step C3, the polystyrene microsphere ethyl alcohol dilution is injected into the glass base that the surface is covered with deionization moisture film
On bottom, and surfactant is added, is then transferred on the water surface of deionized water, so that single layer be made on the deionized water water surface
Polystyrene microsphere.
4. gold nano grain according to claim 1 or 2-zinc-oxide nano cap array preparation method, which is characterized in that
It includes: that the template is put into magnetic control sputtering device that the use magnetron sputtering deposition method, which deposits one layer of zinc film in the template surface,
In, select zinc target as sputtering target material, setting vacuum degree is 30mtor, sputtering current 30mA, sputtering time 6min, thus
One layer of zinc film is deposited in the template surface.
5. gold nano grain according to claim 1 or 2-zinc-oxide nano cap array preparation method, which is characterized in that
It includes: that the template for being deposited with zinc film is put into the crucible of Muffle furnace that the described pair of template for being deposited with zinc film, which carries out annealing,
Setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, arrives zinc oxide after annealing naturally
Nanometer cap array.
6. gold nano grain according to claim 1 or 2-zinc-oxide nano cap array preparation method, which is characterized in that
It includes: that the template is put into ion sputtering instrument that the use ion sputtering deposition method, which deposits one layer of golden film in the template surface,
In, select gold target as sputtering target material, setting vacuum degree is 0.1mbar, and sputtering current 30mA, sputtering time is 45~90s,
To deposit one layer of golden film in the template surface.
7. gold nano grain according to claim 1 or 2-zinc-oxide nano cap array preparation method, which is characterized in that
It includes: that the template for being deposited with golden film is put into the crucible of Muffle furnace that the described pair of template for being deposited with golden film, which carries out annealing,
Setting heating rate is raised to 800 DEG C from room temperature for two hours, keeps the temperature two hours later, arrives gold nano after annealing naturally
Particle-zinc-oxide nano cap array.
8. a kind of gold nano grain-zinc-oxide nano cap array, which is characterized in that using any one of the claims 1 to 7
The gold nano grain-zinc-oxide nano cap array preparation method is prepared.
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