CN106391008A - Method for loading three-dimensional zinc oxide surface with metal nanoparticles - Google Patents
Method for loading three-dimensional zinc oxide surface with metal nanoparticles Download PDFInfo
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- CN106391008A CN106391008A CN201610835841.3A CN201610835841A CN106391008A CN 106391008 A CN106391008 A CN 106391008A CN 201610835841 A CN201610835841 A CN 201610835841A CN 106391008 A CN106391008 A CN 106391008A
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- zinc oxide
- dimensional zinc
- dimensional
- area load
- metal nanoparticle
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 12
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- 238000004528 spin coating Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 6
- XKKVXDJVQGBBFQ-UHFFFAOYSA-L zinc ethanol diacetate Chemical compound C(C)O.C(C)(=O)[O-].[Zn+2].C(C)(=O)[O-] XKKVXDJVQGBBFQ-UHFFFAOYSA-L 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 3
- 239000004312 hexamethylene tetramine Substances 0.000 description 3
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229940024464 emollients and protectives zinc product Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 chlorine palladium acid Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229940003613 zinc oxide 10 mg Drugs 0.000 description 1
Classifications
-
- 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
- B01J23/56—Platinum group metals
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
-
- 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
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B01J35/39—
Abstract
The invention relates to a method for loading a three-dimensional zinc oxide surface with metal nanoparticles. The method comprises (a) adding three-dimensional zinc oxide powder into a container with a metal salt precursor liquid and carrying out an ultrasonic reaction process so that the solution discolors, and (b) carrying out centrifugal separation on the product obtained by the step (a) and carrying out vacuum drying. The metal salt precursor liquid and three-dimensional zinc oxide powder undergo a reaction under action of ultrasonic-assisted treatment. The method is free of a surfactant, is simple and efficient, saves energy and does not produce pollution. The product has uniform morphology and can be massively synthesized. The method provides an effective approach for large-scale effective synthesis of a metal semiconductor composite material.
Description
Technical field
Nano composition field of the present invention is and in particular to one kind is in three-dimensional zinc oxide area load metal nano
The method of grain.
Background technology
In recent years, due to the application prospect in optoelectronic areas, semiconductor material with wide forbidden band has become as a research
Focus.Zinc oxide（ZnO）As a kind of n-type semiconductor oxide, because of its higher catalysis activity, stability, nontoxic, knot
Many advantages, such as configuration looks designability is strong and with low cost is widely used in photocatalytic system.But ZnO has higher electronics
With the recombination rate in hole pair and larger energy gap（3.37 eV）So that its light conversion quantum efficiency is low, and can only
Absorb ultraviolet light（Only account for the 4-5% of sunlight）.How to improve the absorption in visible region for the ZnO, effectively suppression electronics and hole
Compound, thus improving photocatalytic activity and electricity conversion becomes the focus of this area research.
Content of the invention
The invention aims to overcoming the deficiencies in the prior art and providing one kind in three-dimensional zinc oxide area load metal
The method of nano-particle.
For reaching above-mentioned purpose, the technical solution used in the present invention is：One kind is received in three-dimensional zinc oxide area load metal
The method of rice grain, it comprises the following steps：
（a）Add three-dimensional zinc oxide powder in the container fill slaine precursor liquid, ultrasonic reaction makes solution changes color；
（b）By step（a）The product obtaining is centrifuged, and subsequently carries out being vacuum dried.
The synthetic method of above-mentioned three-dimensional zinc oxide comprises the following steps：
（1）Form zinc oxide crystal seed layer in substrate surface；
（2）Will be soluble in water with alkalescence class compound for soluble zinc salt, then be added thereto to additive and be configured to growth solution；
Described additive be selected from one of 1,3- propane diamine, 1,4- butanediamine, 1,6- hexamethylene diamine, ethanolamine and polyethyleneimine or
The mixture of several compositions；
（3）By step（2）In be formed with the substrate of zinc oxide crystal seed layer and put in described growth solution, ultrasonic make described zinc oxide
Crystal seed comes off, and so that described zinc oxide crystal seed is grown in described growth solution after taking out substrate；
（4）By step（3）The product centrifugation obtaining, subsequently carries out being vacuum dried；
（5）By step（4）The product obtaining is placed in natural cooling after 300 ~ 500 DEG C of insulations（Design parameter can be according to need
It is adjusted）.
Optimally, the solute of described slaine precursor liquid be gold chloride, silver nitrate, chloroplatinic acid, chlorine palladium acid or copper chloride,
Further, the solvent of described slaine precursor liquid is selected from deionized water, ethanol, methanol, isopropanol, n-butyl alcohol, first
The mixture of one or more of aldehyde and acetaldehyde composition.
Further, the ratio of described solute and described three-dimensional zinc oxide powder is 1 × 10-5~1×10-4mol：1g.
Optimally, described step（b）In, by step（a）The product obtaining is centrifuged, respectively deionized water and
Absolute ethanol washing purification, then it is placed in 50 ~ 80 DEG C of vacuum drying.
Because technique scheme is used, the present invention compared with prior art has following advantages：The present invention is in three-dimensional oxygen
The method changing zinc surface carried metal nano-particle, makes slaine precursor liquid and three-dimensional zinc oxide powder by using ultrasonic wave added
End is reacted it is not necessary to be added surfactant, has simple, efficient, energy-conservation, free of contamination advantage；Uniform product appearance,
Can synthesize on a large scale, the metal semiconductor composite for extensive synthesizing efficient provides effective approach.
Brief description
Accompanying drawing 1 is the flow chart of the method in three-dimensional zinc oxide area load metal nanoparticle for the present invention；
Accompanying drawing 2 is the present invention figure of zinc oxide SEM used in the method for three-dimensional zinc oxide area load metal nanoparticle；
Accompanying drawing 3 is zinc oxide SEM figure after three-dimensional zinc oxide area load metal nanoparticle for the present invention；
Accompanying drawing 4 is the XRD comparison diagram of the oxidized zinc products before and after carried metal nano-particle in embodiment 1；
Accompanying drawing 5 is the visible absorption spectrum comparison diagram of the oxidized zinc products before and after carried metal nano-particle in embodiment 1；
Accompanying drawing 6 is embodiment 1, zinc oxide 10mg/L methylene blue of degrading under simulated solar irradiation is molten in embodiment 3 to embodiment 5
The comparison diagram of liquid.
Specific embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is further described.
Embodiment 1
The present embodiment provide a kind of method in three-dimensional zinc oxide area load gold nano grain, as shown in figure 1, it include following
Step：
（a）The 0.010 mol/L gold chloride adding 5 mL deionized waters, 5 mL dehydrated alcohol, 0.5 ml in vial is prepared
Become slaine precursor liquid, the nano-zinc oxide powder being then added thereto to 0.1g three-dimensional Herba Taraxaci shape shakes up, and covers bottle cap；Will
Vial is placed in ultrasonic reaction 1h in ultrasonic machine, and solution is gradually changed into kermesinus from light yellow；
（b）By step（a）The product obtaining is centrifuged, and obtains lower floor's kermesinus precipitation powder, then uses deionization respectively
Water and anhydrous alcohol solution centrifugation purification, are finally deposited in 60 DEG C of vacuum drying, you can obtain three-dimensional after purification is dried
Herba Taraxaci shape zinc oxide/gold composite nanometer particle（As shown in Figure 3）；Three-dimensional zinc oxide by the carried metal obtaining nano-particle
Carry out XRD, visible absorption test with unsupported three-dimensional zinc oxide respectively, result is as shown in Figure 4 and Figure 5.
The preparation method of above-mentioned three-dimensional zinc oxide, comprises the following steps：
（1）By glass substrate（1cm×3cm）Use dehydrated alcohol and deionized water to be cleaned by ultrasonic 10 min respectively, and blown with nitrogen
Dry；With the zinc acetate ethanol solution of sol evenning machine spin coating 100 μ L on a glass substrate, rotating speed is 1200 r/min, and spin-coating time is
50s, wherein zinc acetate ethanol solution concentration are 0.005mol/L；By the good substrate of spin coating in Muffle furnace 350 DEG C of heat treatments 30
Min, you can one layer of fine and close zinc oxide crystal seed thin layer is obtained on substrate, as shown in Figure 2.
（2）By zinc nitrate hexahydrate and hexamethylenetetramine with the mixing soluble in water of equimolar concentration in vial, join
Make growth solution（The concentration of the concentration of zinc nitrate hexahydrate and hexamethyl imines is 0.025mol/L）, it is subsequently added interpolation
Agent（The concentration of 1,3- propane diamine is 0.010 mol/L）；
（3）The substrate having zinc oxide nano film to modify is placed in the growth solution preparing, has zinc oxide crystal seed face to incline
Obliquely, ultrasonic 10 min, so that the seed shedding in substrate of glass is dispersed in reaction solution, then will at room temperature
Substrate takes out, and seed-bearing growth-promoting media will be disperseed to grow 2h at 70 DEG C, you can obtain the zinc oxide containing three-dimensional Herba Taraxaci shape
Nanoparticle；
（4）By step（3）In Herba Taraxaci shape burnett's solution separated with the centrifugation of 3000r/min, obtain lower floor's oxidation
Zinc precipitates powder, then deionized water and anhydrous alcohol solution centrifugation cleaning purification respectively, 60 DEG C of last zinc oxide precipitate
Vacuum drying, you can obtain three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle after purification is dried；
（5）By step（4）In isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, be positioned in crucible add a cover in
In Muffle furnace, it is warmed up to 350 DEG C with the speed of 5 DEG C/min, is incubated 2h, then natural cooling puts room temperature；The pattern of final product
As shown in Figure 2.
Embodiment 2
The present embodiment provides a kind of method in three-dimensional zinc oxide area load silver nano-grain, it with embodiment 1 in method
Step is basically identical, except for the difference that：Add the silver nitrate solution of 0.010 mol/L in vial, solution gradually milky white complexion changed
For brownish black.
Embodiment 3
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, different is only：The 1,3- propane diamine concentration adding is 0.015 mol/L.
Embodiment 4
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, different is only：The 1,3- propane diamine concentration adding is 0.020 mol/L.
Embodiment 5
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, except for the difference that：Step（1）In, zinc acetate ethanol solution concentration is 0.001mol/L, using sol evenning machine in glass
Spin coating zinc acetate ethanol solution on substrate, rotating speed is 800r/min, and spin-coating time is 60s；Step（2）In, will in vial
Zinc nitrate hexahydrate（Concentration is 0.01mol/L）And hexamethylenetetramine（Concentration is 0.05mol/L）Mixing soluble in water
It is configured to growth solution, it is degraded respectively with the product in embodiment 1, embodiment 3 and embodiment 4 under simulated solar irradiation
10mg/L methylene blue solution, test data is as shown in Figure 6（C/C0For methylene blue solution concentration after degraded and initial methylene
The ratio of blue solution）
Embodiment 6
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, except for the difference that：Step（1）In, zinc acetate ethanol solution concentration is 0.01mol/L, using sol evenning machine in glass
Spin coating zinc acetate ethanol solution on substrate, rotating speed is 1500r/min, and spin-coating time is 30s；Step（2）In, will in vial
Zinc nitrate hexahydrate（Concentration is 0.05mol/L）And hexamethylenetetramine（Concentration is 0.01mol/L）Mixing soluble in water
It is configured to growth solution.
Embodiment 7
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, except for the difference that：Step（5）Middle will isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, place
Add a cover in crucible in Muffle furnace, be warmed up to 300 DEG C with the speed of 5 DEG C/min, be incubated 5h.
Embodiment 8
The present invention is provided in a kind of method in three-dimensional zinc oxide area load silver nano-grain, its preparation process and embodiment 1
Basically identical, except for the difference that：Step（5）Middle will isolate and purify the three-dimensional Herba Taraxaci shape Zinc oxide nanoparticle obtaining, place
Add a cover in crucible in Muffle furnace, be warmed up to 500 DEG C with the speed of 5 DEG C/min, be incubated 0.5h.
Above-described embodiment only technology design to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implements according to this, can not be limited the scope of the invention with this, all according to the present invention
Equivalence changes or modification that spirit is made, all should be included within the scope of the present invention.
Claims (5)
1. a kind of method in three-dimensional zinc oxide area load metal nanoparticle is it is characterised in that it comprises the following steps：
（a）Add three-dimensional zinc oxide powder in the container fill slaine precursor liquid, ultrasonic reaction makes solution changes color；
（b）By step（a）The product obtaining is centrifuged, and subsequently carries out being vacuum dried.
2. according to claim 1 three-dimensional zinc oxide area load metal nanoparticle method it is characterised in that：Described
The solute of slaine precursor liquid is gold chloride, silver nitrate, chloroplatinic acid, chlorine palladium are sour or copper chloride.
3. the method in three-dimensional zinc oxide area load metal nanoparticle according to claim 1 or claim 2 it is characterised in that：
The solvent of described slaine precursor liquid is in deionized water, ethanol, methanol, isopropanol, n-butyl alcohol, formaldehyde and acetaldehyde
Kind or the mixture of multiple composition.
4. according to claim 3 three-dimensional zinc oxide area load metal nanoparticle method it is characterised in that：Described
The ratio of solute and described three-dimensional zinc oxide powder is 1 × 10-5~1×10-4mol：1g.
5. according to claim 1 three-dimensional zinc oxide area load metal nanoparticle method it is characterised in that：Described
Step（b）In, by step（a）The product obtaining is centrifuged, respectively deionized water and absolute ethanol washing purification, then
It is placed in 50 ~ 80 DEG C of vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610835841.3A CN106391008A (en) | 2016-09-21 | 2016-09-21 | Method for loading three-dimensional zinc oxide surface with metal nanoparticles |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610835841.3A CN106391008A (en) | 2016-09-21 | 2016-09-21 | Method for loading three-dimensional zinc oxide surface with metal nanoparticles |
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| Publication Number | Publication Date |
|---|---|
| CN106391008A true CN106391008A (en) | 2017-02-15 |
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| CN201610835841.3A Pending CN106391008A (en) | 2016-09-21 | 2016-09-21 | Method for loading three-dimensional zinc oxide surface with metal nanoparticles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109225259A (en) * | 2018-11-15 | 2019-01-18 | 西南民族大学 | Copper silver co-doped nano zinc oxide and preparation method thereof as photochemical catalyst |
| CN109507251A (en) * | 2018-09-29 | 2019-03-22 | 中国科学院合肥物质科学研究院 | It palladium modification zinc oxide nanometer sheet, preparation method and its is applied in gas sensor |
| CN112973728A (en) * | 2021-02-01 | 2021-06-18 | 盐城工学院 | Pt-Cu/ZnO plasma photocatalyst and preparation method and application thereof |
Citations (5)
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| CN112973728A (en) * | 2021-02-01 | 2021-06-18 | 盐城工学院 | Pt-Cu/ZnO plasma photocatalyst and preparation method and application thereof |
| CN112973728B (en) * | 2021-02-01 | 2023-03-07 | 盐城工学院 | Pt-Cu/ZnO plasma photocatalyst and preparation method and application thereof |
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