CN108328646A - A method of preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material - Google Patents
A method of preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material Download PDFInfo
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- CN108328646A CN108328646A CN201810205225.9A CN201810205225A CN108328646A CN 108328646 A CN108328646 A CN 108328646A CN 201810205225 A CN201810205225 A CN 201810205225A CN 108328646 A CN108328646 A CN 108328646A
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- 238000000034 method Methods 0.000 title claims abstract description 19
- MQNRINNMYJOTSP-UHFFFAOYSA-N [O-2].[Zn+2].[S-2].[Cd+2] Chemical compound [O-2].[Zn+2].[S-2].[Cd+2] MQNRINNMYJOTSP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002086 nanomaterial Substances 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000011787 zinc oxide Substances 0.000 claims abstract description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000004809 Teflon Substances 0.000 claims abstract description 6
- 229920006362 Teflon® Polymers 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- 239000011701 zinc Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004073 vulcanization Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- -1 zinc oxide-sulphur Cadmium Chemical compound 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical group [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 4
- 102100020720 Calcium channel flower homolog Human genes 0.000 description 3
- 101000932468 Homo sapiens Calcium channel flower homolog Proteins 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UQMZPFKLYHOJDL-UHFFFAOYSA-N zinc;cadmium(2+);disulfide Chemical compound [S-2].[S-2].[Zn+2].[Cd+2] UQMZPFKLYHOJDL-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical 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
- 238000012856 packing Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to a kind of methods preparing three-dimensional flower-shaped zinc oxide cadmium sulfide heterojunction nanometer material, it includes（1）Zinc foil pre-processes；（2）Prepare solution；（3）Zinc foil and mixed solution are put into Teflon inner liner stainless steel reaction kettle and carry out hydro-thermal reaction；（4）By step（3）Obtained product is cleaned with deionized water, is dried；（5）By step（4）Obtained product is annealed in Muffle furnace；（6）Prepare cadmium chloride solution；（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, sample is cleaned after the completion, is dried.Present invention process is simple, without catalyst, and the good three-dimensional ZnO nano-structure of availability at relatively low temperature, and on this basis, using three-dimensional zinc oxide flower-like structure as core, the cadmium sulfide structure for growing cross-linked network is shell, obtains the excellent heterogeneous nano material of nucleocapsid of photocatalytic activity.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of to prepare three-dimensional flower-shaped zinc oxide-cadmium sulfide heterogeneous
The method for tying nano material.
Background technology
Hetero-junctions composite semiconductor light-catalyst is connected by close contact by two or more different component
Composite material together.Its design feature mainly has at 2 points：（1）Outside it can be seen that the appearance of various substances, various objects
Matter all may be with environment interaction；（2）It is independent mutually between different materials to combine closely again, and respectively performance can be superimposed, this is just
Show that hetero-junctions composite semiconductor material performance is better than the performance of single semi-conducting material.Wherein oxide, sulfide nanometer
Heterojunction structure shows special photoelectric property, is widely used in fields such as opto-electronic device, biology, medicine general.
For ZnO as a kind of important wide band gap semiconducter, exciton bind energy is 60 meV, and has high electron mobility
The characteristics of, it is used widely in many fields, such as solar cell, gas sensor, LED and photocatalysis cadmium sulfide
（CdS）Nanocrystalline is a kind of powder of yellow, it has a variety of space structures.Property of the special cadmium sulfide nanostructure to it
It has a very big impact, if the cadmium sulfide of the nanoparticle structure of zero dimension has quantum point effect well, in biomedical science
The leading mark in field has extraordinary effect.Two-dimensional sheet has prodigious specific surface area, this is to visible light catalytic right and wrong
Often it is necessary to.CdS nanocrystal mainly may be attributed to it with the wherein one or two kind of chemical property of electricity, light, magnetic etc. well
Energy gap is 2.42eV, causes it that can will have relatively good light transfer characteristic under light, although we have seen that cadmium sulfide is received
Many superior functions of rice material, but we can not ignore the problems of it, such as when we receive cadmium sulfide
When rice material is as photochemical catalyst, and photoetch reaction easily occurs in aqueous solution for CdS.Result of study shows Ji Husuo
Compared with single semi-conducting material, photocatalytic activity is all significantly improved some n-n hetero-junctions composite semiconductor materials.This
It is because the energy bandmatch caused by hetero-junctions can efficiently separate photo-generated carrier.And in composite catalyst, electronics and
Transfer of the hole between heterogeneous semiconductor becomes most important, in ZnO-CdS heterojunction structures, the carrier at the interfaces ZnO and CdS
Separation and transfer are most important to the raising of photocatalytic activity.
Invention content
Goal of the invention：Purpose of the invention is to overcome the shortcomings in the prior art, provides a kind of simple for process, is not necessarily to
Catalyst, and the good three-dimensional ZnO nano-structure of availability at relatively low temperature, and on this basis, with three
Dimension zinc oxide flower-like structure is core, and the cadmium sulfide structure for growing cross-linked network is shell, and it is different to obtain the excellent core-shell structure copolymer of photocatalytic activity
The preparation method of matter nano material.
Technical solution：In order to solve the above-mentioned technical problem, of the present invention a kind of to prepare three-dimensional flower-shaped zinc oxide-vulcanization
The method of cadmium heterojunction nanometer material, it includes the following steps,
（1）Zinc foil pre-processes：Sanding and polishing is carried out to zinc foil successively with the sand paper of different meshes, then with again successively use acetone,
Absolute ethyl alcohol, deionized water carry out ultrasonic cleaning 5-20min to zinc foil, and drying is for use；
（2）Prepare solution：Weigh 2.6-3.4g NaOH and 7.68 g Zn (Ac)2•2H2O is dissolved in 100 ml deionized waters；
（3）Zinc foil and mixed solution are put into Teflon inner liner stainless steel reaction kettle and carry out hydro-thermal reaction, hydrothermal temperature
It is 60-150 DEG C, reaction time 5-15h；
（4）By step（3）Obtained product is cleaned with deionized water, is dried；
（5）By step（4）Obtained product is annealed in Muffle furnace, and annealing temperature is 300 DEG C -700 DEG C, annealing time 2-
6h obtains three-dimensional ZnO nano self-assembled structures；
（6）Cadmium chloride solution is prepared, and sequentially adds ammonium chloride solution, ammonium hydroxide, thiocarbamide into cadmium chloride solution, is uniformly mixed；
（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, reaction temperature 30-
100 DEG C, reaction time 5-180min, sample is cleaned after the completion, is dried to get to three-dimensional flower-shaped zinc oxide-vulcanization
Cadmium hetero-junctions nanostructure.
By being finely adjusted section to hydroxide ion concentration, three-dimensional zinc oxide nanoassemble structure microscopic appearance is carried out
It controls, and then three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure microscopic appearance is controlled, wherein hydroxide ion
The adjustable range of concentration is 0.1-3.5 mol/Ls.
Regulate and control hydroxide ion concentration in reaction solution by adjusting the concentration of reaction raw materials in reaction solution, adjusts model
It encloses for 0.1-3.5 mol/Ls.
By being finely adjusted section to three-dimensional zinc oxide nanostructure and mixed solution reaction time, to three-dimensional flower-shaped oxidation
Zinc-cadmium sulfide hetero-junctions nanostructure microscopic appearance is controlled.
Step（6）In, caddy concentration range is 1-20 mmol/L, the addition ranging from 1- of ammonium chloride solution
20mmol, the addition ranging from 1-20ml of ammonium hydroxide, the addition ranging from 1-10mmol of thiocarbamide.
Three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material prepared by the present invention can be used as photocatalyst applications in ring
Border pollution control field.
Advantageous effect：Compared with prior art, the present invention its remarkable advantage is：
（1）It selects, using zinc foil as substrate deposition ZnO nano-structure, to reduce cost；
（2）Without using catalyst, reaction temperature is relatively low, process simplification, and avoids and introduce unnecessary impurity, is easier to
Realize the preparation of ZnO nano-structure；
（3）It can be realized to three-dimensional flower-shaped oxygen by technological parameters such as the concentration and the reaction time that simply regulate and control hydroxide ion
Change the regulation and control of zinc-cadmium sulfide hetero-junctions nanostructure microscopic appearance；
（4）Three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure large specific surface area of synthesis, optical property performance is good,
Photocatalysis field degradation of contaminant has very big potentiality.
Description of the drawings
The surface topography for the three-dimensional zinc oxide nanostructure that Fig. 1, which is hydroxyl concentration, to be prepared when being respectively 0.85 mol/L
Figure；
The XRD diagram for the three-dimensional zinc oxide nanostructure that Fig. 2 is prepared when being a concentration of 0.85 mol/L of hydroxyl；
Three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure that Fig. 3 is prepared when being a concentration of 0.85 mol/L of hydroxyl
SEM schemes；
Three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure that Fig. 4 is prepared when being a concentration of 0.65 mol/L of hydroxyl
SEM figure；
Three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure that Fig. 5 is prepared when being a concentration of 0.75 mol/L of hydroxyl
SEM figure.
Specific implementation mode
The present invention is further detailed with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
（1）Zinc foil pre-processes：It is 1.5cm by size1.5cm zinc foil successively use different meshes sand paper sanding and polishing after successively
It is cleaned by ultrasonic 5min with acetone, absolute ethyl alcohol and deionized water, it is for use to dry 1h in baking oven；
（2）Weigh 3.4 g NaOH and 7.68 g Zn (Ac)2•2H2O is dissolved in 100 ml deionized waters, hydroxyl in solution
A concentration of 0.85 mol/L；
（3）The mixed solution of the zinc foil handled well and above-mentioned hydroxyl concentration is put into Teflon inner liner stainless steel reaction kettle difference
Hydro-thermal reaction is carried out, reaction temperature is 70 DEG C, reaction time 12h；
（4）By step（3）In obtained product cleaned with deionized water, be placed in baking oven and dry 2h；
（5）By step（4）In obtained product be placed in Muffle furnace and anneal, annealing temperature is 300 DEG C, and annealing time 4h is obtained
To three-dimensional ZnO nano-structure；
（6）Compound concentration is the caddy of 6 mmol/L（That is the caddy of 0.2 mmol is dissolved in 100 ml deionized waters）,
And the ammonium chloride solution of 3 mmol, 5 ml ammonium hydroxide, 3mmol thiocarbamides are sequentially added into cadmium chloride solution, it is uniformly mixed；
（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, reaction temperature is 80 DEG C,
Reaction time is 30 min, is cleaned, is dried to get to three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions to sample after the completion
Nanostructure.
The scanning electron microscope of three-dimensional ZnO nano-structure is obtained in embodiment 1（SEM）Figure is as shown in Figure 1.Work as hydroxide ion
When a concentration of 0.85 mol/L, there is a large amount of sequence flower shape zinc oxide structure, be evenly distributed.Independent flower-like structure is by ruler
Very little uniform nanometer rods composition, and radial, the symmetry with height is presented.Fig. 2 is a concentration of 0.85 mol/L of hydroxyl
When the XRD spectrum of ZnO nano-structure for preparing.Fig. 2 shows that sample obtained is six side's Wurzite structures, and crystallinity and pure
Spend higher, no other impurities.Fig. 3 is the SEM figures of three-dimensional flower-shaped zinc oxide obtained-cadmium sulfide hetero-junctions nanostructure.From figure
In as can be seen that grown more membranaceous cadmium sulfide structure in radial zinc oxide, and rely on three-dimensional zinc oxide structure
The structure of cross-linked network is formd, this structure is beneficial to carrier separation and transfer between zinc oxide and cadmium sulfide.
Embodiment 2
（1）The pretreatment of zinc foil：It is 1.5cm by size1.5cm zinc foil successively use different meshes sand paper sanding and polishing after according to
Secondary acetone, absolute ethyl alcohol and deionized water are cleaned by ultrasonic 30min, and it is for use to dry 1h in baking oven；
（2）Weigh 2.6 g NaOH and 7.68 g Zn (Ac)2•2H2O is dissolved in 100 ml deionized waters, hydroxyl in solution
Concentration is respectively 0.65 mol/L；
（3）The zinc foil handled well and above-mentioned mixed solution are put into Teflon inner liner stainless steel reaction kettle, and to carry out hydro-thermal respectively anti-
It answers, reaction temperature is 100 DEG C, reaction time 7h；
（4）By step（3）Obtained product is cleaned with deionized water, and 2h is dried in baking oven；
（5）By step（4）Obtained product, which is placed in Muffle furnace, anneals, and annealing temperature is 600 DEG C, and annealing time 3h is obtained
ZnO nano-structure；
（6）Compound concentration is the caddy of 3 mmol/L（That is the caddy of 0.3 mmol is dissolved in 100 ml deionized waters）,
And the ammonium chloride solution of 1 mmol, 5 ml ammonium hydroxide, 1 mmol thiocarbamides are sequentially added into cadmium chloride solution, it is uniformly mixed；
（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, reaction temperature is 50 DEG C,
Reaction time is 10 min, is cleaned, is dried to get to three-dimensional flower-shaped zinc oxide-of the present invention to sample after the completion
Cadmium sulfide hetero-junctions nanostructure.
The scanning electron microscope (SEM) photograph of product obtained is as shown in Figure 4 in embodiment 2.It can be obtained from the figure that when hydroxyl a concentration of 0.65
When mol/L, the negligible amounts of flower shape zinc oxide nanostructure are evenly distributed in some regions, and its basic unit nanometer rods
Length and diameter it is more uniform, and at endpoint pattern rule.Cadmium sulfide cross-linked network negligible amounts and small volume.
Embodiment 3
（1）The pretreatment of zinc foil：It is 1.5cm by sizeAfter 1.5cm zinc foil is successively with difference with the sand paper sanding and polishing of mesh number
Acetone, absolute ethyl alcohol and deionized water is used to be cleaned by ultrasonic 30min successively, it is for use to dry 1h in baking oven；
（2）Weigh 3 g NaOH and 7.68 g Zn (Ac)2•2H2O is dissolved in 100 ml deionized waters, and hydroxyl is dense in solution
Degree is respectively 0.75 mol/L；
（3）The zinc foil handled well and above-mentioned mixed solution are put into Teflon inner liner stainless steel reaction kettle, and to carry out hydro-thermal respectively anti-
It answers, reaction temperature is 100 DEG C, reaction time 12h；
（4）By step（3）Obtained product is cleaned with deionized water, and 2h is dried in baking oven；
（5）By step（4）Obtained product, which is placed in Muffle furnace, anneals, and annealing temperature is 500 DEG C, and annealing time 3h is obtained
Three-dimensional ZnO nano-structure；
（6）Compound concentration is the caddy of 2 mmol/L（That is the caddy of 0.2 mmol is dissolved in 100 ml deionized waters）,
And the ammonium chloride solution of 10 mmol, 5 ml ammonium hydroxide, 3mmol thiocarbamides are sequentially added into cadmium chloride solution, it is uniformly mixed；
（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, reaction temperature is 80 DEG C,
Reaction time is 20 min, is cleaned, is dried to get to three-dimensional flower-shaped zinc oxide-of the present invention to sample after the completion
Cadmium sulfide hetero-junctions nanostructure.
The scanning electron microscope (SEM) photograph of product obtained is as shown in Figure 5 in embodiment 3.It can be obtained from the figure that when hydroxyl a concentration of 0.75
When mol/L, sequence flower shape zinc oxide nanostructure quantity increases, and the length and diameter of basic unit nanometer rods is uniform, and
Pattern rule at endpoint.Cadmium sulfide number of structures is more, and has packing phenomenon, and by cross-linked network by adjacent three
Dimension zinc oxide structures are linked to be an island structure.
The present invention provides a kind of thinking and methods, and there are many method and the approach for implementing the technical solution, the above institute
State only is the preferred embodiment of the present invention, it is noted that for those skilled in the art, is not being departed from
Under the premise of the principle of the invention, several improvements and modifications can also be made, these improvements and modifications also should be regarded as the guarantor of the present invention
Range is protected, all undefined components in this embodiment can be implemented in the prior art.
Claims (5)
1. a kind of method preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material, it is characterised in that：It includes following
Step,
（1）Zinc foil pre-processes：Sanding and polishing is carried out to zinc foil successively with the sand paper of different meshes, then with again successively use acetone,
Absolute ethyl alcohol, deionized water carry out ultrasonic cleaning 5-20min to zinc foil, and drying is for use；
（2）Prepare solution：Weigh 2.6-3.4g NaOH and 7.68 g Zn (Ac)2•2H2O is dissolved in 100 ml deionized waters；
（3）Zinc foil and mixed solution are put into Teflon inner liner stainless steel reaction kettle and carry out hydro-thermal reaction, hydrothermal temperature
It is 60-150 DEG C, reaction time 5-15h；
（4）By step（3）Obtained product is cleaned with deionized water, is dried；
（5）By step（4）Obtained product is annealed in Muffle furnace, and annealing temperature is 300 DEG C -700 DEG C, annealing time 2-
6h obtains three-dimensional ZnO nano self-assembled structures；
（6）Cadmium chloride solution is prepared, and sequentially adds ammonium chloride solution, ammonium hydroxide, thiocarbamide into cadmium chloride solution, is uniformly mixed；
（7）By step（5）Obtained product is put into step（6）It is reacted in obtained mixed solution, reaction temperature 30-
100 DEG C, reaction time 5-180min, sample is cleaned after the completion, is dried to get to three-dimensional flower-shaped zinc oxide-vulcanization
Cadmium hetero-junctions nanostructure.
2. the method according to claim 1 for preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material, feature
It is：By being finely adjusted section to hydroxide ion concentration, three-dimensional zinc oxide nanoassemble structure microscopic appearance is controlled
System, and then three-dimensional flower-shaped zinc oxide-cadmium sulfide hetero-junctions nanostructure microscopic appearance is controlled, wherein hydroxide ion is dense
The adjustable range of degree is 0.1-3.5 mol/Ls.
3. the method according to claim 1 for preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material, feature
It is：Regulate and control hydroxide ion concentration in reaction solution, adjustable range by adjusting the concentration of reaction raw materials in reaction solution
For 0.1-3.5 mol/Ls.
4. the method according to claim 1 for preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material, feature
It is：By being finely adjusted section to three-dimensional zinc oxide nanostructure and mixed solution reaction time, to three-dimensional flower-shaped zinc oxide-sulphur
Cadmium hetero-junctions nanostructure microscopic appearance is controlled.
5. the method according to claim 1 for preparing three-dimensional flower-shaped zinc oxide-cadmium sulfide heterojunction nanometer material, feature
It is：Step（6）In, caddy concentration range be 1-20 mmol/L, the addition ranging from 1-20mmol of ammonium chloride solution,
The addition of ammonium hydroxide ranging from 1-20ml, the addition ranging from 1-10mmol of thiocarbamide.
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| CN109126829B (en) * | 2018-09-18 | 2021-12-14 | 合肥学院 | Preparation method of CdS-MoS2 composite powder with three-dimensional heterostructure |
| CN109201102A (en) * | 2018-09-28 | 2019-01-15 | 商丘师范学院 | A kind of Z-type hetero-junctions M-C3N4The preparation method of/CdS composite photo-catalyst |
| CN109201102B (en) * | 2018-09-28 | 2021-08-13 | 商丘师范学院 | Z-type heterojunction M-C3N4Preparation method of CdS composite photocatalyst |
| CN110606502A (en) * | 2019-10-16 | 2019-12-24 | 江苏巨珩新材料科技有限公司 | Preparation method of self-cleaning surface with photocatalysis synergistic effect |
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| CN115025787A (en) * | 2022-05-24 | 2022-09-09 | 西南科技大学 | Preparation method and application of CdS quantum dot modified ZnO nanoflower heterojunction |
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