CN108408762A - Method for preparing three-dimensional cadmium sulfide nano self-assembly structure - Google Patents
Method for preparing three-dimensional cadmium sulfide nano self-assembly structure Download PDFInfo
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- CN108408762A CN108408762A CN201810205232.9A CN201810205232A CN108408762A CN 108408762 A CN108408762 A CN 108408762A CN 201810205232 A CN201810205232 A CN 201810205232A CN 108408762 A CN108408762 A CN 108408762A
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 95
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001338 self-assembly Methods 0.000 title abstract 3
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 49
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 32
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 16
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 24
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 24
- 239000002202 Polyethylene glycol Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 10
- 239000004809 Teflon Substances 0.000 claims description 7
- 229920006362 Teflon® Polymers 0.000 claims description 7
- 229910000474 mercury oxide Inorganic materials 0.000 claims description 7
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 5
- -1 CTAB cetyl trimethylammonium bromides Chemical class 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 77
- 239000003054 catalyst Substances 0.000 abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract 3
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000007792 addition Methods 0.000 description 31
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 18
- 238000004847 absorption spectroscopy Methods 0.000 description 13
- 239000000654 additive Substances 0.000 description 12
- 230000000996 additive effect Effects 0.000 description 12
- 238000003756 stirring Methods 0.000 description 9
- 238000004020 luminiscence type Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000013019 agitation Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 241000555268 Dendroides Species 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical group [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing a three-dimensional cadmium sulfide nano self-assembly structure, which comprises the following steps of (1) preparing thiourea (NH)2)2CS、CdCl2·2.5H20 mixed solution or thiourea (NH)2)2CS、CdCl2·2.5H20. A surfactant mixed solution; (2) transferring the mixed solution into a Teflon-lined stainless steel reaction kettle for hydrothermal reaction at the temperature of 60-200 ℃ for 3-20 h; (3) respectively centrifugally cleaning the product obtained in the step (2) for 3 times by using distilled water and absolute ethyl alcohol, and centrifugally cleaning the product once by using distilled water; (4) and (4) drying the yellow precipitate product obtained in the step (3) in a drying oven at 60 ℃ for 6 hours to obtain the CdS nano self-assembly structure. The method has simple process, does not need a catalyst, and can obtain the three-dimensional CdS nano structure with good performance and adjustable appearance at relatively low temperature.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to one kind being assembled into three-dimensional vulcanization by low-dimensional cadmium sulfide unit
The method of cadmium nanostructure.
Background technology
Cadmium sulfide (CdS) is a kind of typical II-VI race's semi-conducting material, and at normal temperatures, the direct band gap of Cd S is
2.4 e V.Due to its unique nonlinear optical effect, CdS nano materials are in solar cell, light emitting diode, biology mark
Many fields such as note and photocatalysis are with a wide range of applications.The variation of the morphology and size of nano material is to its many aspect
Property all have an impact, so in recent years, adjusting and the morphology and size of control nano material has become nano science and grinds
Very important aspect in studying carefully.An important factor for prepared by the low cost of CdS nanostructures and controllable preparation is influences its application.
Currently, the preparation method of CdS nanostructures mainly has hydro-thermal(Or solvent heat)Method, microemulsion method, the precipitation method, gas phase
Method, solid phase method.Vapor phase method refers to that first reactant low-pressure heating is evaporated, and so that reactant is formed free atom or molecule, lazy
Property gas molecule or collision effect to each other under offset energy, form nano particle.Physical vaporous deposition and change can be divided into
Learn vapour deposition process.Solid phase method refers in the reaction of formation of CdS nanostructures, and reactant is to exist in solid form,
Chemical combination obtains nano-tube/CdS structure after reactant is decomposed in heating.But there is also preparation works in above-mentioned various methods
Skill is complicated, and reaction temperature is higher, needs to add the defects of catalyst is to introduce unnecessary impurity.Hydro-thermal method(Solvent-thermal method)
The method of synthesizing nano-particle, in general not only can be obtained tiny CdS by hydro-thermal method i.e. under high pressure, hot conditions
Nanostructure, while also having the oxidation that can prevent nanostructure, reaction system is less, easy to operate, to the of less demanding of equipment
The advantages that.
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 availability is good at relatively low temperature, preparation side of the regulatable three-dimensional CdS nanostructures of pattern
Method.
Technical solution:In order to solve the above-mentioned technical problem, of the present invention a kind of to prepare three-dimensional cadmium sulfide nano from group
The method of assembling structure, it includes the following steps,
(1)Prepare thiocarbamide (NH2)2CS、CdCl2· 2.5H20 mixed solution or thiocarbamide (NH2)2CS、CdCl2· 2.5H20, table
Face surfactant mixed solution;
(2)Mixed solution is moved into Teflon inner liner stainless steel reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature 60-
200 DEG C, reaction time 3-20h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product in 60 DEG C of drying boxes dry 6 h to get to CdS nanoassembles
Structure.
By the way that material proportion is adjusted, three-dimensional cadmium sulfide nano self-assembled structures microscopic appearance is controlled,
Middle material proportion CdCl2· 2.5H2O:(NH2)2CS=1:1 or 1:2 or 1:3.
By adding surfactant, three-dimensional cadmium sulfide nano self-assembled structures microscopic appearance is controlled, wherein adding
It is PVA polyvinyl alcohol, PEG polyethylene glycol, SDS lauryl sodium sulfate, CTAB cetyl front threes to add surfactant types
One or more of base ammonium bromide.
Regulate and control the micro- of three-dimensional cadmium sulfide nano self-assembled structures by surfactant addition in adjusting reaction solution
Pattern is seen, the wherein adjustable range of surface modification PVA polyvinyl alcohol concentration is 0- 0.05g/mL, PEG Polyethylene glycols
Adjustable range is 0-0.05g/mL, and the adjustable range of SDS lauryl sodium sulfate concentration is 0- 0.05g/mL, CTAB hexadecanes
The adjustable range of base trimethylammonium bromide concentration is 0-0.05g/mL.
Three-dimensional CdS nanostructures prepared by the present invention can be used as photocatalyst applications in field of environment pollution control.
Advantageous effect:Compared with prior art, the present invention its remarkable advantage is:
(1)Without using catalyst, reaction temperature is relatively low, process simplification, and avoids and introduce unnecessary impurity, is easier to
Realize the preparation of CdS nanostructures;
(2)Material proportion by simply regulating and controlling chromium chloride and thiocarbamide can realize the morphology controllable system of CdS 3-D nano, structures
It is standby;
(3)CdS three-dimensional manometer knots are realized by adding variety classes surfactant and adjusting the additive amount of surfactant
It is prepared by the morphology controllable of structure;
(4)The CdS 3-D nano, structures of synthesis have good photocatalysis performance, have in photocatalysis degradation organic contaminant field
There is prodigious application potential.
Description of the drawings
Fig. 1 is the scanning electron microscope that CdS nanostructures are synthesized under different thiocarbamide additions(SEM)Figure;
Fig. 2 is caddy and thiocarbamide material proportion is 1:The X-ray powder diffraction of the cadmium sulfide nanostructure prepared when 3(XRD)
Figure;
Fig. 3 is caddy and thiocarbamide material proportion is 1:The power spectrum of the cadmium sulfide nanostructure prepared when 3(EDS)Figure;
Fig. 4 is caddy and thiocarbamide material proportion is 1:The cadmium sulfide nanostructure ultraviolet-visible absorption spectroscopy prepared when 3(UV-
vis)Figure;
Fig. 5 is the scanning electron microscope that CdS nanostructures are synthesized under different PVA additions(SEM)Figure;
Fig. 6 is the ultraviolet-visible absorption spectroscopy that CdS nanostructures are synthesized under different PVA additions(UV-vis)Figure;
Fig. 7 is the luminescence generated by light that CdS nanostructures are synthesized under different PVA additions(PL)Collection of illustrative plates;
Fig. 8 is the scanning electron microscope that CdS nanostructures are synthesized under different PEG additions(SEM)Figure;
Fig. 9 is the ultraviolet-visible absorption spectroscopy that CdS nanostructures are synthesized under different PEG additions(UV-vis)Figure;
Figure 10 is the luminescence generated by light that CdS nanostructures are synthesized under different PEG additions(PL)Figure;
Figure 11 is the scanning electron microscope that CdS nanostructures are synthesized under different SDS additions(SEM)Figure;
Figure 12 is the ultraviolet-visible absorption spectroscopy that CdS nanostructures are synthesized under different SDS additions(UV-vis)Figure;
Figure 13 is the luminescence generated by light that CdS nanostructures are synthesized under different SDS additions(PL)Figure;
Figure 14 is the scanning electron microscope that CdS nanostructures are synthesized under different CTAB additions(SEM)Figure;
Figure 15 is the ultraviolet-visible absorption spectroscopy that CdS nanostructures are synthesized under different CTAB additions(UV-vis)Figure;
Figure 16 is the luminescence generated by light that CdS nanostructures are synthesized under different CTAB additions(PL)Figure;
Figure 17 is not add surfactant and add the CdS nanostructures synthesized by 0.0050g/mL surfactants not of the same race
The disposal efficiency curve graph of the sample to simulating pollution object methylene blue.
Specific implementation mode
The present invention is further detailed with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A method of three-dimensional cadmium sulfide nano self-assembled structures are prepared, it includes the following steps,
(1)Weigh four part of 0.01 mol(2.2836 g)CdCl2· 2.5H20, it is separately added into and fills 80 ml deionized waters
In beaker, magnetic agitation makes it fully dissolve, and obtains the solution of clear, then is separately added into 0.01 mol(0.7612 g)、
0.02 mol(1.5224 g)、0.03 mol(2.2836 g)Thiocarbamide, stirring 15 min make its be uniformly mixed;(2)It will be above-mentioned
Mixed solution, which moves into Teflon inner liner stainless steel reaction kettle, carries out hydro-thermal reaction, and hydrothermal temperature is 180 DEG C, the reaction time
For 12h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product dry 6 h in 60 DEG C of drying boxes, obtain CdS nanostructures.
The scanning electron microscope of obtained sample in embodiment 1(SEM)Figure as shown in Figure 1,(a-c)Material proportion is respectively
CdCl2· 2.5H2O:(NH2)2CS=1:1,1:2,1:3.When caddy and thiocarbamide material proportion are 1:When 1, there is sequence branch
Shape cadmium sulfide nanostructure, side shoot is shorter and has preferable symmetry.When caddy and thiocarbamide material proportion are 1:When 2, dendroid
Nanostructured surface is rougher and has corner angle, close to also mutual adhesion at trunk.When caddy and thiocarbamide material proportion are 1:3
When, collateral generation is longer, and crystal side shoot is at regular intervals and away from being separated from each other, and has 2 on its trunk of some CdS nanostructures
Grade collateral generation is in 3 sub-symmetry position of same axial direction, and the side shoot of the same side is in the state that is mutually parallel.Fig. 2 is material
Match CdCl2·2.5H2O:(NH2)2CS=1:The XRD spectrum of 3 cadmium sulfide nanostructures.As can be seen from Figure 2 diffraction peak intensity and
Sharply show that sample crystallinity is good, all diffraction maximums and standard card in figure(JCPDS75-1545)In data be consistent, and
And without miscellaneous peak.Fig. 3 is that material matches CdCl2·2.5H2O:(NH2)2CS=1:The EDS of 3 cadmium sulfide nanostructures is analyzed, from figure
In as can be seen that product is mainly Cd elements and S elements, atom metering is than being 1:1, prove that generated product is in conjunction with XRD diagram
Pure phase.Fig. 4 is caddy and thiocarbamide material proportion is 1:The CdS nanostructures UV-vis figures prepared when 3.Institute as can be seen from Figure
The CdS nanostructures of system have higher absorptivity in 300 ~ 500 nm, it can thus be appreciated that obtained product has visible region
Stronger absorption, the sample direct band gap by can be calculated preparation are 2.33 eV.
Embodiment 2
A method of three-dimensional cadmium sulfide nano self-assembled structures are prepared, it includes the following steps,
(1)Weigh four part of 0.01 mol(2.2836 g)CdCl2· 2.5H20, it is separately added into the burning for filling 80 ml deionized waters
In cup, magnetic agitation makes it fully dissolve, and obtains the solution of clear, then weighs not same amount(0,0.2,1.0,2.0g)PVA
(polyvinyl alcohol)It is respectively added in aforementioned four beaker, continues stirring and dissolving and add 0.03 mol(2.2836 g)Thiocarbamide,
Stirring 15 min makes it be uniformly mixed;(2)Above-mentioned mixed solution is moved into Teflon inner liner stainless steel reaction kettle and carries out hydro-thermal
Reaction, hydrothermal temperature are 180 DEG C, reaction time 12h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product dry 6 h in 60 DEG C of drying boxes, obtain CdS nanostructures.
The scanning electron microscope (SEM) photograph of obtained sample is as shown in Figure 5 in embodiment 2.It can be seen from the figure that not adding
The CdS nanostructures synthesized when PVA are sequence dendritic structure, such as Fig. 5(a).After adding 0.0025 g/mL PVA
Obtained CdS nanostructures are rodlike at trigone, and size is more uniform, and dispersibility is preferable, such as Fig. 5(b).When PVA additive amounts
Increase to 0.0050 g/mL, such as Fig. 5(c)It is shown, three sub-symmetries of the obtained CdS nano bar-shapes structure in trunk
There are short dendritic morphology, sawtooth bottom end that mutually there is adhesion on direction, forms dendritic structure.Continue growing PVA additions
Amount, when PVA additions be 0.0125 g/mL when such as Fig. 5(d)Shown, an obtained CdS nanostructure parts are formed
Dendritic structure small part is still triangular prism shape structure.And dendritic structure side shoot shortens successively from low side to top, and homonymy
The mutual keeping parallelism of crystal side shoot, but the size distribution of nano-particle is more uneven, there is slight reunion.As PVA plus
Enter amount be 0.0250 g/mL when such as Fig. 5(e)It is shown, prepared at this time CdS nanostructures at irregular graininess,
The irregular shapes such as sheet, rodlike, particle size is smaller and particle size range is wider.It can thus be appreciated that being added by controlling in hydrothermal synthesis
Add the amount of PVA, also can effectively control the appearance structure of CdS nanostructures.Fig. 6 is synthesized under different PVA additions
The UV-vis of CdS nanostructures schemes.Curve in left figure(a)It is bent not add the ultraviolet-visible absorption spectroscopy that PVA samples are surveyed
Line,(b)To add 0.4 g PVA sample ultraviolet-visible absorption spectroscopy curves.Fig. 7 is synthesized under different PVA additions
The luminescence generated by light of CdS nanostructures(PL)Figure.
Embodiment 3
A method of three-dimensional cadmium sulfide nano self-assembled structures are prepared, it includes the following steps,
(1)Weigh four part of 0.01 mol(2.2836 g)CdCl2· 2.5H20, it is added separately to fill 80 ml deionized waters
In beaker, magnetic agitation makes it fully dissolve, and obtains the solution of clear, then weighs not same amount(0,0.2,1.0,2.0g)
PEG (polyethylene glycol)It is added into respectively in aforementioned four beaker, continues stirring and dissolving and add 0.03 mol(2.2836 g)Sulphur
Urea, 15 min of stirring make it be uniformly mixed;(2)Above-mentioned mixed solution is moved into Teflon inner liner stainless steel reaction kettle and is carried out
Hydro-thermal reaction, hydrothermal temperature are 180 DEG C, reaction time 12h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product dry 6 h in 60 DEG C of drying boxes, obtain CdS nanostructures.
The scanning electron microscope (SEM) photograph of sample obtained by embodiment 3 is as depicted in figure 8.It can be seen from the figure that not adding PEG
The CdS nanostructures of Shi Hecheng have dendritic structure, such as Fig. 8(a).It is acquired when adding 0.0025 g/mL PEG
CdS nanostructures at trigone bar or granules structure, size is more uneven, dispersibility preferably, and club shaped structure
Symmetry direction three times on have laciniation, such as Fig. 8(b).When PEG additive amounts increase to 0.0050g/mL, such as Fig. 8
(c)Shown and Fig. 8(b)It compares, obtained CdS nano-structured particles size increases, and has slight agglomeration, trigone
Broached-tooth design on column structure slightly increases.With continuing growing for PEG additive amounts, CdS nanostructures have dendroid
Structure also has certain agglomeration, and collateral generation is uneven, and surface is rougher, such as Fig. 8(d)It is shown.When PEG is added
When increasing to 0.0250 g/mL of amount, such as Fig. 8(e)Shown major part CdS nanostructures have dendritic structure, side shoot
Grow more uniform, uniform particle size is smaller, and favorable dispersibility.It can thus be appreciated that by controlling addition PEG in hydrothermal synthesis
Amount, also can effectively control the appearance structure of CdS nanostructures.Fig. 9 is synthesis CdS nano junctions under different PEG additions
The UV-vis of structure schemes.Curve in left figure(a)Not add the ultraviolet-visible absorption spectroscopy curve that PEG samples are surveyed,(b)To add
Add 0.0050 g/mL PEG sample ultraviolet-visible absorption spectroscopy curves.Right figure shows in light-catalyzed reaction, by addition 0.0050
G/mLPEG synthetic samples are not than adding the hole and the summary of photoelectronic redox ability that the sample excitation of PEG synthesis generates
By force.Figure 10 is the luminescence generated by light that PEG nanostructures are synthesized under different PEG additions(PL)Figure.
Embodiment 4
A method of three-dimensional cadmium sulfide nano self-assembled structures are prepared, it includes the following steps,
(1)Weigh four part of 0.01 mol(2.2836 g)CdCl2· 2.5H20, it is separately added into the burning for filling 80 ml deionized waters
In cup, magnetic agitation makes it fully dissolve, and obtains the solution of clear, then weighs not same amount(0,0.2,0.4,0.6,0.8
g)SDS(Lauryl sodium sulfate)It is added into respectively in aforementioned four beaker, continues stirring and dissolving and add 0.03 mol
(2.2836 g)Thiocarbamide, 15 min of stirring make it be uniformly mixed;(2)Above-mentioned mixed solution is moved into Teflon inner liner stainless steel
Hydro-thermal reaction is carried out in reaction kettle, hydrothermal temperature is 180 DEG C, reaction time 12h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product dry 6 h in 60 DEG C of drying boxes, obtain CdS nanostructures.
The scanning electron microscope (SEM) photograph of sample obtained by embodiment 4 is as indicated at 11.It can be seen from the figure that not adding SDS
The CdS nanostructures of Shi Hecheng have dendritic structure, such as Figure 11(a).It is obtained when adding 0.0025 g/mLSDS
For CdS nanostructures at trigone bar or granules structure, size is relatively more uniform, and dispersibility is preferable, and some are rodlike
There are shorter side shoot, such as Figure 11 on the symmetry direction three times of structure(b).As SDS additive amounts increase to 0.0050 g/
ML, such as Figure 11(c)Shown, the nano-particle obtained at this time is at dendritic structure size with respect to Figure 11(b)It is bigger, and nanometer rods
Side shoot length on the symmetry direction three times of shape structure slightly increases, and also occurs some sheets or nutty structure at this time.When
When SDS additive amounts reach 0.0075 g/mL, obtained nanostructure no longer has club shaped structure, irregular at graininess
Accumulation.When SDS additive amounts reach 0.0100 g/mL, obtained nanostructure is fine particle and shape has no rule, and
Agglomeration is serious.It can thus be appreciated that adding the amount of SDS in hydrothermal synthesis by controlling, CdS nanostructures also can be effectively controlled
Appearance structure.Figure 12 is the UV-vis figures that CdS nanostructures are synthesized under different SDS additions.Curve in left figure(a)For not
The ultraviolet-visible absorption spectroscopy curve that addition SDS samples are surveyed,(b)To add 0.4 g SDS sample ultraviolet-visible absorption spectroscopies
Curve.Right figure shows not add the made eV of sample Eg=2.33 of SDS, adds the sample synthesized by 0.0050 g/mLSDS
Eg=2.31 eV.Figure 13 is the luminescence generated by light of synthesizing cadmium sulfide nanostructure under different SDS additions(PL)Figure.
Embodiment 5
A method of three-dimensional cadmium sulfide nano self-assembled structures are prepared, it includes the following steps,
(1)Weigh four part of 0.01 mol(2.2836 g)CdCl2· 2.5H20, it is separately added into the burning for filling 80 ml deionized waters
In cup, magnetic agitation makes it fully dissolve, and obtains the solution of clear, then weighs not same amount(0,0.2,0.4,0.6,0.8
g)CTAB(Cetyl trimethylammonium bromide)It is added into respectively in aforementioned four beaker, continues stirring and dissolving and add 0.03
mol(2.2836 g)Thiocarbamide, 15 min of stirring make it be uniformly mixed;(2)It is stainless that above-mentioned mixed solution is moved into Teflon liner
Hydro-thermal reaction is carried out in steel reaction kettle, hydrothermal temperature is 180 DEG C, reaction time 12h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product dry 6 h in 60 DEG C of drying boxes, obtain CdS nanostructures.
The scanning electron microscope (SEM) photograph of sample obtained by embodiment 5 is as shown at 14.It can be seen from the figure that not adding surface
The CdS nanostructures synthesized when activating agent CTAB have dendritic structure, such as Figure 14(a).And add gained after CTAB
The CdS nanostructures arrived are all bulk structure.When CTAB additive amounts are 0.0025 g/mL, such as Figure 14(b)It is shown, group
Shape nanostructure size is smaller and uneven, good dispersion.When CTAB additive amounts are 0.0050 g/mL, such as Figure 14(c)Institute
Show, bulk nanostructure forms size uniform, favorable dispersibility by sheet accumulation.With the increase of CTAB additive amounts, when
Bulk nanostructure size reaches maximum value, such as Figure 14 when CTAB additive amounts are 0.0075 g/mL(d)It is shown, it rolls into a ball at this time
Shape nanostructure favorable dispersibility, but granular size is more uneven.Obtained bulk nanostructure size as can be seen from Figure
It is obviously increased with CTAB increases, but obtained nanoparticle size can obviously subtract when surfactant additive amount is more than a certain value
It is small, while there is poly- phenomenon, particle size range can also increase, such as Figure 14(e)It is shown.It can thus be appreciated that being added by controlling in hydrothermal synthesis
Add the amount of CTAB, also can effectively control the appearance structure of CdS nanostructures.Figure 15 is synthesized under different CTAB additions
The UV-vis of CdS nanostructures schemes.Curve in left figure(a)It is bent not add the ultraviolet-visible absorption spectroscopy that CTAB samples are surveyed
Line,(b)The ultraviolet-visible absorption spectroscopy curve surveyed for 0.0050 g/mL CTAB samples of addition.Right figure shows not add CTAB
The made eV of sample Eg=2.33 add the eV of sample Eg=2.22 synthesized by 0.0050 g/mLCTAB.Figure 16 is different CTAB
The luminescence generated by light of synthesizing cadmium sulfide nanostructure under addition(PL)Figure.Figure 17 is not add surfactant and addition
Light degradation of the CdS nanostructures sample to simulating pollution object methylene blue synthesized by 0.0050 g/mL different surfaces activating agents
Efficiency curve diagram.A curves are the CdS nanostructure test curves for not adding any surfactant and preparing;B is addition
CdS nanostructure test curves prepared by 0.0050 g/mLPVA;C is the CdS nanometers added 0.0050g/mLPEG and prepared
Structured testing curve;D is the CdS nanostructure test curves for adding 0.0050 g/mLSDS and preparing;E is 0.0050 g/ of addition
CdS nanostructure test curves prepared by mLCTAB.When in 60min 5 samples to the degradation efficiency of methyl blue organic matter
Respectively:A curves 98.7%;B curves 99.9%;C curves 96.4%;D curves 97.8%;E curves 98.8%.Wherein drop
The minimum c curves of solution efficiency have also reached 96.4%, and all samples are basic to the catalytic efficiency of methylene blue in 45 min
Reach peak value.Illustrate that prepared all products all have good photocatalysis performance, has very in field of environment pollution control
Big application potential.
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 (4)
1. a kind of method preparing three-dimensional cadmium sulfide nano self-assembled structures, it is characterised in that:It includes the following steps,
(1)Prepare thiocarbamide (NH2)2CS、CdCl2· 2.5H20 mixed solution or thiocarbamide (NH2)2CS、CdCl2· 2.5H20, surface
Surfactant mixed solution;
(2)Mixed solution is moved into Teflon inner liner stainless steel reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature 60-
200 DEG C, reaction time 3-20h;
(3)By step(2)In obtained product use distilled water and each eccentric cleaning of absolute ethyl alcohol 3 times respectively, then with distilled water from
Heart cleaning is primary;
(4)By step(3)Obtained yellow mercury oxide product in 60 DEG C of drying boxes dry 6 h to get to CdS nanoassembles
Structure.
2. the method according to claim 1 for preparing three-dimensional cadmium sulfide nano self-assembled structures, it is characterised in that:By right
Material proportion is adjusted, and controls three-dimensional cadmium sulfide nano self-assembled structures microscopic appearance, wherein material proportion
CdCl2· 2.5H2O:(NH2)2CS=1:1 or 1:2 or 1:3.
3. the method according to claim 1 for preparing three-dimensional cadmium sulfide nano self-assembled structures, it is characterised in that:By adding
Add surfactant, three-dimensional cadmium sulfide nano self-assembled structures microscopic appearance is controlled, wherein adding surfactant-based
Type is one in PVA polyvinyl alcohol, PEG polyethylene glycol, SDS lauryl sodium sulfate, CTAB cetyl trimethylammonium bromides
Kind.
4. the method according to claim 3 for preparing three-dimensional cadmium sulfide nano self-assembled structures, it is characterised in that:Pass through tune
Surfactant addition regulates and controls the microscopic appearance of three-dimensional cadmium sulfide nano self-assembled structures, wherein surface in section reaction solution
The adjustable range of activating agent PVA polyvinyl alcohol concentrations is 0-0.05g/mL;The adjustable range of PEG Polyethylene glycols is 0-
0.05g/mL;The adjustable range of SDS lauryl sodium sulfate concentration is 0-0.05g/mL;CTAB cetyl trimethylammonium bromides
The adjustable range of concentration is 0-0.05g/mL.
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CN109279644A (en) * | 2018-09-07 | 2019-01-29 | 浙江大学 | A kind of preparation method and product of the rodlike CdS of wolf's fang |
US20220042184A1 (en) * | 2019-08-16 | 2022-02-10 | Jiangnan University | Preparation Method and Application of Non-noble Metal Single Atom Catalyst |
CN110639555A (en) * | 2019-10-09 | 2020-01-03 | 长春工业大学 | CdS/CdIn with visible light response2S4Preparation method and application of composite nano-structured photocatalyst |
CN114984945A (en) * | 2022-06-24 | 2022-09-02 | 陕西科技大学 | CdS/V 2 O 5 Composite photocatalyst and preparation method thereof |
CN114984945B (en) * | 2022-06-24 | 2024-05-14 | 陕西科技大学 | CdS/V2O5Composite photocatalyst and preparation method thereof |
CN116371423A (en) * | 2023-04-14 | 2023-07-04 | 辽宁石油化工大学 | Mn with leaf petal-shaped three-dimensional dendritic structure x Cd 1-x Preparation method and application of S photocatalyst |
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