CN109133155A - The preparation method of CdS nano-rod film - Google Patents
The preparation method of CdS nano-rod film Download PDFInfo
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- CN109133155A CN109133155A CN201710498718.1A CN201710498718A CN109133155A CN 109133155 A CN109133155 A CN 109133155A CN 201710498718 A CN201710498718 A CN 201710498718A CN 109133155 A CN109133155 A CN 109133155A
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- cds nano
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- 239000002073 nanorod Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 17
- UDWCKMMKPOGURO-UHFFFAOYSA-N 1,2-dihydropyrazolo[3,4-b]pyridin-4-one Chemical compound O=C1C=CNC2=C1C=NN2 UDWCKMMKPOGURO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229950004394 ditiocarb Drugs 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 7
- 239000012047 saturated solution Substances 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- UQJQVUOTMVCFHX-UHFFFAOYSA-L nabam Chemical compound [Na+].[Na+].[S-]C(=S)NCCNC([S-])=S UQJQVUOTMVCFHX-UHFFFAOYSA-L 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 5
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- PLXMOAALOJOTIY-FPTXNFDTSA-N Aesculin Natural products OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O)[C@H]1Oc2cc3C=CC(=O)Oc3cc2O PLXMOAALOJOTIY-FPTXNFDTSA-N 0.000 description 1
- QKFSMXLZDRRYNC-UHFFFAOYSA-N C(CCCCC)P(O)(O)O Chemical compound C(CCCCC)P(O)(O)O QKFSMXLZDRRYNC-UHFFFAOYSA-N 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical group [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Photovoltaic Devices (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of CdS nano-rod film, and the preparation method comprises the following steps: S1, by sodium diethyldithiocarbamate and CdCl2·2.5H2O, which reacts, is made cadmium diethyl dithiocarbamate；S2, CdS nano-rod film will be obtained by addition solvent progress solvent thermal reaction in cadmium diethyl dithiocarbamate；S3, CdS nano-rod film is used into CdCl2Carry out wet-treating.The present invention carries out CdCl to CdS nano-rod film2Wet-treating improves the crystallinity of film, reduces defect state density, substantially increase short-circuit current density, battery life can be improved.
Description
Technical field
The invention belongs to photovoltaic technology field, more particularly to a kind of preparation method of CdS nano-rod film.
Background technique
The nanocrystalline peculiar electrical and optical properties different from bulk of one dimension semiconductor, in light emitting diode, the efficient sun
There is huge application prospect in the fields such as energy battery, quantum dot microlaser and the polychrome biomarker based on luminescence generated by light, because
This, synthesizing one-dimensional semiconductor nano has become the hot spot of people's research in recent years.
The nanocrystalline preparation method of one dimension semiconductor can be divided into physical method and chemical method, and general physical method needs precision
Expensive large scale equipment and extreme harsh experiment condition, in comparison, chemical rule has easily operated, cheap and simple
Single effective feature.The nanocrystalline liquid phase chemical method of preparation one dimension semiconductor mainly has at present: solvent-thermal method, liquid crystal templated
Method, polymer assisting growth, electrochemical deposition method, vapour deposition process, the method for partial cation exchange and colloid chemistry methods etc..
Since the report colloid chemistry methods such as Murray in 1993 prepare semiconductor nano, which becomes most widely used at present
Method is for example, Peng etc. assists synthesis CdSe nanometer rods using hexyl phosphorous acid and the stronger coordination ability of cadmium atom earliest；
Cheon etc. is greater than the CdS nanometer rods of 6nm using octadecylamine as ligand pyrolytic unimolecule precursor synthesis diameter；
Prashan etc. is different using coordination ability of the ligand to CdSe cluster and synthesizes CdSe nano wire.
However the crystallinity of CdS nano-rod film in the prior art is lower, defect state density with higher, therefore,
The performance of CdS nano-rod film is greatly affected.
Therefore, in view of the above-mentioned problems, it is necessary to propose a kind of preparation method of CdS nano-rod film.
Summary of the invention
In view of this, the present invention provides a kind of preparation methods of CdS nano-rod film.
In order to achieve the above-mentioned object of the invention, the present invention provides a kind of preparation method of CdS nano-rod film, the preparation side
Method the following steps are included:
S1, by sodium diethyldithiocarbamate and CdCl2·2.5H2O, which reacts, is made cadmium diethyl dithiocarbamate；
S2, CdS nano-rod film will be obtained by addition solvent progress solvent thermal reaction in cadmium diethyl dithiocarbamate；
S3, CdS nano-rod film is used into CdCl2Carry out wet-treating.
As a further improvement of the present invention, sodium diethyldithiocarbamate and CdCl in the step S12·
2.5H2The molar concentration rate of O is 3:1 ~ 4:1.
As a further improvement of the present invention, the step S2 specifically:
Ethylenediamine is added in cadmium diethyl dithiocarbamate and obtains mixed solution, solvent heat is anti-at 200 DEG C~230 DEG C
Answer 12h~for 24 hours.
As a further improvement of the present invention, the step S3 specifically:
S31, by CdS nano-rod film in N2It is carried out dehydrating in atmosphere；
S32, by CdCl2It is added in methanol solution and configures saturated solution, and CdS nano-rod film is placed in 5 in saturated solution ~
It is taken out after 10s；
S33, volatilize CdS nano-rod film surface methanol, in N2Drying is heat-treated in atmosphere.
As a further improvement of the present invention, the temperature of dehydration is 100 ~ 200 DEG C in the step S31, the time 1
~2h。
As a further improvement of the present invention, the temperature of step S33 heat treatment is 200 ~ 300 DEG C, the time is 30 ~
60min。
Compared with prior art, the beneficial effects of the present invention are:
The present invention carries out CdCl to CdS nano-rod film2Wet-treating improves the crystallinity of film, it is close to reduce defect state
Degree, substantially increases short-circuit current density, battery life can be improved.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in invention, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is the preparation method process flow chart of CdS nano-rod film in the embodiment of the invention.
Specific embodiment
Below by a detailed description of the technical solution in the embodiment of the present invention is provided, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Join shown in Fig. 1, the preparation method of one of embodiment of the invention CdS nano-rod film, the preparation
Method the following steps are included:
S1, by sodium diethyldithiocarbamate and CdCl2·2.5H2O, which reacts, is made cadmium diethyl dithiocarbamate；
S2, CdS nano-rod film will be obtained by addition solvent progress solvent thermal reaction in cadmium diethyl dithiocarbamate；
S3, CdS nano-rod film is used into CdCl2Carry out wet-treating.
Specifically, sodium diethyldithiocarbamate and CdCl in step S12·2.5H2The molar concentration rate of O be 3:1 ~
4:1。
In a preferred embodiment of the invention, step S2 specifically:
Ethylenediamine is added in cadmium diethyl dithiocarbamate and obtains mixed solution, solvent heat is anti-at 200 DEG C~230 DEG C
Answer 12h~for 24 hours.
Wherein, step S3 specifically:
S31, by CdS nano-rod film in N2It is carried out dehydrating in atmosphere；
S32, by CdCl2It is added in methanol solution and configures saturated solution, and CdS nano-rod film is placed in 5 in saturated solution ~
It is taken out after 10s；
S33, volatilize CdS nano-rod film surface methanol, in N2Drying is heat-treated in atmosphere.
Preferably, the temperature of dehydration is 100 ~ 200 DEG C in step S31, and the time is 1 ~ 2h；Step S33 heat treatment
Temperature is 200 ~ 300 DEG C, and the time is 30 ~ 60min.
As can be seen from the above technical solutions, the present invention carries out CdCl to CdS nano-rod film2Wet-treating improves
The crystallinity of film, reduces defect state density, substantially increases short-circuit current density, and battery life can be improved.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the embodiments can also be closed suitably, and forming those skilled in the art can
With the other embodiments of understanding.
Claims (6)
1. a kind of preparation method of CdS nano-rod film, which is characterized in that the preparation method comprises the following steps:
S1, by sodium diethyldithiocarbamate and CdCl2·2.5H2O, which reacts, is made cadmium diethyl dithiocarbamate；
S2, CdS nano-rod film will be obtained by addition solvent progress solvent thermal reaction in cadmium diethyl dithiocarbamate；
S3, CdS nano-rod film is used into CdCl2Carry out wet-treating.
2. the preparation method of CdS nano-rod film according to claim 1, which is characterized in that diethyl in the step S1
Base nabam and CdCl2·2.5H2The molar concentration rate of O is 3:1 ~ 4:1.
3. the preparation method of CdS nano-rod film according to claim 1, which is characterized in that the step S2 specifically:
Ethylenediamine is added in cadmium diethyl dithiocarbamate and obtains mixed solution, solvent heat is anti-at 200 DEG C~230 DEG C
Answer 12h~for 24 hours.
4. the preparation method of CdS nano-rod film according to claim 1, which is characterized in that the step S3 specifically:
S31, by CdS nano-rod film in N2It is carried out dehydrating in atmosphere；
S32, by CdCl2It is added in methanol solution and configures saturated solution, and CdS nano-rod film is placed in 5 ~ 10s in saturated solution
After take out；
S33, volatilize CdS nano-rod film surface methanol, in N2Drying is heat-treated in atmosphere.
5. the preparation method of CdS nano-rod film according to claim 4, which is characterized in that be dehydrated in the step S31
The temperature of processing is 100 ~ 200 DEG C, and the time is 1 ~ 2h.
6. the preparation method of CdS nano-rod film according to claim 4, which is characterized in that the step S33 heat treatment
Temperature be 200 ~ 300 DEG C, the time be 30 ~ 60min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710498718.1A CN109133155A (en) | 2017-06-27 | 2017-06-27 | The preparation method of CdS nano-rod film |
| PCT/CN2017/091450 WO2019000478A1 (en) | 2017-06-27 | 2017-07-03 | Preparation method of cds nano-rod film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710498718.1A CN109133155A (en) | 2017-06-27 | 2017-06-27 | The preparation method of CdS nano-rod film |
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| CN109133155A true CN109133155A (en) | 2019-01-04 |
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| CN201710498718.1A Withdrawn CN109133155A (en) | 2017-06-27 | 2017-06-27 | The preparation method of CdS nano-rod film |
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| WO (1) | WO2019000478A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172643A (en) * | 2007-09-30 | 2008-05-07 | 浙江大学 | Method of producing cadmium sulfide nano-stick array |
| CN101698501A (en) * | 2009-10-30 | 2010-04-28 | 陕西科技大学 | Method for preparing floriform cadmium sulfide nano-particles in microwave hydrothermal mode |
| CN101704546B (en) * | 2009-11-12 | 2011-09-14 | 同济大学 | Method for reversely synthesizing cadmium sulfide nano wires by antigravity |
| US9637828B2 (en) * | 2013-03-12 | 2017-05-02 | Ut-Battelle, Llc | Electrochemical method for synthesizing metal-containing particles and other objects |
| CN105688945B (en) * | 2016-03-22 | 2018-06-15 | 福州大学 | MoS2Nanometer sheet/CdS nanowire core shell structure composite photo-catalysts |
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- 2017-06-27 CN CN201710498718.1A patent/CN109133155A/en not_active Withdrawn
- 2017-07-03 WO PCT/CN2017/091450 patent/WO2019000478A1/en active Application Filing
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Application publication date: 20190104 |
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