CN101239735A - Method for preparing cadmium sulfide nano-stick array - Google Patents
Method for preparing cadmium sulfide nano-stick array Download PDFInfo
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- CN101239735A CN101239735A CNA2008100601578A CN200810060157A CN101239735A CN 101239735 A CN101239735 A CN 101239735A CN A2008100601578 A CNA2008100601578 A CN A2008100601578A CN 200810060157 A CN200810060157 A CN 200810060157A CN 101239735 A CN101239735 A CN 101239735A
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- Prior art keywords
- cadmium
- cadmium sulfide
- substrate
- containing precursor
- water
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 23
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000002073 nanorod Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 7
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000011593 sulfur Substances 0.000 claims abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea group Chemical group NC(=S)N UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 108010024636 Glutathione Proteins 0.000 claims description 7
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 3
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 3
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical group OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 238000003491 array Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract 2
- 239000000463 material Substances 0.000 description 6
- 239000003599 detergent Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
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- Photovoltaic Devices (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a method of cadmium sulfide nano rod array, including following steps:cleaning transparent conduction substrate to remove oil stain, and processing ultrasonic treatment in acetone, ethanol and de-ionized water respectively, drying; resolving pre-substance containing cadmium, pre-substance containing sulfur and TAD in water to preparing solution; cadmium sulfide nano rod obtained by placing dried transparent conduction in substrate solution and heating, washing substrate by water after being complete reaction. The provided method of cadmium sulfide nano rod array only needs one step, the process is simple, the length of the cadmium sulfide nano rod is adjusted, the substrate is transparent, suitable for direct preparing electronic apparatus, easy to apply.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing a cadmium sulfide nanorod array.
Background
The CdS band gap is about 2.45eV, and the CdS band gap can be used for preparing quantum devices and changing the light emitting frequency and performance through quantum size effect. And thus has been widely used as a material for photocatalysis, semiconductor devices, light emitting devices, laser or infrared detectors, and light sensitive sensors. In addition, the material is an excellent infrared window and nonlinear optical material. Various optoelectronic devices such as lasers, photodetectors, optical storage devices, quantum dots, and the like have been manufactured by using the optical semiconductor device; meanwhile, the material can be used as a photovoltaic device, such as a solar cell and the like.
One-dimensional nanostructure materials are one of the most important research fronts in material science, and a great deal of research is carried out at home and abroad, particularly, one-dimensional nanowires, nanorods and the like can be synthesized by a plurality of methods, such as thermal evaporation, chemical vapor deposition, gas-liquid-solid (V-L-S) technology and the like. Among a plurality of one-dimensional nanostructures, the nano array is widely regarded as a basic construction material of a nano photoelectric device due to high-efficiency light absorption efficiency, charge separation and charge transmission capability, and thus is widely concerned by a plurality of scientific researchers at home and abroad. The most commonly used methods for the preparation of nanoarrays at present include porous alumina template method (AAO), V-L-S, chemical vapor deposition method, and solution method. For the preparation of the CdS nanorod array, the one-step solution preparation is not reported.
Chinese patent 03150807.3 discloses a method for preparing cadmium sulfide nanorods, which comprises the following steps: 1) adding thioglycollic acid into a cadmium ion-containing solution with the solubility of 0.01M according to the volume ratio of 1: 0.01-100, fully stirring, and then adding sodium sulfide with the concentration of 0.01M according to the volume ratio of 1: 0.01-100; 2) and (3) putting the prepared solution into an autoclave, treating for 1-200 hours at the temperature of 100-500 ℃, centrifuging and drying the solution to obtain the cadmium sulfide nanorod. The nano-rod prepared by the method is not suitable for directly preparing electronic devices and is not easy to popularize and apply.
Disclosure of Invention
A method for preparing cadmium sulfide nanorod arrays comprises the following steps:
(1) cleaning a transparent conductive substrate to remove oil stains, respectively performing ultrasonic treatment in acetone, ethanol and deionized water, and drying;
the transparent conductive substrate can be conductive glass or a conductive silicon wafer, and the ultrasonic treatment time is 10-15 minutes.
(2) Dissolving a cadmium-containing precursor, a sulfur-containing precursor and reduced glutathione in water to prepare a solution;
the cadmium-containing precursor is cadmium nitrate, cadmium acetate or cadmium sulfate.
The sulfur-containing precursor is thiourea, thioacetamide and sublimed sulfur.
The molar ratio of the cadmium-containing precursor to the sulfur-containing precursor to the reduced glutathione is 1: 0.1-1: 10: 1.
(3)And (3) placing the transparent conductive substrate dried in the step (1) into the solution prepared in the step (2), heating, and washing the substrate with water after complete reaction to obtain the cadmium sulfide nanorod array.
The reaction temperature is 90-250 ℃, and the reaction time is 1-24 h.
The above method takes thiourea as an example, and the reaction equation is as follows:
with the continuous rise of the temperature, a layer of CdS nano-particles is firstly formed on the transparent conductive substrate, and then the CdS nano-rod array is formed by taking the layer of nano-particles as seed crystals.
The method for preparing the cadmium sulfide nanorod array can be completed by only one step, the process is simple, the prepared cadmium sulfide nanorod is adjustable in length, and the adopted substrate is a transparent conductive substrate, so that the method is suitable for directly preparing electronic devices and is easy to popularize and apply.
Detailed Description
Example 1
1. Taking conductive glass (ITO), cleaning with detergent to remove oil stain, respectively carrying out ultrasonic treatment in acetone, ethanol and deionized water for 10 minutes in sequence, and drying;
2. dissolving 1mmol of cadmium acetate, 1mmol of thioacetamide and 0.1mmol of reduced glutathione in 80ml of water to prepare a solution;
3. and (3) placing the dried conductive glass into the solution prepared in the step (2), transferring the conductive glass into a reaction kettle, heating at the heating rate of 1 ℃/s, controlling the reaction temperature to be 90 ℃, and washing the substrate with water after reacting for 1h to obtain the cadmium sulfide nanorod array.
Example 2
1. Taking conductive glass (ITO), cleaning with detergent to remove oil stain, respectively performing ultrasonic treatment in acetone, ethanol and deionized water for 15 minutes, and drying;
2. dissolving 1mmol of cadmium nitrate, 10mmol of sublimed sulfur and 0.5mmol of reduced glutathione in 80ml of water to prepare a solution;
3. and (3) putting the dried conductive glass into the solution prepared in the step (2), transferring the conductive glass into a reaction kettle, heating at the heating rate of 1 ℃/s, controlling the reaction temperature to be 250 ℃, and washing the substrate with water after reacting for 12 hours to obtain the cadmium sulfide nanorod array.
Example 3
1. Taking a conductive silicon wafer, cleaning the conductive silicon wafer by using a detergent to remove oil stains, respectively carrying out ultrasonic treatment in acetone, ethanol and deionized water for 15 minutes, and drying;
2. dissolving 1mmol of cadmium sulfate, 5mmol of thiourea and 1mmol of reduced glutathione in 80ml of water to prepare a solution;
3. and (3) placing the dried conductive silicon wafer into the solution prepared in the step (2), transferring the conductive silicon wafer into a reaction kettle, heating at the heating rate of 1 ℃/s, controlling the reaction temperature to be 180 ℃, and washing the substrate with water after reacting for 24 hours to obtain the cadmium sulfide nanorod array.
Claims (7)
1. A method for preparing cadmium sulfide nanorod arrays comprises the following steps:
(1) cleaning a transparent conductive substrate to remove oil stains, respectively performing ultrasonic treatment in acetone, ethanol and deionized water, and drying;
(2) dissolving a cadmium-containing precursor, a sulfur-containing precursor and reduced glutathione in water to prepare a solution;
(3) and (3) placing the transparent conductive substrate dried in the step (1) into the solution prepared in the step (2), heating, and washing the substrate with water after complete reaction to obtain the cadmium sulfide nanorod array.
2. The method of claim 1, wherein: the conductive substrate is conductive glass or a conductive silicon wafer.
3. The method of claim 1, wherein: the ultrasonic treatment time in the step (1) is 10-15 minutes.
4. The method of claim 1, wherein: the cadmium-containing precursor is cadmium nitrate, cadmium acetate or cadmium sulfate.
5. The method of claim 1, wherein: the sulfur-containing precursor is thiourea, thioacetamide or sublimed sulfur.
6. The method of claim 1, wherein: the molar ratio of the cadmium-containing precursor to the sulfur-containing precursor to the reduced glutathione is 1: 0.1-1: 10: 1.
7. The method of claim 1, wherein:the reaction temperature in the step (3) is 90-250 ℃, and the reaction time is 1-24 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100601578A CN101239735B (en) | 2008-03-13 | 2008-03-13 | Method for preparing cadmium sulfide nano-stick array |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100601578A CN101239735B (en) | 2008-03-13 | 2008-03-13 | Method for preparing cadmium sulfide nano-stick array |
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| Publication Number | Publication Date |
|---|---|
| CN101239735A true CN101239735A (en) | 2008-08-13 |
| CN101239735B CN101239735B (en) | 2011-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100601578A Expired - Fee Related CN101239735B (en) | 2008-03-13 | 2008-03-13 | Method for preparing cadmium sulfide nano-stick array |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275870A (en) * | 2010-06-12 | 2011-12-14 | 国家纳米科学中心 | Water-soluble cadmium sulfide nanorod and nanometer heterostructure as well as preparation methods thereof |
| CN103508482A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Preparation method of cadmium sulfide nano-flower array |
| CN107537519A (en) * | 2017-09-30 | 2018-01-05 | 福州大学 | Cadmium sulfide two-dimensional nano rod array catalyst and its preparation method and application |
| CN110841658A (en) * | 2018-08-20 | 2020-02-28 | 南京理工大学 | Preparation method of cobalt-based sulfide nanorod array |
| CN116282133A (en) * | 2023-03-23 | 2023-06-23 | 山东大学 | Method for biosynthesizing cadmium sulfide quantum dots by using thioquinone oxidoreductase |
-
2008
- 2008-03-13 CN CN2008100601578A patent/CN101239735B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275870A (en) * | 2010-06-12 | 2011-12-14 | 国家纳米科学中心 | Water-soluble cadmium sulfide nanorod and nanometer heterostructure as well as preparation methods thereof |
| CN102275870B (en) * | 2010-06-12 | 2014-03-12 | 国家纳米科学中心 | Water-soluble cadmium sulfide nanorod and nanometer heterostructure as well as preparation methods thereof |
| CN103508482A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Preparation method of cadmium sulfide nano-flower array |
| CN107537519A (en) * | 2017-09-30 | 2018-01-05 | 福州大学 | Cadmium sulfide two-dimensional nano rod array catalyst and its preparation method and application |
| CN107537519B (en) * | 2017-09-30 | 2019-08-09 | 福州大学 | Cadmium sulfide two-dimensional nano stick array catalyst and its preparation method and application |
| CN110841658A (en) * | 2018-08-20 | 2020-02-28 | 南京理工大学 | Preparation method of cobalt-based sulfide nanorod array |
| CN116282133A (en) * | 2023-03-23 | 2023-06-23 | 山东大学 | Method for biosynthesizing cadmium sulfide quantum dots by using thioquinone oxidoreductase |
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| Publication number | Publication date |
|---|---|
| CN101239735B (en) | 2011-05-04 |
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Granted publication date: 20110504 Termination date: 20140313 |