CN101239735B - Method for preparing cadmium sulfide nano-stick array - Google Patents
Method for preparing cadmium sulfide nano-stick array Download PDFInfo
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- CN101239735B CN101239735B CN2008100601578A CN200810060157A CN101239735B CN 101239735 B CN101239735 B CN 101239735B CN 2008100601578 A CN2008100601578 A CN 2008100601578A CN 200810060157 A CN200810060157 A CN 200810060157A CN 101239735 B CN101239735 B CN 101239735B
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- China
- Prior art keywords
- cadmium
- sulfide nano
- cadmium sulfide
- presoma
- substrate
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 22
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 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
- 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
- 239000011593 sulfur Substances 0.000 claims abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S 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
- 239000011521 glass Substances 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 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
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound 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
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000004140 cleaning Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 239000002073 nanorod Substances 0.000 abstract 4
- 239000000126 substance Substances 0.000 abstract 2
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000003599 detergent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 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
- 239000004566 building material Substances 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 235000010265 sodium sulphite Nutrition 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 can be adjusted, the adopted substrate is transparent conduction substrate, therefore, the method is suitable for direct preparing electronic apparatus, easy to be popularized and applied.
Description
Technical field
The present invention relates to technical field of nano material, relate in particular to a kind of method for preparing cadmium sulfide nano-stick array.
Background technology
The CdS band gap is about 2.45eV, can be used for preparing quantum device, by quantum size effect, changes glow frequency and performance.Therefore be widely used for material as photochemical catalysis, semiconducter device, luminescent device, laser or infrared eye and photosensor.It still is a kind of good infrared window and nonlinear optical material in addition.Made multiple opto-electronic device now, as laser apparatus, photodetector, light storage device, quantum dot etc. with it; Can also be used to doing photovoltaic device simultaneously, for example solar cell etc.
One-dimensional nano structure material is one of most important research forward position in the Materials science, this has been carried out a large amount of research both at home and abroad, particularly unidimensional nano wire, nanometer rod etc., can be by a lot of methods, such as thermal evaporation, chemical vapour deposition, gas-liquid-solid (V-L-S) technology etc. is synthesized.In numerous one dimension Nano structures, efficiency of light absorption and charge separation and charge transport ability are widely regarded as the basic building material of nano photoelectric device to nano-array owing to having efficiently, thereby are subjected to the extensive concern of lot of domestic and foreign researcher.The most frequently used method for preparing most at present nano-array comprises that porous alumina touches plate method (AAO), V-L-S, chemical Vapor deposition process and solution method.For the preparation of CdS nanometer stick array, the single stage method formulations prepared from solutions yet there are no report.
Chinese patent 03150807.3 discloses a kind of preparation method of cadmium sulfide nano-stick, may further comprise the steps: be containing in the cadmium-ion solution of 0.01M 1) in solubility, 1: 0.01 by volume～100 ratios add Thiovanic acid, after fully stirring, 1: 0.01 by volume～100 ratios adding concentration is 0.01M sodium sulphite again; 2) the above-mentioned solution for preparing is put into autoclave, in 100～500 ℃ of temperature ranges, handled 1～200 hour,, get cadmium sulfide nano-stick then with solution centrifugal, drying.The nanometer rod of this patented method preparation is unsuitable for directly preparing electron device, is not easy to be promoted application.
Summary of the invention
A kind of method for preparing cadmium sulfide nano-stick array may further comprise the steps:
(1) transparent conduction base sheet is cleaned degreasing, and in acetone, ethanol and deionized water, carry out supersound process respectively, oven dry;
Transparent conduction base sheet can be selected conductive glass or conductive silicon chip for use, and the supersound process time is 10～15 minutes.
(2) will contain cadmium presoma, sulfur-bearing presoma and the reduced glutathione solution that makes soluble in water;
Containing the cadmium presoma is cadmium nitrate, cadmium acetate or Cadmium Sulphate.
The sulfur-bearing presoma is thiocarbamide, thioacetamide, sublimed sulphur.
The mol ratio that contains between cadmium presoma, sulfur-bearing presoma and the reduced glutathione is 1: 1: 0.1～1: 10: 1.
(3) transparent conduction base sheet with oven dry in the step (1) places the solution of step (2) preparation also to heat, and the water rinse substrate makes cadmium sulfide nano-stick array after the complete reaction.
Temperature of reaction is for being 90～250 ℃, and the reaction times is 1～24h.
Aforesaid method is example with the thiocarbamide, and its reaction equation is as follows:
Along with the continuous rising of temperature, on transparent conduction base sheet, at first form one deck CdS nanoparticle, then with this layer nanoparticle as crystal seed, form the CdS nanometer stick array.
The method for preparing cadmium sulfide nano-stick array provided by the invention only needs can finish once going on foot, and technology is simple, the cadmium sulfide nano-stick adjustable length that makes, and the substrate of employing is transparent conductive substrate, is suitable for directly preparing electron device, is promoted easily and uses.
Embodiment
Embodiment 1
1. get conductive glass (ITO), after liquid detergent cleaning degreasing, in acetone, ethanol and deionized water, successively carried out supersound process respectively 10 minutes and oven dry;
2. 1mmol cadmium acetate, 1mmol thioacetamide and 0.1mmol reduced glutathione are dissolved in the 80ml water and make solution;
3. the conductive glass with oven dry places the solution of step 2 preparation and is transferred to the reactor heating, and heating rate is 1 ℃/s, and control reaction temperature is 90 ℃, and water rinse substrate behind the reaction 1h makes cadmium sulfide nano-stick array.
Embodiment 2
1. get conductive glass (ITO), after liquid detergent cleaning degreasing, in acetone, ethanol and deionized water, carried out supersound process respectively 15 minutes and oven dry;
2. 1mmol cadmium nitrate, 10mmol sublimed sulphur and 0.5mmol reduced glutathione are dissolved in the 80ml water and make solution;
3. the conductive glass of oven dry is inserted in the solution of step 2 preparation and be transferred to the reactor heating, heating rate is 1 ℃/s, and control reaction temperature is 250 ℃, and water rinse substrate behind the reaction 12h makes cadmium sulfide nano-stick array.
Embodiment 3
1. get conductive silicon chip, after liquid detergent cleaning degreasing, in acetone, ethanol and deionized water, carried out supersound process respectively 15 minutes and oven dry;
2. 1mmol Cadmium Sulphate, 5mmol thiocarbamide and 1mmol reduced glutathione are dissolved in the 80ml water and make solution;
3. the conductive silicon chip with oven dry places the solution of step 2 preparation and is transferred to the reactor heating, and heating rate is 1 ℃/s, and control reaction temperature is 180 ℃, and water rinse substrate behind the reaction 24h makes cadmium sulfide nano-stick array.
Claims (6)
1. method for preparing cadmium sulfide nano-stick array may further comprise the steps:
(1) transparent conduction base sheet is cleaned degreasing, and in acetone, ethanol and deionized water, carry out supersound process respectively, oven dry;
(2) will contain cadmium presoma, sulfur-bearing presoma and the reduced glutathione solution that makes soluble in water;
(3) transparent conduction base sheet of oven dry in the step (1) is placed the solution of step (2) preparation and heat with the speed of 1 ℃/s, at 90～250 ℃ of reaction 1～24h down, water rinse substrate after the complete reaction makes cadmium sulfide nano-stick array.
2. method according to claim 1 is characterized in that: described conductive substrate is conductive glass or conductive silicon chip.
3. method according to claim 1 is characterized in that: the supersound process time is 10～15 minutes in the described step (1).
4. method according to claim 1 is characterized in that: the described cadmium presoma that contains is cadmium nitrate, cadmium acetate or Cadmium Sulphate.
5. method according to claim 1 is characterized in that: described sulfur-bearing presoma is thiocarbamide, thioacetamide or sublimed sulphur.
6. method according to claim 1 is characterized in that: the described mol ratio that contains cadmium presoma, sulfur-bearing presoma and reduced glutathione is 1: 1: 0.1～1: 10: 1.
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 CN101239735A (en) | 2008-08-13 |
| CN101239735B true CN101239735B (en) | 2011-05-04 |
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| CN2008100601578A Expired - Fee Related CN101239735B (en) | 2008-03-13 | 2008-03-13 | Method for preparing cadmium sulfide nano-stick array |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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Granted publication date: 20110504 Termination date: 20140313 |