CN103508482A - Preparation method of cadmium sulfide nano-flower array - Google Patents
Preparation method of cadmium sulfide nano-flower array Download PDFInfo
- Publication number
- CN103508482A CN103508482A CN201210224000.0A CN201210224000A CN103508482A CN 103508482 A CN103508482 A CN 103508482A CN 201210224000 A CN201210224000 A CN 201210224000A CN 103508482 A CN103508482 A CN 103508482A
- Authority
- CN
- China
- Prior art keywords
- cadmium
- glass substrate
- precursor
- sulfide nano
- cadmium sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Surface Treatment Of Glass (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses a preparation method of a cadmium sulfide nano-flower array on a transparent conductive glass substrate. The preparation method mainly comprises the following steps: (1) putting a cleaned transparent conductive glass substrate into an aqueous solution consisting of a cadmium-containing precursor, a sulfur-containing precursor and reduced glutathione, heating, then taking the transparent conductive glass substrate out of the solution after the reaction is complete, and washing with deionized water to obtain a cadmium sulfide nano-rod array; (2) performing oxygen plasma cleaning treatment on the transparent conductive glass substrate on which the cadmium sulfide nano-rod array grows, or treating the surface of the transparent conductive glass substrate by using dilute acid; (3) putting the transparent conductive glass substrate into the aqueous solution consisting of the cadmium-containing precursor, the sulfur-containing precursor and the reduced glutathione again, heating, then taking the transparent conductive glass substrate out of the solution after the reaction is completed, and washing with deionized water to obtain a cadmium sulfide nano-flower array. The preparation method is simple and controllable in operation and is conductive to directly preparing electronic devices.
Description
Technical field
The present invention designs nanotechnology Material Field, relates in particular to a kind of preparation method of cadmium sulfide nano flower array.
Background technology
The nano-array with branched structure, compared with nano particle and monodimension nano stick array, because it has better electric charge transmission and absorbing properties, has caused widely and has paid close attention at material science.Can be used at present the technology of nano-array that preparation has branched structure mainly contains: thermal vapor deposition method, nanometer ball etching method, micella aggregation method, microwave heating method and solution chemical method.Wherein, solution chemical method is simple to operate, both economical.
Cadmium Sulfide is that a kind of band gap is the important II– VI family semi-conductor of 2.4eV, at aspects such as photodiode, panel display screen, electric communication, data storage and solar cells, is widely used.People (the Crystal Growth& such as Sung Oh Cho; Design 8 (2008) 629-630; Crystal Growth& Design 9 (2009) 5259-5265; J.Phys.Chem.C 113 (2009) 10981 – 10989; J.Phys.Chem.C 114 (2010) 14029-14035; Journal ofAlloys and Compounds 509 (2011) L353-L358) in solution system, prepared the cadmium sulfide nano branched structure disperseing, but the cadmium sulfide nano branched structure obtaining is unsuitable for directly preparing electron device, be not easy to be applied.Chinese patent 200810060157.8 discloses a kind of method of preparing cadmium sulfide nano-stick array on conductive substrate, can be directly used in and prepare electron device, but the cadmium sulfide nano that the cadmium sulfide nano-stick array that this method obtains obtains compared with the present invention flower array, specific surface area is little, a little less than absorbing properties.Therefore, be simultaneously with solution chemical method, control cadmium sulfide nano branched structure and in suprabasil nano-array or a kind of challenge, the method that especially solution chemical method is prepared the colored array of cadmium sulfide nano in transparent conductive substrates has no report.
Summary of the invention
A preparation method for cadmium sulfide nano flower array, comprises the following steps:
(1) transparent conducting glass substrate is cleaned and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the transparent conducting glass substrate cleaning up is placed in to the heated in water solution forming containing cadmium precursor, sulfur-bearing precursor and reduced glutathione, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
Transparent conducting glass substrate is the Indium sesquioxide glass of mixing tin, mix the tin oxide glass of fluorine or mix the zinc oxide glass of aluminium, and the ultrasonic cleaning time is 10-30min.
Containing cadmium precursor, be cadmium nitrate, cadmium acetate or Cadmium Sulphate.
Sulfur-bearing precursor is thiocarbamide, thiosemicarbazide, sublimed sulphur or thioacetamide.
Mol ratio containing cadmium precursor, sulfur-bearing precursor and reduced glutathione is: 1:1:0.1 ~ 1:4:1;
Temperature of reaction is 120-250 ℃, and the reaction times is 1-24h;
(2) the long transparent conducting glass substrate that has a cadmium sulfide nano-stick array is carried out in oxygen plasma cleaning apparatus to oxygen plasma clean or with its surface of dilute acid pretreatment;
The power of oxygen plasma clean is 50-200W, and pressure is 0.1-1mbar, and the treatment time is 5-30min;
Diluted acid is that volume ratio is 1% ~ 30% hydrofluoric acid, hydrochloric acid or nitric acid, and the treatment time is 5s ~ 30min;
(3) by processing the transparent conducting glass substrate of surperficial length by cadmium sulfide nano-stick array, be again placed in the heated in water solution forming containing cadmium precursor, sulfur-bearing precursor and reduced glutathione, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano flower array.
Containing cadmium precursor, be cadmium nitrate, cadmium acetate or Cadmium Sulphate.
Sulfur-bearing precursor is thiocarbamide, thiosemicarbazide, sublimed sulphur or thioacetamide.
Mol ratio containing cadmium precursor, sulfur-bearing precursor and reduced glutathione is: 1:1:0.1 ~ 1:4:1;
Temperature of reaction is 120-250 ℃, and the reaction times is 1-24h;
The preparation method of the cadmium sulfide nano flower array that the present invention is used, simple to operate controlled, be conducive to directly prepare electron device.
Accompanying drawing explanation
The SEM figure (low power enlarged view b, high magnification map d) of the cadmium sulfide nano-stick array preparing in transparent conducting glass substrate in Fig. 1 embodiment 1,2,3,4 or 5 (low power enlarged view a, high magnification map c) and cadmium sulfide nano flower array.
Embodiment
In order to further illustrate the present invention, enumerate following examples, but it does not limit the defined invention scope of each accessory claim.
Embodiment 1
1. the Indium sesquioxide substrate of glass of mixing tin is cleaned to 15min and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the Indium sesquioxide substrate of glass of mixing tin cleaning up is placed in and fills the Cadmium Sulphate that mol ratio is 1:1:0.6: thiocarbamide: the reactor of the aqueous solution that reduced glutathione forms (volumetric molar concentration containing cadmium precursor is 48mmol/L) is in 120 ℃ of heating 12h, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
2. by long, have the Indium sesquioxide substrate of glass of mixing tin of cadmium sulfide nano-stick array to carry out oxygen plasma clean, power is 120W, and pressure is 1mbar, and the treatment time is 5min.
3. there is the Indium sesquioxide substrate of glass of mixing tin of cadmium sulfide nano-stick array to be again placed in the length of processing surface and fill the cadmium nitrate that mol ratio is 1:4:1: thiocarbamide: the reactor of reduced glutathione (volumetric molar concentration containing cadmium precursor is 48mmol/L), in 200 ℃ of heating 2h, makes cadmium sulfide nano flower array; Embodiment 2
1. the tin oxide glass substrate of mixing fluorine is cleaned to 20min and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the tin oxide glass substrate of mixing fluorine cleaning up is placed in and fills the cadmium acetate that mol ratio is 1:3:0.2: thiocarbamide: the reactor of the aqueous solution that reduced glutathione forms (volumetric molar concentration containing cadmium precursor is 48mmol/L) is in 220 ℃ of heating 3.5h, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
2. by long, there is the tin oxide glass substrate of mixing fluorine of cadmium sulfide nano-stick array to immerse 2min in the hydrofluoric acid aqueous solution that volume ratio is 10%.
3. there is the tin oxide glass substrate of mixing fluorine of cadmium sulfide nano-stick array to be again placed in the length of processing surface and fill the cadmium acetate that mol ratio is 1:2:0.8: thiocarbamide: the reactor of reduced glutathione (volumetric molar concentration containing cadmium precursor is 48mmol/L), in 140 ℃ of heating 3.5h, makes cadmium sulfide nano flower array;
Embodiment 3
1. the tin oxide glass substrate of mixing fluorine is cleaned to 30min and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the tin oxide glass substrate of mixing fluorine cleaning up is placed in and fills the Cadmium Sulphate that mol ratio is 1:4:1: thioacetamide: the reactor of the aqueous solution that reduced glutathione forms (volumetric molar concentration containing cadmium precursor is 48mmol/L) is in 150 ℃ of heating 4h, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
2. by long, there is the tin oxide glass substrate of mixing fluorine of cadmium sulfide nano-stick array to immerse 5min in the hydrofluoric acid aqueous solution that volume ratio is 15%.
3. there is the tin oxide glass substrate of mixing fluorine of cadmium sulfide nano-stick array to be again placed in the length of processing surface and fill the Cadmium Sulphate that mol ratio is 1:2:0.4: thioacetamide: the reactor of reduced glutathione (volumetric molar concentration containing cadmium precursor is 48mmol/L), in 220 ℃ of heating 3h, makes cadmium sulfide nano flower array;
Embodiment 4
1. the zinc oxide substrate of glass of mixing aluminium is cleaned to 15min and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the zinc oxide substrate of glass of mixing aluminium cleaning up is placed in and fills the cadmium nitrate that mol ratio is 1:1:0.6: thioacetamide: the reactor of the aqueous solution that reduced glutathione forms (volumetric molar concentration containing cadmium precursor is 48mmol/L) is in 200 ℃ of heating 4h, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
2. by long, there is the zinc oxide substrate of glass of mixing aluminium of cadmium sulfide nano-stick array to immerse 25min in the aqueous nitric acid that volume ratio is 5%.
3. there is the zinc oxide substrate of glass of mixing aluminium of cadmium sulfide nano-stick array to be again placed in the length of processing surface and fill the cadmium nitrate that mol ratio is 1:1:0.6: thioacetamide: the reactor of the aqueous solution that reduced glutathione (volumetric molar concentration containing cadmium precursor is 48mmol/L) forms, in 160 ℃ of heating 3h, makes cadmium sulfide nano flower array;
Embodiment 5
1. the Indium sesquioxide substrate of glass of mixing tin is cleaned to 10min and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively, afterwards the Indium sesquioxide substrate of glass of mixing tin cleaning up is placed in and fills the Cadmium Sulphate that mol ratio is 1:2:0.6: thiosemicarbazide: the reactor of the aqueous solution that reduced glutathione forms (volumetric molar concentration containing cadmium precursor is 48mmol/L) is in 170 ℃ of heating 12h, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
2. by long, have the Indium sesquioxide substrate of glass of mixing tin of cadmium sulfide nano-stick array to carry out oxygen plasma clean, power is 200W, and pressure is 0.5mbar, and the treatment time is 15min.
3. there is the Indium sesquioxide substrate of glass of mixing tin of cadmium sulfide nano-stick array to be again placed in the length of processing surface and fill the cadmium nitrate that mol ratio is 1:4:1: sublimed sulphur: the reactor of reduced glutathione (volumetric molar concentration containing cadmium precursor is 48mmol/L), in 130 ℃ of heating 24h, makes cadmium sulfide nano flower array.
Claims (5)
1. cadmium sulfide nano is spent a preparation method for array, comprises the following steps:
(1) the transparent conducting glass substrate cleaning up is placed in to the heated in water solution forming containing cadmium precursor, sulfur-bearing precursor and reduced glutathione, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano-stick array;
Containing cadmium precursor, be cadmium nitrate, cadmium acetate or Cadmium Sulphate; Sulfur-bearing precursor is thiocarbamide, thiosemicarbazide, sublimed sulphur or thioacetamide; Mol ratio containing cadmium precursor, sulfur-bearing precursor and reduced glutathione is: 1:1:0.1 ~ 1:4:1; Temperature of reaction is 120-250 ℃, and the reaction times is 1-24h;
(2) the long transparent conducting glass substrate that has a cadmium sulfide nano-stick array is carried out to oxygen plasma clean or with its surface of dilute acid pretreatment;
The power of oxygen plasma clean is 50-200W, and pressure is 0.1-1mbar, and the treatment time is 5-30min;
Diluted acid is that volume ratio is 1% ~ 30% hydrofluoric acid, hydrochloric acid or nitric acid, and the treatment time is 5s ~ 30min;
(3) by processing the transparent conducting glass substrate of surperficial length by cadmium sulfide nano-stick array, be again placed in the heated in water solution forming containing cadmium precursor, sulfur-bearing precursor and reduced glutathione, after reacting completely, transparent conducting glass substrate is taken out from solution, with deionized water, rinse well, make cadmium sulfide nano flower array;
Containing cadmium precursor, be cadmium nitrate, cadmium acetate or Cadmium Sulphate; Sulfur-bearing precursor is thiocarbamide, thiosemicarbazide, sublimed sulphur or thioacetamide; Mol ratio containing cadmium precursor, sulfur-bearing precursor and reduced glutathione is: 1:1:0.1 ~ 1:4:1; Temperature of reaction is 120-250 ℃, and the reaction times is 1-24h.
2. method according to claim 1, is characterized in that: described transparent conducting glass substrate is the Indium sesquioxide glass of mixing tin, mix the tin oxide glass of fluorine or mix the zinc oxide glass of aluminium.
3. method according to claim 1, is characterized in that:
Volumetric molar concentration containing cadmium precursor in described step (1) aqueous solution is 30-60mmol/L.
4. method according to claim 1, is characterized in that:
The transparent conducting glass substrate cleaning up is that transparent conducting glass substrate is cleaned and dried up in liquid detergent, acetone, Virahol, dehydrated alcohol and deionized water for ultrasonic successively.
5. method according to claim 4, is characterized in that: in described step (1), ultrasonic time is 10-30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210224000.0A CN103508482A (en) | 2012-06-29 | 2012-06-29 | Preparation method of cadmium sulfide nano-flower array |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210224000.0A CN103508482A (en) | 2012-06-29 | 2012-06-29 | Preparation method of cadmium sulfide nano-flower array |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103508482A true CN103508482A (en) | 2014-01-15 |
Family
ID=49891978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210224000.0A Pending CN103508482A (en) | 2012-06-29 | 2012-06-29 | Preparation method of cadmium sulfide nano-flower array |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103508482A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045106A (en) * | 2014-05-22 | 2014-09-17 | 南京邮电大学 | Supercritical carbon dioxide method for preparing cadmium sulfide nanoparticles |
| CN106904650A (en) * | 2017-03-14 | 2017-06-30 | 扬州大学 | A kind of water-soluble CdS nanocrystalline preparation method |
| CN109616550A (en) * | 2018-11-16 | 2019-04-12 | 常州大学 | A kind of raising Sb2Se3The method of film crystal grain columnar growth trend |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239735A (en) * | 2008-03-13 | 2008-08-13 | 浙江大学 | Method for preparing cadmium sulfide nano-stick array |
-
2012
- 2012-06-29 CN CN201210224000.0A patent/CN103508482A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239735A (en) * | 2008-03-13 | 2008-08-13 | 浙江大学 | Method for preparing cadmium sulfide nano-stick array |
Non-Patent Citations (2)
| Title |
|---|
| FEI CHEN ET AL.: "One-Step Fabrication of CdS Nanorod Arrays via Solution Chemistry", 《J. PHYS. CHEM. C》, 31 December 2008 (2008-12-31), pages 13457 * |
| V. I. KORSOUNSKI ET AL.: "Investigation of nanocrystalline CdS±glutathione particles by radial distribution function", 《JOURNAL OF APPLIED CRYSTALLOGRAPHY》, 31 December 2003 (2003-12-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045106A (en) * | 2014-05-22 | 2014-09-17 | 南京邮电大学 | Supercritical carbon dioxide method for preparing cadmium sulfide nanoparticles |
| CN104045106B (en) * | 2014-05-22 | 2015-06-10 | 南京邮电大学 | Supercritical carbon dioxide method for preparing cadmium sulfide nanoparticles |
| CN106904650A (en) * | 2017-03-14 | 2017-06-30 | 扬州大学 | A kind of water-soluble CdS nanocrystalline preparation method |
| CN109616550A (en) * | 2018-11-16 | 2019-04-12 | 常州大学 | A kind of raising Sb2Se3The method of film crystal grain columnar growth trend |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104992990B (en) | A kind of method for reducing surface light reflectivity of silicon chip | |
| CN103523827B (en) | There is the method for making of the dendritic titanium dioxide array of three-dimensional of swift electron transmission performance | |
| CN105039938B (en) | The method that a kind of list source presoma prepares the optoelectronic pole of α-ferric oxide film | |
| CN105498773A (en) | Preparation method for doped iron oxide nanorod catalyst | |
| CN101916670A (en) | Titanium dioxide nanoflower film photoanode and preparation method thereof | |
| CN103882494A (en) | Preparation method of Cu2O/ZnO heterojunction material | |
| CN103746077A (en) | Organic-inorganic composite solar cell and manufacturing method thereof | |
| CN103508482A (en) | Preparation method of cadmium sulfide nano-flower array | |
| CN103618047B (en) | A kind of environmental protection heavy metal free quantum dot solar cell and preparation method thereof | |
| CN109148641A (en) | The method of modifying of copper zinc tin sulfur selenium thin-film solar cells and preparation method thereof and back electrode | |
| CN105761940A (en) | Lanthanum ferrite film photoelectrode and preparation method thereof | |
| CN103151463A (en) | Organic solar battery and preparation method thereof | |
| CN105161572B (en) | A kind of multilayer coated preparation method of the ink of ormolu sulfur solar energy absorbing layer | |
| CN102515248B (en) | Method for preparing ZnO nano-rod array by pulse electromagnetic field | |
| CN103400893B (en) | A kind of method preparing copper zinc tin sulfide optoelectronic film | |
| CN101734866A (en) | Method for preparing nano tungsten trioxide thin film | |
| CN106374011A (en) | Cadmium sulfide sensitized silicon nanowire composite material and preparation and application thereof | |
| CN104022189B (en) | A kind of method preparing ZnO/ZnS composite photoelectric film | |
| CN105568309A (en) | Preparation method for photoelectrode of photoelectrochemical cell | |
| CN104310477A (en) | (NH4)2V4O9 film and preparation method thereof | |
| CN102795665B (en) | Preparation method of titanium dioxide nanotube (rod) array | |
| CN102903456B (en) | Method for preparing triple-doped novel transparent conductive thin film | |
| CN102515559B (en) | Method for preparing copper sulfide film with microwave hydrothermal assisted sol-gel method | |
| CN105957920B (en) | A kind of Cu3BiS3The preparation method of film | |
| CN104167453A (en) | Perovskite solar battery based on CdSe nanocrystals and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140115 |