CN101157437A - Method for preparing carbon nano-tube/CdS nano flower composite material - Google Patents
Method for preparing carbon nano-tube/CdS nano flower composite material Download PDFInfo
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- CN101157437A CN101157437A CNA2007101561874A CN200710156187A CN101157437A CN 101157437 A CN101157437 A CN 101157437A CN A2007101561874 A CNA2007101561874 A CN A2007101561874A CN 200710156187 A CN200710156187 A CN 200710156187A CN 101157437 A CN101157437 A CN 101157437A
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- cnt
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- composite material
- cds
- mixed liquor
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- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 239000002057 nanoflower Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 8
- 239000002041 carbon nanotube Substances 0.000 title abstract description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000000746 purification Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 abstract 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a preparation method of carbon nano-tube/CdS nano-flower composite material in water bath condition. The carbon nano-tubes after purification processing are dispersed to sodium dodecyl benzene sulfonate solution in an ultrasonic way and cadmium chloride solution and thiacetamide solution are added so as to achieve mixed solution. PH value of the mixed solution is adjusted to 1. The mixed solution is processed in water bath which is between 40 DEG C and 65 DEG C for at least 6 hours and then after centrifugal filtration, repeated washing with deionized water and desiccation, the product is achieved. The preparation method provided by the invention has the advantages of simpleness, low reaction temperature and easiness to the industrialized production.
Description
Technical field
The present invention relates to prepare the method for CNT/CdS nano flower composite material.
Background technology
CNT has excellent machinery, calorifics and electric property, has become the focus of domestic and international research since finding always.CNT is carried out surface modification treatment, connect organic and inorganic or biological functional group, can expand the application of CNT greatly in its carbon nano tube surface.In recent years, semiconductor nano crystal grain is coated or is deposited on the popular domain that carbon nano tube surface becomes research.CdS is as a kind of important II-VI family metal sulfide semiconductor material, and photoconductive response wide (green to ultraviolet) can be made the meter of γ and χ ray, also is simultaneously the important materials of making photo-resistor, solar cell.CNT/CdS composite is expected in fields such as light emitting diode and photoelectronic device acquisition important application.
Summary of the invention
The purpose of this invention is to provide a kind of method that under water bath condition, prepares CNT/CdS nano flower composite material.
The method for preparing CNT/CdS nano flower composite material of the present invention, its concrete steps are:
(1) CNT purification process: CNT is soaked in the salpeter solution of 30wt%, ultrasonic processing is filtered, with deionized water rinsing to PH=7, drying;
(2) will ultrasonic dispersion in the neopelex solution of CNT at 0.01～0.02mol/L of above-mentioned purification process, add cadmium chloride solution then, after stirring at least 10min, add the thioacetyl amine aqueous solution again, the mol ratio of CNT, caddy and thioacetamide is 0.003～0.005: 0.01～0.02: 0.01～0.02, stir mixed liquor;
(3) PH=1 of adjusting mixed liquor handles 6h at least with this mixed liquor in 40 ℃～65 ℃ water-baths, centrifugal filtration, and deionized water washes repeatedly, and drying gets final product.
Beneficial effect of the present invention is:
Preparation method provided by the invention is simple, and reaction temperature is low, is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is the transmission electron microscope picture (TEM) of prepared CNT/CdS nano flower composite material;
Fig. 2 is the XRD figure of prepared CNT/CdS nano flower composite material;
Fig. 3 is the sem photograph (SEM) of prepared CNT/CdS nano flower composite material.
The specific embodiment
Embodiment 1
(1) CNT purification process: the 1g CNT is soaked ultrasonic processing 2h in the salpeter solution of 100ml 30wt%, filter and repeatedly wash to PH=7 with deionized water, dry in 60 ℃ of baking ovens;
(2) with 0.04g purifying carbon nano-tube ultrasonic dispersion 30min in the neopelex solution of 50ml 0.02mol/L, the cadmium chloride solution that adds 20ml 0.5mol/L then, stir 10min, add 20ml 0.5mol/L thioacetyl amine aqueous solution again, mixed liquor is stirred 20min;
(3) 1.2ml chemical pure hydrochloric acid is diluted to 6ml with deionized water, to this hydrochloric acid solution of mixed solution and dripping, regulate the PH=1 of mixed liquor, then this mixed liquor is handled 6h in 40 ℃ of water-baths, centrifugal filtration is also repeatedly washed with deionized water, obtains CNT/CdS " nanometer flower " composite in 60 ℃ of baking ovens behind the dry 24h.The transmission electron microscope photo of the CNT that makes/CdS nano flower composite material is seen Fig. 1, and X-ray diffractogram is seen Fig. 2.By Fig. 1, Fig. 2 as seen, the superficial growth at CNT has gone out CdS nanometer flower.
Embodiment 2
(1) CNT purification process: the 1g CNT is soaked ultrasonic processing 2h in the salpeter solution of 100ml 30wt%, filter and repeatedly wash to PH=7 with deionized water, dry in 60 ℃ of baking ovens;
(2) with 0.06g purifying carbon nano-tube ultrasonic dispersion 30min in the neopelex solution of 50ml 0.01mol/L, the cadmium chloride solution that adds 20ml 1mol/L then, stir 10min, add 20ml1mol/L thioacetyl amine aqueous solution again, mixed liquor is stirred 20min;
(3) 1.2ml chemical pure hydrochloric acid is diluted to 6ml with deionized water, to this hydrochloric acid solution of mixed solution and dripping, regulate the PH=1 of mixed liquor, then this mixed liquor is handled 10h in 65 ℃ of water-baths, centrifugal filtration is also repeatedly washed with deionized water, obtains CNT/CdS " nanometer flower " composite in 60 ℃ of baking ovens behind the dry 24h.The stereoscan photograph of the CNT that makes/CdS nano flower composite material is seen Fig. 3.
Embodiment 3
(1) CNT purification process: the 1g CNT is soaked ultrasonic processing 2h in the salpeter solution of 100ml 30wt%, filter and repeatedly wash to PH=7 with deionized water, dry in 60 ℃ of baking ovens;
(2) with 0.05g purifying carbon nano-tube ultrasonic dispersion 30min in the neopelex solution of 50ml 0.01 5mol/L, the cadmium chloride solution that adds 20ml 0.7mol/L then, stir 10min, add 20ml 0.7mol/L thioacetyl amine aqueous solution again, mixed liquor is stirred 20min;
(3) 1.2ml chemical pure hydrochloric acid is diluted to 6ml with deionized water, to this hydrochloric acid solution of mixed solution and dripping, regulate the PH=1 of mixed liquor, then this mixed liquor is handled 12h in 65 ℃ of water-baths, centrifugal filtration is also repeatedly washed with deionized water, obtains CNT/CdS " nanometer flower " composite in 60 ℃ of baking ovens behind the dry 24h.
Claims (1)
1. method for preparing CNT/CdS nano flower composite material, step is as follows:
(1) CNT purification process: CNT is soaked in the salpeter solution of 30wt%, ultrasonic processing is filtered, with deionized water rinsing to PH=7, drying;
(2) will ultrasonic dispersion in the neopelex solution of CNT at 0.01～0.02mol/L of above-mentioned purification process, add cadmium chloride solution then, after stirring at least 10min, add the thioacetyl amine aqueous solution again, the mol ratio of CNT, caddy and thioacetamide is 0.003～0.005: 0.01～0.02: 0.01～0.02, stir mixed liquor;
(3) PH=1 of adjusting mixed liquor handles 6h at least with this mixed liquor in 40 ℃～65 ℃ water-baths, centrifugal filtration, and deionized water washes repeatedly, and drying gets final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710156187A CN100575245C (en) | 2007-10-23 | 2007-10-23 | A kind of method for preparing CNT/CdS nano flower composite material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710156187A CN100575245C (en) | 2007-10-23 | 2007-10-23 | A kind of method for preparing CNT/CdS nano flower composite material |
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| Publication Number | Publication Date |
|---|---|
| CN101157437A true CN101157437A (en) | 2008-04-09 |
| CN100575245C CN100575245C (en) | 2009-12-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200710156187A Expired - Fee Related CN100575245C (en) | 2007-10-23 | 2007-10-23 | A kind of method for preparing CNT/CdS nano flower composite material |
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| CN (1) | CN100575245C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624175B (en) * | 2009-07-30 | 2011-11-30 | 燕山大学 | Controllable synthesis method of hetero-structure of cadmium sulfide/multi-walled carbon nanotube shell core |
| CN102397553A (en) * | 2011-11-24 | 2012-04-04 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN101319404B (en) * | 2008-06-10 | 2012-05-16 | 浙江大学 | Method for preparation of hollow spherical cadmium sulfide nanocrystalline |
| CN101581687B (en) * | 2009-06-24 | 2012-05-30 | 中南大学 | Cadmium sulfide coating carbon nano tube gas-sensitive material and manufacture method of gas-sensitive element |
| CN103979523A (en) * | 2014-04-28 | 2014-08-13 | 中国石油大学(北京) | Method for filling multi-walled carbon nano-tubes with cadmium sulfide |
| CN107759832A (en) * | 2017-11-11 | 2018-03-06 | 蚌埠承永玻璃制品有限公司 | A kind of preparation technology of compounded mix |
| CN107887479A (en) * | 2017-12-19 | 2018-04-06 | 苏州亿沃光电科技有限公司 | A kind of preparation method based on CNT cadmium sulfide photoelectricity composite material |
| CN109331841A (en) * | 2018-12-14 | 2019-02-15 | 青岛大学 | A kind of CdS nanometers of snowflake photochemical catalyst and the preparation method and application thereof |
-
2007
- 2007-10-23 CN CN200710156187A patent/CN100575245C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319404B (en) * | 2008-06-10 | 2012-05-16 | 浙江大学 | Method for preparation of hollow spherical cadmium sulfide nanocrystalline |
| CN101581687B (en) * | 2009-06-24 | 2012-05-30 | 中南大学 | Cadmium sulfide coating carbon nano tube gas-sensitive material and manufacture method of gas-sensitive element |
| CN101624175B (en) * | 2009-07-30 | 2011-11-30 | 燕山大学 | Controllable synthesis method of hetero-structure of cadmium sulfide/multi-walled carbon nanotube shell core |
| CN102397553A (en) * | 2011-11-24 | 2012-04-04 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN102397553B (en) * | 2011-11-24 | 2013-05-22 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN103979523A (en) * | 2014-04-28 | 2014-08-13 | 中国石油大学(北京) | Method for filling multi-walled carbon nano-tubes with cadmium sulfide |
| CN103979523B (en) * | 2014-04-28 | 2015-04-01 | 中国石油大学(北京) | Method for filling multi-walled carbon nano-tubes with cadmium sulfide |
| CN107759832A (en) * | 2017-11-11 | 2018-03-06 | 蚌埠承永玻璃制品有限公司 | A kind of preparation technology of compounded mix |
| CN107887479A (en) * | 2017-12-19 | 2018-04-06 | 苏州亿沃光电科技有限公司 | A kind of preparation method based on CNT cadmium sulfide photoelectricity composite material |
| CN109331841A (en) * | 2018-12-14 | 2019-02-15 | 青岛大学 | A kind of CdS nanometers of snowflake photochemical catalyst and the preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN100575245C (en) | 2009-12-30 |
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