CN103241766A - Preparation method of SiO2 nanorod/CdS - Google Patents
Preparation method of SiO2 nanorod/CdS Download PDFInfo
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- CN103241766A CN103241766A CN201310164066XA CN201310164066A CN103241766A CN 103241766 A CN103241766 A CN 103241766A CN 201310164066X A CN201310164066X A CN 201310164066XA CN 201310164066 A CN201310164066 A CN 201310164066A CN 103241766 A CN103241766 A CN 103241766A
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Abstract
The invention relates to a method for preparing a SiO2 nanorod/CdS composite material. The method is characterized by adopting active SiO2 nanorods obtained from attapulgite clay through acidification treatment as a carrier, taking a cadmium salt as a cadmium source, taking Na2S as a sulfur source, taking EDTA (ethylenediaminetetraacetic acid) and the like as a template agent, and reacting under hydrothermal conditions to obtain the SiO2 nanorod/CdS composite material. The SiO2 nanorod/CdS composite nanomaterial prepared by the method disclosed by the invention can be widely applied in the fields of control of environmental pollution, preparation of photocatalytic functional materials and the like.
Description
Technical field
The present invention relates to inorganic nano composite material and technical field of function materials, especially SiO
2Nanometer rod/CdS composite material and preparation method thereof.
Background technology
Utilizing the conductor photocatalysis hydrogen production by water decomposition is one of desirable approach of solar energy chemical storage.In numerous photocatalysts, TiO
2, SrTiO
3Deng oxide semiconductor stable performance, inexpensive nontoxic, study comparatively deeply, but these semiconductor material greater band gap only absorb UV-light, solar energy utilization ratio is low.Sulfide semiconductor is also paid close attention to always widely, in numerous sulfide, CdS energy gap little (Eg=2.4eV), visible light there is good response, if sulfide semiconductor is carried on the high specific surface carrier, utilize the strong interaction between carrier and the active ingredient, can reduce the reunion of nanoparticle, increase effective reaction active site.In addition, can also control the performances such as light, electricity and catalysis of matrix material flexibly by the The Nomenclature Composition and Structure of Complexes of modulation load active component.
Because in light-catalyzed reaction, the anode dissolution electromotive force of CdS only is 0.32V, is easy to take place the photoetch phenomenon, has reduced photocatalysis efficiency, has limited its practical application.SiO
2Have good dispersiveness and erosion resistance, by composite S iO
2Can reduce CdS photoetch takes place in light-catalyzed reaction, thus the photocatalysis efficiency of raising CdS.
At present, relevant SiO
2The report of the preparation of/CdS composite nano materials emerges in an endless stream, and has reported a kind of novel single presoma Cd[S as U.S.'s " materials chemistry " (Chemistry of Materials,, the 14th volume, 2900-2904 page or leaf in 2002)
2CNRR ˊ]
2Preparation SiO
2/ CdS composite nano materials; Application number is 200610049090 patent " a kind of preparation method of SiO 2 mesoporous material-cadmium sulfide composition nano material "; " Guangxi University's journal " (Journal of Guangxi University (Nat Sci Ed) 2007, the 32nd volume, the 2nd phase, 147-149 page or leaf) reported a kind of " nucleocapsid structure CdS/SiO
2The preparation of nano particle "; Application number be 201210256129.X patented invention " the mesoporous SiO of a kind of preparation
2The method of/CdS composite Nano ball ".But do not see SiO
2Nanometer rod/CdS preparation method's report.
Attapulgite clay is a kind of natural nano-material, has the moisture chain layered magnesium aluminium silicate mineral of specialty fibers shape crystalline structure form, and bigger specific surface area and abundant nano pore are arranged.After the acidified processing, the SiO of gained
2But keep the rhabdolith structure of attapulgite clay, be suitable as carrier.Its report sees that application number is 02148523.2 patent " producing the method for nano bar-shape active silica with attapulgite clay ".Therefore, this patent adopts hydrothermal method successfully the CdS nano particle to be carried on SiO
2Nanometer rod.
Summary of the invention
The present invention relates to attapulgite clay, cadmium salt, Na
2S is main raw material, and hydrochloric acid (36-38%) is solvent, adopts Hydrothermal Preparation inorganic nano composite material SiO
2The method of nanometer rod/CdS has following processing step:
Adopt the acid treatment method, attapulgite is modified as active SiO
2Nanometer rod is then with active SiO
2Nanometer rod is carrier, is cadmium source, Na with the cadmium salt
2S is the sulphur source, is template with EDTA etc., utilizes Hydrothermal Preparation SiO
2Nanometer rod/CdS matrix material.
Described SiO
2Nanometer rod/CdS composite material and preparation method thereof, active SiO wherein
2It is attapulgite clay that nanometer rod prepares raw material;
Described method, the used hydrochloric acid soln volume of wherein acid treatment process is 200mL, concentration is V
Hydrochloric acid: V
Water=1:1, oil bath temperature are 120 ℃, and return time is 4h;
Described method, cadmium source are any in cadmium acetate, Cadmium chloride fine powder, cadmium nitrate, the Cadmium Sulphate, and the sulphur source is Na
2S, its mol ratio n
Cd: n
S=1:1～1:1.5;
Among the described preparation method, template is EDTA, PVP, P123, CTAB, any among the F127;
Among the described preparation method, active SiO
2The CdS that nanometer rod, reaction generate, the mass ratio of template are 1:1:1～1:3:2, and hydrothermal temperature is 100-150 ℃, and the hydro-thermal time is 2-4h.
The SiO of the present invention's preparation
2Nanometer rod/CdS composite nano materials can be widely used in fields such as environmental pollution improvement, photo-catalysis function material preparation.
Description of drawings
Fig. 1 is the XRD spectra after the attapulgite clay acidification.
Fig. 2 is SiO
2The XRD spectra of nanometer rod/CdS composite nano materials.
Fig. 3 is SiO
2The TEM photo of nanometer rod/CdS composite nano materials.
Embodiment
Embodiment 1: gets the 4.0000g attapulgite clay, is dissolved in the 200mL hydrochloric acid soln, and reflux 4h, Heating temperature is 120 ℃.Vacuum-evaporation subsequently is dry must active SiO
2Then get 1.0000g SiO
2Grind in the immigration polytetrafluoroethyllining lining, and add template EDTA, CdCl successively
2, Na
2S, quality is respectively 1.2000g, 1.3960g, 0.6536g, at 120 ℃ of hydro-thermal 2h.Washing at last, drying gets matrix material.The gained sample is carried out the X-ray powder diffraction experiment, and under transmission electron microscope, observe its pattern and structure.
The SiO that makes according to the processing parameter of embodiment 1
2The XRD figure spectrum of nanometer rod as shown in Figure 1.SiO in preparation
2There is tangible SiO in the collection of illustrative plates
2Characteristic diffraction peak, illustrate that attapulgite clay has made SiO through acidification
2Nanometer rod.
SiO
2XRD, the TEM of nanometer rod/CdS sample are shown in Fig. 2,3.As can be seen from the figure, CdS, SiO are arranged in the matrix material
2Exist, and the CdS particulate load is at SiO
2Nanorod surfaces, the about 10-20nm of particle diameter.
Embodiment 2: the change attapulgite clay is 4.0000g, be dissolved in the 200mL hydrochloric acid soln, and reflux 4h, Heating temperature is 120 ℃.Vacuum-evaporation subsequently is dry must active SiO
2Then get 1.0000g SiO
2Grind in the immigration polytetrafluoroethyllining lining, and add template PVP, CdCl successively
2, Na
2S, quality is respectively 1.0000g, 1.2690g, 0.5401g, at 100 ℃ of hydro-thermal 2h.Washing at last, drying gets matrix material.Subsequent detection such as embodiment 1.
Embodiment 3: gets the 4.0000g attapulgite clay, is dissolved in the 200mL hydrochloric acid soln, and reflux 4h, Heating temperature is 120 ℃.Vacuum-evaporation subsequently is dry must active SiO
2Then get 1.0000g SiO
2Grind in the immigration polytetrafluoroethyllining lining, and add template P123, CdCl successively
2, Na
2S, quality is respectively 1.5000g, 2.5380g, 1.2964g, at 130 ℃ of hydro-thermal 3h.Washing at last, drying gets matrix material.Subsequent detection such as embodiment 1.
Embodiment 4: the change attapulgite clay is 4.0000g, be dissolved in the 200mL hydrochloric acid soln, and reflux 4h, Heating temperature is 120 ℃.Vacuum-evaporation subsequently is dry must active SiO
2Then get 1.0000g SiO
2Grind in the immigration polytetrafluoroethyllining lining, and add template CTAB, CdCl successively
2, Na
2S, quality is respectively 2.0000g, 3.8070g, 2.1066g, at 140 ℃ of hydro-thermal 4h.Washing at last, drying gets matrix material.Subsequent detection such as embodiment 1.
Embodiment 5: the change attapulgite clay is 4.0000g, be dissolved in the 200mL hydrochloric acid soln, and reflux 4h, Heating temperature is 120 ℃.Vacuum-evaporation subsequently is dry must active SiO
2Then get 1.0000g SiO
2Grind in the immigration polytetrafluoroethyllining lining, and add template F127, CdCl successively
2, Na
2S, quality is respectively 2.0000g, 2.5380g, 1.6204g, at 150 ℃ of hydro-thermal 4h.Washing at last, drying gets matrix material.Subsequent detection such as embodiment 1.
Claims (6)
1.SiO
2Nanometer rod/CdS composite material and preparation method thereof is characterized in that step is: adopt the acid treatment method, attapulgite is modified as active SiO
2Nanometer rod is then with active SiO
2Nanometer rod is carrier, is cadmium source, Na with the cadmium salt
2S be sulphur source and template together, utilize Hydrothermal Preparation SiO
2Nanometer rod/CdS matrix material.
2. method according to claim 1 is characterized in that described active SiO
2It is attapulgite clay that nanometer rod prepares raw material.
3. method according to claim 1 is characterized in that, the used hydrochloric acid soln volume of acid treatment process is 200mL, and concentration is V
Hydrochloric acid: V
Water=1:1, oil bath temperature are 120 ℃, and return time is 4h.
4. preparation method according to claim 1 is characterized in that described cadmium source is any in cadmium acetate, Cadmium chloride fine powder, cadmium nitrate, the Cadmium Sulphate, and the sulphur source is Na
2S, its mol ratio n
Cd: n
S=1:1～1:1.5.
5. method according to claim 1 is characterized in that described template is EDTA, PVP, P123, CTAB, among the F127 any.
6. method according to claim 1 is characterized in that described active SiO
2The CdS that nanometer rod, reaction generate, the mass ratio of template are 1:1:1～1:3:2, and hydrothermal temperature is 100-150 ℃, and the hydro-thermal time is 2-4h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566952A (en) * | 2013-11-22 | 2014-02-12 | 武汉理工大学 | Preparation method of CdS/Cd2Ge2O6 complex photocatalyst |
| CN104965067A (en) * | 2015-05-15 | 2015-10-07 | 南通明芯微电子有限公司 | Photoelectric responsiveness semiconductor nanomaterial-based biosensor |
| CN106964374A (en) * | 2017-02-21 | 2017-07-21 | 河海大学 | Cadmium sulfide loads the preparation method of the sodium yttrium tetrafluoride composite photo-catalyst of hexagonal phase ytterbium and Er ions |
| CN107804854A (en) * | 2017-11-27 | 2018-03-16 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The method that cupric silicate nanotube is prepared using low-grade attapulgite clay |
| CN109364951A (en) * | 2018-12-21 | 2019-02-22 | 苏州科技大学 | A kind of visible light catalytic composite material and preparation method and application |
| CN110252248A (en) * | 2019-07-09 | 2019-09-20 | 山东百普瑞世环境科技有限公司 | Composite silicon dioxide antibacterial adsorbent material, Preparation method and use |
| CN112892557A (en) * | 2021-02-04 | 2021-06-04 | 常州大学 | SiO (silicon dioxide)2@CdS@SiO2Preparation method and application of core-shell photocatalyst |
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Cited By (13)
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| CN103566952B (en) * | 2013-11-22 | 2015-09-30 | 武汉理工大学 | CdS/Cd 2ge 2o 6the preparation method of composite photo-catalyst |
| CN103566952A (en) * | 2013-11-22 | 2014-02-12 | 武汉理工大学 | Preparation method of CdS/Cd2Ge2O6 complex photocatalyst |
| CN104965067A (en) * | 2015-05-15 | 2015-10-07 | 南通明芯微电子有限公司 | Photoelectric responsiveness semiconductor nanomaterial-based biosensor |
| WO2016184062A1 (en) * | 2015-05-15 | 2016-11-24 | 南通明芯微电子有限公司 | Biosensor based on photoelectrically responsive semiconductor nanomaterial |
| CN106964374B (en) * | 2017-02-21 | 2019-11-12 | 河海大学 | Cadmium sulfide loads the preparation method of the sodium yttrium tetrafluoride composite photo-catalyst of hexagonal phase ytterbium and Er ions |
| CN106964374A (en) * | 2017-02-21 | 2017-07-21 | 河海大学 | Cadmium sulfide loads the preparation method of the sodium yttrium tetrafluoride composite photo-catalyst of hexagonal phase ytterbium and Er ions |
| CN107804854B (en) * | 2017-11-27 | 2020-03-17 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Method for preparing copper silicate nanotube by using low-grade attapulgite clay |
| CN107804854A (en) * | 2017-11-27 | 2018-03-16 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The method that cupric silicate nanotube is prepared using low-grade attapulgite clay |
| CN109364951A (en) * | 2018-12-21 | 2019-02-22 | 苏州科技大学 | A kind of visible light catalytic composite material and preparation method and application |
| CN109364951B (en) * | 2018-12-21 | 2022-09-30 | 苏州科技大学 | Visible light catalytic composite material and preparation method and application thereof |
| CN110252248A (en) * | 2019-07-09 | 2019-09-20 | 山东百普瑞世环境科技有限公司 | Composite silicon dioxide antibacterial adsorbent material, Preparation method and use |
| CN112892557A (en) * | 2021-02-04 | 2021-06-04 | 常州大学 | SiO (silicon dioxide)2@CdS@SiO2Preparation method and application of core-shell photocatalyst |
| CN112892557B (en) * | 2021-02-04 | 2023-05-23 | 常州大学 | SiO (silicon dioxide) 2 @CdS@SiO 2 Preparation method and application of core-shell photocatalyst |
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Effective date of registration: 20201124 Address after: Shandong Yuejin Road 277300 Zaozhuang City Yicheng Economic Development Zone No. 8 Patentee after: Shandong Xuedi Aluminum Technology Co.,Ltd. Address before: 213164 Jiangsu Province, Changzhou city Wujin District Gehu Lake Road No. 1 Patentee before: CHANGZHOU University |
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Denomination of invention: Preparation of SiO2nanorods/CdS Effective date of registration: 20220927 Granted publication date: 20140813 Pledgee: Zaozhuang rural commercial bank Limited by Share Ltd. Yicheng sub branch Pledgor: Shandong Xuedi Aluminum Technology Co.,Ltd. Registration number: Y2022980016328 |
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Date of cancellation: 20230912 Granted publication date: 20140813 Pledgee: Zaozhuang rural commercial bank Limited by Share Ltd. Yicheng sub branch Pledgor: Shandong Xuedi Aluminum Technology Co.,Ltd. Registration number: Y2022980016328 |