CN101559918B - Preparation method of graphene/cadmium sulfide quantum dot composite material applied to photoelectric conversion - Google Patents
Preparation method of graphene/cadmium sulfide quantum dot composite material applied to photoelectric conversion Download PDFInfo
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- CN101559918B CN101559918B CN2009100503334A CN200910050333A CN101559918B CN 101559918 B CN101559918 B CN 101559918B CN 2009100503334 A CN2009100503334 A CN 2009100503334A CN 200910050333 A CN200910050333 A CN 200910050333A CN 101559918 B CN101559918 B CN 101559918B
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Abstract
The invention relates to a preparation method of graphene/cadmium sulfide quantum dot composite materials, and is applied to photoelectric conversion, belonging to the field of nano inorganic materialand energy chemistry. The method comprises the following steps: taking a certain amount of graphite powder, carrying out oxidization to graphite powder under strong oxidizing condition to obtain oxid ized graphite, preparing the oxidized graphite into monolayer oxidized graphite sheet solution with a certain concentration; mixing for 15 hours under the temperature of 95 DEG C in hydrazine hydrate reducing agent solution and then obtaining reduced products, namely monolayer graphene black solid; mixing the graphene solid and cadmium acetate dehydrate according to the molar ratio of 1: 1 into a mixture, dispersing the mixture into dimethylsulfoxide solution with a certain volume, carrying out ultrasonic processing for a period of time, transferring the obtained mixture into a reaction kettle, annealing for 8 to 16 hours under the temperature of 150 to 200 DEG C and carrying out a plurality of times of cleaning to the product by acetone and alcohol and obtaining the graphene/cadmium sulfide quantum dot composite material. The products obtained by the invention can be used as photoelectric conversion material and have higher energy conversion rate.
Description
Technical field
The present invention relates to a kind of preparation method who is applied to the Graphene/cadmium sulfide quantum dot composite material of photoelectricity conversion, belong to nano inorganic material and energy chemical field.
Background technology
Graphene (Graphene) is a kind of new allotrope of carbon, and it has more special cellular two-dimensional structure, and the thickness of being made up of the monolayer carbon atom is the two dimensional crystal structure of 0.34nm.Since finding that it independently existed in 2004; Caused widely and paid close attention to; It not only has the favorable mechanical performance, and unique electrical properties is also arranged, such as the electron mobility of dirac fermion, Brillouin scattering and the superelevation of no quality; Higher 100 times than the electron mobility of silicon semiconductor, higher 20 times than GaAs.Seeing that having caused, the performance of its excellent machinery, electronics, physics, chemical aspect is considered to the extensive concern of each subject have great application prospect, comprising electronic device, energy storage etc. at wide spectrum.Quantum dot is because its unique quantum dimensional effect is widely used in photoelectric field, such as solar cell, luminescent device, biomarker etc.Cadmium sulfide (CdS) has optical transmittance and narrower being with (for 2.42ev) preferably as a kind of semiconductor of important II-VI family.
Our purpose is the advantage of getting two kinds of materials; Make cadmium sulfide (CdS) in Graphene (Graphene) superficial growth; Utilize the optical property of cadmium sulfide (CdS) quantum dot to realize that the absorption photon changes into electronics; Utilize the unique electronic property transportation electric charge of Graphene (Graphene), reach the purpose that photoelectricity transforms.Simultaneously, the selected raw material of this composite is cheap relatively, obtain easily, and the simple and operation easily of preparation method simultaneously, and electricity conversion is high.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who is applied to the Graphene/cadmium sulfide quantum dot composite material of photoelectricity conversion.
A kind of preparation method who is applied to the Graphene/cadmium sulfide quantum dot composite material of photoelectricity conversion of 1 the present invention is characterized in that having following process and step:
A. the preparation of mono-layer graphite oxide sheet and single-layer graphene: use natural graphite powder to be raw material, add a certain amount of concentrated sulfuric acid, potassium peroxydisulfate and phosphorus pentoxide, evenly mix down, make its reaction 4.5 hours at 80 ℃; Mixture is cooled to room temperature, releases the back hold over night, use the CAM isolated by filtration in 0.2 micron hole then, and with a large amount of deionized water washings, product is hold over night at room temperature with deionized water alkene; With above-mentioned product is the graphite limit stirring of pre-oxidation, and the limit adds in the mixed solution of the cold concentrated sulfuric acid and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of hydrogenperoxide steam generator again; Then above-mentioned solution is filtered, and remove metal ion, spend deionised water again and remove unnecessary acid, and repeatedly be washed with water to neutrality with the dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally make the oxidized graphite flake aqueous solution; Again it is carried out sonicated, obtain the mono-layer graphite oxide sheet solution that filemot homogeneous disperses;
Get the mono-layer graphite oxide sheet solution that above-mentioned homogeneous disperses, be incorporated in by a certain percentage in a certain amount of reducing agent hydrazine hydrate solution, stirred 15 hours down, after reduction reaction, products therefrom is filtered, promptly obtain the black solid single-layer graphene at 95 ℃;
B. the preparation of Graphene/cadmium sulfide quantum dot composite material: with the single-layer graphene of above-mentioned gained is raw material, with itself and two hydration cadmium acetate (Cd (CH
3COO)
22H
2O) be dispersed in the dimethyl sulfoxide solution of certain volume with 1: 1 ratio; Single-layer graphene is 1: 1 with the mol ratio that cooperates consumption of two hydration cadmium acetates; The consumption of dimethyl sulfoxide solution serves as to calculate benchmark with the quality of Graphene, and promptly per 1 milligram of Graphene need add 1 milliliter of dimethyl sulfoxide solution; , after a period of time it is being transferred in the agitated reactor through sonicated, 150～200 ℃ of down annealing 8～16 hours, product is after acetone and ethanol repeated multiple times are washed, and drying promptly gets Graphene/cadmium sulfide quantum dot composite material.
Characteristics of the present invention are to use methyl-sulfoxide, both as solution, again as the sulphur source; In the composite that obtains, it is covalently bound not need other molecules between cadmiumsulfide quantum dot and the graphene film.The raw material of gained of the present invention is cheap relatively, obtains easily, and preparation technology is simple, easy to operate simultaneously, and the electricity conversion of product composite is higher.
Description of drawings
Fig. 1 is AFM (AFM) the photo figure of gained mono-layer graphite oxide sheet of the present invention.
Fig. 2 is transmission electron microscope (TEM) the photo figure of gained Graphene/cadmium sulfide composite material of the present invention.
Fig. 3 is X-ray diffraction (XRD) spectrogram of gained Graphene/cadmium sulfide composite material of the present invention.
Fig. 4 is the thermogravimetric and differential scanning calorimetric analysis (TG-DSC) the data and curves figure of gained Graphene/cadmium sulfide composite material of the present invention.
The specific embodiment
After specific embodiment of the present invention being discussed at present.
Embodiment 1
Process and step in the present embodiment are following:
1, the preparation of mono-layer graphite oxide sheet and single-layer graphene: use natural graphite powder to be raw material; Get the natural graphite powder of 3 grams, 325 order fineness, add 12 milliliters of concentrated sulfuric acids, 2.5 gram potassium peroxydisulfates and 2.5 gram phosphorus pentoxides; Evenly mix down at 80 ℃, make its reaction 4.5 hours; Mixture is cooled to room temperature, releases the back hold over night, use the CAM isolated by filtration in 0.2 micron hole then, and with a large amount of deionized water washings, product is hold over night at room temperature with deionized water alkene; With above-mentioned product is the graphite limit stirring of pre-oxidation; The limit slowly adds cold 120 milliliters dense of 0 ℃ the concentrated sulfuric acids and potassium permanganate 15 restrains in the mixed solution of forming; After stirring 2 hours under 35 ℃, release with 250 ml deionized water alkene; Continue to stir the ionized water that adds 700 milliliters after 2 hours again, after stirring, add 20 milliliters of hydrogenperoxide steam generators again; Then above-mentioned solution is filtered, and remove metal ion, spend deionised water again and remove unnecessary acid, and repeatedly use a large amount of water washings to neutral with 1: 10 dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally obtain the oxidized graphite flake aqueous solution; Again it is carried out sonicated 20 minutes, obtain the mono-layer graphite oxide sheet solution that filemot homogeneous disperses;
Get the mono-layer graphite oxide sheet solution that above-mentioned homogeneous disperses, be incorporated in by a certain percentage in a certain amount of reducing agent hydrazine hydrate solution, stirred 15 hours down, after reduction reaction, products therefrom is filtered, promptly obtain the black solid single-layer graphene at 95 ℃;
2, the preparation of Graphene/cadmium sulfide quantum dot composite material: with the single-layer graphene of above-mentioned gained is raw material, with itself and two hydration cadmium acetate (Cd (CH
3COO)
22H
2O) be dispersed in the dimethyl sulfoxide solution of certain volume with 1: 1 ratio; Single-layer graphene is 1: 1 with the mol ratio that cooperates consumption of two hydration cadmium acetates; The consumption of dimethyl sulfoxide solution serves as to calculate benchmark with the quality of Graphene, and promptly per 1 milligram of Graphene need add 1 milliliter of dimethyl sulfoxide solution; , after a period of time it is being transferred in the agitated reactor through sonicated, 180 ℃ of down annealing 12 hours, product is after acetone and ethanol repeated multiple times are washed, and drying promptly gets Graphene/cadmium sulfide quantum dot composite material.
Preparation process in the present embodiment and step and the foregoing description 1 are identical.Different is: also fiery temperature is 150 ℃ in agitated reactor, and annealing time is 8 hours, finally makes composite.
Embodiment 3
Preparation process in the present embodiment and step and the foregoing description 1 are identical.Different is: also fiery temperature is 200 ℃ in agitated reactor, and annealing time is 16 hours, finally makes composite.
Resulting Graphene/cadmium sulfide composite material sample in the present embodiment, through each item instrument detecting, its testing result is seen Fig. 1, Fig. 2, Fig. 3 and the Fig. 4 in the accompanying drawing.
Fig. 1 is AFM (AFM) the photo figure of gained mono-layer graphite oxide sheet in the embodiment of the invention.Visible from figure, the graphite particle in the present embodiment in the graphite oxide solution of gained is an individual layer sheet microstructure.
Fig. 2 is transmission electron microscope (TEM) the photo figure of gained Graphene/cadmium sulfide composite material in the embodiment of the invention.Visible from figure, the nano particle form of gained composite.
Fig. 3 is X-ray diffraction (XRD) spectrogram of gained Graphene/cadmium sulfide composite material in the embodiment of the invention.Peak value place among the figure representes to have the existence of Graphene and CdS.
Fig. 4 is the thermogravimetric and differential scanning calorimetric analysis (TG-DSC) the data and curves figure of gained Graphene/cadmium sulfide composite material in the embodiment of the invention.
Claims (1)
1. preparation method who is applied to Graphene/cadmium sulfide quantum dot composite material that photoelectricity transforms is characterized in that having following process and step:
A. the preparation of mono-layer graphite oxide sheet and single-layer graphene: use natural graphite powder to be raw material, add a certain amount of concentrated sulfuric acid, potassium peroxydisulfate and phosphorus pentoxide, evenly mix down, make its reaction 4.5 hours at 80 ℃; Mixture is cooled to room temperature, releases the back hold over night, use the CAM isolated by filtration in 0.2 micron hole then, and with a large amount of deionized water washings, product is hold over night at room temperature with deionized water alkene; With above-mentioned product is the graphite limit stirring of pre-oxidation, and the limit adds in the mixed solution of the cold concentrated sulfuric acid and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of hydrogenperoxide steam generator again; Then above-mentioned solution is filtered, and remove metal ion, spend deionised water again and remove unnecessary acid, and repeatedly be washed with water to neutrality with the dilute hydrochloric acid solution washing; At last product is dialysed a week, remove the metal remained ion; Finally make the oxidized graphite flake aqueous solution; Again it is carried out sonicated, obtain the mono-layer graphite oxide sheet solution that filemot homogeneous disperses;
Get the mono-layer graphite oxide sheet solution that above-mentioned homogeneous disperses, be incorporated in by a certain percentage in a certain amount of reducing agent hydrazine hydrate solution, stirred 15 hours down, after reduction reaction, products therefrom is filtered, promptly obtain the black solid single-layer graphene at 95 ℃;
B. the preparation of Graphene/cadmium sulfide quantum dot composite material: with the single-layer graphene of above-mentioned gained is raw material, with itself and two hydration cadmium acetate (Cd (CH
3COO)
22H
2O) be dispersed in the dimethyl sulfoxide solution of certain volume with 1: 1 ratio; Single-layer graphene is 1: 1 with the mol ratio that cooperates consumption of two hydration cadmium acetates; The consumption of dimethyl sulfoxide solution serves as to calculate benchmark with the quality of Graphene, and promptly per 1 milligram of Graphene need add 1 milliliter of dimethyl sulfoxide solution; , after a period of time it is being transferred in the agitated reactor through sonicated, 150～200 ℃ of down annealing 8～16 hours, product is after acetone and ethanol repeatedly wash, and drying promptly gets Graphene/cadmium sulfide quantum dot composite material.
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| CN101844762B (en) * | 2010-05-28 | 2012-04-04 | 江苏大学 | Method for preparing hydrophilic graphene |
| CN101913600B (en) * | 2010-08-27 | 2012-07-04 | 上海交通大学 | Method for preparing graphene/semiconductor quantum dot composite material |
| CN102176382B (en) * | 2011-01-31 | 2013-10-16 | 中国科学院上海硅酸盐研究所 | Method for preparing grapheme-quantum dot composite film and solar battery structured by using same |
| CN102225758B (en) * | 2011-04-13 | 2012-10-24 | 昆明物理研究所 | Supersonic chemical preparation method for grapheme quantum dots |
| CN102225754B (en) * | 2011-05-11 | 2013-03-06 | 中国科学技术大学 | Preparation method of graphene oxide and preparation method of graphene |
| CN102649548A (en) * | 2012-05-10 | 2012-08-29 | 上海大学 | Method for directly preparing graphene/cadmium sulfide nanocomposite material by microwave heating one-step method |
| CN102998035A (en) * | 2012-11-21 | 2013-03-27 | 东北大学 | Sensitive element based on pressure volume effect of graphene filled silicone rubber composite material and production method thereof |
| CN103093968B (en) * | 2013-01-21 | 2015-07-08 | 聊城大学 | Graphite oxide-cadmium sulfide compounds applied to electrode materials |
| CN104280447A (en) * | 2014-10-14 | 2015-01-14 | 广州盈思传感科技有限公司 | Method for detecting benzenediol-type substances in water |
| CN104280436A (en) * | 2014-10-14 | 2015-01-14 | 广州盈思传感科技有限公司 | Preparation method of glassy carbon electrode for detecting pyrocatechol and/or paradioxybenzene in water |
| CN105879885B (en) * | 2016-05-04 | 2018-08-07 | 上海大学 | Visible light photolytic hydrogen production catalyst and preparation method thereof |
| CN109971456A (en) * | 2017-12-27 | 2019-07-05 | Tcl集团股份有限公司 | A kind of perovskite quantum dot composite material and preparation method thereof |
| CN112816687B (en) * | 2020-12-31 | 2022-04-22 | 华南农业大学 | Broad-spectrum immunosensor for image matching by using machine learning |
| CN113419048A (en) * | 2021-06-23 | 2021-09-21 | 四川士达特种炭材有限公司 | Method for rapidly identifying oil content of carbon material |
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| CN1986726A (en) * | 2005-12-20 | 2007-06-27 | 中国科学院兰州化学物理研究所 | Preparing process of CdS semiconduct quantum dot |
| CN101125680A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium sulfide |
| WO2008116661A2 (en) * | 2007-03-28 | 2008-10-02 | Centrum Für Angewandte Nanotechnologie Gmbh | A method for the manufacture of nanoparticles on a carbon surface and products therefrom |
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| CN1986726A (en) * | 2005-12-20 | 2007-06-27 | 中国科学院兰州化学物理研究所 | Preparing process of CdS semiconduct quantum dot |
| WO2008116661A2 (en) * | 2007-03-28 | 2008-10-02 | Centrum Für Angewandte Nanotechnologie Gmbh | A method for the manufacture of nanoparticles on a carbon surface and products therefrom |
| CN101125680A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium sulfide |
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