CN103361065B - CdSe quantum dot load Graphene with different-shape feature and uses thereof and preparation method - Google Patents
CdSe quantum dot load Graphene with different-shape feature and uses thereof and preparation method Download PDFInfo
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Abstract
CdSe quantum dot load Graphene with different-shape feature and uses thereof and preparation method.Adopt quadrol solvent-thermal method to reduce to graphene oxide, develop the simple and easy method that single stage method prepares CdSe quantum dot load Graphene.Graphene oxide self is reduced while CdS-loaded e quantum dot, and oxygen level significantly reduces, and the graphenic surface after reduction introduces nitrogen-containing group.The reduction process impact of change on graphene oxide of temperature of reaction is little, and the impact in reaction times is relatively obvious.Along with the prolongation in reaction times, the reducing degree of Graphene is higher, and the CdSe quantum dot of graphenic surface load grows up into nanometer rod and branching nanostructure gradually by particle.By regulation and control reaction conditions can change while controlled oxidization Graphene reducing degree graphenic surface the pattern of CdS-loaded e quantum dot.The CdSe quantum dot load Graphene with different-shape feature can be used for the field such as solar cell and photochemical catalysis.
Description
Technical field
The present invention relates to field of nanometer material technology, be specifically related to CdSe quantum dot load Graphene with different-shape feature and uses thereof and preparation method's method field.
Background technology
Graphene is the elementary cell forming other carbon nanomaterials.Graphene is nano material thin, the hardest in the world at present.Because Graphene has some very unique character, it all has broad application prospects in fields such as electron device, stored energy, solar cell, sensor and photo-detectors.Develop the multiple method preparing Graphene in recent years, comprise micromechanics stripping method, silicon carbide epitaxial growth method, chemical Vapor deposition process, oxidation reduction process and other arc process, microwave method, quench hot method and carbon nanotube stripping method etc.Oxidation reduction process is prepare the common method of Graphene, mainly contains Brodie method, Hummer method and Staudenmaier method
[16].Quantum dot is because of the size-dependent of its uniqueness, and the narrow and emmission spectrum of symmetry, wide and continuous print absorption spectrum, fabulous biocompatibility, causes extensive concern and the great interest of scientific circles.But quantum dot all existence and stability problems of preparation at present, quantum dot is after placement certain hour, fluorescence decline can be caused very serious due to reasons such as gatherings, so the quantum dot of preparation at present is generally made up of inorganic semiconductor core and stablizer shell, stablizer shell keeps the stable of quantum dot, but the coupling between quantum dot can be hindered simultaneously, add the randomness of system, cause the specific conductivity of quantum dot and photoconductivity extremely low.Quantum dot is implanted in appropriate semiconductor substrate, effectively can reduce the restructuring of electron-hole, improve the generation of photoelectric current.Wherein CdSe quantum dot is the model system of research quantum dot size effect, for the research of the size of other semiconductor-quantum-points, the structure of reconfigurable and photoelectric property provides example.The optical property of the CdSe quantum dot size adjustable carrier mobility high with Graphene is combined and can obtains a kind of desirable energy transformation system, and wherein CdSe quantum dot is as photovoltaic material, has the Flexible graphene electrode of high conductivity as support.In a word, although the research of quantum dot load Graphene achieves some achievements, but still practical needs can not be met.The weak point of these methods is the uncontrollability that graphenic surface reacts at present, and then causes the size uncontrollability of quantum dot in mixture and the character of Size dependence to be restricted.
Summary of the invention
Goal of the invention: existingly prepare in the process of Graphene composite inorganic quantum dot, due to the uncontrollability of graphenic surface reaction, and then causes the size uncontrollability of quantum dot in mixture and the character of Size dependence to be restricted.The invention provides a kind of CdSe quantum dot load Graphene with different-shape feature and uses thereof and preparation method.
Summary of the invention: adopt quadrol solvothermal method, developed the simple and easy method that one kettle way prepares CdSe quantum dot load Graphene.Show the phenetic analysis result of CdSe quantum dot load Graphene, graphene oxide self is reduced while CdS-loaded e quantum dot, and oxygen level significantly reduces, and the graphenic surface after reduction introduces nitrogen-containing group.Investigated the impact of temperature of reaction and reaction times, the reduction process impact of change on graphene oxide of temperature of reaction is little, and the impact in reaction times is relatively obvious.Along with the prolongation in reaction times, the reducing degree of Graphene is higher, and the CdSe of graphenic surface load is then grown up into the starlike nanostructure of nanometer rod and branching gradually by particle by quantum dot.By regulation and control reaction conditions can change while controlled oxidization Graphene reducing degree graphenic surface the pattern of CdS-loaded e quantum dot, this is that the preparation of the CdSe quantum dot load Graphene of morphology controllable provides a kind of effective ways.
A kind of CdSe quantum dot load Graphene with different-shape feature, graphenic surface has abundant N structure, the CdSe quantum dot of area load can change while controlled oxidization Graphene reducing degree graphenic surface the pattern of CdS-loaded e quantum dot.For electricity storage, solar cell and photocatalytic device.
Have the CdSe quantum dot load graphene preparation method of different-shape feature, it is characterized in that, concrete steps are as follows:
The preparation of a graphene oxide
The concrete operation step of graphene oxide is as follows: take a certain amount of natural graphite powder in large beaker in, slowly add the vitriol oil.Beaker is placed in ice-water bath, under stirring, in beaker, slowly adds KMnO
4, now solution gradually becomes deep green.After completing, taken out by beaker from ice-water bath, ice-water bath temperature controls in 0 (± 1) DEG C.Then, after stirring at room temperature for some time, in beaker, slowly deionized water is dripped with separating funnel.In the process that adds water, solution becomes grey from green gradually, last pinkiness.After stirring for some time, beaker is placed in hot oil bath, temperature is 90 DEG C, and taken out by beaker after heating for some time, add deionized water, add hydrogen peroxide, solution becomes glassy yellow.Leave standstill, abandoning supernatant, collecting precipitation thing, with a large amount of water and ethanol repetitive scrubbing, until solution is in neutral.Lyophilize, collects product and is graphene oxide.Graphene oxide is added in deionized water, ultrasonic stripping, obtain the graphene oxide suspension liquid of stable dispersion.Graphene oxide suspension liquid is 1mg/mL.
The preparation of bCdSe quantum dot load Graphene
Adopt solvent-thermal method one step to prepare CdSe quantum dot load Graphene, concrete operation step is as follows: get certain density CdCl
2the aqueous solution is in flask, and concentration is 0.25mmol/L.Add selenium powder, then add the graphene oxide suspension liquid through centrifugal treating, finally add reductive agent, reductive agent is quadrol.Cumulative volume is made to be 20ml, ultrasonic disperse certain hour after stirring.Above-mentioned mixed solution being transferred to liner is in the stainless steel cauldron of tetrafluoroethylene, insulation reaction certain hour in constant temperature oven.Naturally cool to room temperature.Gained solution is carried out suction filtration, and with a large amount of water and ethanol repetitive scrubbing, collects solid, high-temperature vacuum is dry.Temperature is 50 DEG C.
Beneficial effect: using quadrol as reductive agent, adopts a step solvent-thermal method to prepare CdSe quantum dot load Graphene.Whole preparation process is simple, inexpensive, workable, the reducing degree of Graphene and the pattern of CdSe quantum dot in gained mixture can be controlled in a big way by controlling the parameters such as reactant ratio, reaction times and temperature of reaction, possessing the potentiality that industrialization magnanimity is produced.
Accompanying drawing explanation
The FT-IR spectrogram of the CdSe quantum dot load Graphene (G-CdSe) prepared under Fig. 1 graphene oxide (GO), CdSe quantum dot and differing temps;
Prepare at the XPS collection of illustrative plates (C1s) 120 DEG C of Fig. 2 (a) CdSe quantum dot load Graphene
Prepare at the XPS collection of illustrative plates (C1s) 180 DEG C of Fig. 2 (b) CdSe quantum dot load Graphene
The FT-IR spectrogram of the CdSe quantum dot load Graphene (G-CdSe) prepared under Fig. 3 graphene oxide (GO), CdSe quantum dot and different time
XPS collection of illustrative plates (C1s) 3h of Fig. 4 (a) CdSe quantum dot load Graphene
XPS collection of illustrative plates (C1s) 6h of Fig. 4 (b) CdSe quantum dot load Graphene
SEM spectrogram (A) 3h that Fig. 5 CdSe quantum dot load Graphene changed with the reaction times, (B) 6h, (C) 12h, (D) 24h,
With TEM spectrogram (E) 6h, (F) 12h, (G) 24h.
Embodiment
The concrete steps preparing the CdSe quantum dot load Graphene of different-shape feature are as follows:
The preparation of a graphene oxide
The concrete operation step of graphene oxide is as follows: take a certain amount of natural graphite powder in the large beaker of 1000ml, slowly add the certain volume vitriol oil.Beaker is placed in ice-water bath, and holding temperature, in 0 (± 1) DEG C, slowly adds a certain amount of KMnO under stirring in beaker
4, now solution gradually becomes deep green.After completing, beaker is taken out from ice-water bath, then after stirring at room temperature 1h, in beaker, slowly drip certain volume deionized water with separating funnel.In the process that adds water, solution becomes grey from green gradually, last pinkiness.After stirring 1h, beaker is placed in the oil bath of 90 DEG C, taken out by beaker after heating 30min, add certain volume deionized water, add certain volume hydrogen peroxide (30%), solution becomes glassy yellow.Leave standstill, abandoning supernatant, collecting precipitation thing, with a large amount of water and ethanol repetitive scrubbing, until solution is in neutral.Lyophilize, collects product and is graphene oxide.Graphene oxide is added in deionized water, ultrasonic stripping, obtain the graphene oxide suspension liquid of stable dispersion.The graphene oxide suspension liquid prepared in this patent is 1mg/mL, and if no special instructions, described graphene oxide turbid liquid concentration is all taken this as the standard.
The preparation of bCdSe quantum dot load Graphene
Adopt solvent-thermal method one step to prepare CdSe quantum dot load Graphene, concrete operation step is as follows: getting certain volume concentration is finite concentration CdCl
2the aqueous solution, in the flask of 50ml, adds a certain amount of selenium powder, then adds the graphene oxide suspension liquid of certain volume through centrifugal treating, finally adds certain volume quadrol, make cumulative volume keep certain l, ultrasonic disperse 30min after stirring.Above-mentioned mixed solution being transferred to liner is (amount of fill is 80%) in the stainless steel cauldron of tetrafluoroethylene, insulation reaction certain hour in constant temperature oven.Naturally cool to room temperature.Gained solution is carried out suction filtration, and with a large amount of water and ethanol repetitive scrubbing, collects solid, at a certain temperature vacuum-drying.。This patent has investigated differential responses temperature and differential responses time respectively on the impact of composite physical chemical property.
Result characterizes situation:
Temperature of reaction is on the impact of CdSe quantum dot load Graphene
(1) the FT-IR phenetic analysis of the CdSe quantum dot load Graphene prepared at differential responses temperature
Fig. 1 is the FT-IR spectrogram of the CdSe quantum dot load Graphene (G-CdSe) prepared under graphene oxide, CdSe quantum dot and differing temps.As seen from Figure 1, wherein 1728cm
-1the stretching vibration absorption peak of neighbouring C=O all disappears, typical hydroxyl stretching vibration absorption peak (3354cm
-1) obviously weaken.And all at 3400cm
-1there is the stretching vibration absorption peak of carbon nitrogen singly-bound, and all at 1590cm
-1near there is place's band multiplicity, and peak value is more weak, is secondary amine δ
n-Hflexural vibration.In the CdSe quantum dot load Graphene prepared under above-mentioned three temperature are described, Graphene not only obtains good reduction, and achieves chemically modified to it.But as can be seen from figure also, prepare the reduction of Graphene under differing temps and finishing degree is different, 3400cm at 120 DEG C
-1near absorption peak faint, and absorption peak at 210 DEG C is stronger.Hydroxyl stretching vibration absorption peak (3354cm
-1) also weaken gradually along with the rising of temperature of reaction, but not obvious.Illustrate thus, the reducing degree impact of temperature on graphene oxide is less, and raised temperature can increase the content of graphenic surface nitrogen-containing group.
(2) the XPS phenetic analysis of the CdSe quantum dot load Graphene prepared at differential responses temperature
Fig. 2 is the XPS collection of illustrative plates (C1s) of the CdSe quantum dot load Graphene prepared at differential responses temperature.(A) preparation at 120 DEG C; (B) prepare as seen from Figure 2 at 180 DEG C, in CdSe quantum dot load Graphene, the oxy radical of Graphene obviously reduces, and oxygen level obviously reduces, and illustrates that the reducing degree of recombination process graphene oxide is good.N1s peak in XPS, illustrates and introduce nitrogen-containing group in recombination process.Comparison diagram (A) and (B) can confirm further, and after compound, the oxygen level of Graphene reduces further along with the raising of temperature, but not obvious, illustrate that the surface functional group impact of temperature on Graphene in reduction process is less.
Reaction times is on the impact of CdSe quantum dot load Graphene
(1) the FT-IR phenetic analysis of the CdSe quantum dot load Graphene prepared under the differential responses time
Fig. 3 is the FT-IR spectrogram of the CdSe quantum dot load Graphene prepared under graphene oxide, CdSe quantum dot and different time.(A) 3h; (B) 6h, as seen from Figure 3, when the reaction times is 3h, the functional group content of its surface significantly weakens, simultaneously 3400cm
-1near occurred one significantly sharp-pointed absorption band be the stretching vibration absorption peak of carbon nitrogen singly-bound, 1590cm
-1near there is place's band multiplicity, and peak value is more weak, is secondary amine δ
n-Hflexural vibration.Along with the reaction times extend to more than 6h time, 1728cm
-1neighbouring carbonylic stretching vibration absorption peak and 3354cm
-1neighbouring wide typical hydroxy stretching vibration absorption peak disappears all substantially, and the functional group absorption peak of nitrogen strengthens all to some extent.Illustrate thus, the length changing the reaction times not only can regulate and control the reducing degree of graphene oxide, and can regulate the content of its surperficial nitrogen-containing group.Fig. 4 is the XPS collection of illustrative plates of the CdSe quantum dot load Graphene obtained after the different thermal reduction time.As seen from Figure 4, after the reaction times extends to 6h by 3h, the nitrogen peak in mixture on Graphene obviously strengthens, and illustrates that nitrogen modification effect is further strengthened
[39].
(2) the shape characteristic analysis of the CdSe quantum dot load Graphene prepared after the differential responses time
Fig. 5 is the prolongation along with the reaction times, SEM and the TEM collection of illustrative plates of the CdSe quantum dot load Graphene of preparation.A)3h，(B)6h，(C)12h，(D)24h，(E)6h，(F)12h，(G)24h。Obviously can be observed the structure layer by layer of Graphene by figure, the graphene complex under each reaction conditions is all laminate structure, and dispersed better all can be observed few layer even single layer structure, its on the surface growth in situ stub and granular CdSe quantum dot.The successful load of CdSe quantum dot can strengthen the interlamellar spacing of Graphene, and then improves its dispersiveness, is conducive to the raising of performance.Grown up to bar-shaped even forked gradually by particle with CdSe in the prolongation mixture in reaction times, and when the time is shorter, the load number of particle is less.Illustrate thus, the length controlling the reaction times can also control the pattern of CdSe quantum dot while regulating Graphene reducing degree, and then is that the performance adjusting product provides convenient means.As for the concrete growth mechanism of CdSe quantum dot under solvothermal condition and Graphene derivative in the process role it be not immediately clear.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should be appreciated that; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by its equivalent of appending claims.
Claims (8)
1. one kind has the preparation method of the CdSe quantum dot load Graphene of different-shape feature, it is characterized in that, graphenic surface has abundant N structure, the CdSe quantum dot of area load can change while controlled oxidization Graphene reducing degree graphenic surface the pattern of CdS-loaded e quantum dot; Concrete steps are as follows:
The preparation of a graphene oxide
The concrete operation step of graphene oxide is as follows: take natural graphite powder in large beaker, slowly add the vitriol oil; Beaker is placed in ice-water bath, under stirring, in beaker, slowly adds KMnO
4, now solution gradually becomes deep green; After completing, beaker is taken out from ice-water bath, then after stirring at room temperature, in beaker, slowly drip deionized water with separating funnel; In the process that adds water, solution becomes grey from green gradually, last pinkiness; After stirring, beaker is placed in hot oil bath, taken out by beaker after heating, add deionized water, add hydrogen peroxide, solution becomes glassy yellow; Leave standstill, abandoning supernatant, collecting precipitation thing, with water and ethanol repetitive scrubbing, until solution is in neutral; Lyophilize, collects product and is graphene oxide; Graphene oxide is added in deionized water, ultrasonic stripping, obtain the graphene oxide suspension liquid of stable dispersion;
The preparation of bCdSe quantum dot load Graphene
Adopt solvent-thermal method one step to prepare CdSe quantum dot load Graphene, concrete operation step is as follows: get CdCl
2the aqueous solution, in flask, adds selenium powder, then adds the graphene oxide suspension liquid through centrifugal treating, finally adds reductive agent, makes cumulative volume be 20mL, ultrasonic disperse after stirring; Above-mentioned mixed solution being transferred to liner is in the stainless steel cauldron of tetrafluoroethylene, insulation reaction in constant temperature oven, and in constant temperature oven, temperature of reaction is 180 DEG C; Naturally cool to room temperature; Gained solution is carried out suction filtration, and with water and ethanol repetitive scrubbing, collects solid, high-temperature vacuum is dry; The temperature of high-temperature vacuum drying is 50 DEG C.
2. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1, is characterized in that, prepares the Graphene of gained for electricity storage, solar cell and photocatalytic device.
3. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1, it is characterized in that, in step a, graphene oxide suspension liquid is 1mg/mL.
4. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1 or 3, it is characterized in that, in step a, ice-water bath temperature controls at 0 ± 1 DEG C.
5. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1 or 3, it is characterized in that, in step a, hot oil bath temperature is 90 DEG C.
6. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1 or 3, it is characterized in that, the reductive agent in step b is quadrol.
7. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1 or 3, is characterized in that, CdCl in step b
2concentration is 0.25mmol/L.
8. the preparation method with the CdSe quantum dot load Graphene of different-shape feature according to claim 1 or 3, it is characterized in that, in step b, reaction obtains particulate state CdSe quantum dot for 6 hours, react and within 12 hours, obtain bar-shaped CdSe quantum dot, react and within 24 hours, obtain dendroid CdSe quantum dot.
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| CN104477854B (en) * | 2014-11-17 | 2016-06-22 | 武汉理工大学 | Ternary semiconductor quantum dot Graphene functional composite material and preparation method thereof |
| CN104588044B (en) * | 2014-12-30 | 2015-11-25 | 吉首大学 | Quantum dot sensitized graphene-based mesoporous coated CdSeMT/GR visible light catalytic composite nano materials and preparation technology |
| CN105293475A (en) * | 2015-10-26 | 2016-02-03 | 李修兵 | Graphene and nickel diselenide composite and preparation method thereof |
| CN107591248B (en) * | 2017-08-04 | 2019-03-12 | 天津师范大学 | Quantum dot-graphene-carbon nano-tube film composite and flexible solar battery photoanode and preparation method thereof |
| CN110320195B (en) * | 2019-08-21 | 2021-12-28 | 合肥工业大学 | Colorimetric fluorescent probe and preparation method and application thereof |
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