CN101696002A - Graphene and semiconductor nano particle compound system and synthesizing method thereof - Google Patents
Graphene and semiconductor nano particle compound system and synthesizing method thereof Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 98
- 239000004065 semiconductor Substances 0.000 title claims abstract description 95
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 92
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- 238000000034 method Methods 0.000 title claims abstract description 14
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Abstract
The invention discloses a graphene and semiconductor nano particle compound system and a synthesizing method thereof in the field of nano materials. The compound system comprises a single or multiple graphite sheet layers and semiconductor nano particles, wherein the graphite sheet layers and the semiconductor nano particles are carried out noncovalent compounding with graphene in solution by pyridine, pyrene or a derivative containing a pi bond or hydroxyl or carboxyl is modified on the graphite sheet layers by a chemical oxidation reduction method, and the amino modification is carried out on the surface of the semiconductor nano particles; and the graphene and semiconductor nano particle compound system is formed by the covalent combination of the hydroxyl or carboxyl and amino. The invention can really improve the interface geometrical contact and energy matching of the graphene and the semiconductor nano particles and creates beneficial condition for the industrial application of a photoelectric device based on the compound system.
Description
Technical field
The present invention relates to a kind of compound system and synthetic method thereof of semiconductor nano material, relate in particular to the nano material and the synthetic method thereof of the good compound one of semiconductor nanoparticle of the Graphene of a kind of specific surface area big and electricity and thermal property excellence and light sensitive characteristic, belong to the semiconductor material preparing technical field.
Background technology
Graphene (Graphene) is the carbon nano-structured material by the accurate two dimension of monolayer carbon atomic building, has big specific surface area and excellent electricity and thermal property.The mobility height of Graphene can surpass 10
4Cm
2/ Vs is hopeful to be applied at aspects such as high speed nano electron device in the future, biochemical sensors.But since it the zero gap semiconductor energy band structure and the monoatomic layer thickness limits its photoelectric properties, single-layer graphene almost is transparent to visible light, and minimum photoconduction is only arranged.So the photoelectric properties of improving carbon nanotube, Graphene are problems that needs solve.
Semiconductor nanocrystal also is known as nano particle, is to cause that people greatly study another nano material of interest.Its distribution of sizes in several nanometers to tens nanometer range.Semiconductor nanoparticle has important potential application aspect biological fluorescent labelling, electroluminescent, the photoelectric device.Semiconductor nanoparticle has the level spacing and the band gap of discrete electronic level and size dependence, therefore has good optical character.CdSe, the semiconductor nanoparticle of spatia zonularises such as PbSe is found the exciton doubling effect, is expected to be applied aspect high performance solar batteries.Semiconductor nanoparticle is made up of the core of inorganic semiconductor and the shell of organic ligand, and the organism part of coating plays in nano particle synthesizes and deposits and prevents to reunite and stabilization.But the existence of these insulation organic ligands, greatly reduce the coupling between the nanocrystal, and cause existing in the semiconductor nanoparticle assembly system a large amount of unordered, if unorderedly on energy surpassed coupling, whole system will be in similar Anderson-Mott insulator state.Therefore, semiconductor nanoparticle has utmost point low conductivity and photoconduction, and this has seriously limited nano particle and has used aspect photoelectricity.Semiconductor nanoparticle is used solar photovoltaic device has become an important research direction, and therefore, the specific conductivity of improving the semiconductor nanoparticle system is significant in the application of photoelectricity conversion aspect to them.
A common advantage of carbon nanotube, Graphene and semiconductor nanoparticle is to be easy to be made into big film of area and device.In carbon nano-tube film, the carbon nano-tube film of directed assembling causes people's very big concern, because directional property, high-density can be made into high-performance, device that homogeneity is good.In chemical vapor deposition (CVD) synthesizing carbon nanotubes process, utilize control air-flow, thermograde, electric field leading and employing single crystal quartz substrate can generate directed carbon nano pipe array.Recently, a large amount of preparations of Graphene have also obtained some impressive progresses, and the graphite oxide of chemical reduction can be by the electrostatic interaction stable dispersion in the aqueous solution.Directly the Graphene transparent conductive film with synthetic individual layer of CVD method and several layers also makes progress.These progress provide possibility for realizing based on the compound system of aligned carbon nanotube, Graphene.
Because the light sensitive characteristic of semiconductor nanoparticle, and carbon nanomaterial provides the conduction percolation path and improves mobility, and carbon nanomaterial and semiconductor nanoparticle compound system material cause people's intensive interest.Covalently boundly need carry out oxide treatment, cause carbon nanotube sp carbon nanotube
2Structural damage can the serious electroconductibility that reduces carbon nanotube.
Present both at home and abroad preliminary stage such as nano particle and the non-covalent compound work of carbon nanotube also only limits to synthesize, structure and optical property sign.How to design with synthesize nano carbon material and semiconductor nanoparticle non-covalent compound, make novel high transformation efficiency photoelectric device and be applied to the medium a lot of problems of photovoltaic device still unresolved.The non-covalent compound system of directionally assembled carbon nanotube and nanocrystal is not also carried out.The Graphene of aqueous solution dispersive chemical reduction and CVD prepare Graphene and just have breakthrough recently, and the non-covalent compound system preparation of Graphene and semiconductor nanoparticle still gets nowhere.Realizing that Graphene and semiconductor nanoparticle compound system also exist will solve both and dissolve each other in solution and interactional problem.The interface of how to improve carbon nanomaterial and semiconductor nanoparticle contacts for how much with energy flux matched so that can provide more effective charge migration to be still waiting research.Realize field-effect modulation carbon nanomaterial for the carrier concentration in the control carbon nanomaterial, problems such as carrier type also all have to be solved.
Summary of the invention
Purpose of the present invention aims to provide a kind of Graphene and semiconductor nanoparticle compound system and synthetic method thereof, solving both dissolves each other in solution and interactional problem, the interface how much of improving Graphene (or carbon nanomaterial) and semiconductor nanoparticle contact and energy flux matched, so that more effective charge migration to be provided.
First purpose of the present invention will be achieved through the following technical solutions:
Graphene and semiconductor nanoparticle compound system, it is characterized in that: the formation of described compound system comprises the graphite flake layer and the semiconductor nanoparticle of single or multiple lift, wherein said graphite flake layer size is between 20nm～600 μ m, the size of described semiconductor nanoparticle is between 2nm～100nm, graphite flake layer and semiconductor nanoparticle are combined into covalent structure, non-covalent structure, perhaps covalency and non-covalent and deposit structure.
Further, aforesaid Graphene and semiconductor nanoparticle compound system, wherein this graphite flake layer is by the dispersion Graphene with hydroxyl or carboxyl of Graphite Powder 99 through the chemistry redox preparation, or the Graphene lamella of thermal expansion cleavage intercalated graphite gained, or the carbon source graphene film that pyrolytic decomposition is made under metallic film catalysis.
Further, aforesaid Graphene and semiconductor nanoparticle compound system, wherein this Graphite Powder 99 that is used for chemistry redox comprises natural graphite powder, crystalline graphite powder, graphous graphite powder and expanded graphite powder; The intercalated graphite that is used for the thermal expansion cleavage comprises sulfuric acid intercalated graphite, sodium hydroxide intercalated graphite, potassium hydroxide intercalated graphite and basic metal potassium intercalated graphite; Described under metallic film catalysis the carbon source of pyrolytic decomposition be hydrocarbon polymer, comprise CH
4, C
2H
2, ethanol and benzene.
Further, aforesaid Graphene and semiconductor nanoparticle compound system, wherein this semiconductor nanoparticle has the part that contains the π key, this part is pyridine, pyrene, or the two one of derivative, or chemically modified is useful on and the covalently bound amino of Graphene on this semiconductor nanoparticle.
Second purpose of the present invention will be achieved through the following technical solutions:
The synthetic method of Graphene and semiconductor nanoparticle compound system is characterized in that: pyridine, the pyrene of described semiconductor nanoparticle by containing the π key, or the two one of derivative, in solution, carry out non-covalent compound with Graphene.Wherein said semiconductor nanoparticle is synthetic through chemical liquid phase, then with pyridine, pyrene, or the two one of derivative, semiconductor nanoparticle is carried out the part displacement forms.
Second purpose of the present invention can also be achieved through the following technical solutions:
The synthetic method of Graphene and semiconductor nanoparticle compound system, it is characterized in that: passing through hydroxyl or carboxyl in the modification of chemistry redox method on the described graphite flake layer, and carry out amido modified to described semiconductor nanoparticle surface, by hydroxyl or carboxyl and amino covalent attachment, form Graphene and semiconductor nanoparticle compound system.
After Graphene of the present invention and semiconductor nanoparticle compound system and the synthetic method application implementation thereof, can improve Graphene conscientiously contacts with energy flux matched how much with the interface of semiconductor nanoparticle, Graphene and the feasible synthetic method of semiconductor nanoparticle compound system are provided, for the industrial application based on the photoelectric device of this compound system has been created precondition.
Description of drawings
Fig. 1 is the non-covalent composite chemical equation that chemical reduction oxidation of the present invention prepares Graphene and semiconductor nanoparticle compound system;
Fig. 2 is the covalency composite chemical equation that chemical reduction oxidation of the present invention prepares Graphene and semiconductor nanoparticle compound system;
Fig. 3 a is the electron scanning micrograph that chemical reduction oxidation of the present invention prepares Graphene;
Fig. 3 b is the atomic force microscope photo that chemical reduction oxidation of the present invention prepares Graphene;
The abosrption spectrogram of Fig. 4 Graphene of the present invention and semiconductor nanoparticle compound system;
The transmission electron microscope picture of Fig. 5 Graphene of the present invention and semiconductor nanoparticle compound system.
Embodiment
The invention provides a kind of Graphene and semiconductor nanoparticle compound system and synthetic method thereof, being intended to solve both dissolves each other in solution and interactional problem, the interface how much of improving Graphene (or carbon nanomaterial) and semiconductor nanoparticle contact and energy flux matched, so that more effective charge migration performance to be provided.
As a whole, the formation of this compound system comprises the graphite flake layer and the semiconductor nanoparticle of single or multiple lift, is combined into covalent structure, non-covalent structure, perhaps covalency and non-covalent and deposit structure.Wherein:
This graphite flake layer size is between 20nm～600 μ m, it can be the dispersion Graphene for preparing and have hydroxyl or carboxyl by Graphite Powder 99 through chemistry redox, can be the Graphene lamella of thermal expansion cleavage intercalated graphite gained, also can be the carbon source graphene film that pyrolytic decomposition is made under metallic film catalysis.And this Graphite Powder 99 that is used for chemistry redox comprises natural graphite powder, crystalline graphite powder, graphous graphite powder and expanded graphite powder; The intercalated graphite that is used for the thermal expansion cleavage comprises sulfuric acid intercalated graphite, sodium hydroxide intercalated graphite, potassium hydroxide intercalated graphite and basic metal potassium intercalated graphite; The carbon source of the pyrolytic decomposition overwhelming majority is a hydrocarbon polymer under metallic film catalysis, comprises CH
4, C
2H
2, ethanol and benzene also can be hydrocarbon, for example CO.
The size of this semiconductor nanoparticle can adopt selenizing chromium (CdSe), tellurium chromium (CdTe), lead selenide (PbSe), lead telluride (PbTe), lead sulfide (PbS), chromic sulfide (CdS), zinc selenide (ZnSe), zinc sulphide (ZnS), zinc oxide (ZnO) and titanium oxide (TiO between 2nm～100nm
2) etc.Those semiconductor nanoparticles have the part that contains the π key, and this part can be pyridine, pyrene, or the two one of derivative, or chemically modified is useful on and the covalently bound amino of Graphene.
For further being convenient to understand the synthetic method of compound system of the present invention, below just with the Graphene of chemical reduction oxidation style preparation and two synthetic embodiment and the Graphene of other method preparation and the some synthetic embodiment of semi-conductor nano particles of semi-conductor nano particles, details are as follows:
Embodiment 1
Chemical reduction oxidation of the present invention as shown in Figure 1 prepares the non-covalent composite chemical equation of Graphene and semiconductor nanoparticle compound system, can be understood as: 1. after the Graphite Powder 99 process vitriol oil, potassium persulfate, the Vanadium Pentoxide in FLAKES oxidation, wash neutrality with deionized water, pass through the vitriol oil, the profound oxidation of potassium permanganate again, by adding a large amount of deionized waters and a certain amount of hydrogen peroxide termination reaction, wash neutrality by deionization once more.Obtain graphite oxide.Graphite oxide 1a process is ultrasonic, hydrazine hydrate reduction, and ammoniacal liquor is stable, obtains single-layer graphene 1b (shown in Fig. 3 a and Fig. 3 b, being electron scanning micrograph and the atomic force microscope photo that chemical reduction graphite oxide of the present invention prepares Graphene).2. the CdSe nano particle is synthetic, mainly adopt chromic oxide, octadecyl phosphoric acid (ODPA), three n-octyl phosphorus oxygen (TOPO) with the selenium powder that is dissolved in three n-octyl phosphorus (TOP) again 280 ℃ react half an hour down.Obtain the selenizing chromium 2 (CdSe-TOPO) that three n-octyl phosphorus oxygen are part.Selenizing chromium 2 is that the acquisition of part is to adopt CdSe-TOPO in anhydrous pyridine 118 ℃ with the pyridine; nitrogen protection was reacted 24 hours down; reaction product is through normal hexane precipitation, is solvent reaction 1 hour with the pyridine under 65 ℃ further after centrifugal, and this process repeats 3 times.Obtaining with the pyridine is the selenizing chromium 2a (CdSe-Py) of part.The acquisition of Graphene and nano particle compound system is to utilize the π key of pyridine among the π key of six-ring in the Graphene and the CdSe-Py to interact to obtain.After main process is diluted the Graphene that obtains, when stirring, add the pyridine solution of CdSe-Py, continue to stir, obtain Graphene-nano particle compound system 3.
Chemical reduction oxidation of the present invention as shown in Figure 2 prepares the non-covalent composite chemical equation of Graphene and semiconductor nanoparticle compound system, can be understood as: after the Graphite Powder 99 process vitriol oil, potassium persulfate, the Vanadium Pentoxide in FLAKES oxidation, wash neutrality with deionized water, pass through the vitriol oil, the profound oxidation of potassium permanganate again, by adding a large amount of deionized waters and a certain amount of hydrogen peroxide termination reaction, wash neutrality by deionization once more.Obtain graphite oxide.The graphite oxide process is ultrasonic, hydrazine hydrate reduction, and ammoniacal liquor is stable, obtains having the single-layer graphene 1 of hydroxyl or carboxyl.By the part displacement, utilize sulphur to link to each other CdSe semiconductor nanoparticle 2 with amino 2b, the Graphene with the preparation of chemical reduction graphite oxide mixes then, by amino 2b and carboxyl dehydration reaction, the Graphene of preparation and semiconductor nanoparticle covalency compound system.
The Graphene of the intercalated graphite of thermal expansion cleavage preparation and semiconductor nanoparticle non-covalent compound:
The Graphene lamella of intercalated graphite cleavage, put into autoclave or flask after it is characterized in that the natural or crystalline flake graphite of micro/nano level (100nm-800 μ m) and sulfuric acid or alkali mixed, between 250 ℃-400 ℃, carry out intercalation, reaction times surpasses 36 hours, forms the intercalated graphite material.After carrying out mechanical mill, between 900-1800 ℃, under high vacuum and hydrogen condition, carry out fast or thermal expansion at a slow speed, prepare the Graphene lamella.Then with contain pyridine, pyrene (Pyrene) with π key, or the two one of the semiconductor nanoparticle of derivative carry out non-covalent compound.
Embodiment 4
The Graphene and the semiconductor nanoparticle of chemical vapour deposition preparation are non-covalent compound:
The Graphene of chemical vapour deposition, the graphene film that it is characterized in that the chemical vapour deposition preparation are to adopt with metallic film (Fe, Ni, Co, Ag is Cu) as catalyzer, its film can adopt the electron beam evaporation preparation, also can adopt the magnetically controlled sputter method preparation, carries out anneal before the growth.Hydrocarbon polymer (CH
4, C
2H
2, ethanol, benzene) and be carbon source, the graphene film of high temperature (750 ℃-950 ℃) catalytic decomposition preparation.Then with contain pyridine, pyrene with π key, or the two one of the semiconductor nanoparticle of derivative carry out non-covalent compound.
By the description of above synthetic embodiment, the composite structure and the synthetic method of Graphene of the present invention and semiconductor nanoparticle compound system have been done comprehensive and full and accurate narration.For proving that it has the nano ZnO of marked improvement.As shown in Figure 4 and Figure 5, be the abosrption spectrogram and the transmission electron microscope picture of Graphene of the present invention and semiconductor nanoparticle compound system, wherein X-coordinate is a spectral wavelength among Fig. 4, ordinate zou is an absorptivity, three absorptivity change curves are represented the photoabsorption of the photoabsorption of Graphene and semiconductor nanoparticle compound system, pure Graphene, the photoabsorption of pure semiconductor nano particle respectively from top to bottom in the coordinate.Fig. 5 is the transmission electron microscope picture of Graphene and semiconductor nanoparticle compound system, can know and see a large amount of quantum dots there be (the straight fine rule of black that gathers among the figure) on the Graphene.This shows, the interface that the present invention can improve Graphene (or carbon nanomaterial) and semiconductor nanoparticle conscientiously contacts with energy flux matched how much, the effective ways of preparation Graphene and semiconductor nanoparticle compound system are provided, for the industrial application based on the photoelectric device of this compound system has been created precondition.
Claims (10)
1. Graphene and semiconductor nanoparticle compound system, it is characterized in that: the formation of described compound system comprises the graphite flake layer and the semiconductor nanoparticle of single or multiple lift, wherein said graphite flake layer size is between 20nm～600 μ m, the size of described semiconductor nanoparticle is between 2nm～100nm, graphite flake layer and semiconductor nanoparticle are combined into covalent structure, non-covalent structure, perhaps covalency and non-covalent and deposit structure.
2. Graphene according to claim 1 and semiconductor nanoparticle compound system, it is characterized in that: the dispersion Graphene with hydroxyl or carboxyl of described graphite flake layer for preparing through chemistry redox by Graphite Powder 99, or the Graphene lamella of thermal expansion cleavage intercalated graphite gained, or the carbon source graphene film that pyrolytic decomposition is made under metallic film catalysis.
3. Graphene according to claim 2 and semiconductor nanoparticle compound system is characterized in that: the described Graphite Powder 99 that is used for chemistry redox comprises natural graphite powder, crystalline graphite powder, graphous graphite powder and expanded graphite powder.
4. Graphene according to claim 2 and semiconductor nanoparticle compound system is characterized in that: the described intercalated graphite that is used for the thermal expansion cleavage comprises sulfuric acid intercalated graphite, sodium hydroxide intercalated graphite, potassium hydroxide intercalated graphite and basic metal potassium intercalated graphite.
5. Graphene according to claim 2 and semiconductor nanoparticle compound system is characterized in that: described under metallic film catalysis the carbon source of pyrolytic decomposition be hydrocarbon polymer, comprise CH
4, C
2H
2, ethanol and benzene.
6. Graphene according to claim 1 and semiconductor nanoparticle compound system is characterized in that: described semiconductor nanoparticle has the part that contains the π key, and this part is pyridine, pyrene, or the two one of derivative.
7. Graphene according to claim 1 and semiconductor nanoparticle compound system is characterized in that: described semiconductor nanoparticle chemically modified is useful on and the covalently bound amino of Graphene.
8. the synthetic method of described Graphene of claim 1 and semiconductor nanoparticle compound system, it is characterized in that: pyridine, the pyrene of described semiconductor nanoparticle by containing the π key, or the two one of derivative, in solution, carry out non-covalent compound with Graphene.
9. the synthetic method of Graphene according to claim 8 and semiconductor nanoparticle compound system, it is characterized in that: described semiconductor nanoparticle is synthetic through chemical liquid phase, then with pyridine, pyrene, or the two one of derivative, semiconductor nanoparticle is carried out the part displacement.
10. the synthetic method of described Graphene of claim 1 and semiconductor nanoparticle compound system, it is characterized in that: passing through hydroxyl or carboxyl in the modification of chemistry redox method on the described graphite flake layer, and carry out amido modified to described semiconductor nanoparticle surface, by hydroxyl or carboxyl and amino covalent attachment, form Graphene and semiconductor nanoparticle compound system.
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