CN101157851A - Preparation method of quantum dot self-assembling nano structural material - Google Patents
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- CN101157851A CN101157851A CNA2007100530563A CN200710053056A CN101157851A CN 101157851 A CN101157851 A CN 101157851A CN A2007100530563 A CNA2007100530563 A CN A2007100530563A CN 200710053056 A CN200710053056 A CN 200710053056A CN 101157851 A CN101157851 A CN 101157851A
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Abstract
The invention discloses a preparation method of a super nanostructure material formed by quantum dots self-assembly. That the alcohols are used as solvent to prepare nano-metal oxides and sulphides or metal oxides and sulphides are reduced to get nano-metal is a widely used method. The super nanostructure material formed by the quantum dots self-assembly draws much attention because of the superior comprehensive properties. The application prospect is wide enough. The invention adopts a method of using the alcohols as the solvent that a super nanostructure with different appearances and is formed by the quantum dots self-assembly which is obtained by changing the condition under the existence condition of surfactant. According to the invention, precursor, namely organic metal compound is dissolved in the alcohol solvent by ultrasonic, stirring and being laid down quietly. Under the effect of the surfactant, the precursor has a nucleation and grows into a plurality of quantum dots, the size of which is similar to nano. Then the dots form a super nanostructure which has a certain shape or space structure along the defined growing direction of the surfactant.
Description
Technical field
The invention belongs to the preparation method of quantum dot self-assembling nano structural material.Super nano structural material has application prospect at transmitter, nano electron device, superelevation magnetic recording multi-media, lithium cell with based on aspects such as the solar cell of nanostructure and new catalyst, sterilant, algicides.
Background technology
Recently, method by self-assembly forms super nanostructure and has caused great concern, this is because preparation-obtained super nano structural material has a wide range of applications in fields such as catalysis, medicine, electronics, potteries (Chem.Commun.2004,2182).A large amount of experimental techniques such as molecule crosslinked method (Adv.Mater.1995,7,795), (Nature 1996 for the dna profiling method, 382,607), chemistry and little preparation method (Adv.Mater.2001,13,427), self-assembly superlattice method (Adv.Mater.1998,10,13) etc. the quilt development prepares high-sequential, has the structure of space diagram.Simultaneously, use bionical pattern strategy also to be used to template and prepare inorganic super nanostructure (Angew.Chem.Int.Ed.2005,44,6004) with self-assembly characteristic.Though these methods can prepare various patterns, have the nanostructure of certain space figure, owing to reasons such as preparation process complexity, processing requirement height are difficult to realize that a large amount of preparations is to satisfy the market requirement in the future.
Synthesize various metals as solvent or metal oxide nano-material is a kind of widely used method (Angew.Chem.Int.Ed.2001,40,359) with alcohols, utilize this method TiO
2, CoO, ZnO, Cu
2O, Fe
2O
3, Nb
2O
3, Ta
2O
3, Al
2O
3Can both prepare etc. a lot of inorganic nano materials.In this method, alcoholic solvent can not only play the effect of hydrolysis, and some solvent can also reduce the compound that is in unstable valence state, even it is reverted to metal simple-substance.The main advantage of this method is to control homogeneity (J.Mater.Chem.1996,6,1047 of the shape, size and the granular size that are precipitated out particulate by changing experiment condition; Science, 2000,287,1989), can make single the dispersion or the nanostructure (J.Solid State Chem.2005,178,1489) of self-assembly, simple, the easy row of preparation process can be realized large-scale production simultaneously.
Summary of the invention
The objective of the invention is to utilize organometallic compound with " soft " template--the arrangement mode of precursor is controlled in the surfactant molecule interphase interaction, hydrolysis and/or reduction are arranged by " soft " template and precursor interaction mode with nano particle or even quantum dot with acquisition under the effect of alcoholic solvent then, and finally obtain quantum dot self-assembling nano structural.
Principle of the present invention is:
Usually preparing metal oxide, sulfide or metal with the polyvalent alcohol method relates generally to three steps: the one, and the dissolving of metal-salt (organometallic compound), two are intended for and store mutually and control GOLD FROM PLATING SOLUTION and belong to ion supersaturated concentration intermediate solid separating out mutually, the 3rd, the growth (J.Mater.Chem.2003 of intermediate solid phase nucleation and solid particulate under near the temperature of polyol solvent boiling point, 13,312).
The principles of chemistry that the polyvalent alcohol legal system is equipped with metal oxide, metal are: under the effect of alcoholic solvent, and organometallic compound generation hydrolysis reaction, its expression formula is as follows:
Me(OR)
m+mR’-OH→Me(OH)
m+mROR’
In the formula: m represents any positive integer, R '=H or alkyl;
Behind the reaction last very long, decomposition reaction can take place in solution metal oxyhydroxide, generates metal oxide.When solvent itself has certain reducing power, can obtain metal oxide at a low price and finally can reduce obtaining metal.
The principles of chemistry that the polyvalent alcohol legal system is equipped with metallic sulfide are: under the effect of alcoholic solvent, organometallic compound reacts with sulfide or thioamides in the different pH values environment, and its expression formula is as follows:
2Me (OR)
m+ mS
2-(inorganic sulfur source)+2mR '-OH → Me
2S
m+ 2OH
2-+ 2mROR '
M represents any positive integer in the formula, R '=H or alkyl;
2Me (OR)
m+ 2mR '-OH+mR " CSNH
2(organosulfur source) → Me
2S
m+ 2mROR '+mNH
3+ mR " COOH
R in the formula " be arbitrary alkyl or the vinyl except that methyl.
When solvent itself had certain reducing power, the sulfide of generation further reaction obtain metal oxide at a low price, and finally can reduce and obtain metal.
Because tensio-active agent is different with micellar state of aggregation in the pH environment in the different solvents system, its existence in system can influence the state of aggregation of pre-reaction material, thereby the pattern of final product is exerted an influence.Generally, by long-time ultrasonic and/or stirring precursor is fully scatter, organometallic compound has an opportunity to contact with tensio-active agent as much as possible; Leave standstill the influence of nucleation state of aggregation in the time of can changing tensio-active agent to reactant reaction for a long time.By selecting suitable solvent, methods such as the concentration of control reaction, time, temperature, can control the generation of different valence state product, and nucleation is grown up be several nano-quantum points to tens nano particle, be self-assembled into super nanostructure by tensio-active agent accumulative mode.
The scheme that realizes the object of the invention is:
A kind of method for preparing the quantum dot self-assembling nano structural material is characterized in that, uses alcohol solvent method, comprises the preparatory phase of mixed reactant preprocessing process and matrix material,
Mixed reactant preprocessing process: select suitable organic solvent, the precursor organometallic compound of metal oxide, sulfide or metal is dissolved in the organic solvent, add tensio-active agent or reactant, or/and stir or/and leave standstill, the precursor organometallic compound of metal oxide, sulfide or metal and tensio-active agent or reactant are combined by ultrasonic;
The preparatory phase of matrix material: make the super nano structural material of assembling, be arranged in certain pattern or certain space structure by the particle that is of a size of several nanometers to tens nanometer by control reactant concn, kinds of surfactants, reaction times and temperature.
State in realization in the preprocessing process of mixed reactant of scheme, selected organic solvent is absolute alcohol or alcohol solution, described absolute alcohol is ethanol, propyl alcohol, Virahol, ethylene glycol, glycerol, glycol ether, triglycol, two glycerine, 1,2-n-Hexadecane glycol or polyvinyl alcohol.
In such scheme, employed organometallic compound is various metals, metal oxide or sulfide precursor, and these organometallic compounds are anhydrous or water-containing acetic acid salt crystal, salicylate, contain oxygen based metallization thing, metallic carbonyls thing, metal acid esters.
In the preprocessing process of the mixed reactant of such scheme, the concentration of organometallic compound in organic solvent is 1 * 10
-5-30 mol.
State in realization in the preprocessing process of mixed reactant of scheme, the concentration of tensio-active agent in organic solvent is 1 * 10
-7-10 mol, described tensio-active agent is selected from glucose, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, ethanamide, RCONH
2Acid amides, wherein R is arbitrary alkyl or vinyl, thioacetamide, thiobenzamide or RCSNH except that methyl
2Thioamides, its R is arbitrary alkyl or vinyl except that methyl.
State in realization in the preprocessing process of mixed reactant of scheme, mixture is ultrasonic or/and to stir the needed time be 5 minutes-5 hours.
State in realization in the preprocessing process of mixed reactant of scheme, it is ultrasonic or/and the mode that leaves standstill after mixing is open or/and closed, time of repose is 0.5-72 hour, and open is that solution directly is exposed in the air, and closed is that solution and outside air are isolated.
For realizing such scheme, in the mixed reactant preprocessing process of preparation sulfide, selected sulphur source can be sodium sulphite, potassium sulphide, sulfuration ammonia, Sodium sulfhydrate, potassium bisulfide, thioacetamide, thiobenzamide, RCSNH
2Deng thioamides, its R is arbitrary alkyl or vinyl except that methyl; It needed to be dissolved in the alcoholic solvent before joining reaction system, and its concentration is 1 * 10
-6-10 mol; Again by above-mentioned dissolving with leave standstill operating process and carry out.
State the preparatory phase of the matrix material of scheme in realization, the temperature of reaction is 50-300 ℃, is controlled in 2 (1) hours by the heating-up time of room temperature to temperature of reaction.
Realize such scheme, can obtain the different-shape CuO, the Cu that form by the quantum dot self-assembly
2O, Cu, ZnO, CdO, NiO, Ni, CoO, Co, TiO
2, Al
2O
3, Fe
2O
3, Fe, Nb
2O
5, WO
3, V
2O
5, Sb
2O
5, Sb
2O
3, SnO
2, SnO, Sn, MoO
3, MoO, Mo, Ta
2O
5, Bi
2O
3, La
2O
3, Y
2O
3, ZrO
2, Ag, Pt, Pa, Cu
2S, CuS, CdS, ZnS, Ag
2Numerous nano structural materials such as S, SnS or MoS.
Description of drawings
The transmission (left figure) of the upright nanometer stick array of Fig. 1 cuprous sulfide quantum dot self-assembly and stereoscan photograph (right figure neutralizes)
The stereoscan photograph of Fig. 2 cuprous sulfide quantum dot self-assembled nanometer rod flower-like structure
The transmission (left figure) of Fig. 3 cuprous sulfide quantum dot self-assembled nanowires and stereoscan photograph (right figure)
The scanning (last figure) of the flower-shaped super nanostructure of Fig. 4 Red copper oxide quantum dot self-assembly and transmission (figure below) electromicroscopic photograph
The uv-visible absorption spectra of super nanostructure of Fig. 5 Red copper oxide (A curve) and 200 nanocubes (B curve) (the little figure of insertion is the bandwidth calculated curve).
The stereoscan photograph of the super nanostructure of Fig. 6 zinc oxide: low power figure (left side) and high power figure (right side)
The XRD spectra of the super nanostructure of Fig. 7 zinc oxide
Embodiment
Embodiment 1: a water acetic acid copper 0.4 gram is dissolved in 70 milliliters of glycol ethers, and this solution under agitation is warmed up to 180 ℃.In this simultaneously, 0.075 gram thioacetamide is dissolved in 30 milliliters of glycol ethers by ultransonic method, and this solution of sealing and standing 3 hours, join then in 180 ℃ of above-mentioned neutralized verdigris solution, react the suspension that obtains black after 3 hours.After this system naturally cools to room temperature, isolate the black product, and with this product of absolute ethanol washing 3 times, dryly in vacuum drying oven obtain the final upright nanometer stick array of cuprous sulfide quantum dot self-assembly with centrifugation method.By transmission and stereoscan photograph (Fig. 1) as can be seen, this upright nanometer stick array is to be got up by the small-particle self-assembly of about 5 nanometers.
Keep above-mentioned same preparation condition, just change time to 5 hour of thioacetamide diethylene glycol solution sealing and standing, the stereoscan photograph of the product that obtains as shown in Figure 2, visible cuprous sulfide quantum dot has been self-assembled into by the flower-shaped arrangement of nanometer rod.
Keep above-mentioned same preparation condition, in neutralized verdigris solution, add 0.08 gram sodium hydroxide solution, after its temperature arrives 180 ℃, immediately the thioacetamide diethylene glycol solution for preparing is added and begins and react, finally obtain the cuprous sulfide nano wire (Fig. 3) that is assembled into by twin.
The Cu of method for preparing
2The super nanostructure of S has identical visible absorption spectrum, and the semiconductor material bandwidth that calculates by this spectrometer is 1.35 electron-volts, than micron order Cu
2Wanting of S is high 0.15 electron-volt, and this proves absolutely the existence of quantum effect, and this nanostructure of more abundant proof is formed by the quantum dot self-assembly.
Change the solvent in the above-mentioned system into ethanol, with the super nanostructure of the different shape for preparing CuS; Use other solvents can prepare ZnS, SnS, MoS, Ag
2The S quantum dot self-assembling nano structural.
Embodiment 2: with 2.3 mmoles/rise Glacial acetic acid copper and 4.3 mmoles/rise the ethanamide ultrasonic dissolution in 50 milliliters of glycol ether solvents, this solution is heated to 180 ℃, and after keeping 8 hours under this temperature, separates out the xanchromatic throw out.Behind this aaerosol solution cool to room temperature, the centrifugation throw out, and, in vacuum drying oven, obtain the xanchromatic product after dry 5 hours with ethanol flush away solvent.This product is the flower-shaped super nanostructure that is formed by 3～5 nano-quantum point self-assemblies, and its scanning and transmission electron microscope photo are as shown in Figure 4.What Fig. 5 showed is the spectrogram and the corresponding calculated bandwidth (band-gap energy) (curve A among the figure) of the uv drs of this structured material, compare with Red copper oxide 200 nanocubes (curve B among the figure) that we prepare ourselves, absorption peak by the flower-like nanostructure of quantum dot assembling has bigger blue shift, bandwidth reaches 2.25eV, big 0.25eV than macroscopic body material, than the cubical also big nearly 0.1eV of homemade 200nm, this has proved absolutely the existence of quantum limit threshold effect in super nanostructure of quantum dot.
Embodiment 3: 3 gram zinc acetates are mixed with 300 milliliters of ethylene glycol solvents, be warmed up to 250 ℃ behind the ultrasonic dissolution under vigorous stirring, hydrolysis reaction continued after 2 hours, cool to room temperature.By centrifugation, washing, and repeatedly after 3 times, put into the super nanostructure of ZnO that the baking oven oven dry promptly obtains white.High-resolution-ration transmission electric-lens observe to find, this nanostructure is the dendritic structure that forms of the monocrystalline self-assembly by the 3-10 nanometer (shown in Figure 6).It is the ZnO (see figure 7) that XRD detects the proof crystal.
The preparation process of CdO quantum dot self-assembling nano structural and above-mentioned basically identical, just solvent is a butyleneglycol.
Embodiment 4: the tetrabutyl titanate of 1 gram is dispersed in by vigorous stirring in 400 milliliter 2% the polyvinyl alcohol solution, remain under 200 ℃ the condition reaction in temperature 10 hours, centrifugation behind the stopped reaction, washing are repeatedly after 3 times, with the product oven dry, obtain the TiO of white
2Super nanostructure.Electron microscopic observation finds that titanium dioxide is is several microns nano wire by the length that the quantum dot about 5 nanometers is assembled into.The existence of uv-visible absorption spectra proof quantum effect.XRD analysis proves that the titanium dioxide crystal in this matrix material mainly is sharp attitude type, but also has red stone type of a spot of crystalline substance and plate attitude ore deposit to exist.
SiO
2, SnO
2, ZrO
2The preparation of quantum dot self-assembling nano structural and TiO
2Similar, be that employed hydrolysising solvent is respectively glycol ether, triglycol and glycerol.
Embodiment 5: the oxyethyl group niobium of 1 gram is put into reactor with 500 milliliters of glycerol solvents, under vigorous stirring, temperature is raised to 250 ℃, reacts and stop after 5 hours, with the centrifugation of gained suspension, and, put into the vacuum drying oven oven dry and promptly obtain Nb with distilled water wash throw out 3 times
2O
5Super nanostructure.Electronic microscope photos shows Nb
2O
5Be the hollow ball that is assembled into by the 4-8 nano particle, have good quantum effect but ultraviolet-visible absorbs the test shows material.XRD analysis shows that granular quantum dot exists with crystalline form.
V
2O
5, Sb
2O
5, Ta
2O
5The preparation method and the said process of quantum dot self-assembling nano structural are similar.
Embodiment 6: the platinum acetate of 0.5 gram is put into reactor with 300 milliliter 1,2-n-Hexadecane diol solvent, vigorous stirring, add initiator oleic acid and be raised to 200 ℃ in temperature, react and stop after 8 hours, with the centrifugation of gained suspension, and, put into the super nanostructure that the baking oven oven dry promptly obtains the self-assembly of Pt quantum dot with distilled water wash throw out 3 times.Spectroscopic analysis has quantum effect.XRD analysis proof nano particle is the Pt metal simple-substance.
The preparation process basically identical of the preparation process of Ag, Pa quantum dot self-assembling nano structural and Pt.
Embodiment 7: 2 gram nickel acetates are put into reactor with 300 milliliters of glycol ether solvents, vigorous stirring, be raised to 180 ℃ in temperature, react and stop after 3 hours, with the centrifugation of gained suspension, and with distilled water wash throw out 3 times, promptly obtain the super nanostructure of the NiO quantum dot self-assembly of black after the oven dry.Electronic microscope photos show NiO for the 2-3 nano-quantum point be assembled into by the compact arranged array of nanometer rod, the ultraviolet-visible light absorption analysis proves that this structure has quantum effect.XRD analysis proof nano particle is a nickel oxide.
Fe
2O
3, CoO and MoO quantum dot self-assembling nano structural preparation process and NiO preparation method similar, just hydrolysising solvent needs also need extend to more than 6 hours with the reaction time with having three hydroxyls, glycerol or triglycol that reductibility is stronger.
Embodiment 8: 1 gram tin oxalate (II) is put into reactor with 300 milliliters of ethylene glycol solvents, vigorous stirring, be raised to 150 ℃ in temperature, react and stop after 6 hours, with the centrifugation of gained suspension, and, promptly obtain the SnO quantum dot self-assembling nano structural after the oven dry with distilled water wash throw out 3 times.Electronic microscope photos shows that SnO is that the length of side that quantum dot is self-assembled into is the cubes of 200 nanometers.Spectroscopic analysis has quantum effect.XRD analysis proof nano particle is a tin protoxide.
Change hydrolysising solvent into triglycol or glycerol in this reaction process, the reaction times extends to 10 hours, finally obtains the Sn quantum dot self-assembling nano structural.
Embodiment 9: six carbonylation tungsten of 1 gram are put into reactor with 500 milliliters of alcohol solvents, and vigorous stirring is raised to 120 ℃ in temperature, back flow reaction stopped after 8 hours, with the centrifugation of gained suspension, and, promptly obtain WO after the oven dry with distilled water wash throw out 3 times
3Quantum dot self-assembling nano structural.Electronic microscope photos shows WO
3Be the flower-like nanostructure that is self-assembled into by quantum dot.Spectroscopic analysis has quantum effect.XRD analysis proof nano particle is a tungstic oxide.
MoO
3The preparation process of quantum dot self-assembling nano structural and WO
3Similar.
Embodiment 10: 0.3 gram bismuth salicylate is put into reactor with 200 milliliters of propyl alcohol solvents, and vigorous stirring, when temperature is 150 ℃, back flow reaction 10 hours, after the suspension centrifugation was handled, oven dry promptly obtained Bi
2O
3Quantum dot self-assembling nano structural.TEM shows Bi
2O
3The diameter that is self-assembled into by the quantum dot about 5 nanometers is 1 micron, and thickness is the disk of 200 nanometers.Spectroscopic analysis has quantum effect.XRD analysis shows that this crystal is Bi
2O
3
La
2O
3, Y
2O and Sb
2O
3The preparation process of quantum dot self-assembling nano structural and Bi
2O
3Similar.
Claims (10)
1. method for preparing the quantum dot self-assembling nano structural material, it is characterized in that, use alcohol solvent method, the preparatory phase that comprises mixed reactant preprocessing process and matrix material, mixed reactant preprocessing process: select suitable organic solvent, the precursor organometallic compound of metal oxide, sulfide or metal is dissolved in wherein, add tensio-active agent or reactant, or/and stir or/and leave standstill, the precursor organometallic compound of metal oxide, sulfide or metal and tensio-active agent or reactant are combined by ultrasonic;
The preparatory phase of matrix material: make the super nano structural material of assembling, be arranged in certain pattern or certain space structure by the particle that is of a size of several nanometers to tens nanometer by control reactant concn, kinds of surfactants, reaction times and temperature.
2. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1, it is characterized in that, in the mixed reactant preprocessing process, selected organic solvent is absolute alcohol or alcohol solution, described absolute alcohol is ethanol, propyl alcohol, Virahol, ethylene glycol, glycerol, glycol ether, triglycol, two glycerine, 1,2-n-Hexadecane glycol or polyvinyl alcohol.
3. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1, it is characterized in that, employed organometallic compound is metal, metal oxide or sulfide precursor, and these organometallic compounds are anhydrous or water-containing acetic acid salt crystal, salicylate, contain oxygen based metallization thing, metallic carbonyls thing, metal acid esters.
4. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1 is characterized in that, in the preprocessing process of mixed reactant, the concentration of organometallic compound in organic solvent is 1 * 10
-5-30 mol.
5. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1 is characterized in that, in the preprocessing process of mixed reactant, the concentration of tensio-active agent in organic solvent is 1 * 10
-7-10 mol, described tensio-active agent is selected from glucose, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, ethanamide, RCONH
2Acid amides, wherein R is alkyl or vinyl, thioacetamide, thiobenzamide or RCSNH except that methyl
2Thioamides, wherein R is alkyl or vinyl except that methyl.
6. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1 is characterized in that, in the preprocessing process of mixed reactant, ultrasonic or/and time of stirring is 5 minutes-5 hours.
7. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1, it is characterized in that, in the preprocessing process of mixed reactant, the mode that leaves standstill is open or/and closed, time of repose is 0-72 hour, openly directly be exposed in the air for solution, closed is that solution and outside air are isolated.
8. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1, it is characterized in that, in the mixed reactant preprocessing process of preparation sulfide, selected sulfide is sodium sulphite, potassium sulphide, sulfuration ammonia, Sodium sulfhydrate, potassium bisulfide, thioacetamide, thiobenzamide or RCSNH
2Thioamides, its R is alkyl or vinyl except that methyl; Above-mentioned sulfide was dissolved in before joining reaction system in the alcoholic solvent, and its concentration is 1 * 10
-6-10 mol.Then, undertaken by the dissolving of claim 6 and the operating process of leaving standstill of claim 7 again.
9. the method for preparing the quantum dot self-assembling nano structural material as claimed in claim 1 is characterized in that, at the preparatory phase of matrix material, the temperature of reaction is 50-300 ℃, is controlled in 2 hours by the heating-up time of room temperature to temperature of reaction; The pH value of reaction soln is controlled between the 2-12.
10. the described application for preparing the method for quantum dot self-assembling nano structural material of claim 1 is characterized in that, the super nano structural material that is used to prepare the quantum dot self-assembly comprises: CuO, Cu
2O, Cu, ZnO, CdO, NiO, Ni, CoO, Co, TiO
2, Al
2O
3, Fe
2O
3, Fe, Nb
2O
5, WO
3, V
2O
5, Sb
2O
5, Sb
2O
3, SnO
2, SnO, Sn, MoO
3, MoO, Mo, Ta
2O
5, Bi
2O
3, La
2O
3, Y
2O
3, ZrO
2, Ag, Pt, Pa, Cu
2S, CuS, CdS, ZnS, Ag
2S, SnS or MoS.
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