CN101380625B - Preparation method of large-area nano-microparticles monolayer film - Google Patents
Preparation method of large-area nano-microparticles monolayer film Download PDFInfo
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Abstract
The invention provides a method for preparing a large-area nanometer particulate monofilm. In terms of nanometer particulate aqueous solvent, water-soluble nano-particles are extracted from colloid solution by adding (water-soluble organic substances, non-water-soluble liquid organic substances and water) in sequence, thereby preparing the nanometer particulate monofilm on a water-soluble/non-water-soluble liquid organic interface; regarding nano-particle alcoholic solution, the water-soluble nano-particles are extracted from the colloid solvent by adding (non-water-soluble liquid organic substances and water) in sequence, thereby preparing the nanometer particulate monofilm on the water-soluble/non-water-soluble liquid organic interface. The method can realize large-area preparation of the nanometer particulate monofilm, and has the advantages of low cost, simple operation, rapidness, non toxicity or low toxicity.
Description
Technical field:
The present invention relates generally to the method that a kind of self assembly prepares large-area nano-microparticles monolayer film.
Background technology:
Thin-film material always is the key factor that influences a national productivity, and this is determined by its critical role in national economy.Thin-film material can be used in numerous research fields such as sensor, magnetic storage, electronic circuit, catalysis and functional coating material.The broad research of nano material causes the new round upsurge of thin-film material research.This will inevitably lead the further develop rapidly of a lot of high-tech areas.
Up to now, following several method is adopted in the preparation of nanoparticle film substantially:
(1) natural evaporation construction from part.The nanoparticle drips of solution is added to used substrate surface, obtains the nanoparticle film by evaporating solvent gradually.This method is that the nanoparticle ratio of stabilizing agent is easier to form uniform nano-microparticles monolayer film (list of references: Murray, C.B. for mercapto alkane, trioctylphosphine oxide (TOPO) and organic amine; Kagan, C.R.; Bawendi, M.G.Science1995,270,1335-1338), but for the stable water miscible nanoparticle of non-sulfhydryl compound, nanoparticle is easy to reunite, and is unfavorable for forming uniform nanoparticle film.And this method to the requirement of substrate than higher, need the whole surface of substrate to have uniform physicochemical characteristics.And the area of the nanoparticle film that obtains is less, generally is in submicron order, can not use on a large scale.
(2) absorption construction from part.The characteristics of this method be at first substrate surface modify one deck can with the interactional molecule of nanoparticle of assembling, then substrate is placed the solution of nanoparticle, leave standstill a period of time, just obtain the film modified base material of nanoparticle (list of references: Raj, C.R. then; Jena, B.K.Chem.Commun.2005,2005-2007).The key of this method be seek can with the bifunctional molecule of substrate, nanoparticle effect.The type of this bifunctional molecule is very restricted on the one hand, has restricted nanoparticle and substrate range of choice; This class bifunctional molecule is relatively more expensive on the other hand, is unfavorable for industrial production.In addition, the particle coverage of this method is not high yet, greatly about 60%.
(3) the even glue method of rotation.The characteristics of this method are that certain amount of nano particulate drips of solution is added in the substrate, then by this substrate of rotation, make solvent evaporation and the nanoparticle film (list of references: Das.G. that obtains; Ferraioli, L.; Bettotti, P; De Angelis, F.; Mariotto, G.; Pavesi, L.; Di Fabrizio.E.; Soraru, G.D.Thin Solid Films2008,516,6804-6807).The solvent of solution must be the material that is easy to volatilize in this method, otherwise is difficult to obtain uniform nanoparticle film.The particle of resulting nanoparticle film is very low in suprabasil coverage.
(4) LB pushes away membrane technology.The characteristics of this technology are that non-water-soluble nanoparticle solution is distributed on the water surface, treat to adopt LB to push away the film instrument nanoparticle is forced into film (list of references: Tao, A. closely after the solvent evaporation; Kim, F.; Hess, C.; Goldberger, J.; He, R.R.; Sun, Y.G.; Xia, Y.N.; Yang, P D.Nano Lett.2003,3,1229-1233).The general volatile nonaqueous solvents of solvent in this method.This non-water-soluble nano-particle surface generally adopts mercapto alkane protection, causes the reactivity on surface to descend, and the costing an arm and a leg of instrument.
(5) chemical vapour deposition technique.The characteristics of this method are by utilizing the material that has become gas that thermal decomposition, reduction or other chemical reaction take place under certain conditions, obtain the desired substance of gaseous state, and then it is deposited to specific substrate surface, form nanoparticle film (list of references: Blanco, A.; Chomski, E.; Grabtchak, S.; Ibisate, M.; John, S.; Leonard, S.W.; Lopez, C.; Meseguer, F.; Miguez, H.; Mondia, J.P; Ozin, G.A.; Toader, O.; Van Driel, H.M.Nature2000,405,437-440).This method can suitability for industrialized production, but at the material of required film, this method has certain limitation, and requires very high to equipment.
(6) sputtering method.The characteristics of this method are the particle bombardment surfaces of solids with the lotus energy, solid atom (or molecule) is penetrated from the surface, and deposit to film forming method (list of references: Dixon, M.C. on the substrate surface; Daniel, T.A.; Hieda, M.; Smilgies, D.M.; Chan, M.H.W.; Allara, D.L.Langmuir2007,23,2414-2422).This method can be carried out in industrialization, and is very high to the equipment requirement equally, and, the yardstick skewness one of nanoparticle in the nano thin-film of preparation.
(7) using vaporization condensation process.The characteristics of this method are in the atmosphere of ultravacuum or low-pressure inert gas, by the heat effect of evaporation source, make metal to be prepared, alloy or compound become gas, and condensation forms nano film material (list of references: Pan, Z.W. then; Mahurin, S.M.; Dai, S.; Lowndes, D.H.Nano Lett.2005,5,723-727).This method also can be carried out in industrialization, and is also very high to the equipment requirement, and, the yardstick skewness one of nanoparticle in the nano thin-film of preparation.
From above method, substantially as can be seen, (1-5) method be " from small to large " technology-by little nanoparticle directly assembling obtain big nanoparticle film.And (6,7) method is the technology-prepare nanoparticulate thin films by big block materials of " from big to small ".Though (1-4) method is simple to operate, the particle size big or small homogeneous that distributes in the nano thin-film that obtains, and waywardly obtain large-area film, in industrial its great application value that also do not highlight; Although (5-7) method all needs expensive equipment, these three kinds of methods all can be used in suitability for industrialized production.But, it is inhomogenous adopting in the nano thin-film that (5-7) method obtains particle size to distribute.Above method respectively has pluses and minuses, and Given this, it is necessary invent a kind of simple, quick and technology of preparing nanoparticle film that can large-scale production.
Summary of the invention:
The present invention wants institute's technical solution problem to be, at the deficiency that prior art exists, provides a kind of simple, technology that can prepare the large-area nano-microparticles film.The characteristics of this technology: 1. do not need expensive equipment; 2. the area of nanoparticle film changeable (square centimeter-square metre); 3. the particle in the nano thin-film is individual layer and arranges; 4. the coverage of particle can reach more than 90% in the film; 5. the particle size in the nano thin-film is controlled; 6. agents useful for same can be reused through simple process.With low cost, simple to operate, quick, the nontoxic or low toxicity of this method, be easy to industrial production.
Technical scheme of the present invention is, the described method for preparing the nanoparticle film is, with water-soluble nano particulate, water soluble organic substance, water-insoluble liquid state organics and water is raw material, for the nanoparticle aqueous solution, adding (water soluble organic substance, water-insoluble liquid state organics and water) by in turn extracts water soluble nanometer particles from colloidal solution, prepare nano-microparticles monolayer film at water/water-insoluble liquid state organics on the interface; For the nanoparticle alcoholic solution, the adding (water-insoluble liquid state organics and water) by in turn extracts water soluble nanometer particles from colloidal solution, prepare nano-microparticles monolayer film at water/water-insoluble liquid state organics on the interface.
Below the present invention made further specify, the preparation method of a kind of large-area nano-microparticles monolayer film provided by the invention may further comprise the steps: (1) is 1.0g/L～10 to the quality volumetric concentration
-5Add water soluble organic substance in the aqueous solution of the nanoparticle of g/L, forming nanoparticle solution or directly adopting the quality volumetric concentration is 1.0g/L～10
-5The alcoholic solution of the nanoparticle of g/L;
(2) be that 10%～100% non-water-soluble liquid state organics of step (1) liquor capacity is poured in the solution that above-mentioned steps (1) obtains with volume;
(3) be that 10%～100% water of step (2) overall solution volume is poured in the solution that above-mentioned steps (2) obtains with volume, nano-microparticles monolayer film forms on the interface of water/water-insoluble liquid state organics;
(4) above-mentioned nano-microparticles monolayer film is transferred to solid substrate (referring to Fig. 3-5,6-12).
Compare with the self-assembling technique of routine, the present invention does not have the stabilizing agent and the polyelectrolyte of use and nanoparticle strong bonding, and the nano-particle surface that constitutes nano thin-film maintains higher chemical reactivity, can be used for surface reaction carrier, catalyst.
The nanoparticle aqueous solution that the present invention is used and alcoholic solution can be that nano-powder is distributed to the nanoparticle solution that forms in the dispersant, also can be directly synthetic nanoparticle original solutions
The dispersant of above-mentioned nanoparticle is water or 5 unary alcohols that carbon atom is following.
Above-mentioned water soluble organic substance is following unary alcohol, ketone or organic acids of water-soluble 5 carbon atoms.
Above-mentioned water-insoluble liquid state organics is heptane, carbon tetrachloride, cyclohexane, benzene, toluene or chlorobenzene.
If when using the nanoparticle aqueous solution, used water soluble organic substance volumetric usage is 1:10～10:1 with nanoparticle liquor capacity ratio among the present invention, preferred 2:5～6:5.
If when using the nanoparticle alcoholic solution, do not need to add water soluble organic substance, and directly carry out step (2).
The liquor capacity ratio that the volumetric usage of used water-insoluble liquid state organics and step (1) obtain among the present invention is 10%～100%.
The nanoparticle film for preparing among the present invention has the thickness of a particle.
Consumption and the preparation volume of a container of the present invention by changing raw material can be realized control to the area of nanoparticle film, generally at 1 square centimeter to 1000 square centimeters, and preferred 1 square centimeter to 200 square centimeters.
The present invention adopts the organic matter suction-operated to reduce the nanoparticle surface electric charge, under the triggering of water, a large amount of nano particles in the solution are extracted into form the stabilized nano particle film on the two-dimentional interface of water-insoluble liquid state organics/water, nanoparticle is transferred to the technology of preparing of suprabasil a kind of nanoparticle film arbitrarily by the way that lifts.
As known from the above, the present invention can realize the extensive assembling to water soluble nanometer particles, and described method is with low cost, simple to operate, quick, nontoxic or low toxicity for a kind of technology of assembling preparation nanoparticle film.
Description of drawings:
Fig. 1 is nano-microparticles monolayer film preparation method's a operational flowchart;
Fig. 2 is the digital pictures that the golden particle film of 18nm is transferred to the crystallising dish bottom, and area is approximately 200 square centimeters;
Fig. 3 is that the non-water-soluble liquid state organics of adding is the transmission electron micrograph of the 18nm gold nano particulate film of benzene;
Fig. 4 is that the non-water-soluble liquid state organics of adding is the transmission electron micrograph of the 18nm gold nano particulate film of toluene;
Fig. 5 is that the non-water-soluble liquid state organics of adding is the transmission electron micrograph of the 18nm gold nano particulate film of cyclohexane;
Fig. 6 is that to add non-water-soluble liquid state organics be that the average length of side of benzene is the transmission electron micrograph of the silver nano-particle film of 35nm;
Fig. 7 is that to add non-water-soluble liquid state organics be that the average length of side of heptane is the transmission electron micrograph of the silver nano-particle film of 35nm;
Fig. 8 is that to add non-water-soluble liquid state organics be that the average length of side of carbon tetrachloride is the transmission electron micrograph of the silver nano-particle film of 35nm;
Fig. 9 is that to add non-water-soluble liquid state organics be that the average length of side of chlorobenzene is the transmission electron micrograph of the platinum nanoparticle film of 3.3nm;
Figure 10 is that to add non-water-soluble liquid state organics be that the average length of side of carbon tetrachloride is the transmission electron micrograph of the platinum nanoparticle film of 3.3nm;
Figure 11 is that to add non-water-soluble liquid state organics be that the average length of side of chlorobenzene is the transmission electron micrograph of 200nm silica nanoparticles film;
Figure 12 is that to add non-water-soluble liquid state organics be that the average length of side of heptane is the transmission electron micrograph of 200nm silica nanoparticles film.
The specific embodiment:
Embodiment 1
To 5mL concentration is to add the 3mL propyl alcohol in the gold nano particulate aqueous solution of 0.91g/L, add 2mL benzene then, form benzene/water termination, after injecting 2mL water, the gold nano particulate film just forms on benzene/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 3).
Embodiment 2
To 5mL concentration is to add the 2mL butanone in the gold nano particulate aqueous solution of 0.074g/L, add 2mL toluene then, form toluene, after injecting 2mL water, the gold nano particulate film just forms on toluene, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 4).
Embodiment 3
To 5mL concentration is to add the 4mL butyric acid in the gold nano particulate aqueous solution of 0.00043g/L, add the 2mL cyclohexane then, form cyclohexane/water termination, after injecting 2mL water, the gold nano particulate film just forms on cyclohexane/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 5).
Embodiment 4
To 5mL concentration is to add 5mL acetone in the silver nano-particle aqueous solution of 0.00006g/L, add 3mL benzene then, form benzene/water termination, after injecting 2mL water, the silver nano-particle film just forms on benzene/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 6).
Embodiment 5
To 5mL concentration is to add 6mL acetone in the silver nano-particle aqueous solution of 0.038g/L, add the 2mL heptane then, form heptane/water termination, after injecting 2mL water, the silver nano-particle film just forms on heptane/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 7).
Embodiment 6
To 5mL concentration is to add 3mL acetone in the silver nano-particle aqueous solution of 0.16g/L, add the 2.5mL carbon tetrachloride then, form carbon tetrachloride/water termination, after injecting 2mL water, the silver nano-particle film just forms on carbon tetrachloride/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (see figure 8).
Embodiment 7
In being the methanol solution of platinum nanoparticle of 0.00072g/L, 5mL concentration adds the 2mL chlorobenzene, after injecting 2mL water, platinum nanoparticle film just forms on the chlorobenzene/water interface, film is transferred to by the method that lifts carried out transmission electron microscopy observation (see figure 9) in the substrate subsequently.
Embodiment 8
In being the methanol solution of platinum nanoparticle of 0.022g/L, 5mL concentration adds the 2mL carbon tetrachloride, after injecting 2mL water, platinum nanoparticle film just forms on carbon tetrachloride/water termination, subsequently film is transferred in the substrate by the method that lifts, and carries out transmission electron microscopy and observes (see figure 10).
Embodiment 9
In being the ethanolic solution of silicon dioxide microparticle of 0.045g/L, 5mL concentration adds the 3mL chlorobenzene, after injecting 2mL water, the silicon dioxide microparticle film just forms on the chlorobenzene/water interface, subsequently film is transferred in the substrate by the method that lifts, and carries out transmission electron microscopy and observes (seeing Figure 11).
Embodiment 10
In being the ethanolic solution of silicon dioxide microparticle of 0.00058g/L, 5mL concentration adds the 2.5mL heptane, after injecting 3mL water, the silica nanoparticles film just forms on heptane/water termination, subsequently film is transferred in the substrate by the method that lifts, carried out transmission electron microscopy and observe (seeing Figure 12).
Claims (6)
1. the preparation method of a large-area nano-microparticles monolayer film is characterized in that, adopts following steps:
(1) be 1.0g/L～10 to the quality volumetric concentration
-5Add water soluble organic substance in the aqueous solution of the nanoparticle of g/L, form nanoparticle solution, the aqueous solution of described nanoparticle and the volume ratio of water soluble organic substance are 1: 0.4-1.2; Perhaps directly adopting the quality volumetric concentration is 1.0g/L～10
-5The alcoholic solution of the nanoparticle of g/L;
(2) be that 10%～100% non-water-soluble liquid state organics of step (1) liquor capacity is poured in the solution that above-mentioned steps (1) obtains with volume;
(3) be that 10%～100% water of step (2) overall solution volume is poured in the solution that above-mentioned steps (2) obtains with volume, nano-microparticles monolayer film forms on the interface of water/water-insoluble liquid state organics;
(4) above-mentioned nano-microparticles monolayer film is transferred to solid substrate;
Described water soluble organic substance is the following unary alcohol of 5 carbon atoms or ketone, organic acid compound;
Described non-water-soluble liquid state organics is heptane, carbon tetrachloride, cyclohexane, benzene, toluene or chlorobenzene.
2. according to the preparation method of the described large-area nano-microparticles monolayer film of claim 1, it is characterized in that the described nanoparticle aqueous solution and alcoholic solution are that nano-powder is distributed to nanoparticle solution or the directly synthetic nanoparticle original solution that forms in the dispersant.
3. according to the preparation method of the described large-area nano-microparticles monolayer film of claim 2, it is characterized in that the dispersant of described nanoparticle solution is water or 5 unary alcohol compounds that carbon atom is following.
4. according to the method for the described large-area preparation nano-microparticles monolayer film of claim 1, it is characterized in that described nano-microparticles monolayer film has the thickness of single nanoparticle.
5. according to the method for the described large-area preparation nano-microparticles monolayer film of claim 1, it is characterized in that the area of described nano-microparticles monolayer film is 1 square centimeter～1000 square centimeters.
6. according to the method for the described large-area preparation nano-microparticles monolayer film of claim 5, it is characterized in that the area of described nano-microparticles monolayer film is 1 square centimeter～200 square centimeters.
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| TWI421209B (en) * | 2010-08-12 | 2014-01-01 | Academia Sinica | Large-area particle-monolayer and method for fabricating the same |
| CN103966655B (en) * | 2014-05-07 | 2016-08-10 | 哈尔滨工业大学 | A kind of preparation method of opal structural 2 D photon crystal |
| CN109689329B (en) * | 2016-06-10 | 2021-10-19 | 迈克尔·波珀 | Method and apparatus for producing large area monolayer films of solution dispersed nanomaterials |
| CN108642487A (en) * | 2018-05-23 | 2018-10-12 | 厦门斯贝克科技有限责任公司 | A kind of preparation method of two-dimension single layer Ag SHINs films |
| CN111974612A (en) * | 2020-08-25 | 2020-11-24 | 中国科学院长春光学精密机械与物理研究所 | Film preparation equipment and method |
| CN113707769B (en) * | 2021-08-24 | 2023-10-17 | 福州大学 | High-precision patterned LED leakage current blocking layer based on transfer printing insulating Langmuir monolayer and preparation method thereof |
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| FR2848476A1 (en) * | 2002-12-16 | 2004-06-18 | Univ Aix Marseille Ii | Method for micro-deposition of molecules on a substrate by utilizing an atomic force microscope tip, by dispersing molecules in a solution of very low saturated vapour tension |
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