CN102828176A - Preparation method for uniform gold nanoparticle film - Google Patents
Preparation method for uniform gold nanoparticle film Download PDFInfo
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- CN102828176A CN102828176A CN2012102694376A CN201210269437A CN102828176A CN 102828176 A CN102828176 A CN 102828176A CN 2012102694376 A CN2012102694376 A CN 2012102694376A CN 201210269437 A CN201210269437 A CN 201210269437A CN 102828176 A CN102828176 A CN 102828176A
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Abstract
The invention discloses a preparation method for a uniform gold nanoparticle film, which belongs to the field of preparation of nanomaterials. The method comprises the following steps: 1, preparing a nanometer solution (2) containing gold nanoparticles (1); 2, preparing a solution (3) containing polyvinylpyrrolidone and ascorbic acid; and 3, inserting a substrate material (4) for self-assembly deposition, wherein a layer of a gold nanoparticle film (5) is self-assembled on the substrate material after deposition is finished. The method is advantaged in that the deposition rate of the gold nanoparticles can be adjusted based on the concentrations of the gold nanoparticles, polyvinylpyrrolidone and ascorbic acid in the solutions. The gold nanoparticle film prepared by using the method has the characteristics of uniform distribution of the nanoparticles, no occurrence of accumulation, controllable spacing among the nanoparticles, strong adhesion of the gold nanoparticles and is extensively applicable to fields like surface-enhanced Raman scattering, photovoltaic synergism and light emitting diodes.
Description
Technical field
The invention belongs to the nano material preparation technical field, specifically is the method for the even gold nano grain film of a kind of large-area preparation.
Background technology
In recent years rice, the gold nano grain film is because its unique optics, electronics and catalytic performance and caused extensive interest in fields such as biology, medical science, optics, catalysis and nanoelectronicss.Why the gold nano grain film shows these peculiar characteristics with relevant attached to the nano particle character on the film, especially relevant with the metal nano material optical property.Metal nanoparticle will produce surface plasma excimer under the excitation of extraneous incident light.Surface plasma excimer is a kind of electromagnetic transmission pattern that the interaction between the unbound electron of light and metal or semiconductor material surface forms.This mode of electromagnetic wave can form resonance and transmission with the hertzian wave local in the scope of sub-wavelength, hertzian wave forms high optics local effect at Nanosurface.When incident electromagnetic wave shone the metal nanoparticle surface with nanoscale, the electric field composition in the incident electromagnetic wave and the free charge of nano grain surface formed consumingly and interact, and light field enhanced amplitude can reach 10
3-10
7Doubly.For field of solar energy, the gold nano grain film can improve the action intensity of incident light in photovoltaic material, increases the transmission range of incident light in material, thereby promotes photovoltaic material to absorption of incident light, improves the efficient of solar cell.For the bio-sensing field, the gold nano grain film increases by near the distribution of light intensity the detecting material through the surface plasma reinforcing effect, and then the strength of signal of raising detecting material etc.In addition, film of metal nano-particles also can be widely used in fields such as electrooptic modulator, photodiode, catalyzed reactions.
Gold nano grain can be according to the diverse microcosmic characteristic, like the difference of the couple state between particulate volume, shape, packaging assembly and the particle and have different character.Through the selection of gold nano grain arrangement mode and the difference of settled density, can realize the blue shift or the red shift of gold nano-material surface plasma body resonant vibration resonance peak.On the other hand, the application of every field has the requirement that has nothing in common with each other again to the microtexture of gold nano grain film, and the gold nano grain film that therefore prepares multiple structure, different settled densities is one of indispensable gordian technique of field of nano material preparation.
Summary of the invention
Technical problem: the objective of the invention is to overcome the deficiency of prior art, a kind of method for preparing even gold nano grain film is provided.Utilize the self-assembly behavior of metal nanoparticle in special chemical solution, regulate the microscopic appearance and the settled density of gold nano grain in several ways, realize big area uniform preparation gold nano grain film.
Technical scheme: for solving the problems of the technologies described above, the present invention provides a kind of method for preparing even gold nano grain film, and this method comprises the steps:
Step 1: preparation contains the nano-solution of gold nano grain;
Step 2: configuration contains the solution of Vinylpyrrolidone polymer and xitix;
Step 3: insert substrate material and carry out the self-assembly deposition, deposition will independently be adorned one deck gold nano grain film after accomplishing on substrate material.
Preferably, in the step 1:
Adopt any method in seed mediated growth method, xitix reduction method, Trisodium Citrate method, Peng Qinghuana method, electrochemical process, photoreduction method, the sonochemistry synthesis method to prepare the nano-solution that contains gold nano grain;
The gold nano grain that nano particle in the nano-solution is prepared various different shapeies and size according to the concentration and the preparation condition rice of reactant materials in each class methods.
Preferably, in the step 2, the method that configuration contains the solution of Vinylpyrrolidone polymer and xitix is:
In containing the nano-solution of gold nano grain, add Vinylpyrrolidone polymer and these two kinds of chemical substances of xitix; The PVP K120 concentration of adding is 0.01 mole and whenever is raised to 0.5 mole every liter that the concentration of the xitix of interpolation is 0.005 mole and whenever is raised to 0.6 mole every liter; Through adding PVP K120 and xitix, nano particle will be realized the modification of surface energy, facilitate nano grain surface can with the coupling of deposition substrate.
Preferably, in the step 3, when the insertion substrate material carries out the self-assembly deposition,
Use in the solution after clean substrate material vertically is inserted into interpolation PVP K120 and xitix, the self-assembly behavior will take place in gold nano grain this moment, spontaneously be deposited on the surface of substrate material, realize the preparation of even gold nano grain film.
Preferably, gold nano grain is the nanostructure of nanometer ball or nanometer rod or nanometer dish or nanometer square or nano flower-like, and size is that 1 nanometer is to 200 nanometers.
Preferably, substrate material is any in polished silicon slice, metal, glass, quartz plate, the transparent conducting glass matrix material.
Beneficial effect:
1, the method for the even gold nano grain film of this large-area preparation; Be to adopt the solution that contains gold nano grain to prepare starting material as nanometer particle film; This liquid preparation process comprises multiple preparation method, and the nano particle of various preparing method's preparations has the variety of size, pattern.Therefore adopt this method for preparing the even gold nano grain film of big area, the size of nanometer gold grain that is deposited, pattern will can not suffer restraints yet, and can prepare the gold nano grain film of different-shape requirement.
2, the method for the even gold nano grain film of this large-area preparation is regulated the sedimentation velocity and the final settled density of nano particle in the gold nano grain film through factors such as the concentration of control GOLD FROM PLATING SOLUTION nano particle, the amount of adding chemical substance, depositing times.Therefore can prepare the gold nano grain film of different settled density requirements through these factors easily.
3, adopt the even gold nano grain film process of this large-area preparation to have the variation of preparation process; Be applicable to all kinds of gold nano grains of deposition, have nano particle simultaneously and be evenly distributed, do not produce characteristics such as accumulation, nano particle spacing are controlled, gold nano grain adhere firmly.In addition, but the film preparation process is simple, the short large-area preparation of preparation time, and attenuating film preparation cost can obtain considerable economic.
Description of drawings
Fig. 1 is a preparation gold nano grain film schematic flow sheet;
Fig. 2 is a deposition back gold nano grain thin film planar microcosmic synoptic diagram.
Sign as follows among the figure: gold nano grain 1; The solution 2 that contains gold nano grain; Solution 3 behind interpolation Vinylpyrrolidone polymer and the xitix; Substrate material 4; Gold nano grain film 5.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.
The invention provides the method for the even gold nano grain film of a kind of large-area preparation, this method comprises the steps:
Step 1: preparation contains the nano-solution 2 of gold nano grain 1;
Step 2: configuration contains the solution 3 of Vinylpyrrolidone polymer and xitix;
Step 3: insert substrate material 4 and carry out the self-assembly deposition, deposition will independently be adorned one deck gold nano grain film 5 after accomplishing on substrate material.
In the step 1: adopt any method in seed mediated growth method, xitix reduction method, Trisodium Citrate method, Peng Qinghuana method, electrochemical process, photoreduction method, the sonochemistry synthesis method to prepare the nano-solution 2 that contains gold nano grain 1; The gold nano grain that nano particle in the nano-solution 2 is prepared various different shapeies and size according to the concentration and the preparation condition of reactant materials in each class methods.
In the step 2; The method that configuration contains the solution 3 of Vinylpyrrolidone polymer and xitix is: in the nano-solution that contains gold nano grain 12, add Vinylpyrrolidone polymer and these two kinds of chemical substances of xitix; The PVP K120 concentration of adding is 0.01 mole and whenever is raised to 0.5 mole every liter that the concentration of the xitix of interpolation is 0.005 mole and whenever is raised to 0.6 mole every liter; Through adding PVP K120 and xitix, nano particle will be realized the modification of surface energy, facilitate nano grain surface can with the coupling of deposition substrate.
In the step 3; When the insertion substrate material carries out the self-assembly deposition; Use in the solution 3 after clean substrate material 4 vertically is inserted into interpolation PVP K120 and xitix; The self-assembly behavior will take place in gold nano grain this moment, spontaneously be deposited on the surface of substrate material 4, realize the preparation of even gold nano grain film.
Gold nano grain 1 is the nanostructure of nanometer ball or nanometer rod or nanometer dish or nanometer square or nano flower-like, and size is that 1 nanometer is to 200 nanometers.
Technical scheme of the present invention mainly comprises three steps: 1, adopt the chemical process preparation to contain the solution of gold nano grain, and 2, configuration contains the solution of Vinylpyrrolidone polymer and xitix, 3, insert substrate material and carry out the self-assembly deposition.The concrete realization as follows:
Step 1: adopt the chemical process preparation to contain the solution of gold nano grain
At first adopt a kind of method in the different chemical methods such as seed mediated growth method, xitix reduction method, Trisodium Citrate method, Peng Qinghuana method, electrochemical process, photoreduction method, sonochemistry synthesis method to prepare the solution that contains gold nano grain.The gold nano grain that nano particle in the solution can be prepared various different shapeies and size according to the concentration and the preparation condition of reactant materials in each class methods.The gold nano grain microscopic appearance that this mode prepares has variety, and shape mainly contains other multiple patterns such as sphere, trilateral, cubes, bar-shaped, hexagon.Size of nanometer gold grain can be several nanometers between hundreds of nanometers.And the nano material of different-shape and size, character such as the electricity on its performance mountain, optics, catalysis are different.Therefore, for the requirement of different gold nano grain photoelectric characteristics, can realize through the gold nano grain that the control chemical reaction condition prepares different-shape and size.
Step 2: configuration contains the solution of Vinylpyrrolidone polymer and xitix
Adopt the solution that the chemical process configuration contains gold nano grain to can be the starting material that the gold nano grain film provides gold nano grain, deposition is to obtain the gold nano grain film in this solution but directly be inserted into substrate material.Add Vinylpyrrolidone polymer and these two kinds of chemistry of xitix in the solution that contains gold nano grain that core of the present invention is in step 1, to prepare; The PVP K120 concentration of adding can be 0.01 mole and whenever is raised to 0.5 mole every liter and does not wait, and the concentration of xitix is 0.005 mole and whenever is raised to 0.6 mole every liter and does not wait.Through adding chemical substance PVP K120 and xitix material, nano particle will be realized the modification of surface energy, facilitate nano grain surface can with the coupling of deposition substrate.
Step 3: insert substrate material and carry out the self-assembly deposition
Use in the solution after clean substrate material such as polished silicon slice, metal, glass, quartz plate, transparent conducting glass matrix material etc. vertically are inserted into interpolation PVP K120 and xitix; The self-assembly behavior will take place in gold nano grain this moment; Spontaneously be deposited on the surface of substrate, realize the preparation of the even gold nano grain film of big area.The region area of deposited gold nano particle is by the chip area decision of immersing in the solution.
Embodiment 1: adopt seed mediated growth method to prepare gold nano grain
Be that to add 0.3 ml concn in 0.1 mole every liter the cetyl trimethylammonium bromide be 0.01 mole every liter golden solution chlorate at 8 ml concns at first, the sodium borohydride solution that adds 0.5 ml concn again and be 0.01 mole every liter forms gold seeds solution.More than the configuration solvent all is a deionized water.In beaker, adding 40 ml deionized water, 6 ml concns then successively is that 0.1 mole of every liter of cetyl trimethylammonium bromide, 1.5 ml concns are that 0.01 mole every liter golden chloric acid, the xitix that 3 ml concns are 0.01 mole every liter form growth solution; Get 10 microlitres to gold seeds solution again and splash in the above-mentioned growth solution and stirring, growth obtains gold nano grain 1 and solution 2.
Embodiment 2: add Vinylpyrrolidone polymer and xitix
Interpolation Vinylpyrrolidone polymer and xitix obtain solution 3 in the solution in embodiment 1, and these two kinds of substance purity are more than the analytical pure.Adding Vinylpyrrolidone polymer concentration is 0.1 mole about every liter, and the concentration of xitix is 0.05 mole about every liter, after interpolation finishes, utilizes ultrasonic cleaning agent, and sonic oscillation dissolved it in 5 minutes fully.
Embodiment 3: insert substrate material and carry out the self-assembly deposition
This method advantage is to regulate according to the concentration of GOLD FROM PLATING SOLUTION nano particle, PVP K120, xitix the sedimentation rate of gold nano grain.The gold nano grain film of preparing by this method possesses nano particle and is evenly distributed, does not produce characteristics such as accumulation, nano particle spacing are controlled, gold nano grain adhere firmly, can strengthen at surface-enhanced raman scattering, field such as photovoltaic synergy, photodiode has a wide range of applications.
The above is merely preferred embodiments of the present invention; Protection scope of the present invention is not exceeded with above-mentioned embodiment; As long as the equivalence that those of ordinary skills do according to disclosed content is modified or changed, all should include in the protection domain of putting down in writing in claims.
Claims (6)
1. a method for preparing even gold nano grain film is characterized in that, this method comprises the steps:
Step 1: preparation contains the nano-solution (2) of gold nano grain (1);
Step 2: configuration contains the solution (3) of Vinylpyrrolidone polymer and xitix;
Step 3: insert substrate material (4) and carry out the self-assembly deposition, deposition will independently be adorned one deck gold nano grain film (5) after accomplishing on substrate material.
2. the method for the even gold nano grain film of preparation according to claim 1 is characterized in that, in the step 1:
Adopt any method in seed mediated growth method, xitix reduction method, Trisodium Citrate method, Peng Qinghuana method, electrochemical process, photoreduction method, the sonochemistry synthesis method to prepare the nano-solution (2) that contains gold nano grain (1);
The gold nano grain that nano particle in the nano-solution (2) is prepared various different shapeies and size according to the concentration and the preparation condition of reactant materials in each class methods.
3. the method for the even gold nano grain film of preparation according to claim 1 is characterized in that, in the step 2, the method that configuration contains the solution (3) of Vinylpyrrolidone polymer and xitix is:
In the nano-solution that contains gold nano grain (1) (2), add Vinylpyrrolidone polymer and these two kinds of chemical substances of xitix; The PVP K120 concentration of adding is 0.01 mole and whenever is raised to 0.5 mole every liter that the concentration of the xitix of interpolation is 0.005 mole and whenever is raised to 0.6 mole every liter; Through adding PVP K120 and xitix, nano particle will be realized the modification of surface energy, facilitate nano grain surface can with the coupling of deposition substrate.
4. according to the method for claim 1 or the even gold nano grain film of 3 described preparations, it is characterized in that, in the step 3, when the insertion substrate material carries out the self-assembly deposition,
Use in the solution (3) after clean substrate material (4) vertically is inserted into interpolation PVP K120 and xitix; The self-assembly behavior will take place in gold nano grain this moment; Spontaneously be deposited on the surface of substrate material (4), realize the preparation of even gold nano grain film.
5. the method for the even gold nano grain film of preparation according to claim 1 is characterized in that, gold nano grain (1) is the nanostructure of nanometer ball or nanometer rod or nanometer dish or nanometer square or nano flower-like, and size is that 1 nanometer is to 200 nanometers.
6. the method for the even gold nano grain film of preparation according to claim 4 is characterized in that, substrate material (4) is any in polished silicon slice, metal, glass, quartz plate, the transparent conducting glass matrix material.
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