CN110116217B - Method for constructing two-dimensional gold nanoparticle pattern - Google Patents
Method for constructing two-dimensional gold nanoparticle pattern Download PDFInfo
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- CN110116217B CN110116217B CN201910453422.7A CN201910453422A CN110116217B CN 110116217 B CN110116217 B CN 110116217B CN 201910453422 A CN201910453422 A CN 201910453422A CN 110116217 B CN110116217 B CN 110116217B
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- B22F9/00—Making metallic powder or suspensions thereof
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Abstract
The invention discloses a method for constructing a two-dimensional gold nanoparticle pattern, which comprises the following steps of using polyoxyethylene-bPreparing diversified crystallization templates by a film self-nucleation method by taking a poly-2-vinylpyridine block copolymer as a means, then immersing the crystallization templates in a chloroauric acid solution with a certain concentration for carrying gold ions, and then cleaning a sample by using a plasma cleaning machine to obtain a two-dimensional gold nanoparticle pattern; the method for self-nucleation is simple and easy to implement, the processing conditions are not harsh, the method has guiding significance for the preparation and research of the two-dimensional metal nano conductive structure, and a new thought is provided for the application of the polymer film in the fields of nano materials and the like.
Description
The technical field is as follows:
the invention relates to the field of high polymer materials, in particular to a method for constructing a two-dimensional gold nanoparticle pattern.
Background art:
nowadays, more and more crystalline polymer films are used in various industries such as optical and electrical communication. In the polymer film system, the crystal morphology structure of the film is greatly different from the bulk due to the influence of space limitation and interface effect. By researching the crystallization behavior of the crystallized polymer film, the effective regulation and control of the crystal morphological structure of the polymer film can be realized.
Polyethylene oxide-bPoly 2-vinylpyridine, which is a diblock copolymer with stronger crystallization ability formed by combining a crystallizable PEO segment and an amorphous P2VP segment through chemical bonds, having the name of Poly (ethylene oxide) -blockPoly (2-vinyl pyridine), abbreviated PEO-b-P2 VP. It not only has a certain crystallization ability, but also the amorphous P2VP segment can generate complex reaction with a plurality of metal ions such as Au, Ag, Pt, Ni, Cu and the like to generate a metal complex with stable chemical property, so PEO-bP2VP is mostly applied in zero-dimensional, one-dimensionalThe preparation of metal nano conductive materials, and the research on two-dimensional metal nano conductive structures is not yet common. Therefore, the method for preparing the two-dimensional metal nano conductive structure has important theoretical significance and application value.
The self-nucleation (self-nucleation) method for preparing crystals utilizes the memory effect of macromolecules, small crystal grains are left after the macromolecule lamella is partially melted, and the small crystal grains can be used as crystal nuclei when the temperature is reduced, so that the crystallization can be carried out. In PEO-bIn the P2VP film, a two-dimensional crystallization template with a certain shape, size and distribution can be prepared by a self-nucleation method, which is greatly different from a zero-dimensional structure formed in a solution and a one-dimensional structure formed by phase separation in the film. Although the self-nucleation method is a simple and easy method, most of documents focus on the research of the self-nucleation behavior of the high molecular material, and the construction of the two-dimensional gold nanoparticle pattern by the high molecular self-nucleation method is not reported.
The invention content is as follows:
the technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides a polyoxyethylene-containing material which is simple and easy to operate and has excellent crystallization performancebPoly-2-vinylpyridine (PEO-b-P2 VP) block copolymer as a means, preparing diversified crystallization templates by a thin film self-nucleation method, immersing the crystallization templates in a chloroauric acid solution with a certain concentration for carrying gold ions, and then cleaning a sample by a plasma cleaning machine to obtain a two-dimensional gold nanoparticle pattern.
The technical scheme of the invention is as follows: a method for constructing a two-dimensional gold nanoparticle pattern by using polyethylene oxide with excellent crystallization performancebPoly-2-vinylpyridine (PEO-b-P2 VP) block copolymer as a means, preparing a diversified crystallization template by a thin film self-nucleation method, then immersing the crystallization template in a chloroauric acid solution with a certain concentration for carrying gold ions, and then cleaning with a plasma cleaning machine to obtain a two-dimensional gold nanoparticle pattern, wherein the method comprises the following specific steps: step 1) toCarrying out surface treatment on the silicon wafer;
step 2) weighing a certain mass of PEO-b-P2VP raw material, using toluene as solvent to prepare solution with certain concentration;
step 3) placing the solution on a heating table, heating for several hours at a certain temperature until the solute is fully dissolved;
step 4) preparing a film by taking the processed silicon wafer as a substrate and utilizing a spin coating instrument and a spin coating method;
step 5) placing the prepared PEO film on a Linkam hot table, and obtaining PEO-ion by adopting a self-nucleation method under the protection of nitrogen atmosphereb-P2VP thin film crystallization template;
step 6) completely washing out disordered molecular chains in the film sample and thin platelets formed in the quenching process by using a cold toluene solution through a spin coating method;
step 7) immersing the completely washed sample in a chloroauric acid solution with a certain concentration for several hours;
and 8) cleaning the loaded sample by using a plasma cleaning machine.
Further, in the step 1), the surface treatment of the silicon wafer is carried out for 1 hour by using ultraviolet ozone.
Further, in the step 2), PEO-bP2VP, the number-average molecular weight of which is 4000-2000g/mol, the mass fraction of the solution being 0.5%.
Further, in the step 3), the prepared solution is placed in a 70 ℃ hot stage to be heated for 1 hour to fully dissolve the solute.
Further, in the step 4), the thin film is prepared in a spin coater by rotating at 4000 rpm for 30 s.
Further, in the step 5), the temperature of the sample is increased from room temperature to 75 ℃ at a temperature increase rate of 30 ℃/min, the sample is kept at 75 ℃ for 10 min to eliminate thermal history, then the temperature is decreased to 35 ℃ at a rate of 20 ℃/min to perform isothermal crystallization for 10 min, then the temperature is increased to a partial melting temperature of 47 ℃ to 48 ℃ at a temperature increase rate of 1 ℃ to 20 ℃/min, and the temperature is decreased to 43 ℃ for growth for 4 min after the temperature is kept for 10 min.
Further, in the step 6), the prepared film sample with the crystallization template is completely washed away by a Spin-coating method by using a cold toluene solvent at 8 ℃ to remove disordered molecular chains in the film and thin platelets formed in the quenching process.
Further, in the step 7), the completely washed sample is immersed in a 1.0% chloroauric acid/n-octanol solution and is kept away from light for 16 h to ensure the sufficient loading of gold ions.
Further, in the step 8), the loaded sample is cleaned by a plasma cleaning machine, wherein the gas is air, the flow rate is 20 sccm, the power is 100 w, and the time is 20 min.
The invention has the beneficial effects that: the invention provides a simple and feasible method for constructing a two-dimensional gold nanoparticle pattern, which not only has guiding significance for the preparation and research of a two-dimensional metal nano conductive structure, but also provides a new thought for the application of a polymer film in the fields of nano materials and the like.
Description of the drawings:
FIG. 1 is a representation of a first two-dimensional pattern of gold nanoparticles with varying reaction conditions.
FIG. 2 is a representation of a second two-dimensional pattern of gold nanoparticles with varying reaction conditions.
FIG. 3 is a representation of a third two-dimensional gold nanoparticle pattern with varying reaction conditions.
The specific implementation mode is as follows:
example (b): see fig. 1, 2 and 3.
The method for constructing two-dimensional gold nanoparticle pattern uses polyethylene oxide with excellent crystallization performancebPoly-2-vinylpyridine (PEO-b-P2 VP) block copolymer as a means, preparing a diversified crystallization template by a thin film self-nucleation method, then immersing the crystallization template in a chloroauric acid solution with a certain concentration for carrying gold ions, and then cleaning with a plasma cleaning machine to obtain a two-dimensional gold nanoparticle pattern.
The specific operation steps of the present application are described in detail below according to specific examples.
The first embodiment is as follows: see FIG. 1
Step 1) treating the surface of a silicon wafer with ultraviolet ozone for 1h (the silicon wafer is a P100 type silicon wafer purchased from Zhejiang Lijing optical-electronic technology Co., Ltd.).
Step 2) weighing a certain mass of PEO-b-P2VP raw material, using toluene as solvent to prepare solution with certain concentration; PEO-bP2VP having a number-average molecular weight (4000-2000) g/mol (from Polymer Source, Canada), the mass fraction of the solution being 0.5%;
step 3) placing the solution on a 70 ℃ hot bench to heat for 1h until the solute is fully dissolved;
step 4) taking the processed silicon wafer as a substrate, and rotating the substrate in a spin coater at the speed of 4000 rpm for 30 s to prepare a film (the spin coater is KW-4A type produced by micro-electronic research institute of Chinese academy of sciences);
step 5) placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate thermal history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (47 ℃) at a certain heating rate (1 ℃/min), preserving heat for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template;
step 6) completely washing out disordered molecular chains in the prepared film sample with the crystallization template and thin platelets formed in the quenching process by using a 8-DEG C cold toluene solution through a spin coating method;
step 7) immersing the completely washed sample in a 1.0% chloroauric acid/n-octanol solution for 16 h in the dark to ensure the sufficient carrying of gold ions;
and 8) cleaning the loaded sample by using a plasma cleaner (the gas is air, the flow rate is 20 sccm, the power is 100 w, and the time is 20 min), wherein the used plasma cleaner is a small-sized plasma cleaner produced by Zhengzhou Ke Probe instruments and Equipment Limited.
Example two:
the second embodiment is carried out on the basis of the first embodiment 1,the operation procedure is substantially the same as that of the first embodiment, and the difference is only the change of the partial heat treatment conditions, and the difference is that: placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate heat history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (48 ℃) at a certain heating rate (1 ℃) for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template.
Example three:
example three was carried out on the basis of example 1, which was substantially the same as the procedure of example one except for the change in the partial heat treatment conditions, except that: placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate heat history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (47 ℃) at a certain heating rate (5 ℃) for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template.
The remaining steps are the same as those in the first embodiment, and are not described herein.
Example four: see FIG. 2
The fourth example was carried out on the basis of example 1, which was substantially the same as the first example except for the change in the partial heat treatment conditions, except that: placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate heat history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (47.5 ℃) at a certain heating rate (5 ℃) for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template。
The remaining steps are the same as those in the first embodiment, and are not described herein.
Example five:
example five was carried out on the basis of example 1, which was substantially the same as the procedure of example one except for the change in the partial heat treatment conditions, except that: placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate heat history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (48 ℃) at a certain heating rate (5 ℃) for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template.
The remaining steps are the same as those in the first embodiment, and are not described herein.
Example six:
the sixth embodiment is based on the embodiment 1, and basically has the same operation steps as the first embodiment, and is different only in the change of the partial heat treatment conditions, and the difference is that: placing the prepared PEO film on a Linkam hot table, heating the sample from room temperature to 75 ℃ (higher than the nominal melting point) at a heating rate of 30 ℃/min under the protection of nitrogen atmosphere, preserving heat at 75 ℃ for 10 min to eliminate heat history, cooling to 35 ℃ at a rate of 20 ℃/min for isothermal crystallization for 10 min, then increasing to a partial melting temperature (47 ℃) at a certain heating rate (20 ℃/min), preserving heat for 10 min, and then reducing to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template.
The remaining steps are the same as those in the first embodiment, and are not described herein.
Example seven: see FIG. 3
Example seven was conducted on the basis of example 1, which was substantially the same as the procedure of example one except for the change in the partial heat treatment conditions, except that: placing the prepared PEO film on a Linkam hot table, and heating the sample at a temperature rise rate of 30 ℃ per min under the protection of nitrogen atmosphereRaising the temperature from room temperature to 75 ℃ (higher than the nominal melting point), preserving heat at 75 ℃ for 10 min to eliminate thermal history, then lowering the temperature to 35 ℃ at the rate of 20 ℃/min for isothermal crystallization for 10 min, then raising the temperature to partial melting temperature (48 ℃) at a certain raising rate (20 ℃/min), preserving heat for 10 min, and then lowering the temperature to 43 ℃ for growth for 4 min; obtain PEO-b-P2VP thin film crystallization template.
The remaining steps are the same as those in the first embodiment, and are not described herein.
In the above embodiments, the characterization of the two-dimensional gold nanopatterns was achieved by atomic force microscopy.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent variations and modifications made to the above embodiment according to the technical spirit of the present invention still fall within the scope of the technical solution of the present invention.
Claims (9)
1. A method for constructing a two-dimensional gold nanoparticle pattern by using polyethylene oxide with excellent crystallization performancebPoly-2-vinylpyridine (PEO-b-P2 VP) block copolymer as a means, preparing a diversified crystallization template by a thin film self-nucleation method, then immersing the crystallization template in a chloroauric acid solution with a certain concentration for carrying gold ions, and then cleaning with a plasma cleaning machine to obtain a two-dimensional gold nanoparticle pattern, wherein the method comprises the following specific steps: step 1) carrying out surface treatment on a silicon wafer;
step 2) weighing a certain mass of PEO-b-P2VP raw material, using toluene as solvent to prepare solution with certain concentration;
step 3) placing the solution on a heating table, heating for several hours at a certain temperature until the solute is fully dissolved;
step 4) preparing a film by taking the processed silicon wafer as a substrate and utilizing a spin coater and a spin coating method;
step 5) placing the prepared PEO film on a Linkam hot table, and obtaining PEO-ion by adopting a self-nucleation method under the protection of nitrogen atmosphereb-P2VP thin film crystallization template;
step 6) completely washing out disordered molecular chains in the film sample and thin platelets formed in the quenching process by using a cold toluene solution through a spin coating method;
step 7) immersing the completely washed sample in a chloroauric acid solution with a certain concentration for several hours;
and 8) cleaning the loaded sample by using a plasma cleaning machine.
2. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 1), the surface treatment of the silicon wafer is ultraviolet ozone treatment for 1 hour.
3. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: PEO-bP2VP, the number-average molecular weight of which is 4000-2000g/mol, the mass fraction of the solution being 0.5%.
4. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 3), the prepared solution is placed in a 70 ℃ hot stage to be heated for 1 hour to fully dissolve the solute.
5. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 4), the film was prepared by spinning in a spin coater at 4000 rpm for 30 seconds.
6. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 5), the temperature of the sample is increased from room temperature to 75 ℃ at the temperature increase rate of 30 ℃/min, the temperature is maintained at 75 ℃ for 10 min to eliminate thermal history, then the temperature is decreased to 35 ℃ at the speed of 20 ℃/min to perform isothermal crystallization for 10 min, then the temperature is increased to the partial melting temperature of 47 ℃ to 48 ℃ at the temperature increase rate of 1 ℃ to 20 ℃/min, and the temperature is decreased to 43 ℃ after the temperature is maintained for 10 min to grow for 4 min.
7. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 6), the prepared film sample with the crystallization template is completely washed away by using a 8 ℃ cold toluene solvent and a spin coating method for disordered molecular chains in the film and thin platelets formed in the quenching process.
8. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: in the step 7), the completely washed sample is immersed in a 1.0% chloroauric acid/n-octanol solution and is protected from light for 16 h to ensure the sufficient loading of gold ions.
9. The method of constructing a two-dimensional pattern of gold nanoparticles of claim 1, wherein: and in the step 8), cleaning the carried sample by using a plasma cleaning machine, wherein the gas is air, the flow rate is 20 sccm, the power is 100 w, and the time is 20 min.
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