CN111690917A - Method for preparing material surface metal nano array by stable block copolymer micelle template method - Google Patents
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- CN111690917A CN111690917A CN202010457170.8A CN202010457170A CN111690917A CN 111690917 A CN111690917 A CN 111690917A CN 202010457170 A CN202010457170 A CN 202010457170A CN 111690917 A CN111690917 A CN 111690917A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1658—Process features with two steps starting with metal deposition followed by addition of reducing agent
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Abstract
The invention belongs to the technical field of surface modification of nano materials, and discloses a method for preparing a metal nano array on the surface of a material by a stable block copolymer micelle template method, wherein the method for preparing the metal nano array on the surface of the traditional material comprises the following steps: preparing a micelle solution of the block copolymer; loading a metal precursor in the micelle; forming a micelle array on the surface of the material; the plasma removes the micelle template. However, the metal nano-array on the surface of the material obtained by the above preparation method often has the condition of metal nano-particle agglomeration or metal nano-particle shedding in the long-term storage process, which hinders batch preparation and subsequent experiments. After the metal nano array on the surface of the material is prepared, the material is soaked in a reducing solvent, the metal nano particles and the surface of the material are reduced gently and quickly, and organic matters possibly remained on the surface of the material are dissolved and removed, so that the metal nano array is kept stable on the surface of the material for a long time.
Description
Technical Field
The invention belongs to the technical field of material surface modification, and particularly relates to a method for preparing a material surface metal nano array by a stable block copolymer micelle template method.
Background
The nano patterning of the material surface has important application in the fields of catalysis, optics, electronics, biology and biological materials.
An important method for realizing the nano patterning of the material surface is a block copolymer micelle template method. The method utilizes the solubility difference of different blocks of the block copolymer to form micelles by self-assembly in a specific solvent; loading metal precursors or nanoparticles in the micelle; forming a micelle solution liquid film on the surface of the material by a spin coating or dip coating method; the micelle spontaneously forms a periodic ordered array on the surface of the material along with solvent volatilization; finally, removing the copolymer by using gas plasma, and forming an ordered nano array on the surface of the material. The metal nano array prepared by the method can realize free regulation and control of the size, the interval and the degree of order of the structural units.
However, the metal nano-array prepared on the surface of the material by the above method often has the phenomenon of metal nano-particle agglomeration or metal nano-particle dropping during long-term storage. The instability hinders the batch preparation of the metal nano-array on the surface of the material, is not beneficial to the experimental repeatability and experimental design, and simultaneously increases the economic cost and time cost of scientific research invisibly.
Therefore, the development of a method for rapidly and mildly stabilizing a material surface metal nano-array prepared by a block copolymer micelle template method becomes a problem which needs to be solved by the technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a method for rapidly and gently stabilizing a material surface metal nano-array prepared by a block copolymer micelle template method, aiming at the problems existing in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for stabilizing a material surface metal nano array prepared by a block copolymer micelle template method comprises the following steps:
I. preparing a micelle solution of a segmented copolymer for encapsulating a metal precursor;
II. Preparing a micelle array for encapsulating a metal precursor on the surface of the material;
III, removing a micelle template formed by the segmented copolymer on the surface of the material by using a plasma cleaning instrument;
IV, soaking and reducing the materials by using a reducing solvent.
It is worth to be noted that the metal nano array on the surface of the material refers to patterned elemental metal dots, the diameter of which is nano-scale, and the patterned elemental metal dots are periodically regularly or irregularly arranged on the surface of the material.
Researches find that the instability of the metal nano array is mainly caused by the possibility of oxidation of metal nano particles after high-power plasma treatment, and the stability of the nano metal points in an oxidation state is poor; partly due to the oxidation activation of the material surface itself, or the incomplete removal of the micelle template and the organic residue on the material surface. High power and long plasma treatment process are necessary to ensure that the polymer template is removed; on the other hand, the use of oxygen and nitrogen plasmas is more common than that of hydrogen plasmas for safety reasons, so that the metal nanoarrays on the surface of the material subjected to plasma treatment are inevitably oxidized to affect the long-term stability. Therefore, the material after plasma treatment can be quickly and mildly reduced by adopting the reducing solvent for soaking reduction, and simultaneously, possible residual organic matters are cleaned, so that the aim of stabilizing the metal nano array on the surface of the material is fulfilled.
It is worth to say that the invention adds the reduction treatment step after the plasma treatment, and besides improving the success rate of self-assembly patterning and the stability of nano metal point preservation and post-treatment, the surface property of the substrate material with the metal nano array pattern after the reduction treatment is consistent with the surface property of the material treated by the traditional block copolymer micelle template method, and the subsequent processing can be directly carried out without other process steps.
Further, the metal precursor in step I is chloroauric acid, iridium chloroplatinate, chlororhodic acid, chloropalladic acid, chloroiridic acid or osmium chloroosmic acid.
Furthermore, the block copolymer in the step I is polystyrene-block-polyvinylpyridine PS-b-P2VP, the molecular weight of the PS-b-P2VP is 19500-290000 g/mol, and the molecular weight dispersion index is less than 1.5; the solvent of the micelle solution of the block copolymer is one of anhydrous toluene and anhydrous o-xylene, and the concentration of the micelle solution of the block copolymer is greater than the corresponding critical micelle concentration.
Further, the molar ratio of the metal precursor to the polyvinylpyridine P2VP in the step I is 0.5: 1.
Further, the material in step II includes one of quartz glass, common glass, silicon, and metal.
Furthermore, the preparation method of the material surface micelle array in the step II is an immersion pulling method.
Further, the gas used for plasma cleaning in step III is one or more of oxygen and nitrogen.
Further, the reducing solvent in step IV includes one or more of borohydride, sodium citrate, potassium tartrate, amine compound, ascorbic acid, and absolute ethyl alcohol.
In some embodiments, the metal precursor in step I is chloroauric acid and the reducing solvent in step IV is absolute ethanol.
In some embodiments, the method for stabilizing the metal nano array on the surface of the material prepared by the block copolymer micelle template method comprises the following steps:
I. preparing a micellar solution of polystyrene-block-polyvinyl pyridine PS-b-P2VP carrying chloroauric acid;
II. Preparing a polystyrene-block-polyvinylpyridine PS-b-P2VP array coated with chloroauric acid on the surface of the material by adopting a dip-coating method;
III, removing a micelle template formed by the polystyrene-block-polyvinyl pyridine PS-b-P2VP on the surface of the material by using a plasma cleaning instrument;
IV, soaking the materials in absolute ethyl alcohol to reduce the materials
Compared with the prior art, the invention has the advantages that:
1. the invention utilizes the block copolymer micelle self-assembly technology to carry out patterning modification on the surface of the material, is a metal nano-array patterning modification technology which is relatively simple and easy to implement and relatively low in cost, can prepare a nano-scale metal dot array, and has controllable space among metal nano-dots;
2. the method reduces the metal nano array oxidized by the plasma and the surface of the material by using the solution with the reduction property, can dissolve and remove possible residual organic matters, does not influence the appearance of the metal nano array, and solves the problem that the metal nano array on the surface of the material is unstable in the long-term storage process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an image of P3808-200 characterized by a field emission scanning electron microscope in example 1.
FIG. 2 is an image of P3808-300 characterized by a field emission scanning electron microscope in example 2.
FIG. 3 is an image of P5052-300 of example 3 as characterized by a field emission scanning electron microscope.
Fig. 4 is an image of P5052 of comparative example 1 characterized by field emission scanning electron microscopy.
FIG. 5 is a schematic view of the preparation process of examples 1 to 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
Example 1
A method for preparing a material surface metal nano array by a stable block copolymer micelle template method comprises the steps of weighing 2.92mg of polystyrene-block-polyvinyl pyridine (P3808-S2VP) in a 25ml brown reagent bottle, weighing 10ml of o-xylene, and stirring for 24 hours in a dry environment until a solution is clear and transparent. 14.7mg of chloroauric acid trihydrate (HAuCl) was added43H2O) and stirring for 24H in a dry environment protected from light until the solution is clear and transparent. The block copolymer micelle solution carrying chloroauric acid was allowed to stand for 1 hour. The slide was immersed in the micelle solution for 5 seconds and then pulled up at a constant rate of 200 μm/s. And (3) drying and standing the dipped and pulled material for 24 hours in a dark place, and putting the material into an oxygen plasma cleaning instrument after the solvent is completely volatilized. Setting the parameters of the plasma cleaning instrument to be 8Pa in vacuum degree and 120W in power, and processing 3600s to obtain the gold nano array on the surface of the glass. The material is soaked in absolute ethyl alcohol for 1h after being cooled, and is dried by high-purity nitrogen gas, and the mark is P3808-200.
The obtained glass surface gold nano dot array is characterized by a field emission scanning electron microscope (FE-SEM), a secondary electron (SE2) detector, a 30-micron objective lens diaphragm (alert), a working distance of 4.2mm and an acceleration voltage (EHT) of 3.00kV are used.
Example 2
A method for preparing a material surface metal nano array by a stable block copolymer micelle template method comprises the steps of weighing 3.02mg of polystyrene-block-polyvinyl pyridine (P3808-S2VP) in a 25ml brown reagent bottle, weighing 10ml of o-xylene, and stirring for 24 hours in a dry environment until a solution is clear and transparent. 11.5mg chloroauric acid trihydrate (HAuCl) was added43H2O) and stirring for 24H in a dry environment protected from light until the solution is clear and transparent. The block copolymer micelle solution carrying chloroauric acid was allowed to stand for 1 hour. Immersing quartz plate into micelleThe solution, immersed for 5s, was then pulled up at a constant rate of 300 μm/s. And (3) drying and standing the dipped and pulled material for 24 hours in a dark place, and putting the material into an oxygen plasma cleaning instrument after the solvent is completely volatilized. Setting parameters of the plasma cleaning instrument to be 8Pa in vacuum degree and 150W in power, and processing 3600s to obtain the gold nano array on the surface of the quartz. After cooling, the material is soaked in absolute ethyl alcohol for 1h, and is dried by high-purity nitrogen, and the mark is P3808-300.
The quartz surface gold nano dot array obtained above is characterized by using a field emission scanning electron microscope (FE-SEM), and a secondary electron (SE2) detector, a 30mm objective lens diaphragm (alert), a working distance of 4.2mm and an acceleration voltage (EHT) of 2.00kV are used.
Example 3
A method for preparing a material surface metal nano array by a stable block copolymer micelle template method comprises the steps of weighing 3.01mg of polystyrene-block-polyvinyl pyridine (P5052-S2VP) in a 25ml brown reagent bottle, weighing 10ml of o-xylene, and stirring for 24 hours under a dry environment until a solution is clear and transparent. 8.2mg chloroauric acid trihydrate (HAuCl) was added43H2O) and stirring for 24H in a dry environment protected from light until the solution is clear and transparent. The block copolymer micelle solution carrying chloroauric acid was allowed to stand for 1 hour. The quartz plate was immersed in the micellar solution and after 5s of immersion, pulled up at a constant rate of 300 μm/s. And (3) drying and standing the dipped and pulled material for 24 hours in a dark place, and putting the material into an oxygen plasma cleaning instrument after the solvent is completely volatilized. Setting the parameters of the plasma cleaning instrument to be 8Pa in vacuum degree and 150W in power, and processing 3600s to obtain the gold nano array on the surface of the glass. After cooling, the materials are soaked in absolute ethyl alcohol for 1h, and are dried by high-purity nitrogen, and the mark is P5052-300.
The quartz surface gold nano dot array obtained above is characterized by using a field emission scanning electron microscope (FE-SEM), and a secondary electron (SE2) detector, a 30mm objective lens diaphragm (alert), a working distance of 4.2mm and an acceleration voltage (EHT) of 2.00kV are used.
The basic physical properties of the polystyrene-block-polyvinylpyridine (PS-b-P2VP) used in examples 1-3 are shown in Table 1:
TABLE 1
The basic properties of the gold nanoarrays on the surface of the materials prepared in examples 1-3 are shown in Table 2:
TABLE 2
| Sample name | Base material | Amount of gold carried | Nano dot spacing |
| P3808-200 | Glass | 0.67 | 171±7nm |
| P3808-300 | Quartz crystal | 0.51 | 114±7nm |
| P5052-300 | Quartz crystal | 0.49 | 125±1nm |
In order to further prove the beneficial effects of the present invention and to better understand the present invention, the following comparative examples further illustrate the properties and application properties of the method for preparing metal nano-arrays on the surface of materials by the micelle template method of the block copolymer, which is not to be construed as a limitation of the present invention, and the properties of the products obtained by other determination experiments performed by those skilled in the art according to the above summary of the invention and the applications performed according to the above properties are also considered to fall within the protection scope of the present invention.
Comparative example 1
3.00mg of polystyrene-block-polyvinylpyridine (P5052-S2VP) is weighed into a 25ml brown reagent bottle, 10ml of o-xylene is weighed out, and the solution is stirred for 24h under a dry environment until the solution is clear and transparent. 8.0mg chloroauric acid trihydrate (HAuCl) was added43H2O) and stirring for 24H in a dry environment protected from light until the solution is clear and transparent. The block copolymer micelle solution carrying chloroauric acid was allowed to stand for 1 hour. The quartz plate was immersed in the micellar solution and after 5s of immersion, pulled up at a constant rate of 300 μm/s. And (3) drying and standing the dipped and pulled material for 24 hours in a dark place, and putting the material into an oxygen plasma cleaning instrument after the solvent is completely volatilized. The parameters of the plasma cleaning instrument are set to be 8Pa in vacuum degree and 150W in power, and the gold nano array on the surface of the glass is obtained after 3600s of treatment without further treatment.
The quartz surface gold nano dot array obtained above is characterized by a field emission scanning electron microscope (FE-SEM), a secondary electron (SE2) detector, a 30mm objective lens diaphragm (alert), a working distance of 4.0mm and an acceleration voltage (EHT) of 2.00 kV.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for stabilizing a material surface metal nano array prepared by a block copolymer micelle template method is characterized by comprising the following steps:
I. preparing a micelle solution of a segmented copolymer for encapsulating a metal precursor;
II. Preparing a micelle array for encapsulating a metal precursor on the surface of the material;
III, removing a micelle template formed by the segmented copolymer on the surface of the material by using a plasma cleaning instrument;
IV, soaking and reducing the materials by using a reducing solvent.
2. The method for stabilizing the metal nanoarray on the surface of the material prepared by the block copolymer micelle template method according to claim 1, wherein the metal precursor in the step I is chloroauric acid, iridium chloroplatinate, chlororhodic acid, chloropalladic acid, chloroiridic acid or chloroosmic acid.
3. The method for stabilizing the material surface metal nano-array prepared by the block copolymer micelle template method according to claim 2, wherein the block copolymer in the step I is polystyrene-block-polyvinylpyridine PS-b-P2VP, the molecular weight of the PS-b-P2VP is 19500-290000 g/mol, and the molecular weight dispersion index is less than 1.5; the solvent of the micelle solution of the block copolymer is one of anhydrous toluene and anhydrous o-xylene, and the micelle solution concentration of the block copolymer is greater than the corresponding critical micelle concentration.
4. The method for stabilizing the metal nano-array on the surface of the material prepared by the block copolymer micelle template method according to the claim 3, wherein the molar ratio of the metal precursor to the monomer unit of the polyvinylpyridine P2VP in the step I is 0.5: 1.
5. The method for stabilizing the metal nano-array on the surface of the material prepared by the block copolymer micelle template method according to claim 1, wherein the material in the step II comprises one of quartz glass, common glass, silicon and metal.
6. The method for stabilizing the material surface metal nano-array prepared by the block copolymer micelle template method according to claim 5, wherein the material surface micelle array preparation method in the step II is a dip-coating method.
7. The method for stabilizing the metal nano-array on the surface of the material prepared by the block copolymer micelle template method according to the claim 1, wherein the gas used for the plasma cleaning in the step III is one or more of oxygen and nitrogen.
8. The method for stabilizing the metal nano-array on the surface of the material prepared by the block copolymer micelle template method according to claim 1, wherein the reducing solvent in the step IV comprises one or more of borohydride, sodium citrate, potassium tartrate, amine compounds, ascorbic acid and absolute ethyl alcohol.
9. The method for stabilizing the metal nano-array on the surface of the material prepared by the block copolymer micelle template method according to claim 1, wherein the metal precursor in the step I is chloroauric acid, and the reducing solvent in the step IV is absolute ethyl alcohol.
10. The method for stabilizing the metal nano array on the surface of the material prepared by the block copolymer micelle template method according to claim 1, which is characterized by comprising the following steps:
I. preparing a micellar solution of polystyrene-block-polyvinyl pyridine PS-b-P2VP carrying chloroauric acid;
II. Preparing a polystyrene-block-polyvinylpyridine PS-b-P2VP array coated with chloroauric acid on the surface of the material by adopting a dip-coating method;
III, removing a micelle template formed by the polystyrene-block-polyvinyl pyridine PS-b-P2VP on the surface of the material by using a plasma cleaning instrument;
IV, soaking the materials in absolute ethyl alcohol to reduce the materials.
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| CN112680403A (en) * | 2021-01-12 | 2021-04-20 | 复旦大学 | Gradient nano material and preparation method and application thereof |
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Application publication date: 20200922 |
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| RJ01 | Rejection of invention patent application after publication |