CN109609935A - A method of preparing high density single dispersion metal nano particle on the surface of the material - Google Patents
A method of preparing high density single dispersion metal nano particle on the surface of the material Download PDFInfo
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- CN109609935A CN109609935A CN201910025430.1A CN201910025430A CN109609935A CN 109609935 A CN109609935 A CN 109609935A CN 201910025430 A CN201910025430 A CN 201910025430A CN 109609935 A CN109609935 A CN 109609935A
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- high density
- nano particle
- metal nano
- single dispersion
- density single
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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
- C23C18/166—Process features with two steps starting with addition of reducing agent followed by metal deposition
-
- 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
-
- 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
- C23C18/1603—Process or apparatus coating on selected surface areas
- C23C18/1605—Process or apparatus coating on selected surface areas by masking
-
- 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
- C23C18/1664—Process features with additional means during the plating process
- C23C18/1667—Radiant energy, e.g. laser
-
- 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
Abstract
The invention discloses the methods that one kind prepares high density single dispersion metal nano particle on the surface of the material, it is characterized by: method includes the following steps: 1) upper on the surface of the material prepare poly-dopamine coating: material is dipped into Dopamine hydrochloride solution, it stands or is taken out after stirring a period of time, by material clean and drying, the substrate (a) with poly-dopamine coating is obtained;2) it prepares high density single dispersion metal nano particle: the substrate (a) with poly-dopamine coating is soaked in metal salt solution (b), illumination is taken out from metal salt solution (b) after a certain period of time, after material clean and drying, high density single dispersion metal nano particle is obtained on the surface of the material.This method can rapidly, space-time controllably realize arbitrary surfaces metallize, metalized surface obtained contains highdensity, the good metal nanoparticle of monodispersity, can be widely applied to the fields such as nanocomposite optical, biochemical catalyst, medical diagnosis and therapy.
Description
Technical field
The present invention relates to the methods that one kind prepares high density single dispersion metal nano particle on the surface of the material, belong to materialized
Field.
Background technique
Exactly because the continuous development of functional material meets the development of the every field such as biology, chemistry, physics, medicine
It is required that.Wherein metal nanoparticle is widely used in each research and application field because of its unique physicochemical properties.Example
Such as, metal nanoparticle has unique phasmon effect, can be applied to nanocomposite optical research;Metal nanoparticle has
Small-size effect, reactivity is high, the catalysis reaction being widely used in biochemistry;Metal nanoparticle is imitated with photo-thermal
It answers, can be used for oncotherapy;Metal nanoparticle is electrically conductive after being enriched with to a certain extent, and many researchs have been used
In electronic sensor.However, prepare the conventional method of metal nanoparticle, either physical vapour deposition (PVD) or chemical liquid phase be also
Original all has and maintains metal nanoparticle small size difficult, and metal nanoparticle is poor with substrate adhesion, can not in time, sky
Between upper controllable preparation metal nanoparticle limitation.
Photochemical reaction is referred mainly to by light activated chemical reaction.Photochemical reaction has very high reaction efficiency, can be
Several seconds to completion in several minutes is reacted.In addition, light is a kind of splendid energy source, can make endergonic reaction room temperature, normal pressure with
And occur in mild solvent, this is that other means institute is irrealizable.Also, light has supereminent space-time controllability.
By controlling the irradiation zone and irradiation intensity of illumination, the fixed point generation and extent control of reaction can be accurately realized.
Since light has good penetrability for transparent medium, it is light-operated with untouchable compared to other control means
Feature.Exactly because the photochemically reactive above advantage, is prepared based on photochemically reactive material and modification has been developing progressively
For a subject with bright prospects.
The deficiency of metal nanoparticle is prepared on surface for the prior art, in conjunction with photochemistry unique advantage, the present invention
A kind of method in any material surface preparation high density single dispersion metal nano particle is provided.This method can rapidly, when
Empty expectation wheat flour controllably in office adheres to for high density single dispersion metal nano particle, prepared metal nanoparticle and substrate
Property is good, and monodispersity is good.Also, metal nanoparticle remains to very stably keep its small when suitable high density
Size.
Summary of the invention
Technical problem: the object of the present invention is to provide one kind to prepare high density single dispersion metal nano particle on the surface of the material
Method, this method can rapidly, space-time controllably realize that arbitrary surfaces metallize, metalized surface obtained contains height
Density, the good metal nanoparticle of monodispersity, and metal nanoparticle and substrate adhesion are good, and can be very stable
Ground maintains its small size, can be widely applied to the fields such as nanocomposite optical, biochemical catalyst, medical diagnosis and therapy, great
Scientific research and application value.
Technical solution: the present invention provides the sides that one kind prepares high density single dispersion metal nano particle on the surface of the material
Method, method includes the following steps:
1) upper on the surface of the material to prepare poly-dopamine coating: material is dipped into Dopamine hydrochloride solution, stand or
It is taken out after stirring a period of time, by material clean and drying, obtains the substrate with poly-dopamine coating;
2) it prepares high density single dispersion metal nano particle: it is molten that the substrate with poly-dopamine coating being soaked in metal salt
In liquid, illumination is taken out from metal salt solution after a certain period of time, after substrate is washed and dried, obtains high density on the surface of the material
Single dispersion metal nano particle.
Wherein:
The material be any material with interface, including but not limited to glass, silicon, quartz, plastics, metal, knit
Object or PE.
The concentration of the Dopamine hydrochloride solution is 0.1~10mg/mL;Its configuration method is to dissolve Dopamine hydrochloride
In 10Mm Tris-HCl buffer (pH=8.5).
The standing perhaps stirs take out after a period of time in stand or the time of stirring is 1~72h, stirring
Revolving speed is 500~2000r/min.
In washing and drying described in step 1) and step 2), cleaning way is alternately to be cleaned using ethyl alcohol and pure water, is done
Dry is to dry under room temperature.
Metal salt solution described in step 2) is Ag+Salting liquid or Au3+Salting liquid.
The Ag+Salting liquid in Ag+Concentration is 0.001~1mol/L;The Au3+Salting liquid in Au3+It is dense
Degree is 0.0001~1mol/L.
The Ag+Salting liquid or Au3+Salting liquid in, solvent is aqueous solution, methanol, ethyl alcohol, formic acid or contains
There is the aqueous solution of methanol, ethyl alcohol or formic acid.
During the illumination, the wave-length coverage of light is from ultraviolet light to visible light region, intensity of illumination is 0.1~
1000mW/cm-2, light application time is 10s~120min.
In the During Illumination, light is irradiated by lithography mask version.
By the region of control illumination and the time and intensity of illumination in this method, to control the area of surface metalation
The density and pattern of domain and prepared metal nanoparticle.
The utility model has the advantages that compared with prior art, present invention has the advantage that
1, the method proposed by the present invention for preparing high density single dispersion metal nano particle on the surface of the material has versatility;
For material without selectivity, any materials such as glass, silicon, quartz, plastics, metal, woven fabric etc. can be completed this method
The preparation of high density single dispersion metal nano particle;
2, the method proposed by the present invention for preparing high density single dispersion metal nano particle on the surface of the material can be tens
It completes to prepare high density single dispersion metal nano particle in any material surface in minute or even a few minutes, overcomes other systems
Time-consuming for Preparation Method, step is complicated, by the limitation of large-scale instrument;
3, the method proposed by the present invention for preparing high density single dispersion metal nano particle on the surface of the material has very good
Good space-time controllability;By controlling the region (such as using lithography mask version) of illumination and the time and intensity of illumination, come
Control the region of surface metalation and the density and pattern of prepared metal nanoparticle;
4, gold prepared by the method proposed by the present invention for preparing high density single dispersion metal nano particle on the surface of the material
The monodispersity of metal nano-particle is good, can stablize the small size for maintaining itself in the case where keeping highdensity situation, for being based on
The maintenance of nano material small-size effect is extremely important;
5, gold prepared by the method proposed by the present invention for preparing high density single dispersion metal nano particle on the surface of the material
Metal nano-particle solves material in other preparation methods and needs pre-treatment and metal nano to material substrate good adhesion
The problem of grain is to material substrate poor adhesion.
Detailed description of the invention
Fig. 1 is the signal of the method provided by the invention for preparing high density single dispersion metal nano particle on the surface of the material
Figure;
Fig. 2 is the scanning electron microscope (SEM) photograph of high density monodisperse silver nano-grain prepared by the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of high density monodisperse gold particle prepared by the present invention;
Wherein: a has the substrate of poly-dopamine coating, b metal salt solution, c lithography mask version.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, and the present embodiment is with technical solution of the present invention
Premised under implemented, it should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Embodiment 1
A method of preparing high density single dispersion metal nano particle on the surface of the material, method includes the following steps:
1) slide is dipped into Dopamine hydrochloride solution (2mg/mL, 10mM tris-HCl buffer, pH=8.5), is soaked
After steeping for 24 hours, material is taken out, is alternately cleaned using ethyl alcohol and pure water, and drying at room temperature, has obtained the glass with poly-dopamine coating
Piece a;
2) the slide a with poly-dopamine coating is dipped into the silver nitrate solution b of 0.1mol/L (solvent is water), and
The material being soaked in silver nitrate solution b is irradiated through lithography mask version c using the ultraviolet light that wavelength is 365nm afterwards, irradiation is strong
Degree is 5mW/cm2, irradiation time 30min takes out slide after completing illumination from silver nitrate solution b, uses ethyl alcohol and pure
Water alternately cleans, and drying at room temperature, obtains high density single dispersion metal nano particle, such as Fig. 2 in surface of glass slide.
Embodiment 2
A method of preparing high density single dispersion metal nano particle on the surface of the material, method includes the following steps:
1) silicon wafer is dipped into Dopamine hydrochloride solution (0.1mg/mL, 10mM tris-HCl buffer, pH=8.5),
After stirring 1h (revolving speed 1500r/min), material is taken out, is alternately cleaned, and drying at room temperature, is had using ethyl alcohol and pure water
The silicon wafer a of poly-dopamine coating;
2) the slide a with poly-dopamine coating is dipped into the silver nitrate solution b of 1mol/L to (solvent is 50% second
Alcohol), the material being soaked in silver nitrate solution b then is irradiated through lithography mask version c using the ultraviolet light that wavelength is 365nm,
Exposure intensity is 1000mW/cm2, irradiation time 10s, after completing illumination, material takes out from solution b, uses ethyl alcohol and pure
Water alternately cleans, and drying at room temperature, obtains high density single dispersion metal nano particle in silicon chip surface.
Embodiment 3
A method of preparing high density single dispersion metal nano particle on the surface of the material, method includes the following steps:
1) PE piece is dipped into Dopamine hydrochloride solution (2mg/mL, 10mM tris-HCl buffer, pH=8.5), is soaked
After steeping 72h, material is taken out, is alternately cleaned using ethyl alcohol and pure water, and drying at room temperature, has obtained the PE with poly-dopamine coating
Piece a;
2) the PE piece a with poly-dopamine coating is dipped into the chlorauric acid solution b of 10mmol/L to (solvent is water, is made
PH=7 is adjusted with sodium hydroxide), this then, which is irradiated, through lithography mask version c using the ultraviolet light that wavelength is 365nm is soaked in chlorine gold
Material in acid solution b, exposure intensity 5mW/cm2, irradiation time 10min, after completing illumination, material takes from solution b
Out, it is alternately cleaned using ethyl alcohol and pure water, and drying at room temperature, obtains high density single dispersion metal nano particle on PE piece surface,
Such as Fig. 3.
Embodiment 4
A method of preparing high density single dispersion metal nano particle on the surface of the material, method includes the following steps:
1) fabric is dipped into Dopamine hydrochloride solution (10mg/mL, 10mM tris-HCl buffer, pH=8.5),
After impregnating for 24 hours, material is taken out, is alternately cleaned, and drying at room temperature, has been obtained with poly-dopamine coating using ethyl alcohol and pure water
Fabric a;
2) the fabric a with poly-dopamine coating is dipped into the silver nitrate solution b of 0.1mol/mL (solvent is water).
The material being soaked in silver nitrate solution b then is irradiated through lithography mask version c using the blue light that wavelength is 455nm, irradiation is strong
Degree is 30mW/cm2, irradiation time 120min, after completing illumination, material takes out from solution b, is replaced using ethyl alcohol and pure water
Cleaning, and drying at room temperature, obtain high density single dispersion metal nano particle on PE piece surface.
It should be pointed out that for those skilled in the art, without departing from the principle of the present invention,
Several improvements and modifications can also be made, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (10)
1. the method that one kind prepares high density single dispersion metal nano particle on the surface of the material, it is characterised in that: this method includes
Following steps:
1) upper on the surface of the material to prepare poly-dopamine coating: material being dipped into Dopamine hydrochloride solution, stands or stirs
It is taken out after a period of time, by material clean and drying, obtains the substrate (a) with poly-dopamine coating;
2) it prepares high density single dispersion metal nano particle: it is molten that the substrate (a) with poly-dopamine coating being soaked in metal salt
In liquid (b), illumination is taken out from metal salt solution (b) after a certain period of time, after substrate is washed and dried, is obtained on the surface of the material
High density single dispersion metal nano particle.
2. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: the material is any material with interface.
3. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: the concentration of the Dopamine hydrochloride solution is 0.1~10mg/mL.
4. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: the standing perhaps stirs take out after a period of time in stand or the time of stirring is 1~72h, stirring turns
Speed is 500~2000r/min.
5. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: in washing and drying described in step 1) and step 2), cleaning way is alternately to be cleaned using ethyl alcohol and pure water, is done
Dry is to dry under room temperature.
6. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: metal salt solution (b) described in step 2) is Ag+Salting liquid or Au3+Salting liquid.
7. the method that one kind as claimed in claim 6 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: the Ag+Salting liquid in Ag+Concentration is 0.001~1mol/L;The Au3+Salting liquid in Au3+Concentration
For 0.0001~1mol/L.
8. the method that one kind as claimed in claim 6 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: the Ag+Salting liquid or Au3+Salting liquid in, solvent is aqueous solution, methanol, ethyl alcohol, formic acid or contains
The aqueous solution of methanol, ethyl alcohol or formic acid.
9. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: in During Illumination described in step 2), the wave-length coverage of light is from ultraviolet light to visible light region, and intensity of illumination is
0.1~1000mW/cm-2, light application time is 10s~120min.
10. the method that one kind as described in claim 1 prepares high density single dispersion metal nano particle on the surface of the material, special
Sign is: in the During Illumination, light is irradiated by lithography mask version (c).
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Cited By (2)
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CN111940143A (en) * | 2020-07-24 | 2020-11-17 | 合肥百诺金科技股份有限公司 | Sterilizing, disinfecting and ozone-removing electrostatic adsorption electrode and preparation method thereof |
CN113663139A (en) * | 2021-07-02 | 2021-11-19 | 福州市微纳新创医疗科技有限公司 | Multi-spine nano-gold memory alloy stent with radiotherapy sensitization function and preparation method and application thereof |
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CN105671525A (en) * | 2016-01-27 | 2016-06-15 | 西南大学 | Method for manufacturing patterned metal film based on poly-dopamine and product thereof |
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CN113663139A (en) * | 2021-07-02 | 2021-11-19 | 福州市微纳新创医疗科技有限公司 | Multi-spine nano-gold memory alloy stent with radiotherapy sensitization function and preparation method and application thereof |
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