CN103539958B - Substrate is coated with the transfer method of super thin metal nano material film - Google Patents
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- CN103539958B CN103539958B CN201310535290.5A CN201310535290A CN103539958B CN 103539958 B CN103539958 B CN 103539958B CN 201310535290 A CN201310535290 A CN 201310535290A CN 103539958 B CN103539958 B CN 103539958B
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Abstract
A kind of substrate is coated with the transfer method of super thin metal nano material film, it is made up of following step: polymeric laminate is placed into the thickness prepared in substrate and is less than on the metal nano material film of 10 atomic shells, be heated to polymeric laminate and substrate bonds together, naturally cool to room temperature; Coherent polymeric laminate and substrate are placed in acid or alkali, after substrate is eliminated completely, metal nano material film transfer is on polymeric laminate.The platinum film that embodiment 1 aluminum foil substrate is plated transfer to molecular-weight average be 2000 ethylene-vinyl acetate copolymer adhesive film on sample, test with atomic force microscope and x-ray photoelectron spectroscopy, the photo of atomic force microscope shows, platinum metal film is evenly distributed on polymeric laminate, and size is 0.3nm, x-ray photoelectron power spectrum graphs is bright, and it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum metal film is present in molecular-weight average.
Description
Technical field
The invention belongs to thin-film material technical field, be specifically related to the thin-film material be plated on substrate to transfer on another kind of substrate.
Background technology
Ultrathin nanometer material, particularly thickness is less than the nano material of 10 atomic shells, as Graphene and derivative, the noble metal film of Graphene, chemically modified, as Pt, Pd, Au, Ag, Cu etc., sull is as zinc-oxide film, nitride film, as boron nitride etc., has very unique character, has attracted to study interest widely.Narrowly, Graphene is a kind of bidimensional C film of monoatomic layer thickness.The room temperature electron mobility of Graphene far exceedes other known species all, the highest Young mould constant and physical strength.At higher current densities, the stability of Graphene is higher than copper 1,000,000 times, is best gas, water vapour and chemical vapors block film, has high conductance and heat-conduction coefficient.Meanwhile, Graphene is not only transparent but also conduct electricity, and can make good transparent conductive film etc.Graphene will inevitably replace a lot of common used material in a lot of fields.Such as; Graphene can make flexible electronic device, gas shield film, water vapour and barrier layer for gases, electromagnetic shielding material, heat sink material, ultracapacitor, is applied to the transparent conductive film on solar cell and indicating meter, photosensor, ultra-high frequency generator, supper-fast laser, lithium cell, fuel cell and molecular device electrode materials, support of the catalyst, function sensor etc.The extreme thickness of Graphene, chemical stability, conduction, heat conduction, transparent and physical strength also become the focus for the research of cancer photoelectric therapy.
The Atomic layer deposition method of oxide compound and nitride semi-conductor and electron device industry noticeable.Monoatomic layer thicknesses of metal film, although there is a lot of potential use, because evenly prepare the technical difficulty of large area film, up to the present, research rests on the primary stage.Although underpotential deposition technology has been used to prepare monoatomic layer film, have a lot about the report of monoatomic layer thin film deposition, but because of the formation of surface when the first layer deposits always with three-dimensional structure, make uniformity of film and Quality Down, strict theory is not uniform big area Atomic layer deposition.During as deposit multilayer, after one deck always reduce than one deck fraction of coverage above, backmost the material of one deck deposition is less, and extensive high quality applications is restricted.
2012, the human hairs such as Moffat understood a new Atomic layer deposition method [Yihua Liu, DincerGokcen, Ugo Bertocci, Thomas P.Moffat, Science, 338,1327 (2012)].When metal platinum deposits, due to underpotential deposition, one deck hydrogen can be formed immediately on the surface of platinum.They find, this layer of hydrogen can stop the further deposition of platinum, thus deposition process is limited in an atomic shell, avoids the formation of 3 D defects structure simultaneously, and deposition process is stopped after evenly completing an atomic layer level thin film.When applying reverse voltage, Surface Hydrogen can oxidizedly be removed, and forms a unsalted surface.Repeat said process, an atomic shell can be deposited at every turn, in layer do plane SH wave.They, with the gentle x-ray photoelectron spectroscopy analysis in micro-sky, confirm that the thickness of every one deck and quality are all identical.
The shortcoming of Moffat method is: employ gold-plated silicon chip and make substrate, and after platinum has deposited, platinum nature combines with gold, has no idea separately.The method is only limited to the deposition of metal platinum, is not generalized to other material.
But another shortcoming of aforesaid method is: the monomolecular film prepared depends on substrate, effectively can not be transferred on other substrates, which limits the application of monomolecular film.
Summary of the invention
Technical problem to be solved by this invention is the shortcoming overcoming prior art, provides the transfer method a kind of method is simple, substrate flexibility is curling substrate being coated with super thin metal nano material film.
It is made up of following step to solve the problems of the technologies described above adopted technical scheme:
1, polymeric laminate is placed into the thickness prepared in substrate to be less than on the metal nano material film of 10 atomic shells, is heated to polymeric laminate and substrate bonds together, naturally cool to room temperature.
2, be placed in acid or alkali by coherent polymeric laminate and substrate, after substrate is eliminated completely, above-mentioned metal nano material film transfer is on polymeric laminate.
Polymeric laminate of the present invention is any one in ethylene-vinyl acetate copolymer, polyvinyl butyral acetal, polyethylene, polypropylene, polystyrene, polymethylmethacrylate, polyvinyl chloride, nylon, polycarbonate, urethane, tetrafluoroethylene, polyethylene terephthalate, polyimide, melamine formaldehyde resin, vinyl acetate between to for plastic.
Substrate of the present invention is the substrate that flexible curling substrate or thickness are less than 3.3mm.
Substrate of the present invention be at the bottom of the stainless steel-based end, the substrate of ITO conductive glass, the substrate of FTO conductive glass, silicon wafer-based in any one.
The curling substrate of flexibility of the present invention is that thickness is less than the tinsel of 1mm or conductive polymer film substrate or metal-doped organic conductive macromolecule film substrate.
Tinsel of the present invention is any one in stainless steel foil, nickel foil, cobalt paper tinsel, titanium foil, aluminium foil.
Conductive polymer film of the present invention is any one in polyacetylene, Polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, poly-two alkynes conductive polymer film; Described metal-doped organism conductive polymer film is any one in iron, cobalt, nickel, copper, gold and silver, indium, platinum, sodium, magnesium, aluminium, titanium, molybdenum, cadmium, manganese, zinc, silicon, tin, is doped to any one the conductive polymer film in polyacetylene, Polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, poly-two alkynes.
Metal nano material film of the present invention is any one in platinum, gold and silver, copper, iron, nickel, aluminium film.
The composition of any one or any two kinds in the chromic acid of the phosphoric acid of the hydrochloric acid of acid of the present invention to be concentration be 0.001 ~ 0.05mol/L, the sulfuric acid of 0.001 ~ 0.05mol/L, 0.001 ~ 0.05mol/L, the hydrofluoric acid of 0.001 ~ 0.05mol/L, 0.001 ~ 0.05mol/L.
Alkali of the present invention is concentration is the NaOH of 0.001 ~ 0.05mol/L, the NaHCO of 0.001 ~ 0.05mol/L
3, 0.001 ~ 0.05mol/L NaCO
3, the KOH of 0.001 ~ 0.05mol/L, the MgOH of 0.001 ~ 0.05mol/L, 0.001 ~ 0.05mol/L CaOH in the composition of any one or any two kinds.：
Adopt the platinum film that the aluminum foil substrate prepared of the inventive method is plated transfer to molecular-weight average be 2000 ethylene-vinyl acetate copolymer adhesive film on sample, test with atomic force microscope and x-ray photoelectron spectroscopy, the photo of atomic force microscope shows, platinum metal film is evenly distributed on polymeric laminate, and size is 0.3nm, x-ray photoelectron power spectrum graphs is bright, and it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum metal film is present in molecular-weight average.
Accompanying drawing explanation
Fig. 1 is the atomic force microscopy that the platinum film that embodiment 1 aluminum foil substrate is plated transfers to ethylene-vinyl acetate copolymer adhesive film.
Fig. 2 is that the transfer method real substrate being coated with super thin metal nano material film executes the x-ray photoelectron energy spectrogram that the platinum film that example 1 aluminum foil substrate is plated transfers to ethylene-vinyl acetate copolymer adhesive film.
Specific implementation method
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the invention is not restricted to these embodiments.
Embodiment 1
To be coated with the transfer method of platinum film in aluminum foil substrate, its step is as follows:
In aluminum foil substrate, the method for plating platinum film is: be that the flexible curling aluminium foil conductive substrates of 0.3mm is put into and prepared vessel 1 and as the first electrode 2 with thickness, platinized platinum conductive electrode is as the second electrode 3, distance between first electrode 2 and the second electrode 3 is 5cm, is preparing the K adding 3mM in vessel 1
2ptCl
6the sodium-chlor of the aqueous solution and 1.5M, K
2ptCl
6be 1:500 with the mol ratio of sodium-chlor, be prepared into deposit solution, the add-on of deposit solution is to the flexible curling aluminium foil conductive substrates of submergence, adjust ph to 4, is heated to 25 DEG C, switches on power, voltage is-0.60V, and aluminium foil conductive substrates deposits one deck monoatomic layer thickness platinum metal film.
1, by molecular-weight average be 2000 ethylene-vinyl acetate copolymer adhesive film be placed into and be coated with in aluminum foil substrate that thickness is 0.3nm platinum film, substrate is thickness is the flexible curling substrate of 0.5mm, also thickness can be adopted to be less than the flexible curling substrate of 1mm, be heated to ethylene-vinyl acetate copolymer adhesive film and substrate bonds together, naturally cool to room temperature.
Above-mentioned substrate also can adopt thickness to be less than the flexible curling stainless steel foil substrate of 1mm, also thickness can be adopted to be less than the flexible curling nickel foil substrate of 1mm, also thickness can be adopted to be less than the flexible curling cobalt paper tinsel substrate of 1mm, thickness can be adopted to be less than the flexible curling titanium foil substrate of 1mm.Also can adopt the polymerization degree be 30 ~ 500,000 polyacetylene, Polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, any one in poly-two alkynes.
Substrate also can adopt the polymerization degree be 30 ~ 500,000 iron, cobalt, nickel, copper, gold and silver, indium, platinum, sodium, magnesium, aluminium, titanium, molybdenum, cadmium, manganese, zinc, silicon, any one in tin be doped to any one conductive polymer film in polyacetylene, Polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene, poly-two alkynes.
Substrate also can adopt at the bottom of the stainless steel-based end, the substrate of ITO conductive glass, the substrate of FTO conductive glass, silicon wafer-based any one.
The 0.3nm platinum film that substrate is plated, also can adopt in the plating gold and silver of same thickness, copper, iron, nickel, aluminium film any one.
Above-mentioned ethylene-vinyl acetate copolymer adhesive film also can adopt in polyvinyl butyral acetal, polyethylene, polypropylene, polystyrene, polymethylmethacrylate, polyvinyl chloride, nylon, polycarbonate, urethane, tetrafluoroethylene, polyethylene terephthalate, polyimide, melamine formaldehyde resin, vinyl acetate between to for plastic any one.
2, coherent ethylene-vinyl acetate copolymer adhesive film and aluminum foil substrate being placed on concentration is in the aqueous hydrochloric acid of 0.01mol/L, and after aluminum foil substrate is eliminated completely, platinum film is transferred on ethylene-vinyl acetate copolymer adhesive film.
To transfer to molecular-weight average be that the method for the ethylene-vinyl acetate copolymer adhesive film of 2000 is identical with being coated with platinum film in aluminum foil substrate to the method on any one polymeric laminate above-mentioned to adopt the metal nano material film transfer of other substrate above-mentioned plating.
Embodiment 2
To be coated with the transfer method of platinum film in aluminum foil substrate, its step is as follows:
Step 1 is identical with embodiment 1.In step 2, coherent ethylene-vinyl acetate copolymer adhesive film and aluminum foil substrate being placed on concentration is in the aqueous hydrochloric acid of 0.001mol/L, after aluminum foil substrate is eliminated completely, it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum film transfers to molecular-weight average.
Embodiment 3
To be coated with the transfer method of platinum film in aluminum foil substrate, its step is as follows:
Step 1 is identical with embodiment 1.In step 2, coherent ethylene-vinyl acetate copolymer adhesive film and aluminum foil substrate being placed on concentration is in the aqueous hydrochloric acid of 0.05mol/L, after aluminum foil substrate is eliminated completely, it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum film transfers to molecular-weight average.
Embodiment 4
To be coated with the transfer method of platinum film in aluminum foil substrate, its step is as follows:
In the step 2 of above embodiment 1 ~ 3, aqueous hydrochloric acid aqueous sulfuric acid used is replaced, and the concentration of aqueous sulfuric acid is identical with corresponding embodiment; The aqueous hydrochloric acid used also phosphoric acid aqueous solution is replaced, and the concentration of phosphate aqueous solution is identical with corresponding embodiment; Aqueous hydrochloric acid used also available hydrogen aqueous fluorine acid solution is replaced, and the concentration of hydrofluoric acid aqueous solution is identical with corresponding embodiment; Aqueous hydrochloric acid used also can be replaced with chromic acid aqueous solution, and the concentration of chromic acid aqueous solution is identical with corresponding embodiment.Acid solution any proportioning composition between the two of acid solution used also available above-mentioned concentration.After aluminum foil substrate is eliminated completely, it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum film transfers to molecular-weight average.
Other steps are identical with embodiment 1.
Embodiment 5
To be coated with the transfer method of platinum film in aluminum foil substrate, its step is as follows:
In the step 2 of above embodiment 1 ~ 3, the aqueous hydrochloric acid NaOH aqueous solution used is replaced, and the concentration of the NaOH aqueous solution is identical with the concentration of acid solution in corresponding embodiment; Aqueous hydrochloric acid used also can use NaHCO
3the aqueous solution is replaced, NaHCO
3the concentration of the aqueous solution is identical with corresponding embodiment; Aqueous hydrochloric acid used also can use NaCO
3the aqueous solution is replaced, NaCO
3the concentration of the aqueous solution is identical with the concentration of acid solution in corresponding embodiment; Aqueous hydrochloric acid used also can be replaced with the MgOH aqueous solution, and the concentration of the MgOH aqueous solution is identical with corresponding embodiment, and aqueous hydrochloric acid used also can be replaced with the CaOH aqueous solution, and the concentration of the CaOH aqueous solution is identical with corresponding embodiment.The acid solution arbitrary composition between the two of acid solution used also available above-mentioned concentration, the alkaline solution arbitrary composition between the two of alkaline solution used also available above-mentioned concentration.After aluminum foil substrate is eliminated completely, it is on the ethylene-vinyl acetate copolymer adhesive film of 2000 that platinum film transfers to molecular-weight average.
Other steps are identical with embodiment 1.
In order to verify beneficial effect of the present invention, the platinum film that contriver adopts the embodiment of the present invention 1 to plate in aluminum foil substrate transfer to molecular-weight average be 2000 ethylene-vinyl acetate copolymer adhesive film on test, various experimental conditions is as follows:
The platinum film that aluminum foil substrate is plated transfer to molecular-weight average be 2000 ethylene-vinyl acetate copolymer adhesive film on experimental technique identical with embodiment 1.Get 2 × 2cm
2sample atomic force microscope and x-ray photoelectron spectroscopy test by the using method of instrument, Fig. 1 is shown in by the photo of atomic force microscope.As seen from Figure 1, platinum metal film is evenly distributed on polymeric laminate, and size is 0.3nm.X-ray photoelectron energy spectrogram is shown in Fig. 2, and as seen from Figure 2, platinum metal film is present on polymeric laminate.
Claims (9)
1. substrate is coated with a transfer method for super thin metal nano material film, it is characterized in that it is made up of following step:
(1) polymeric laminate is placed into the thickness prepared in substrate to be less than on the metal nano material film of 10 atomic shells, is heated to polymeric laminate and substrate bonds together, naturally cool to room temperature;
(2) be placed in acid or alkali by coherent polymeric laminate and substrate, after substrate is eliminated completely, above-mentioned metal nano material film transfer is on polymeric laminate.
2. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described polymeric laminate is any one in ethylene-vinyl acetate copolymer, polyvinyl butyral acetal, polyethylene, polypropylene, polystyrene, polymethylmethacrylate, polyvinyl chloride, nylon, polycarbonate, urethane, polyethylene terephthalate, polyimide, trimeric cyanamide, formaldehyde resin, vinyl acetate between to for plastic.
3. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described substrate is the substrate that flexible curling substrate or thickness are less than 3.3mm.
4. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described substrate be at the bottom of the stainless steel-based end, the substrate of ITO conductive glass, the substrate of FTO conductive glass, silicon wafer-based in any one.
5. substrate according to claim 3 is coated with the transfer method of super thin metal nano material film, it is characterized in that: the curling substrate of described flexibility is the tinsel that thickness is less than 1mm.
6. substrate according to claim 5 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described tinsel is any one in stainless steel foil, nickel foil, cobalt paper tinsel, titanium foil, aluminium foil.
7. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described metal nano material film is any one in platinum, gold and silver, copper, iron, nickel, aluminium film.
8. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: the composition of any one or any two kinds in the chromic acid of the phosphoric acid of the hydrochloric acid of described acid to be concentration be 0.001 ~ 0.05mol/L, the sulfuric acid of 0.001 ~ 0.05mol/L, 0.001 ~ 0.05mol/L, the hydrofluoric acid of 0.001 ~ 0.05mol/L, 0.001 ~ 0.05mol/L.
9. substrate according to claim 1 is coated with the transfer method of super thin metal nano material film, it is characterized in that: described alkali is concentration is the NaOH of 0.001 ~ 0.05mol/L, the NaHCO of 0.001 ~ 0.05mol/L
3, 0.001 ~ 0.05mol/L Na
2cO
3, the KOH of 0.001 ~ 0.05mol/L, the Ca (OH) of 0.001 ~ 0.05mol/L
2in the composition of any one or any two kinds.
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| CN109722007B (en) * | 2018-12-05 | 2021-08-31 | 江汉大学 | Conductive polymer composite material under action of magnetic field and preparation method thereof |
| CN113346038A (en) * | 2020-03-03 | 2021-09-03 | 宁德新能源科技有限公司 | Preparation method and preparation device of composite current collector |
| CN112552544B (en) * | 2020-11-20 | 2023-07-25 | 广东工业大学 | Surface metallized polymer material and preparation method and application thereof |
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