CN103556197B - The method of monoatomic layer thicknesses of metal film prepared by flexible curling conductive substrates - Google Patents
The method of monoatomic layer thicknesses of metal film prepared by flexible curling conductive substrates Download PDFInfo
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- CN103556197B CN103556197B CN201310535381.9A CN201310535381A CN103556197B CN 103556197 B CN103556197 B CN 103556197B CN 201310535381 A CN201310535381 A CN 201310535381A CN 103556197 B CN103556197 B CN 103556197B
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Abstract
The method of monoatomic layer thicknesses of metal film prepared by a kind of flexibility curling conductive substrates, be made up of following step: curling for flexibility conductive substrates is put into and prepares vessel 1 and be connected to the first electrode 2, the second electrode 3 is made with inert metal sheet, two interelectrode distances are 0.2 ~ 10cm, preparing in vessel 1 deposit solution added containing plating metal salt, the add-on of deposit fluid is to the flexible curling conductive substrates of submergence, adjust ph to 2.0 ~ 7.5, heating is no more than 90 DEG C, switch on power, voltage between two electrodes is regulated to be-10 ~ 10V, deposit layer of metal film on conductive substrates or repeat above-mentioned steps at least deposition layer of metal film or on conductive substrates alternating deposit at least two kinds of metals at least double layer of metal film on conductive substrates.It can flexible curling, coating be the advantages such as atomic shell that the present invention has method substrate simple, used, can be used for flexible curling conductive substrates deposits monoatomic layer thicknesses of metal film.
Description
Technical field
The invention belongs to deposition arts, be specifically related at metal substrate or high molecular polymer deposited on substrates monoatomic layer thicknesses of metal film.
Background technology
Known monoatomic layer material, mainly contains Graphene and several oxide compound, nitride etc.Graphene, because of the structures and characteristics of its uniqueness, has attracted to study interest widely.
Graphene is a kind of bidimensional C film of monoatomic layer thickness.In known substance, it has the highest room temperature electron mobility, 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 transparent conductive film etc. well.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, but not yet find because of monoatomic layer film, application successively prepares high-quality multilayered film material with Atomic layer deposition method at present.
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, because surface is usually with the formation of 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 [YihuaLiu, DincerGokcen, UgoBertocci, ThomasP.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.
Technical problem to be solved by this invention is the shortcoming overcoming prior art, provides the deposition method of the monoatomic layer thicknesses of metal film that a kind of method is simple, substrate flexibility is curling, coating is atomic shell.
Solve the problems of the technologies described above adopted technical scheme to be made up of following step:
1, prepared by flexibility curling conductive substrates a method for monoatomic layer thicknesses of metal film, is made up of following step:
Curling for flexibility conductive substrates is put into and prepares vessel 1 and be connected to the first electrode 2, the second electrode 3 is made with inert metal sheet, two interelectrode distances are 0.2 ~ 10cm, preparing in vessel 1 deposit solution added containing plating metal salt, the add-on of deposit fluid is to the flexible curling conductive substrates of submergence, adjust ph to 2.0 ~ 7.5, heating is no more than 90 DEG C, switch on power, voltage between two electrodes is regulated to be-10 ~ 10V, deposit layer of metal film on conductive substrates or repeat above-mentioned steps at least deposition layer of metal film or on conductive substrates alternating deposit at least two kinds of metals at least double layer of metal film on conductive substrates.
Above-mentioned plating metal is any one in manganese, iron, cobalt, nickel, copper, zinc, molybdenum, palladium, silver, platinum, gold, aluminium, tin, bismuth, and deposit solution is the aqueous solution containing plating metal salt.
Inert metal sheet of the present invention is any one in platinized platinum, gold plaque, palladium sheet, rhodium sheet.
Deposit solution containing plating metal salt of the present invention is by the composition of concentration to be first group of inorganic salt solution of 0.1 ~ 10mM and concentration be second group of inorganic salt solution of 0.1 ~ 10mM, and the mol ratio of first group of inorganic salt solution and second group of inorganic salt solution is 1:10 ~ 1000; First group of above-mentioned inorganic salt are any one in nitrate, muriate, vitriol, perchlorate, and second group of inorganic salt are any one in the nitrate of lithium or sodium or potassium or magnesium or calcium, muriate, vitriol, perchlorate.
The curling conductive substrates of flexibility of the present invention is that thickness is less than the tinsel of 0.5mm or is coated with the conductive polymer film that thickness is 100 ~ 500nm metallic film.
Above-mentioned tinsel is any one in nickel foil, cobalt paper tinsel, titanium foil, aluminium foil, red copper foil.
Above-mentioned thickness to be the metallic film of 100 ~ 500nm be in Ag films, Copper thin film, platinum film, aluminium film any one.
Conductive polymer film of the present invention is any one in polythiophene film, poly(p-phenylene) film, polyaniline film, film of poly pyrrole, D-A type conjugated polymer thin films, carbon fiber-polypropylene film.
Monoatomic layer thicknesses of metal film not of the same race of the present invention is alternately plate different metallic films, and this metallic film is different metallic film is alternately plate different metallic films.
Owing to present invention employs deposition method, the curling conductive substrates of flexibility deposits at least a layer thickness and is less than the same of 1.0nm or the monoatomic layer thicknesses of metal film replaced not of the same race, it can flexible curling, coating be the advantages such as atomic shell that the present invention has method substrate simple, used, can be used for flexible curling conductive substrates deposits monoatomic layer thicknesses of metal film.
Accompanying drawing explanation
Fig. 1 is the structural representation preparing vessel 1.
Fig. 2 is the x-ray photoelectron energy spectrogram depositing platinum individual layer atomic layer level thin film in aluminum substrates.
Fig. 3 is the scanning tunnel microscope figure depositing platinum individual layer atomic layer level thin film in aluminum substrates.
Embodiment
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
For the deposition method of platinum monoatomic layer thicknesses of metal film, its step is as follows:
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, platinized platinum conductive electrode is 5cm as the distance between the second electrode 3, first electrode 2 and the second electrode 3, is preparing the K adding 3mM in vessel 1 with thickness
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.
Embodiment 2
For the deposition method of platinum monoatomic layer thicknesses of metal film, its step is as follows:
Be that the flexible curling aluminium foil conductive substrates of 0.1mm is put into and prepared vessel 1 and as the first electrode 2, platinized platinum conductive electrode is 0.2cm as the distance between the second electrode 3, first electrode 2 and the second electrode 3, is preparing the K adding 0.1mM in vessel 1 with thickness
2ptCl
6the sodium-chlor of the aqueous solution and 0.01M, K
2ptCl
6be 1:10 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 2, is heated to 89 DEG C, switches on power, voltage is-10V, and aluminium foil conductive substrates deposits one deck monoatomic layer thickness platinum metal film.
Embodiment 3
For the deposition method of platinum monoatomic layer thicknesses of metal film, its step is as follows:
Be that the flexible curling aluminium foil conductive substrates of 0.5mm is put into and prepared vessel 1 and as the first electrode 2, platinized platinum conductive electrode is 10cm as the distance between the second electrode 3, first electrode 2 and the second electrode 3, is preparing the K adding 10mM in vessel 1 with thickness
2ptCl
6the sodium-chlor of the aqueous solution and 10M, K
2ptCl
6be 1:1000 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 7.5, is heated to 25 DEG C, switches on power, voltage is 10V, and aluminium foil conductive substrates deposits one deck monoatomic layer thickness platinum metal film.
Embodiment 4
In above embodiment 1 ~ 3, deposit solution used is the composition of first group of inorganic salt solution and second group of inorganic salt solution, first group of inorganic salt solution is identical with corresponding embodiment with the concentration of second group of inorganic salt solution, the K in first group of inorganic salt solution
2ptCl
6also any one muriate in manganese, iron, copper, cobalt, nickel, zinc, molybdenum, palladium, silver, platinum, gold, aluminium, tin, bismuth or nitrate or vitriol or perchlorate can be used to replace, sodium-chlor in second group of inorganic salt solution also can use any one nitrate in lithium, sodium, potassium, magnesium, calcium or muriate or acetate or vitriol or perchlorate to replace, first group of inorganic salt solution is identical with corresponding embodiment with the concentration of second group of inorganic salt solution, and first group of inorganic salt is identical with corresponding embodiment with the mol ratio of second group of inorganic salt.
Embodiment 5
In above embodiment 1 ~ 3, the curling conductive substrates of flexibility used is flexible curling nickel foil, and thickness is identical with corresponding embodiment; Also can use flexible curling cobalt paper tinsel, thickness is identical with corresponding embodiment; Also can use flexible curling titanium foil, thickness is identical with corresponding embodiment; Also can use flexible curling red copper foil, thickness is identical with corresponding embodiment.Other steps are identical with corresponding embodiment, and tinsel conductive substrates is plated one deck monoatomic layer thickness platinum metal film.
Embodiment 6
In above embodiment 1 ~ 3, the curling conductive substrates of flexibility used is coated with the conductive polythiophene film that thickness is 300nm Ag films, and other steps are identical with corresponding embodiment, plates one deck monoatomic layer thickness platinum metal film on conductive substrates.
Embodiment 7
In above embodiment 1 ~ 3, the curling conductive substrates of flexibility used is coated with the conductive polythiophene film that thickness is 100nm Ag films, and other steps are identical with corresponding embodiment, plates one deck monoatomic layer thickness platinum metal film on conductive substrates.
Embodiment 8
In above embodiment 1 ~ 3, the curling conductive substrates of flexibility used is coated with the conductive polythiophene film that thickness is 500nm Ag films, and other steps are identical with corresponding embodiment, plates one deck monoatomic layer thickness platinum metal film on conductive substrates.
Embodiment 9
In above embodiment 6 ~ 8, the curling conductive substrates of flexibility used is the polythiophene film being coated with Ag films, and the thickness of Ag films is identical with corresponding embodiment; Also the adoptable polythiophene film being coated with Copper thin film, the thickness of Copper thin film is identical with corresponding embodiment; Also the adoptable polythiophene film being coated with platinum film, the thickness of platinum film is identical with corresponding embodiment; Also the adoptable polythiophene film being coated with aluminium film, the thickness of aluminium film is identical with corresponding embodiment.Other steps are identical with corresponding embodiment, plate one deck monoatomic layer thicknesses of metal film on conductive substrates.
Embodiment 10
In above embodiment 6 ~ 8, the curling conductive substrates of flexibility used is the poly(p-phenylene) film of metal-plated membrane, the metallic membrane plated and the thickness of metallic membrane identical with corresponding embodiment; The curling conductive substrates of flexibility used is the polyaniline film of metal-plated membrane, the metallic membrane plated and the thickness of metallic membrane identical with corresponding embodiment; The curling conductive substrates of flexibility used is the film of poly pyrrole of metal-plated membrane, the metallic membrane plated and the thickness of metallic membrane identical with corresponding embodiment; The curling conductive substrates of flexibility used is the D-A type conjugated polymer thin films of metal-plated membrane, the metallic membrane plated and the thickness of metallic membrane identical with corresponding embodiment; The curling conductive substrates of flexibility used is the carbon fiber-polypropylene film of metal-plated membrane, the metallic membrane plated and the thickness of metallic membrane identical with corresponding embodiment.Other steps are identical with corresponding embodiment, plate one deck monoatomic layer thicknesses of metal film on conductive substrates.
Embodiment 11
In above embodiment 1 ~ 10, first group of inorganic salt solution is identical with corresponding embodiment with the concentration of second group of inorganic salt solution, and first group of inorganic salt is identical with corresponding embodiment with the mol ratio of second group of inorganic salt.Other steps are identical with corresponding embodiment.The curling conductive substrates of flexibility is plated a kind of monoatomic layer thicknesses of metal of one deck film.Before plating second layer monoatomic layer thicknesses of metal film, switch on power, voltage is-0.6V, repeats above-mentioned steps, and plating the first layer monoatomic layer thicknesses of metal film plates one deck same monoatomic layer thicknesses of metal film again.Repeat above-mentioned steps 9 times, the curling conductive substrates of flexibility plates 10 layers of same monoatomic layer thicknesses of metal film.The concrete metallic membrane of the monoatomic layer thicknesses of metal film plated, the thickness of every one deck and the number of plies of plating should be determined according to institute's metallizing.
Embodiment 12
In above embodiment 1 ~ 10, first group of inorganic salt solution is identical with corresponding embodiment with the concentration of second group of inorganic salt solution, first group of inorganic salt is identical with corresponding embodiment with the mol ratio of second group of inorganic salt, other steps are identical with corresponding embodiment, and the curling conductive substrates of flexibility is plated a kind of monoatomic layer thicknesses of metal of one deck film.Before plating second layer monoatomic layer thicknesses of metal film, switch on power, voltage is-0.6V, deposit solution used and the first layer are not identical, repeat above-mentioned steps, plating the first layer monoatomic layer thicknesses of metal film plates the monoatomic layer thicknesses of metal film of one deck the first layer monoatomic layer metallic film different metal again.Repeat above-mentioned steps 9 times, the curling conductive substrates of flexibility plates 10 layers two kinds monoatomic layer thicknesses of metal films, the concrete metallic membrane of the monoatomic layer thicknesses of metal film plated, the thickness of every one deck and the number of plies of plating should be determined according to institute's metallizing.
Embodiment 13
First group of inorganic salt solution is identical with corresponding embodiment with the concentration of second group of inorganic salt solution, and first group of inorganic salt is identical with corresponding embodiment with the mol ratio of second group of inorganic salt.Other steps are identical with corresponding embodiment, and the curling conductive substrates of flexibility is plated a kind of monoatomic layer thicknesses of metal of one deck film.Before plating second layer monoatomic layer thicknesses of metal film, switch on power, voltage is-0.6V, deposit solution used and the first layer are not identical, other steps are identical with corresponding embodiment, and plating the first layer monoatomic layer thicknesses of metal film plates the monoatomic layer thicknesses of metal film of one deck and the first layer monoatomic layer thicknesses of metal film different metal again.Before plating third layer monoatomic layer thicknesses of metal film, switch on power, voltage is-0.6V, deposit solution used is not identical with the first layer, the second layer, other steps are identical with corresponding embodiment, and plating second layer monoatomic layer thicknesses of metal film plates the monoatomic layer thicknesses of metal film of one deck and the first layer, second layer monoatomic layer thicknesses of metal film different metal again.Repeat above-mentioned steps 14 times, the curling conductive substrates of flexibility plates 15 layers three kinds monoatomic layer thicknesses of metal films.The concrete metallic membrane of the monoatomic layer thicknesses of metal film plated, the thickness of every one deck and the number of plies of plating should be determined according to institute's metallizing.
In order to verify beneficial effect of the present invention, contriver adopts the embodiment of the present invention 1 to be that the flexible curling aluminium foil conductive substrates of 0.3mm deposits one deck platinum monoatomic layer thicknesses of metal film Multifunctional imaging photoelectron spectrograph and atomic force microscope is tested at thickness, and experimental conditions is as follows:
Aluminium foil conductive substrates is deposited one deck platinum monoatomic layer thicknesses of metal film Multifunctional imaging photoelectron spectrograph to test by the testing method of this instrument, test result is shown in Fig. 2.As seen from Figure 2, near 70.9eV and 74.6eV, there is the 4f of metal platinum respectively
7/2and 4f
5/2peak, illustrates that the platinum metal film using the method to obtain is the atom of 0 valence state.
Aluminium foil conductive substrates is deposited one deck platinum monoatomic layer thicknesses of metal film atomic force microscope to test by the testing method of this instrument, test result is shown in Fig. 3.As seen from Figure 3, the size of one deck platinum monoatomic layer that aluminium foil conductive substrates deposits is only 0.4nm, and the pt atom that aluminium foil conductive substrates deposited one deck monoatomic layer is uniformly described.
Claims (3)
1. prepared by flexibility curling conductive substrates a method for monoatomic layer thicknesses of metal film, is made up of following step:
Curling for flexibility conductive substrates is put into and prepares vessel 1 and be connected to the first electrode 2, the second electrode 3 is made with inert metal sheet, two interelectrode distances are 0.2 ~ 10cm, preparing in vessel 1 deposit solution added containing plating metal salt, the add-on of deposit fluid is to the flexible curling conductive substrates of submergence, adjust ph to 2.0 ~ 7.5, heating is no more than 90 DEG C, switch on power, voltage between two electrodes is regulated to be-10 ~ 10V, deposit layer of metal film on conductive substrates or repeat above-mentioned steps at least deposition layer of metal film or on conductive substrates alternating deposit at least two kinds of metals at least double layer of metal film on conductive substrates,
Above-mentioned plating metal is any one in manganese, iron, cobalt, nickel, copper, zinc, molybdenum, palladium, silver, platinum, gold, aluminium, tin, bismuth, and deposit solution is the aqueous solution containing plating metal salt;
Above-mentioned inert metal sheet is any one in platinized platinum, gold plaque, palladium sheet, rhodium sheet;
The above-mentioned deposit solution containing plating metal salt is by the composition of concentration to be first group of inorganic salt solution of 0.1 ~ 10mM and concentration be second group of inorganic salt solution of 0.1 ~ 10mM, and the mol ratio of first group of inorganic salt solution and second group of inorganic salt solution is 1:10 ~ 1000; First group of above-mentioned inorganic salt are any one in nitrate, muriate, perchlorate, and second group of inorganic salt are any one in the nitrate of lithium or sodium or potassium or magnesium or calcium, muriate, perchlorate.
2. prepared by flexibility according to claim 1 curling conductive substrates the method for monoatomic layer thicknesses of metal film, it is characterized in that: the curling conductive substrates of described flexibility is that thickness is less than the tinsel of 0.5mm or is coated with the conductive polymer film that thickness is 100 ~ 500nm metallic film;
Above-mentioned tinsel is any one in nickel foil, cobalt paper tinsel, titanium foil, aluminium foil, red copper foil;
Above-mentioned thickness to be the metallic film of 100 ~ 500nm be in Ag films, Copper thin film, platinum film, aluminium film any one.
3. prepared by flexibility according to claim 1 curling conductive substrates the method for monoatomic layer thicknesses of metal film, it is characterized in that: described monoatomic layer thicknesses of metal film not of the same race is alternately plate different metallic films.
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| CN113373472B (en) * | 2021-06-16 | 2023-04-25 | 西北大学 | Polypyrrole/rhodium nanoparticle composite flexible electrode and preparation method and application thereof |
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| CN101651046A (en) * | 2009-07-22 | 2010-02-17 | 电子科技大学 | Preparation method of Al2O3/TiO2 compound dielectric film aluminum electrode foil |
| CN101841043A (en) * | 2010-01-25 | 2010-09-22 | 上海电力学院 | Method for preparing Ru-based/Pt skin film nano-film electrode for fuel cell |
| CN102154661A (en) * | 2011-03-22 | 2011-08-17 | 中国科学院过程工程研究所 | Method for preparing aluminum ingot by low-temperature electrolysis of metal monocrystal surface electrodes |
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|---|---|---|---|---|
| CN101651046A (en) * | 2009-07-22 | 2010-02-17 | 电子科技大学 | Preparation method of Al2O3/TiO2 compound dielectric film aluminum electrode foil |
| CN101841043A (en) * | 2010-01-25 | 2010-09-22 | 上海电力学院 | Method for preparing Ru-based/Pt skin film nano-film electrode for fuel cell |
| CN102154661A (en) * | 2011-03-22 | 2011-08-17 | 中国科学院过程工程研究所 | Method for preparing aluminum ingot by low-temperature electrolysis of metal monocrystal surface electrodes |
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| Self-terminating growth of Platinum films by electrochemical deposition;Yihua Liu etal.;《Science》;20121206;第338卷(第1327期);1327-1330 * |
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