CN105023627A - Film having high conductivity and oxidation resistance and preparing method thereof - Google Patents
Film having high conductivity and oxidation resistance and preparing method thereof Download PDFInfo
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- CN105023627A CN105023627A CN201510402001.3A CN201510402001A CN105023627A CN 105023627 A CN105023627 A CN 105023627A CN 201510402001 A CN201510402001 A CN 201510402001A CN 105023627 A CN105023627 A CN 105023627A
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Abstract
Provided is a film having high conductivity and oxidation resistance. The film is formed by a substrate. The substrate is provided with a transition layer. The transition layer is provided with a layer of amorphous silver alloy reflection film. The amorphous silver alloy reflection film is provided with a layer of metal protection film. The silver alloy reflection film comprises a silver element and rare earth elements, wherein the rare earth elements occupy, in mass percentage, 0.0001%-15% of the silver alloy reflection film. The silver alloy reflection film also comprises, in mass percentage, 0.001%-25% of any one or more than one of the elements of iron, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium and ruthenium, and balance being the silver element. The invention also provides a preparing method of the film above. The film has adjustable visible light reflectance, resistance to electrochemical corrosion and excellent conductivity, solves the problem of oxidation of the silver film, and is suitable for preparing an LCD device, an OLED device, an LED device, an EC device or a dye-sensitized solar cell device.
Description
Technical field
The present invention relates to electricity field, particularly relate to the conducting reflective film for LCD device or LED component or OLED or EC device etc., particularly a kind of have film of high connductivity and non-oxidizability and preparation method thereof.
Background technology
The electronic structure of rare earth element is different from other elements, in their atomic electrons layer, has one deck not by internal layer one 4f electronic shell that electronics fills up.Due to the existence of unsaturated electronic shell, rare earth element is made to have unique characteristic.Add a small amount of rare earth element and just can greatly affect materials microstructure and performance.Rare earth can refinement casting alloy crystal grain, reduce or eliminate column crystal, expand the effect such as equiax crystal district.
Existing conducting reflective film is all adopt evaporation coating, sputter coating, ion film plating or chemical vapour deposition (CVD) mode that required metal targets is coated with surface of the work under vacuum conditions by equipment, reaches various functional requirement.But because the characteristic of self can contact with air, there is the problem of oxidation in various metal in the process of film preparation, or the corrosion-resistant problem after film forming, makes performance have a greatly reduced quality, and do not reach the requirement that expection is actual.
Summary of the invention
The object of the present invention is to provide a kind of film with high connductivity and non-oxidizability, the described this film with high connductivity and non-oxidizability will solve the problem of the high and decrease in efficiency of energy consumption that conducting reflective film in prior art causes because of resistance, and the silver alloy film that simultaneously will solve crystalline state also exists the technical problem that potential difference is easy to suffer electrochemical corrosion.
A kind of film with high connductivity and non-oxidizability of the present invention, a substrate is had to form, described substrate is provided with one deck transition zone, described transition zone is provided with one deck amorphous state silver alloy reflective film, described amorphous state silver alloy reflective film is provided with layer of metal diaphragm, described silver alloy reflective film includes silver element and rare earth element, the mass percent of described rare earth element in silver alloy reflective film is 0.0001% ~ 15%, also containing the iron accounting for silver alloy reflective film mass percent 0.001% ~ 25%, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, the combination of any one or more than one the element in ruthenium, surplus is silver element.
Further, described rare earth element is lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, any one or more than one the combination in ytterbium, lutetium or scandium.
Further, described metal protective film is made up of any one element in titanium, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum, tantalum, niobium, cobalt, hafnium, vanadium, tin or zinc, and thickness is 5-50nm.
Further, described transition zone is made up of any one in chromium, aluminium, titanium, silicon dioxide, nickel or iron, and the thickness of described transition zone is 2nm ~ 100nm.
Further, the thickness of described silver alloy reflective film is 10nm ~ 1000nm.
Further, square resistance≤6 ohm of above-mentioned silver alloy reflective film, the reflectivity being 550nm place at visible wavelength is 25% ~ 98%.
Further, the E Θ/V (reduction potential) of described silver alloy reflective film is greater than the+0.7996V of fine silver.
Present invention also offers above-mentioned a kind of preparation method with the film of high connductivity and non-oxidizability, comprise the steps:
1) on substrate, adopt vacuum evaporation, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD) or plating and the method for chemical plating to be coated with thin film as transition zone, described transition zone is made up of any one in chromium, aluminium, titanium, silicon dioxide, nickel or iron, and the thickness of described transition zone is 2nm ~ 100nm;
2) on transition zone, vacuum evaporation is adopted, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD), or the method for plating and chemical plating prepares amorphous state silver alloy reflective film, described silver alloy reflective film includes silver element and rare earth element, the mass percent of described rare earth element in silver alloy reflective film is 0.0001% ~ 15%, also containing the iron accounting for silver alloy reflective film mass percent 0.001% ~ 25%, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, the combination of any one or more than one the element in ruthenium, surplus is silver element, by vacuum chamber spare interface in the process of preparation, be filled with nitrogen, helium, neon, argon gas, Krypton, xenon wherein any one, , the chance that workpiece is contacted with oxygen reduces, and improves the oxidation resistance of film.
3) any one element in amorphous state silver alloy reflective film ti coat on diamond, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum, tantalum, niobium, cobalt, hafnium, vanadium, tin or zinc, thickness is 5-50nm.
When rare earth element joins in silver and alloy thereof, the interfacial tension of silver alloy liquid can be made to reduce, the forming core function reduction of crystal grain, critical nucleus radius reduces, and nucleation is easy, nucleus refinement.Also hinder growing up of silver alloy crystal grain at annealing process middle rare earth, rare earth exists and adds the quantity of fault, effectively hinders recrystal grain seam and grows up, and makes the obvious refinement of crystal grain after cold roller and deformed, recrystallization annealing.Therefore, the amorphous state silver alloy film adding rare earth element can suppress film to produce the phenomenon of structural relaxation and crystallization under certain external condition.Rare earth element suppresses except crystallization except having in silver alloy, important function is the metallic element generation intermetallic compound in same alloy in addition, and these effects improve intensity, plasticity, corrosion resistance, resistance to wear, the heat-resisting and Properties of High Temperature Creep of silver alloy.Silver alloy film due to crystalline state also exists potential difference and is easy to suffer electrochemical corrosion, and thus amorphous silver alloy film has good electrochemical corrosion resistant.Therefore silver alloy reflective film uses vacuum evaporation, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD), plating and chemical plating method, thus obtains amorphous silver alloy film.
Silverskin is that 550nm place has higher reflectivity in optical wavelength, and silver has excellent electric conductivity, but the corrosion resistance of silverskin is poor, be easy to condense balling-up, reduce reflectivity, increase diffuse reflection, greatly reduce reflectivity and the electric conductivity of silverskin, have a strong impact on its serviceability.For this reason, with the addition of iron, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium and ruthenium one or more metal wherein as silver alloy composition.Simultaneously in order to improve the oxidizing potential of silverskin, thermal endurance, Properties of High Temperature Creep and suppress the crystallization phenomenon of silver alloy film, with the addition of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, one or more in ytterbium, lutetium, scandium.
By adding above metal and although heating makes the non-oxidizability of silverskin strengthen, but also thoroughly do not solve, because the overlong time of heating in production in enormous quantities, serious restriction production efficiency, in order to solve this 2 problems, in the present invention, first on filming equipment, the vacuum chamber of the vacuum cavity of silverskin and the bottoming of prime plated film is separated, be filled with nitrogen again, helium, neon, argon gas, Krypton, xenon one wherein, the problem of oxidation obtains good solution, on this basis, again the one in the metals such as silverskin plated surface one deck titanium (ti) nickel (ni) zirconium (zr) chromium (cr) aluminium (al) copper (cu) tungsten (w) molybdenum (mo) tantalum (ta) niobium (ni) cobalt (co) hafnium (hf) vanadium (v) tin (sn) zinc (zn).Coating film thickness is between 5nm-55nm.Substantially negligible on the impact of conductance, this tunic provides good protection to silverskin, further ensure that the non-oxidizability of silverskin, and follow-up heated baking link can dispense, and the production efficiency of product is greatly improved.
Because silver alloy film and diaphragm have adjustable visible reflectance, excellent electrochemical corrosion resistant performance and good electric conductivity, be specially adapted to the field that LCD device, LED component, OLED, EC device or dye sensitization solar battery device etc. are relevant to conducting reflective film.
The main component of amorphous state silver alloy film of the present invention is silver element, adds other metallic element to improve the correlated performance of film.Iron, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium or ruthenium is added mainly in order to suppress silverskin to cause because of self-coagulation balling-up to decline to visible reflectance and conductance declines in amorphous state silver alloy film, addition is 0.001% ~ 25% (mass fraction), is preferably 0.5% ~ 15% (mass fraction).
In order to improve the corrosion resistance of silver alloy, suppress silver element crystallization, resistance to wear, heat-resisting and Properties of High Temperature Creep, with the addition of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, one or more in scandium, addition is 0.0001% ~ 15% (mass fraction), be preferably 0.05% ~ 2% (mass fraction), improve the reduction potential of Ag films simultaneously, amorphous state silver alloy film reduction potential is made to have exceeded+the 0.7996V of silverskin, improve the electrochemical corrosion resistant of amorphous state silver alloy film.The thickness of amorphous state silver alloy reflective film is 1nm ~ 1000nm, and be preferably 5nm ~ 500nm, the thickness of rete regulates and controls according to actual needs, and its reflectivity at visible ray 550nm place can regulate according to thickness between 25% ~ 98%.
Because amorphous state silver alloy film is lower with the binding ability of glass substrate, therefore need between amorphous state silver alloy film and glass or other substrate, to be coated with one deck transition zone, to improve the stability of amorphous state silver alloy film.Transition zone selected is in the present invention chromium, aluminium, titanium, silicon dioxide, nickel, iron etc., based on the consideration on cost, be preferably chromium, iron, nickel or silicon dioxide, the thickness of transition zone is 2nm ~ 100nm, be preferably 5nm ~ 50nm, the thickness of transition zone carries out selecting according to different demands.
The preparation method of amorphous state silver alloy reflective mainly adopts vacuum evaporation, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD), plating and chemical plating method.Due to the conforming requirement of demand fulfillment large-area coating film, the preparation method of amorphous state silver alloy reflective is preferably the physical preparation method of vacuum evaporation, magnetron sputtering and ion sputtering, in addition the element composition due to silver alloy is more, is more preferably magnetron sputtering and ion sputtering process.
The present invention compares with prior art, and its technique effect is obvious.Conductive reflective has regulatable reflectivity; there is excellent electric conductivity; there is higher reduction potential; pour certain inert gas in the preparation; and at plated surface layer protecting film; substantially there are not how many impacts on electric conductivity, solve the problem of oxidation of silverskin well, be applicable to manufacture LCD device, OLED, LED component, EC device or dye sensitization solar battery device.The present invention has the electric conductivity of adjustable visible reflectance, electrochemical corrosion resistant and excellence.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment of the present invention device.
Embodiment
Embodiment 1
A kind of film with high connductivity and non-oxidizability of the present invention, a substrate 1 is had to form, described substrate 1 is provided with one deck transition zone 2, described transition zone 2 is provided with one deck amorphous state silver alloy reflective film 3, described amorphous state silver alloy reflective film 3 is provided with layer of metal diaphragm 4, described silver alloy reflective film 3 includes silver element and rare earth element, the mass percent of described rare earth element in silver alloy reflective film is 0.0001% ~ 15%, also containing the iron accounting for silver alloy reflective film 3 mass percent 0.001% ~ 25%, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, the combination of any one or more than one the element in ruthenium, surplus is silver element.
Further, described rare earth element is lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, any one or more than one the combination in ytterbium, lutetium or scandium.
Further, described metal protective film 4 is made up of any one element in titanium, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum, tantalum, niobium, cobalt, hafnium, vanadium, tin or zinc, and thickness is 5-50nm.
Further, described transition zone 2 is made up of any one in chromium, aluminium, titanium, silicon dioxide, nickel or iron, and the thickness of described transition zone 2 is 2nm ~ 100nm.
Further, the thickness of described silver alloy reflective film 3 is 10nm ~ 1000nm.
Further, square resistance≤6 ohm of above-mentioned silver alloy reflective film 3, the reflectivity being 550nm place at visible wavelength is 25% ~ 98%.
Further, the E Θ/V (reduction potential) of described silver alloy reflective film 3 is greater than the+0.7996V of fine silver.
Present invention also offers above-mentioned a kind of preparation method with the film of high connductivity and non-oxidizability, comprise the steps:
1) adopt on the substrate 1 vacuum evaporation, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD) or
The method of plating and chemical plating is coated with thin film as transition zone 2, and material is chromium, aluminium, titanium, dioxy
Any one in SiClx, nickel or iron is formed;
2) on transition zone 2, the preparation amorphous state silver alloy reflective film 3 that uses the same method is adopted, described silver alloy reflective film 3 includes silver element and rare earth element, the mass percent of described rare earth element in silver alloy reflective film 3 is 0.0001% ~ 15%, combination also containing any one or more than one the element accounted in the iron of silver alloy reflective film 3 mass percent 0.001% ~ 25%, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, ruthenium, surplus is silver element.By vacuum chamber spare interface in the process of preparation, be filled with nitrogen, helium, neon, argon gas, Krypton, xenon wherein any one, the chance that workpiece is contacted with oxygen reduces, and improves the oxidation resistance of film.
3) amorphous state silver alloy reflective film 3 ti coat on diamond, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum,
Any one element in tantalum, niobium, cobalt, hafnium, vanadium (v) tin or zinc.Thickness is 5-50nm.
Silver element when using in the present invention purity be 99.99% (mass fraction), purity is the chromium of 99.99% (mass fraction), silicon, aluminium, titanium, iron, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium and ruthenium, rare-earth elements of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, the thulium of purity 99.5% (mass fraction), ytterbium, lutetium and scandium.Adopt vacuum Alloy melting technology to be prepared into required target with the mass fraction of following table composition above-mentioned element, then adopt vacuum evaporation respectively, the mode of magnetron sputtering and ion sputtering is coated with amorphous state silver alloy film.Its coating is as shown in schematic diagram 1, and wherein 1 is film plating substrate, and 2 is transition zone, and 3 is amorphous state silver alloy reflective film layer, and 4 is metal film protective layer.
The each element composition of table 1 silver alloy film
Above-mentioned silver alloy is coated with on a glass substrate through certain coating process, then plates layer of metal film as protection, carry out correlated performance contrast with amorphous state silver alloy film.Data measured by below only using plating chromium as protective layer, its test result is as follows:
The correlated performance test result of table 2 amorphous state silver alloy film and plating protection crome metal film
Amorphous silver alloy film has higher reflectivity as can be seen from the above table, and higher electrochemical reduction current potential and low-resistivity are after protective film coating, and corresponding reflectivity declines, and resistance raises, but the antioxygenic property of film improves greatly.
Claims (8)
1. one kind has the film of high connductivity and non-oxidizability, comprise a substrate, described substrate is provided with one deck transition zone, it is characterized in that: described transition zone is provided with one deck amorphous state silver alloy reflective film, described amorphous state silver alloy reflective film is provided with layer of metal diaphragm, described amorphous state silver alloy reflective film includes silver element and rare earth element, the mass percent of described rare earth element in amorphous state silver alloy reflective film is 0.0001% ~ 15%, also containing the iron accounting for amorphous state silver alloy reflective film mass percent 0.001% ~ 25% in amorphous state silver alloy reflective film, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, any one element in ruthenium or the combination of more than one element, surplus is silver element.
2. the film with high connductivity and non-oxidizability according to claim 1, it is characterized in that: described rare earth element is lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, any one or more than one the combination in ytterbium, lutetium or scandium.
3. the film with high connductivity and non-oxidizability according to claim 1; it is characterized in that: described metal protective film is made up of any one element in titanium, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum, tantalum, niobium, cobalt, hafnium, vanadium, tin or zinc, thickness is 5-50nm.
4. the film with high connductivity and non-oxidizability according to claim 1, is characterized in that: described transition zone is made up of any one element in chromium, aluminium, titanium, silicon dioxide, nickel or iron, and the thickness of described transition zone is 2nm ~ 100nm.
5. the film with high connductivity and non-oxidizability according to claim 1, is characterized in that: the thickness of described amorphous state silver alloy reflective film is 10nm ~ 1000nm.
6. the film with high connductivity and non-oxidizability according to claim 1, is characterized in that: square resistance≤6 ohm of amorphous state silver alloy reflective film, and the reflectivity being 550nm place at visible wavelength is 25% ~ 98%.
7. the film with high connductivity and non-oxidizability according to claim 1, is characterized in that: the E Θ/V (reduction potential) of described silver alloy reflective film is greater than the+0.7996V of fine silver.
8. prepare a method with the film of high connductivity and non-oxidizability according to claim 1, it is characterized in that comprising the steps:
1) on substrate, adopt vacuum evaporation, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD) or plating and the method for chemical plating to be coated with thin film as transition zone, described transition zone is made up of any one in chromium, aluminium, titanium, silicon dioxide, nickel or iron, and the thickness of described transition zone is 2nm ~ 100nm;
2) on transition zone, vacuum evaporation is adopted, magnetron sputtering, ion sputtering, chemical vapour deposition (CVD), or the method for plating and chemical plating prepares amorphous state silver alloy reflective film, described silver alloy reflective film includes silver element and rare earth element, the mass percent of described rare earth element in silver alloy reflective film is 0.0001% ~ 15%, also containing the iron accounting for silver alloy reflective film mass percent 0.001% ~ 25%, cobalt, nickel, tungsten, tin, palladium, gold, rhodium, iridium, the combination of any one or more than one the element in ruthenium, surplus is silver element, by vacuum chamber spare interface in the process of preparation, be filled with nitrogen, helium, neon, argon gas, Krypton, xenon wherein any one,
3) any one element in amorphous state silver alloy reflective film ti coat on diamond, nickel, zirconium, chromium, aluminium, copper, tungsten, molybdenum, tantalum, niobium, cobalt, hafnium, vanadium, tin or zinc, thickness is 5-50nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107093500A (en) * | 2017-03-30 | 2017-08-25 | 华南理工大学 | A kind of graphic method of nano silver wire flexible transparent conductive film |
| CN111763919A (en) * | 2020-09-03 | 2020-10-13 | 宁波瑞凌新能源科技有限公司 | Reflecting film and preparation method and application thereof |
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| CN101083896A (en) * | 2006-05-31 | 2007-12-05 | 柏腾科技股份有限公司 | A method of forming an electromagnetic wave interference shielding film on a non-conductive material and its structure |
| CN102943221A (en) * | 2012-11-14 | 2013-02-27 | 仝泽彬 | Silver alloy reflecting film with high conductivity and electrochemical corrosion resisting performance and manufacture method thereof |
| CN103474494A (en) * | 2012-06-05 | 2013-12-25 | 爱博福欧有限公司 | Back-sheet for photovoltaic modules comprising back-contact solar cells |
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| JPH06329496A (en) * | 1992-08-26 | 1994-11-29 | Mitsubishi Kasei Corp | Method for preparing deposited thin film |
| US20030143342A1 (en) * | 2002-01-25 | 2003-07-31 | Kabushiki Kaisha Kobe Seiko Sho ( Kobe Steel, Ltd) | Reflective film, reflection type liquid crystal display, and sputtering target for forming the reflective film |
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| CN107093500B (en) * | 2017-03-30 | 2019-04-09 | 华南理工大学 | A kind of patterning method of silver nanowire flexible transparent conductive film |
| CN111763919A (en) * | 2020-09-03 | 2020-10-13 | 宁波瑞凌新能源科技有限公司 | Reflecting film and preparation method and application thereof |
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Application publication date: 20151104 |