CN104505149A - Laminated transparent electrode and preparation method thereof - Google Patents
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Abstract
The invention provides a laminated transparent electrode and a preparation method thereof. The laminated transparent electrode sequentially comprises a transparent substrate, a first-layer metal oxide film on the transparent substrate, a metal nanowire network layer on the first-layer metal oxide film, and a second-layer metal oxide film covering the metal nanowire network layer and the first-layer metal oxide film not covered by the metal nanowire network layer. A preparation method of the metal nanowire network layer comprises the steps of preparing a metal film layer on the first-layer metal oxide film, preparing a high-polymer nanofiber network on the metal film layer by using an electrostatic spinning technique, removing the metal film that is not covered by the high-polymer nanofiber network through etching by taking high-polymer nanofiber as a mask, and removing the high-polymer nanofiber network. The laminated transparent electrode has the advantages of high light transmissivity, low resistivity, firm contact with the substrate, smooth surface, low preparation and growth temperature, low cost and the like, and can be widely applied to various organic and inorganic photoelectric devices.
Description
Technical field
The invention belongs to electrode preparation field, be specifically related to a kind of stacked laminated transparent electrode and preparation method thereof.
Background technology
The photoelectric devices such as the touch-screen be widely used at present, flat-panel monitor and solar cell all need light transmission good and the transparency electrode of conduction.For transparency electrode, surface resistance and light transmittance are two major parameters determining its quality and application.Such as: the transparency electrode of high-performance touch-screen needs its light transmittance to be greater than 95%, but allows its surface resistance between 400 Ω/ to 600 Ω/; Solar cell and large area display then require that the surface resistance of transparency electrode is less than 20 Ω/.Traditional transparency electrode mainly refers to the metal oxide adulterated, and wherein, ITO relies on higher visible light transmissivity and lower surface resistance, in occupation of the transparent conductive film market share of more than 90%.But over nearly 10 years, the electronic device fast developments such as smart mobile phone, display, solar cell, surge to transparent conductive film demand, phosphide element reserves are limited, cause indium price to improve year by year in addition.Therefore, researcher is exploring novel transparent electric conducting material and is being used as transparency electrode with traditional materials such as alternative ITO.Novel transparent electric conducting material mainly comprises: conducting polymer, c-based nanomaterial and metal Nano structure electric conducting material.Wherein, the conductivity of organic conductive polymer is relatively low, is of limited application; C-based nanomaterial mainly comprises Graphene and carbon nano-tube, and the individual conductivity of these materials is better, but due to the contact area between adjoining graphite alkene or adjacent carbon nanotubes little, cause their stability and conductivity not satisfactory.Metal Nano structure mainly comprises conductive grid and nano wire.Wherein, the technology such as the photoetching that formation conducting metal network needs process costs high usually, electron beam or ion beam etching, are difficult to large-scale production practicality.The metal nanometer line conductive network prepared by solwution method has high conductivity and light transmission rate, and process costs is low simultaneously, is considered to the most promising novel transparent electrode material at present.But, the metal nanometer line in transparent substrates is distributed to by coating process, weak with substrate absorption affinity, and between adjacent nanowires, connection electrical resistance is comparatively large, often needs the means such as extra thermal annealing or laser treatment to improve its conductivity.
To sum up: novel transparent electrode needs to possess higher conductivity and light transmission rate, should prepare under alap raw material and process costs simultaneously, and current transparent electrode material and technology also have not as people's will part.Therefore, the transparency electrode of development of new and simple manufacture method, to obtain photoelectric properties excellence, strong with substrate adsorptivity and that surface smoothness is high transparency electrode has important value.
Summary of the invention
An object of the present invention is to provide a kind of stacked laminated transparent electrode and preparation method thereof.The transparency electrode obtained by the present invention has good visible ray and infrared light transmittance, and has the resistivity compared favourably with commercial transparency electrode.
Stacked laminated transparent electrode provided by the present invention, comprises from bottom to top successively: transparent substrates, the first layer metal sull be positioned in described transparent substrates, be positioned at the metal nanowire network layer on described first layer metal sull and be covered in the second layer metal sull on described metal nanowire network layer and the first layer metal oxide that do not hidden by described metal nanowire network layer.
Described stacked laminated transparent electrode prepares according to the method comprised the steps:
Step 1, provide described transparent substrates;
Step 2, prepare described first layer metal sull on the transparent substrate;
Step 3, on described first layer metal sull, prepare described metal nanowire network layer, following (a)-(e) of concrete grammar:
(a) depositing metal films layer on the clean surface of described first layer metal sull;
(b) by high molecular polymer (be called for short: high polymer) the nanofiber network of electrostatic spinning technique in described metal film layer surface preparative chemistry stable in properties,---first layer metal sull---metal film layer---the high polymer nano network of fibers lamination that obtains stacking transparent substrates from bottom to top;
C () is to above-mentioned transparent substrates---first layer metal sull---metal film layer---high polymer nano network of fibers laminated construction carries out Low Temperature Thermal annealing, make high polymer and metal film surfaces close contact, thus form the mask of high polymer nano network of fibers;
D () for mask with described high polymer nano network of fibers, utilizes corrosion of metals liquid corrosion to carve and removes not by metal that described high polymer nano network of fibers is covered;
E () selects suitable solvent clean to remove described high polymer nano network of fibers, obtain the metal nanowire network layer with high polymer network similar geometry shape;
Step 4, in above-mentioned transparent substrates---first layer metal sull---second layer metal sull prepared by metal nano spider lines, described second layer metal sull is covered on described metal nanowire network layer and the first layer metal oxide that do not hidden by described metal nanowire network layer, obtains described stacked laminated transparent electrode.
In said method step 1, described transparent substrates can be the transparent substrates of rigidity or flexibility, as glass substrate or PET substrate etc.The thickness range of described transparent substrates is 0.1mm-5mm.
In said method step 2, the Main Function of described first layer metal sull strengthens the tack between metal nano network layer and substrate, and serve as barrier layer and avoid corrosion of metals liquid to the etching of substrate.
Described first layer metal sull is made up of following at least one material: other transparent oxides of aluminium oxide, zinc oxide, indium oxide, tin oxide, gallium oxide and titanium oxide and same nature, specifically can be titanium oxide.
In said method step 2, the preparation method of described first layer metal sull is conventional method, as magnetron sputtering, electron beam evaporation, pulsed laser deposition or sol-gal process.
In said method step 2, the thickness of described first layer metal sull is 5nm-50nm.
In said method step 3 (a), the preparation method of described metal film layer is physical vapour deposition (PVD), such as vacuum evaporation or magnetron sputtering, or electroplates and chemical plating method.
Described metal is selected from following at least one: nickel, chromium, aluminium, copper, silver, gold, platinum and their alloy, considers cost and electric conductivity, specifically can be copper or aluminium.
The thickness of described metal film layer, by the process parameter control of physical vapour deposition (PVD), plating and chemical plating, specifically can be 20nm-200nm.
In said method step 3 (b), described high polymer can be following at least one: polyvinyl alcohol, polyoxyethylene, PLA, polymethyl methacrylate, polyacrylonitrile, polyurethane, polystyrene and polyvinylpyrrolidone, and described high polymer specifically can be the polyacrylonitrile (PAN) that point quantum is 130000.
In said method step 3 (b), the technological parameter of described electrostatic spinning is: spinning voltage is 3kV-50kV, and spinning nozzle is 5cm-50cm to the distance of collecting plate, and the mass concentration of spinning solution is 6%-15%.
Diameter continuously adjustabe in the scope of 100nm-2000nm of the high polymer nano fiber prepared.
In said method step 3 (c), described Low Temperature Thermal annealing adopts the heating of baking oven, hot plate or adopts solution vapor heating to carry out.The temperature of described Low Temperature Thermal annealing is 50-150 DEG C, and the time is 0.5-30min.
In said method step 3 (d), described corrosion of metals liquid is by solute and solvent composition, described solute is selected from following at least one: ferric nitrate, iron chloride, potassium bichromate, potassium cyanide, sulfate of ammoniac, hydrogen peroxide, hydrochloric acid, nitric acid, acetic acid and ammonia, described solvent for can dissolve above-mentioned solute arbitrarily, but can not dissolve the solvent of described high polymer nano fiber.
The molar concentration of described corrosion of metals liquid is 0.01-1M; Select depending on corrosion rate.
In said method step 3 (e), the described solvent for removing high polymer nano fiber is low toxicity and the low cost solvent that can dissolve described high polymer nano fiber, as when as described in high polymer nano fiber be polyacrylonitrile (PAN) nanofiber time, described solvent is dimethyl formamide (DMF).
After the described operation of said method step 3 (e) completes, the width of the metal nanometer line of gained is determined by the thickness of the diameter of high polymer nano fiber and metal film layer, and the diameter that size is about high polymer nano fiber deducts the thickness of the metal level of two times.Concrete scope can between 60nm-1600nm continuously adjustabe.
Described metal nanowire network layer is made up of random distribution or the metal nanometer line with rule orientating, and concrete condition is selected according to the equipment structure of electrostatic spinning.
In said method step 4, described second layer metal sull is made up of doping transparent metal oxide, and its crystalline state can be polycrystalline or amorphous.Described doping transparent metal oxide is selected from following at least one: Zinc-aluminium, indium tin oxide, fluorine tin-oxide, indium-zinc oxide and indium gallium zinc oxide, specifically can be Zinc-aluminium.
In said method step 4, the preparation method of described second layer metal sull can select chemical synthesis process easy and simple to handle, as sol-gal process, atomic layer deposition sum CVD, or physical gas-phase deposite method, as magnetron sputtering, ion sputtering plating, electron beam evaporation, pulsed laser deposition etc.
In said method step 4, the thickness of described second layer metal sull is 50nm-200nm.Its effect is protection metal nano network layer, reduces its oxidation rate to greatest extent, strengthens the adhesive force of metal nanometer line and substrate simultaneously.
Comprise the photoelectric device of stacked laminated transparent electrode provided by the present invention, as touch-screen, solar cell, light-emitting diode and flat-panel monitor etc. also belong to protection scope of the present invention.
In the present invention, rigidity or flexible transparent substrate are formed the first layer metal sull of thickness within the scope of 5-50nm, its on the one hand can increase the adsorptivity of metal level to substrate, and corrosion of metals liquid can be prevented in formation second layer metal nanometer line network process on the other hand to the erosion on photoelectric device surface; When preparing described metal nano spider lines, electrostatic spinning technique is adopted on continuous print metal film layer, directly to form high polymer fibre network as mask, recycling corrosion of metals liquid is removed not by metal that high polymer fibre is covered, high polymer fibre mask plate is removed in finally cleaning, can form the metal nano spider lines consistent with template; The second layer metal sull that metal nano spider lines is formed; fill up the space between metal nanometer line; reduce the surface roughness of electrode; add the adhesive force of metal nano spider lines and substrate; metal nanometer line is played to the effect of protection simultaneously, thereby is achieved the high-quality transparency electrode with excellent photoelectric property and mechanical performance.
Invention applies characterization method: electrostatic spinning.Electrostatic spinning technique is simple, is conducive to large area manufacture.Adopt fiber prepared by electrostatic spinning technique, diameter is continuously adjustabe in the scope of 100nm-2000nm, can realize the accurate control of metal nano line width simultaneously; By regulating electrostatic spinning time and voltage parameter, the special collection structure of employing, can draw ratio be prepared different with gap length, or having the network of fibers of certain rule orientating, thus obtain transmitance and the adjustable metal nano spider lines of resistivity.Because metal nano spider lines is formed after being corroded by metal film layer, connect so the connection between metal nanometer line is mutual melting, synthesize compared to chemical method and the metal nano spider lines piled up and formed, the metal nano spider lines that the present invention is formed has larger draw ratio, less crosslinked resistance, less surface roughness and stronger substrate adhesive force.In addition, the method that the present invention relates to is implemented at a lower temperature, can be used for large area on flexible substrates to prepare high-quality transparency electrode, realizes the application in flexible device.
Metal nanometer line transport network layer is clipped in the middle of two-layer oxide electroconductive film, metal nano spider lines can be avoided directly to contact with the external world, metal nanometer line is played to the effect of protection.The second layer metal oxide simultaneously conducted electricity has filled up the internetwork hole of metal nanometer line, be conducive to the carrier injection in metal nano spider lines space or photo-generated carrier collection, reduce the surface roughness of film, and the transmittance of incident light can be improved, stacked laminated transparent electrode provided by the present invention has that light transmission rate is high, resistivity is low, with substrate contact firmly, surfacing, preparation and the advantage such as growth temperature is low, with low cost, various organic and inorganic photoelectric device can be widely used in.
Accompanying drawing explanation
Fig. 1 is the manufacture process schematic diagram of stacked laminated transparent electrode of the present invention.
Fig. 2 is the schematic cross-section of stacked laminated transparent electrode of the present invention.
Fig. 3 is the stereoscan photograph of the PAN fiber of preparation.
Fig. 4 is optical microscope photograph and the electron micrograph of copper nano-wire network on the slide substrate prepared of the embodiment of the present invention.
Fig. 5 is the light transmittance of glass substrate prepared by the embodiment of the present invention---titanium deoxid film---copper nano-wire network lamination and the relation curve of wavelength.
Fig. 6 is light transmittance and the wavelength plot of stacked laminated transparent electrode prepared by the embodiment of the present invention.
Fig. 7 is the electron scanning micrograph of stacked laminated transparent electrode surface prepared by the embodiment of the present invention.
Embodiment
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.
The experimental technique used in following embodiment if no special instructions, is conventional method; Reagent used in following embodiment, material etc., if no special instructions, all can obtain from commercial channels.
Embodiment
1. first, 4cm × 4cm glass substrate carried out deoiling and cleaning according to the chemical cleaning procedure of standard, the cleaning agent of use is commercialization simple glass cleaning agent.After deionized water rinsing, dry rear for subsequent use for 150 DEG C in an oven.
2., under room temperature, utilize magnetron sputtering apparatus deposition of titanium oxide film in above-mentioned clean glass substrate.Wherein, deposition power is 200 watts, deposits the gases used gaseous mixture for argon gas and oxygen, and corresponding flow-rate ratio is 3:1.Sedimentation time is 2 minutes, and the titanium deoxid film thickness of formation is 8nm;
3. utilize vacuum vapour deposition in the layers of copper of titanium deoxid film surface deposition 80nm; During evaporation, the temperature of glass substrate is controlled at 200 DEG C by heater.Film thickness can be controlled by film thickness monitoring device;
4. by evaporation, the glass substrate of Copper thin film, as on the cathode collector plate of electrostatic spinning system, utilizes electrostatic spinning technique layers of copper surface deposition cyclization (diameter of cyclization is 500nm).Spinning voltage 8kV, spinning nozzle to the distance 9 centimetres of collecting plate, the DMF colloidal sol of spinning precursor to be mass concentration the be polyacrylonitrile of 12%; As shown in Figure 3, the uniform diameter of PAN fiber that prepared by electrostatic spinning is 500nm.
5. the compressed air band dynamic temperature utilizing flow velocity to be 1L/min is that the DMF liquid of 75 DEG C carries out vapours to sample and fumigates 1min, makes PAN and substrate surface form firm close contact;
6. utilize 1 liter of concentration be the iron chloride of 0.003 mole often liter the aqueous solution rinse sample, washing time is 2.5 minutes; Then continue to rinse this sample with the ferric chloride in aqueous solution that concentration is 0.0015 mole often liter, washing time is 2.5 minutes, to remove remaining copper;
7. utilize the DMF solution of 50 DEG C soak sample to dissolve PAN fiber, then with distilled water flushing, nitrogen dry up, 120 DEG C of oven for drying samples; The width of the copper nano-wire on the slide substrate prepared is about 300nm, has larger draw ratio, is interconnected to each other and on substrate, defines good conductive channel, as shown in Figure 4.Obtained copper nano-wire network all has good transmitance within the scope of 200-1000nm, and light transmittance is the highest can reach more than 90%, as shown in Figure 5.
8. prepare the metal oxide of second layer electrically conducting transparent, select the zinc oxide (thickness is 100nm) of sol-gal process synthesis aluminium doping.Concrete technology is as follows: first, and configuration concentration is than the zinc acetylacetonate and the zinc nitrate mixed solution that are 1:1, and solvent is EGME, and wherein precursor total concentration is 0.15 mole often liter; Then aluminum nitrate is mixed in precursor solution, the atomic ratio controlling aluminium and zinc is 2:98, and after completing, under room temperature, ageing obtains zinc oxide aluminum colloidal sol in 24 hours;
9. utilize spin coating technique zinc oxide aluminum colloidal sol to be spun to copper nano-wire network layer surface, it is 30 seconds that spin-coating time controls, and it is 2000 rpms that rotating speed controls.The heating plate that sample after spin coating is placed in 150 DEG C is dried 60 seconds, then repeats spin coating and dry run 5 times;
10. described sample is placed in Muffle furnace to anneal one hour under 200 DEG C of conditions, obtains final product.The final laminate electrode visible light transmissivity prepared reaches as high as 85%, as shown in Figure 6.
Structural parameters and the photoelectric parameter of final stacked laminated transparent electrode are as shown in table 1.
The structural parameters of the stacked laminated transparent electrode that table 1 prepares and photoelectric parameter
Claims (8)
1. a stacked laminated transparent electrode, it comprises from bottom to top successively: transparent substrates, the first layer metal sull be positioned in described transparent substrates, be positioned at the metal nanowire network layer on described first layer metal sull and be covered in the second layer metal sull on described metal nanowire network layer and the first layer metal oxide that do not hidden by described metal nanowire network layer.
2. stacked laminated transparent electrode according to claim 1, is characterized in that:
In described stacked laminated transparent electrode structure, described transparent substrates is the transparent substrates of rigidity or flexibility;
Described first layer metal sull is made up of following at least one material: other transparent oxides of aluminium oxide, zinc oxide, indium oxide, tin oxide, gallium oxide and titanium oxide and same nature;
The thickness of described first layer metal sull is 5nm-50nm;
Described metal nanowire network layer is made up of random distribution or the metal nanometer line with rule orientating;
Width continuously adjustabe between 60nm-1600nm of described metal nanometer line;
The metal forming described metal nanowire network layer is selected from following at least one: nickel, chromium, aluminium, copper, silver, gold, platinum and their alloy;
Described second layer metal sull is made up of doping transparent metal oxide, and described doping transparent metal oxide is selected from following at least one: Zinc-aluminium, indium tin oxide, fluorine tin-oxide, indium-zinc oxide and indium gallium zinc oxide;
The thickness of described second layer metal sull is 50nm-200nm.
3. prepare a method for the stacked laminated transparent electrode described in claim 1 or 2, comprise the steps:
Step 1, provide described transparent substrates;
Step 2, prepare described first layer metal sull on the transparent substrate;
Step 3, on described first layer metal sull, prepare described metal nanowire network layer, following (a)-(e) of concrete grammar:
(a) depositing metal films layer on the clean surface of described first layer metal sull;
(b) by the high polymer nano network of fibers of electrostatic spinning technique in described metal film layer surface preparative chemistry stable in properties,---first layer metal sull---metal film layer---the high polymer nano network of fibers lamination that obtains stacking transparent substrates from bottom to top;
C () is to above-mentioned transparent substrates---first layer metal sull---metal film layer---high polymer nano network of fibers laminated construction carries out Low Temperature Thermal annealing, make high polymer and metal film surfaces close contact, thus form the mask of high polymer nano network of fibers;
D () for mask with described high polymer nano network of fibers, utilizes corrosion of metals liquid corrosion to carve and removes not by metal that described high polymer nano network of fibers is covered;
E () selects suitable solvent clean to remove described high polymer nano network of fibers, namely obtain the metal nanowire network layer with high polymer network similar geometry shape;
Step 4, in above-mentioned transparent substrates---first layer metal sull---second layer metal sull prepared by metal nano spider lines, obtain described stacked laminated transparent electrode.
4. method according to claim 3, is characterized in that: in described method step 1, and described transparent substrates is the transparent substrates of rigidity or flexibility; The thickness of described transparent substrates is 0.1mm-5mm.
5. method according to claim 3, it is characterized in that: in described method step 2, described first layer metal sull is made up of following at least one material: other transparent oxides of aluminium oxide, zinc oxide, indium oxide, tin oxide, gallium oxide and titanium oxide and same nature;
The thickness of described first layer metal sull is 5nm-50nm.
6. method according to claim 3, is characterized in that: in described method step 3 (a), and the preparation method of described metal film layer is physical vaporous deposition or plating and chemical plating method;
Described metal is selected from following at least one: nickel, chromium, aluminium, copper, silver, gold, platinum and their alloy;
The thickness of described metal film layer is 20nm-200nm;
In described method step 3 (b), described high polymer is selected from following at least one: polyvinyl alcohol, polyoxyethylene, PLA, polymethyl methacrylate, polyacrylonitrile, polyurethane, polystyrene and polyvinylpyrrolidone;
In described method step 3 (b), the technological parameter of described electrostatic spinning is: spinning voltage is 3kV-50kV, and spinning nozzle is 5cm-50cm to the distance of collecting plate, and the mass concentration of spinning solution is 6%-15%;
Diameter continuously adjustabe in the scope of 100nm-2000nm of the high polymer nano fiber prepared;
In described method step 3 (c), described Low Temperature Thermal annealing adopts the heating of baking oven, hot plate or adopts solution vapor heating to carry out; The temperature of described Low Temperature Thermal annealing is 50-150 DEG C, and the time is 0.5-30min;
In described method step 3 (d), described corrosion of metals liquid is by solute and solvent composition, described solute is selected from following at least one: ferric nitrate, iron chloride, potassium bichromate, potassium cyanide, sulfate of ammoniac, hydrogen peroxide, hydrochloric acid, nitric acid, acetic acid and ammonia, described solvent for can dissolve above-mentioned solute arbitrarily, but can not dissolve the solvent of described high polymer nano fiber;
In described method step 3 (e), the described solvent for removing high polymer nano fiber is low toxicity and the low cost solvent that can dissolve described high polymer nano fiber;
Width continuously adjustabe between 60nm-1600nm of the metal nanometer line of gained after the described operation of described method step 3 (e) completes;
Described metal nanowire network layer is made up of random distribution or the metal nanometer line with rule orientating.
7. method according to claim 3, it is characterized in that: in described method step 4, described second layer metal sull is made up of doping transparent metal oxide, and described doping transparent metal oxide is selected from following at least one: Zinc-aluminium, indium tin oxide, fluorine tin-oxide, indium-zinc oxide and indium gallium zinc oxide;
The thickness of described second layer metal sull is 50nm-200nm.
8. a photoelectric device, is characterized in that: described photoelectric device comprises the stacked laminated transparent electrode described in claim 1 or 2.
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