CN105355675A - Preparation method for high-haze composite transparent conductive electrode - Google Patents
Preparation method for high-haze composite transparent conductive electrode Download PDFInfo
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- CN105355675A CN105355675A CN201510779814.4A CN201510779814A CN105355675A CN 105355675 A CN105355675 A CN 105355675A CN 201510779814 A CN201510779814 A CN 201510779814A CN 105355675 A CN105355675 A CN 105355675A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/022433—Particular geometry of the grid contacts
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- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
- H01L31/1888—Manufacture of transparent electrodes, e.g. TCO, ITO methods for etching transparent electrodes
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Abstract
The invention discloses a preparation method for a high-haze composite transparent conductive electrode. The method comprises the following steps that (1) a cracking liquid is prepared; (2) a cracking template is prepared; (3) a metal film is deposited; (4) a cracking template is removed; (5) a metal oxide is deposited; (6) an etching liquid is prepared; and (7) a composite film is etched to obtain the high-haze composite transparent conductive electrode. The electrode prepared by the method is higher in the haze, can effectively scatter incident light, greatly enhances light absorption of a film cell semiconductor layer, increases the short-circuit light current density, and finally improves the photoelectric conversion efficiency of a solar cell; and in addition, the composite electrode also has the advantages including low surface resistance, higher light transmittance and high environmental stability.
Description
Technical field
The invention belongs to transparency conductive electrode preparing technical field, be specifically related to a kind of preparation method of haze composite transparent conductive electrode.
Background technology
Before electrically conducting transparent, electrode is solar cell extremely important part, and to the short circuit current of solar cell, fill factor, curve factor etc. have significant impact.In general, transparency conductive electrode refers to and is greater than 80% to the transmissivity of the spectrum of lambda1-wavelength scope between 380nm to 780nm, and resistivity is lower than 10
-3the membrane electrode of Ω cm.Badeker reported first translucent conduction CdO material in 1907.Until World War II, transparent conductive film material just obtains enough attention and application.Nowadays, transparent conductive film material (as ITO (Indiumtinoxide), FTO (fluorine-dopedtinoxide)) is widely used in flat panel display, in intelligent glass and solar cell.From physical angle, the light transmission of material and conductivity are a pair basic contradictions.Material will possess a good conductivity, must have higher carrier concentration and higher carrier mobility simultaneously, but the charge carrier of higher concentration can improve the absorptivity of material to light by absorb photons, thus reduces its transmissivity.From CdO, ITO to AZO (Al-dopedZnO); From metallic film to thin polymer film; From one-component to multicomponent material; The research of transparent conductive film is launched around this contradiction always.Metal oxide ITO has higher light transmission rate and lower resistivity in visible region, be the focus of transparency conductive electrode investigation and application in the past over 50 years always.But stable not and ITO Surface Texture is difficult to prepare and limits its use on the solar cell to improve its mist degree etc. in the plasma when in crisp frangible, the ITO of ITO matter, high, the ITO of phosphide element price is applied to solar cell.Compared with ITO, the photoelectric properties of AZO film are suitable, and have nontoxic, be easy to realize doping, be easy to etching (to improve mist degree), the advantage such as chemical stability high, aboundresources, low price in hydrogen plasma, become study hotspot.
In recent years along with the development of nanometer new material and new construction, a frontier of transparency conductive electrode developing is two-dimensional nano new material, with structural membrane electrode, such as high polymer conductive film, carbon nano-tube film, graphene film, nano metal line film and metal grill film.The conductivity of high polymer conductive film itself is not fine; Graphene film has well flexible and high carrier mobility, but volume production technology is not yet ripe; Carbon nano-tube film needs comparatively big L/D ratio, and the Ohmic resistance problem between the dispersed and carbon pipe of carbon pipe limit film face in conductivity; Although metal nanowire film adopts liquid phase method to reduce costs, dispersed metal nanometer line is also difficult problem, and the contact resistance of metal nanometer line and substrate or active layer and adhesion problem thereof are difficult to solve.Transparent conductive film, except excellent conductivity, also needs excellent light transmission, the ratio (σ of photoconductivity
dc/ σ
opt, σ
dcdetermining electrode surface resistance, σ
optdetermine film light transmitance) the good photoelectric properties describing transparent conductive film.Research shows: the ratio of general carbon nano-tube photoconductivity is 6 ~ 14, and Graphene is ~ 70, ITO is 120-200, and nanometer metallic silver line electrode is 215, and metal grid electrode can reach higher.This shows that metal grill has excellent conductivity and light transmission.In addition, metal grid electrode also has excellent adhesive force, good profile pattern and stronger resistance to rich song, and thus metal grid electrode will become the favourable competitor of ITO.But the mist degree of metal grid electrode is very little, solar cell transparency conductive electrode used then requires certain mist degree, therefore needs to take measures to improve its mist degree.
In sum, single transparent electrode always has some defects, which has limited its application.In order to meet the demands, we compensate its shortcoming by the mode of electrode compound, keep respective advantage simultaneously.Such as, the compound of metal silver nanowires (AgNW) and Graphene, the Graphene covered on nano silver wire has completely cut off nano silver wire and external environment, thus improves the environmental stability of nano silver wire, and the conductivity of nano silver wire excellence makes this combination electrode conductivity splendid.Metal grill photoelectric properties are good but mist degree is very low, and thinner textured metal oxide mist degree is high but photoelectric properties are not good; Thus, we expect the compound by metal grill and metal oxide, realize preferably translucidus, less resistance and higher mist degree, thus improve the photoelectric conversion efficiency of solar cell.
Summary of the invention
First object of the present invention is the preparation method providing a kind of haze composite transparent conductive electrode, this preparation method is by the metal oxide compound of metal grill and Surface Texture, can prepare that sheet resistance is low, light transmittance and the high front electrode of mist degree, the efficiency of solar cell can be improved, be applicable to large area and produce.
The present invention also aims to provide the haze composite transparent conductive electrode adopting the preparation method of above-mentioned haze composite transparent conductive electrode to make, this haze composite transparent conductive circuit electrode surface resistance is low, light transmittance and mist degree high, and there is good machinery and environmental stability.
First object of the present invention is achieved by the following technical solution: a kind of preparation method of haze composite transparent conductive electrode, comprises the following steps:
(1) modulation be full of cracks liquid: adopt high-molecular organic material to be modulated into be full of cracks liquid;
(2) make be full of cracks template: get substrate, adopt be full of cracks liquid to chap uniformly film at deposited on substrates one deck, described be full of cracks film exposure cracking forms be full of cracks template;
(3) depositing metal films: adopt magnetron sputtering method to deposit the metallic film of one deck densification in be full of cracks template;
(4) be full of cracks template is removed: the be full of cracks template on substrate removed, substrate is formed metal grill transparent membrane;
(5) depositing metal oxide: at the metal oxide of metal grill transparent conductive film surface deposition one deck densification, obtain low haze composite transparent conductive electrode;
(6) etching liquid is prepared: adopt glacial acetic acid, concentrated hydrochloric acid and deionized water to make etching liquid;
(7) etch laminated film: after being soaked in etching liquid by low haze composite transparent conductive electrode, after taking out cleaning, namely obtain haze composite transparent conductive electrode.
Further, the preparation method of above-mentioned haze composite transparent conductive electrode, specifically comprises the following steps:
(1) modulation be full of cracks liquid: some high-molecular organic materials are modulated into solution, obtain be full of cracks liquid;
(2) be full of cracks template is made: be full of cracks liquid spin-coating method or Meyer rod method to be chapped uniformly film at deposited on substrates one deck, and the condition such as control temperature, humidity, make be full of cracks film exposure cracking form the template that chaps;
(3) depositing metal films: adopt magnetron sputtering to deposit the metallic film of one deck densification in be full of cracks template;
(4) be full of cracks template is removed: the be full of cracks template on substrate removed, substrate is formed metal grill transparent membrane;
(5) depositing metal oxide: at the metal oxide of metal grill transparent membrane surface deposition one deck densification, obtain low haze composite transparent conductive electrode;
(6) etching liquid is prepared: the concentration ratio regulating glacial acetic acid, concentrated hydrochloric acid and water, obtains etching liquid;
(7) etch laminated film: after low haze composite transparent conductive electrode is dipped in etching liquid certain hour, take out cleaning, obtain haze composite transparent conductive electrode and namely prepare composite transparent conductive electrode based on metal grill and Surface Texture metal oxide.
In the preparation method of above-mentioned haze composite transparent conductive electrode:
High-molecular organic material described in step of the present invention (1) is egg white solution, the modulated process of described be full of cracks liquid is: get egg white solution, add deionized water, centrifugal after ultrasonic dissolution, remove lower floor's impurity, obtain be full of cracks liquid, wherein the volume ratio of deionized water and egg white solution is 0 ~ 2:1, time centrifugal, centrifuge speed is 2000 ~ 4000r/min, and centrifugation time is 3 ~ 10min.
Further, the be full of cracks liquid described in step of the present invention (1) is prepared by following method: get egg white solution, add deionized water, and the volume ratio of deionized water and egg white solution is preferably 0 ~ 2:1; Ultrasonic cleaning (time is 1 ~ 30min preferably) is preferably used egg white solution and deionized water fully to be dissolved each other; Preferably use centrifuge (rotating speed is 2000 ~ 4000r/min preferably) centrifugal 3 ~ 10min, remove lower floor's impurity, obtain be full of cracks liquid.
Substrate described in step of the present invention (2) can choose different materials, as transparent materials such as PETG (PET), glass, dimethyl silicone polymer (PDMS), polyimides (PI) or polytetrafluoroethylene (PTFE).
Be full of cracks liquid is adopted in step of the present invention (2) to be Meyer rod method or spin-coating method in chap the uniformly method of film of deposited on substrates one deck; When described be full of cracks film exposure cracking forms be full of cracks template, control temperature condition is 30 ~ 70 DEG C, and damp condition is 20 ~ 40%, and the be full of cracks time is 5 ~ 60min.
Adopt the detailed process of Meyer rod method preferably: the drop that will chap is on substrate, and thickness is preferably 0.5 ~ 3mm, the Meyer rod speed of service is preferably 0.5 ~ 15cm/s, and the thickness of be full of cracks film is 10 ~ 50 μm.
Adopt the detailed process of spin-coating method preferably: the drop that will chap is on substrate, with spin coater with the speed continuous service 5 ~ 20s of 100 ~ 300r/min, continue spin coating 0 ~ 60s with the rotating speed of 500 ~ 1000r/min again, namely obtain be full of cracks film, the thickness of described be full of cracks film is 2 ~ 20 μm.
When adopting magnetron sputtering method to deposit the metallic film of one deck densification in step of the present invention (3) in be full of cracks template, sputtering power is preferably 100 ~ 200W, magnetic control chamber indoor temperature is preferably 20 ~ 25 DEG C, and be full of cracks template surface temperature is preferably 30 ~ 60 DEG C; Described in step (3), the thickness of metallic film is preferably 50 ~ 250nm; In described metallic film, metal is preferably one or more in silver, copper, aluminium, gold and nickel.
Preferably adopt WATER-WASHING METHOD the be full of cracks template on substrate to be removed in step (4), the mesh size that substrate is formed metal grill transparent membrane is preferably 5 ~ 150 μm, and metal line-width is preferably 0.5 ~ 12 μm.
The detailed process that be full of cracks template on substrate is removed is by employing WATER-WASHING METHOD: metallic film is cooled to room temperature, and use current to wash away template, the complexity that can be combined with substrate according to template suitably regulates the speed of current.
Adopt magnetron sputtering method at the metal oxide of metal grill transparent conductive film surface deposition one deck densification in step of the present invention (5), described metal oxide is preferably aluminium-doped zinc oxide AZO, its thickness is preferably 400 ~ 1000nm, the power of magnetron sputtering is preferably 100 ~ 200W, during magnetron sputtering, chamber indoor temperature is preferably 20 ~ 200 DEG C, and the surface temperature of metal grill transparent membrane is preferably 30 ~ 200 DEG C.
Described in step of the present invention (6), the volume ratio of glacial acetic acid, concentrated hydrochloric acid and deionized water is preferably 0.5 ~ 1.5:1 ~ 3:200.
Because of concentrated hydrochloric acid highly volatile, the contact of concentrated hydrochloric acid and air in process for preparation, to be reduced as far as possible, thus reduce its volatilization, make formula more accurate.
After the low haze composite transparent conductive electrode of preparation in step (5) preferably being soaked 10 ~ 30s in etching liquid in step of the present invention (7), rapid taking-up also adopts washed with de-ionized water clean, namely obtains haze composite transparent conductive electrode after drying.
The dry deionized water adopting nitrogen gun or purification of compressed air rifle to dry up remained on surface.
Principle of the present invention is: be full of cracks liquid is coated in substrate surface, and the moisture in be full of cracks sol solutions volatilizees in a heated condition, and shrink when be full of cracks colloidal sol forms gel film and create internal stresses release, thus crack, have a close grain small and dense collection.After magnetron sputtering plating, sample surfaces cover by metal film, use deionized water rinsing sample, remove be full of cracks template, now formed a continuous print metalolic network.And then with magnetron sputtering layer of metal oxide, carry out etching certain hour with etching liquid, thus define the composite transparent conductive electrode based on metal grill and Surface Texture metal oxide.Metal grill can reduce sheet resistance, and Surface Texture metal oxide can increase mist degree, regulate the inhomogeneities of metal grill distribution of resistance, and the two complements each other, and promotes the collection of charge carrier and transports, being conducive to the raising of conversion efficiency of solar cell.
Second object of the present invention is achieved through the following technical solutions: adopt the haze composite transparent conductive electrode that the preparation method of above-mentioned haze composite transparent conductive electrode makes.
Compared with prior art, tool of the present invention has the following advantages:
(1) the present invention is on the metal grill of be full of cracks template synthesis, and depositing metal oxide also etches, and effectively improves mist degree and the conductivity of electrode;
(2) the present invention is by the compound by metal grill and metal oxide, effectively improves the inhomogeneities of metal grill sheet resistance distribution;
(3) the present invention easily regulates metal mesh structure, thus realizes the balance of electrode light transmission and conductivity;
(4) what the present invention proposed prepares based on metal grill and Surface Texture metal oxide the contenders that composite transparent conductive electrode is INVENTIONConventional metal-oxide transparency conductive electrode, the conversion efficiency of solar cell can be improved, indirectly reduce the production cost of battery;
(5) the composite transparent conductive electrode that the method is made has higher mist degree, to incident light, there is good scattering power, the very big enhanced film cell semiconductor layer of energy to the absorption of light, and then increases circuit photocurrent density, the final photoelectric conversion efficiency improving solar cell;
(6) combination electrode cost relative moderate of the present invention, productive rate is higher, is easy to industrialization, and the electrode simultaneously made has that good conductivity, light transmittance are high, mist degree high, and expectability improves carrier collection efficiency, improves the conversion efficiency of solar cell.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure preparing composite transparent conductive electrode in embodiment of the present invention 1-4 based on metal grill and Surface Texture metal oxide, wherein (1) represents the deposition of be full of cracks liquid, (2) formation of be full of cracks film is represented, (3) formation of be full of cracks template is represented, (4) deposition of metallic film and the removal of be full of cracks template is represented, the formation of composite transparent conductive electrode after deposition (6) the expression corrosive liquid etching of formation metal grill (5) expression metal oxide.In figure, 1 represents substrate, and 2 represent metal grill, 3 presentation surface textured metal oxides;
Fig. 2 is the light microscope figure of the metal grill made in the embodiment of the present invention 1, and amplify 50 times, length of the scale shown in figure is 100 microns;
Fig. 3 is the SEM figure after AZO (being distributed in metal grill) the etching 30S of 1000nm (thickness) in the embodiment of the present invention 1, amplifies 5000 times;
Fig. 4 is the SEM figure of the composite transparent conductive electrode prepared based on metal grill and Surface Texture metal oxide in the embodiment of the present invention 1, amplifies 2000 times;
Fig. 5 is light transmittance in the embodiment of the present invention 1 after metal grill surface coverage textured metal oxide and sheet resistance figure;
Fig. 6 is the mist degree comparison diagram in the embodiment of the present invention 1 before and after metal grill surface coverage textured metal oxide.
Embodiment
Embodiment 1
As shown in Figure 1, present embodiments provide a kind of preparation method of haze composite transparent conductive electrode, namely the preparation method of composite transparent conductive electrode is namely prepared based on metal grill and Surface Texture metal oxide, wherein (1) represents the deposition of be full of cracks template liquid, (2) formation of be full of cracks template is represented, (3) deposition of metallic film is represented, (4) removal of be full of cracks template is represented, also be the formation of metal grill, (5) deposition of metal oxide is represented, (6) etching of metal oxide is represented, also be the formation of metal grill and Surface Texture metal oxide composite transparent conductive electrode, wherein: 1 represents wire netting winding thread, 2 represent mesh, 3 presentation surface textured metal oxides.
The detailed process of each step is as follows:
(1) chap the preparation of liquid and the deposition of be full of cracks film
Take egg white solution as raw material, add deionized water (wherein the volume ratio of deionized water and egg white solution is 1:2), ultrasonic 10min in egg white solution, centrifuge, with the centrifugation 5min of 3000r/min, removes lower floor's impurity, obtains clear pale yellow look be full of cracks liquid.Then adopt spin-coating method to deposit be full of cracks film on a glass substrate, specifically: on substrate, drip be full of cracks liquid, adopt spin coater to continue 5s with the speed of 100r/min, then continue with the rotating speed of 600r/min the be full of cracks film that spin coating 20s acquisition thickness is about 15 μm.
(2) formation of the template that chaps
Lain in by sample in (one) (heating station surface temperature is set to 50 DEG C) on heating station, damp condition is 30%, and heating 10min, can obtain be full of cracks template.
(3) magnetron sputtering deposition metallic film
What the present embodiment deposited is that thickness of metal film is about 200nm, the metal adopted is silver, and other metal outside desilver such as copper, aluminium, gold, silver nickel alloy etc. are also feasible, regulates magnetron sputtering power to be 200W, magnetic control chamber indoor temperature is about 25 DEG C, and sample surface temperature is about 60 DEG C.
(4) remove be full of cracks template, form metal grill
The method that be full of cracks template adopts current to rinse is removed, specifically: the sample of depositing metal films is cooled to room temperature, the method using current to rinse removes template, suitably water velocity is regulated according to removal complexity, the mesh size of the metal grill transparent conductive film obtained is about 70 μm, metal line-width is about 5 μm, as shown in Figure 2.
(5) magnetron sputtering deposition metal-oxide film
By the sample deposition metal-oxide film obtained in (four), the metal-oxide film deposited in the present embodiment is AZO, and thickness is about 1000nm, and adjustment magnetron sputtering power is 200W, magnetic control chamber indoor temperature is about 200 DEG C, and sample surface temperature is about 200 DEG C.
(6) preparation of etching liquid and the etching of metal oxide
The formula of etching liquid is glacial acetic acid: concentrated hydrochloric acid: the volume ratio of deionized water is 0.5:1:200.Sample in (five) is dipped in etching liquid and takes out rapidly after 30s, AZO in metal grill etches the SEM figure after 30S as shown in Figure 3, namely haze composite transparent conductive electrode is obtained after deionized water cleaning down, compressor gun dry up, as shown in Figure 4, the preparation giving over to solar cell is saved.
The present embodiment has good photoelectric properties and higher mist degree based on composite transparent conductive electrode prepared by argent grid and Surface Texture metal oxide, as shwon in Figures 5 and 6, as can be seen from Figure 5, the resistance of sample 1 (i.e. the present embodiment make composite transparent conductive electrode) combination electrode is 10.40 Ω/sq, light transmission is 78.95%, and mist degree is 45.95%.Assisting by metal oxide, the resistance of electrode has had larger decline, and the resistance of sample 1 drops to about 10.40 Ω/sq from initial about 20.06 Ω/sq; The mist degree of electrode is greatly improved, and the mist degree of sample 1, from initial about 4.29%, is changed to about 45.95%.
Embodiment 2
Present embodiments provide and a kind ofly prepare the preparation method of composite transparent conductive electrode as shown in Figure 1 based on metal grill and Surface Texture metal oxide, wherein (1) represents the deposition of be full of cracks template liquid, (2) formation of be full of cracks template is represented, (3) deposition of metallic film is represented, (4) removal of be full of cracks template is represented, also be the formation of metal grill, (5) deposition of metal oxide is represented, (6) etching of metal oxide is represented, also be the formation of metal grill and Surface Texture metal oxide composite transparent conductive electrode, wherein: 1 represents wire netting winding thread, 2 represent mesh, 3 presentation surface textured metal oxides.
The detailed process of each step is as follows:
(1) chap the preparation of liquid and the deposition of be full of cracks film
With the egg white solution of egg for raw material, in egg white solution, add deionized water (wherein the volume ratio of deionized water and egg white solution is 0:1), ultrasonic 30min, centrifuge is with the centrifugation 10min of 2000r/min, remove lower floor's impurity, obtain clear pale yellow look be full of cracks liquid.Then employing spin-coating method deposits be full of cracks film on PI, specifically: on substrate, drip be full of cracks liquid, adopts spin coater to continue 10s with the speed of 300r/min, then continues with the rotating speed of 800r/min the be full of cracks film that spin coating 60s acquisition thickness is about 8 μm.
(2) formation of the template that chaps
Lain in by sample in (one) (heating station surface temperature is set to 30 DEG C) on heating station, relative humidity is 20%, and heating 30min, can obtain be full of cracks template.
(3) magnetron sputtering deposition metallic film
What the present embodiment deposited is that thickness of metal film is about 150nm, the metal adopted is silver, and other metal outside desilver such as copper, aluminium, gold, silver nickel alloy etc. are also feasible, regulates magnetron sputtering power to be 150W, magnetic control chamber indoor temperature is about 20 DEG C, and sample surface temperature is about 50 DEG C.
(4) remove be full of cracks template, form metal grill
The method that be full of cracks template adopts current to rinse is removed, specifically: the sample of depositing metal films is cooled to room temperature, the method using current to rinse removes template, suitably water velocity is regulated according to removal complexity, the mesh size of the metal grill transparent conductive film obtained is about 50 μm, and metal line-width is about 3 μm.
(5) magnetron sputtering deposition metal-oxide film
By the sample deposition metal-oxide film obtained in (four), the metal-oxide film deposited in the present embodiment is AZO, and thickness is about 600nm, and adjustment magnetron sputtering power is 150W, magnetic control chamber indoor temperature is about 100 DEG C, and sample surface temperature is about 100 DEG C.
(6) preparation of etching liquid and the etching of metal oxide
The formula of etching liquid is glacial acetic acid: concentrated hydrochloric acid: deionized water=1:1:200 (volume ratio).Sample in (five) is dipped in etching liquid and takes out rapidly after 20s, after deionized water cleaning down, compressor gun dry up, save the preparation giving over to solar cell.
The present embodiment has good photoelectric properties and higher mist degree based on composite transparent conductive electrode prepared by argent grid and Surface Texture metal oxide.
Embodiment 3
Present embodiments provide and a kind ofly prepare the preparation method of composite transparent conductive electrode as shown in Figure 1 based on metal grill and Surface Texture metal oxide, wherein (1) represents the deposition of be full of cracks template liquid, (2) formation of be full of cracks template is represented, (3) deposition of metallic film is represented, (4) removal of be full of cracks template is represented, also be the formation of metal grill, (5) deposition of metal oxide is represented, (6) etching of metal oxide is represented, also be the formation of metal grill and Surface Texture metal oxide composite transparent conductive electrode, wherein: 1 represents wire netting winding thread, 2 represent mesh, 3 presentation surface textured metal oxides.
The detailed process of each step is as follows:
(1) chap the preparation of liquid and the deposition of be full of cracks film
Take egg white solution as raw material, add deionized water (wherein the volume ratio of deionized water and egg white solution is 2:1), ultrasonic 5min in egg white solution, centrifuge, with the centrifugation 3min of 4000r/min, removes lower floor's impurity, obtains clear pale yellow look be full of cracks liquid.Then adopt spin-coating method to deposit be full of cracks film on a glass substrate, specifically: on substrate, drip be full of cracks liquid, adopt spin coater to continue 20s with the speed of 200r/min, then continue with the rotating speed of 1000r/min the be full of cracks film that spin coating 10s acquisition thickness is about 5 μm.
(2) formation of the template that chaps
Lain in by sample in (one) (heating station surface temperature is set to 60 DEG C) on heating station, relative humidity is 30%, and heating 50min, can obtain be full of cracks template.
(3) magnetron sputtering deposition metallic film
What the present embodiment deposited is that thickness of metal film is about 250nm, the metal adopted is silver, and other metal outside desilver such as copper, aluminium, gold, silver nickel alloy etc. are also feasible, regulates magnetron sputtering power to be 100W, magnetic control chamber indoor temperature is about 25 DEG C, and sample surface temperature is about 45 DEG C.
(4) remove be full of cracks template, form metal grill
The method that be full of cracks template adopts current to rinse is removed, specifically: the sample of depositing metal films is cooled to room temperature, the method using current to rinse removes template, suitably water velocity is regulated according to removal complexity, the mesh size of the metal grill transparent conductive film obtained is about 150 μm, and metal line-width is about 10 μm.
(5) magnetron sputtering deposition metal-oxide film
By the sample deposition metal-oxide film obtained in (four), the metal-oxide film deposited in the present embodiment is AZO, and thickness is about 400nm, and adjustment magnetron sputtering power is 100W, magnetic control chamber indoor temperature is about 20 DEG C, and sample surface temperature is about 30 DEG C.
(6) preparation of etching liquid and the etching of metal oxide
The formula of etching liquid is glacial acetic acid: concentrated hydrochloric acid: deionized water=1:2:200 (volume ratio).Sample in (five) is dipped in etching liquid and takes out rapidly after 10s, after deionized water cleaning down, compressor gun dry up, save the preparation giving over to solar cell.
Because of concentrated hydrochloric acid highly volatile, the contact of concentrated hydrochloric acid and air in process for preparation, to be reduced as far as possible, thus reduce its volatilization, make formula more accurate.
The present embodiment has good photoelectric properties and higher mist degree based on composite transparent conductive electrode prepared by argent grid and Surface Texture metal oxide.
Embodiment 4
Present embodiments provide and a kind ofly prepare the preparation method of composite transparent conductive electrode as shown in Figure 1 based on metal grill and Surface Texture metal oxide, wherein (1) represents the deposition of be full of cracks template liquid, (2) formation of be full of cracks template is represented, (3) deposition of metallic film is represented, (4) removal of be full of cracks template is represented, also be the formation of metal grill, (5) deposition of metal oxide is represented, (6) etching of metal oxide is represented, also be the formation of metal grill and Surface Texture metal oxide composite transparent conductive electrode, wherein: 1 represents wire netting winding thread, 2 represent mesh, 3 presentation surface textured metal oxides.
The detailed process of each step is as follows:
(1) chap the preparation of liquid and the deposition of be full of cracks film
Take egg white solution as raw material, add deionized water (wherein the volume ratio of deionized water and egg white solution is 1:1), ultrasonic 1min in egg white solution, centrifuge, with the centrifugation 8min of 3500r/min, removes lower floor's impurity, obtains clear pale yellow look be full of cracks liquid.Then adopt Meyer rod method to deposit be full of cracks film on a glass substrate, detailed process is: the drop that will chap is on substrate, and thickness is about 2mm, and Meyer rod pace is about 2cm/s, and the thickness of be full of cracks film is about 20 μm.
(2) formation of the template that chaps
Lain in by sample in (one) (heating station surface temperature is set to 70 DEG C) on heating station, relative humidity is 40%, and heating 10min, can obtain be full of cracks template.
(3) magnetron sputtering deposition metallic film
What the present embodiment deposited is that thickness of metal film is about 50nm, the metal adopted is gold, and other metal in addition to gold such as copper, aluminium, silver-nickel etc. are also feasible, and adjustment magnetron sputtering power is 100W, magnetic control chamber indoor temperature is about 25 DEG C, and sample surface temperature is about 35 DEG C.
(4) remove be full of cracks template, form metal grill
The method that be full of cracks template adopts current to rinse is removed, specifically: the sample of depositing metal films is cooled to room temperature, the method using current to rinse removes template, suitably water velocity is regulated according to removal complexity, the mesh size of the metal grill transparent conductive film obtained is about 100 μm, and metal line-width is about 2 μm.
(5) magnetron sputtering deposition metal-oxide film
By the sample deposition metal-oxide film obtained in (four), the metal-oxide film deposited in the present embodiment is AZO, and thickness is about 800nm, and adjustment magnetron sputtering power is 150W, magnetic control chamber indoor temperature is about 180 DEG C, and sample surface temperature is about 180 DEG C.
(6) preparation of etching liquid and the etching of metal oxide
The formula of etching liquid is glacial acetic acid: concentrated hydrochloric acid: deionized water=1.5:1:200 (volume ratio).Sample in (five) is dipped in etching liquid and takes out rapidly after 25s, after deionized water cleaning down, nitrogen gun dry up, save the preparation giving over to solar cell.
The present embodiment has good photoelectric properties and higher mist degree based on composite transparent conductive electrode prepared by argent grid and Surface Texture metal oxide.
Above-described embodiment is the present invention's preferably execution mode, but embodiments of the present invention are not restricted to the described embodiments, and such as transparent conductive metal oxide is except AZO, also can be the metal oxide that other is easy to etch; The etching liquid of metal oxide, except the mixture of glacial acetic acid and concentrated hydrochloric acid, also can be any one in them, or other acid, as nitric acid etc.; Metal grill in addition to silver, also can be one or more in gold, copper, silver-nickel; The parameter of magnetron sputtering also can carry out suitable adjustment because machine is different.Other are any do not deviate from Spirit Essence of the present invention and principle under do change, modification, substitute, combine, simplify, all should be the substitute mode of equivalence, be included in protection scope of the present invention.
Claims (10)
1. a preparation method for haze composite transparent conductive electrode, is characterized in that comprising the following steps:
(1) modulation be full of cracks liquid: adopt high-molecular organic material to be modulated into be full of cracks liquid;
(2) make be full of cracks template: get substrate, adopt be full of cracks liquid to chap uniformly film at deposited on substrates one deck, described be full of cracks film exposure cracking forms be full of cracks template;
(3) depositing metal films: adopt magnetron sputtering method to deposit the metallic film of one deck densification in be full of cracks template;
(4) be full of cracks template is removed: the be full of cracks template on substrate removed, substrate is formed metal grill transparent membrane;
(5) depositing metal oxide: at the metal oxide of metal grill transparent conductive film surface deposition one deck densification, obtain low haze composite transparent conductive electrode;
(6) etching liquid is prepared: adopt glacial acetic acid, concentrated hydrochloric acid and deionized water to make etching liquid;
(7) etch laminated film: after being soaked in etching liquid by low haze composite transparent conductive electrode, after taking out cleaning, namely obtain haze composite transparent conductive electrode.
2. the preparation method of haze composite transparent conductive electrode according to claim 1, it is characterized in that: the high-molecular organic material described in step (1) is egg white solution, the modulated process of described be full of cracks liquid is: get egg white solution, add deionized water, centrifugal after ultrasonic dissolution, remove lower floor's impurity, obtain be full of cracks liquid, wherein the volume ratio of deionized water and egg white solution is 0 ~ 2:1, and time centrifugal, centrifuge speed is 2000 ~ 4000r/min, and centrifugation time is 3 ~ 10min.
3. the preparation method of haze composite transparent conductive electrode according to claim 1, is characterized in that: substrate described in step (2) is transparent material polyethylene terephtalate, glass, polydimethylsiloxane, polyimides PI or polytetrafluoroethylene PTFE.
4. the preparation method of haze composite transparent conductive electrode according to claim 1, is characterized in that: adopt in step (2) be full of cracks liquid to be Meyer rod method or spin-coating method in chap the uniformly method of film of deposited on substrates one deck; When described be full of cracks film exposure cracking forms be full of cracks template, control temperature condition is 30 ~ 70 DEG C, and damp condition is 20 ~ 40%, and the be full of cracks time is 5 ~ 60min.
5. the preparation method of haze composite transparent conductive electrode according to claim 1, it is characterized in that: when adopting magnetron sputtering method to deposit the metallic film of one deck densification in step (3) in be full of cracks template, sputtering power is 100 ~ 200W, magnetic control chamber indoor temperature is 20 ~ 25 DEG C, and be full of cracks template surface temperature is 30 ~ 60 DEG C; Described in step (3), the thickness of metallic film is 50 ~ 250nm; In described metallic film, metal is one or more in silver, copper, aluminium, gold and nickel.
6. the preparation method of haze composite transparent conductive electrode according to claim 1, it is characterized in that: in step (4), adopt WATER-WASHING METHOD the be full of cracks template on substrate to be removed, the mesh size that substrate is formed metal grill transparent membrane is 5 ~ 150 μm, and metal line-width is 0.5 ~ 12 μm.
7. the preparation method of haze composite transparent conductive electrode according to claim 1, it is characterized in that: in step (5), adopt magnetron sputtering method at the metal oxide of metal grill transparent conductive film surface deposition one deck densification, described metal oxide is aluminium-doped zinc oxide AZO, its thickness is 400 ~ 1000nm, the power of magnetron sputtering is 100 ~ 200W, during magnetron sputtering, chamber indoor temperature is 20 ~ 200 DEG C, and the surface temperature of metal grill transparent membrane is 30 ~ 200 DEG C.
8. the preparation method of haze composite transparent conductive electrode according to claim 1, is characterized in that: described in step (6), the volume ratio of glacial acetic acid, concentrated hydrochloric acid and deionized water is 0.5 ~ 1.5:1 ~ 3:200.
9. the preparation method of haze composite transparent conductive electrode according to claim 1, it is characterized in that: after low haze composite transparent conductive electrode being soaked 10 ~ 30s in etching liquid in step (7), rapid taking-up also adopts washed with de-ionized water clean, namely obtains haze composite transparent conductive electrode after drying.
10. adopt the haze composite transparent conductive electrode that the preparation method of the haze composite transparent conductive electrode described in any one of claim 1-9 makes.
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