CN104124386A - Flexible conductive electrode and preparation method thereof - Google Patents

Flexible conductive electrode and preparation method thereof Download PDF

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Publication number
CN104124386A
CN104124386A CN201310157835.3A CN201310157835A CN104124386A CN 104124386 A CN104124386 A CN 104124386A CN 201310157835 A CN201310157835 A CN 201310157835A CN 104124386 A CN104124386 A CN 104124386A
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Prior art keywords
film
conductive electrode
stainless steel
thickness
compliant conductive
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周明杰
冯小明
陈吉星
王平
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Priority to CN201310157835.3A priority Critical patent/CN104124386A/en
Publication of CN104124386A publication Critical patent/CN104124386A/en
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates
    • H10K77/111—Flexible substrates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Abstract

The invention provides a flexible conductive electrode. The flexible conductive electrode comprises a stainless steel substrate, a mixed buffer layer and a conductive layer, all of which are orderly stacked on each other; the mixed buffer layer comprises a polyimide film and a silicon oxide film formed on the surface of the polyimide film. The flexible conductive electrode is excellent in stability. The invention also provides a preparation method of the flexible conductive electrode.

Description

Compliant conductive electrode and preparation method thereof
Technical field
The present invention relates to a kind of compliant conductive electrode and preparation method thereof.
Background technology
Organic electroluminescence device (OLED) uses ultra-thin glass conventionally, thin polymer film, sheet metal etc. are as flexible substrate, than more frivolous, the more impact-resistant advantage of having of glass substrate, and the preparation of flexible device can adopt volume to volume mode to produce, thereby reduces manufacturing cost significantly.
But stainless steel thin slice shows that roughness is larger conventionally, and its surface roughness Ra can reach more than 0.6 micron conventionally.General by stainless steel thin slice plated surface last layer silicon monoxide (SiO) film, as the surface roughness of flatness layer reduction stainless steel thin slice, then on this flatness layer, prepare conductive layer.Because SiO belongs to a kind of inorganic matter, in the time of preparation SiO, easily there is internal stress in blocked up film, thereby make stainless steel thin slice in the time carrying out bending, SiO film can produce slight crack, thereby destroys film integrity, produces pin hole and defect, make the conductive film on SiO surface destroyed, make the less stable of compliant conductive electrode.
Summary of the invention
Based on this, be necessary to provide good compliant conductive electrode of a kind of stability and preparation method thereof.
A kind of compliant conductive electrode, at the bottom of comprising the stainless steel lining stacking gradually, mix resilient coating and conductive layer, described mixing resilient coating comprises polyimide film and is formed at the silicon monoxide film on described polyimide film surface.
In an embodiment, the thickness at the bottom of described stainless steel lining is 0.05mm～0.2mm therein.
In an embodiment, the thickness of described polyimide film is 100nm～300nm therein, and the thickness of described silicon monoxide film is 200nm～800nm.
In an embodiment, the material of described conductive layer is selected from least one in indium tin oxide, indium-zinc oxide, aluminium zinc oxide and gallium zinc oxide therein.
In an embodiment, the material of described conductive layer is selected from least one in aluminium, silver and gold therein.
In an embodiment, described mixing resilient coating is 2～5 therein, and multiple mixing resilient coatings stack gradually.
A preparation method for compliant conductive electrode, comprises the following steps:
In vacuum coating system, by pyromellitic acid anhydride and 4,4, ' diaminodiphenyl ether is placed in respectively two crucibles, makes pyromellitic acid anhydride and 4,4 ' ratio of the evaporation rate of diaminodiphenyl ether is 1:0.8～1.2, at stainless steel lining basal surface deposition polyimide prepolymer film;
Under vacuum environment, by the bottom of described stainless steel lining and be deposited on the polyimide prepolymer film heating to 120 DEG C of described stainless steel lining basal surface～200 DEG C and carry out processed, make polyimide prepolymer film dehydration form polyimide film;
Surperficial evaporation at described polyimide film is prepared silicon monoxide film; And
Prepare conductive layer at described silicon monoxide film surface.
In an embodiment, the thickness of described polyimide film is 100nm～300nm therein, and the thickness of described silicon monoxide film is 200nm～800nm.
In an embodiment, described mixing resilient coating is 2～5 therein, and multiple mixing resilient coatings stack gradually.
In an embodiment, the thickness at the bottom of described stainless steel lining is 0.05mm～0.2mm therein.
Above-mentioned compliant conductive electrode and preparation method thereof, mixing resilient coating is set between stainless steel thin slice and conductive layer, mix the silicon monoxide film that resilient coating comprises polyimide film and is formed at polyimide film surface, silicon monoxide film can smooth stainless steel lining at the bottom of, reduce surface roughness, polyimide film can absorb the two-layer stress producing in bending being in contact with it, thereby avoid silicon monoxide film cracking, and then avoid the conductive layer that is formed on silicon monoxide film surface to produce the defects such as pin hole, thereby the stability of this compliant conductive electrode is better.
Brief description of the drawings
Fig. 1 is the structural representation of the compliant conductive electrode of an execution mode;
Fig. 2 is the preparation method's of the compliant conductive electrode of an execution mode flow chart;
Fig. 3 is the schematic diagram that compliant conductive electrode carries out flexibility test;
Fig. 4 is the sheet resistance change curve of the compliant conductive electrode prepared of embodiment 1 and comparative example under different number of flexings.
Embodiment
Below in conjunction with the drawings and specific embodiments, compliant conductive electrode and preparation method thereof is further illustrated.
Refer to Fig. 1, the compliant conductive electrode 100 of an execution mode comprises at the bottom of the stainless steel lining stacking gradually 10, mixes resilient coating 30 and conductive layer 50.
At the bottom of stainless steel lining, 10 material is the stainless steel such as American Standard AISI304, AISI303 type.At the bottom of stainless steel lining, 10 thickness is 0.05mm～0.2mm.Preferably, at the bottom of stainless steel lining, 10 surface roughness (Ra) is less than 0.6 μ m.
Mix silicon monoxide (SiO) film 34 that resilient coating 30 comprises polyimides (PI) film 32 and is formed at polyimide film surface.The thickness of polyimide film 32 is 100nm～30nm, and the thickness of silicon monoxide film 34 is 200nm～800nm.
Further, mixing resilient coating 30 is 2～5, and multiple mixing resilient coatings 30 stack gradually, and forms as PI/SiO/PI/SiO/PI/SiO/ ... the structure of/SiO.Thereby the stress producing in the time that the polyimide film 32 between two silicon monoxide films 34 can absorb the silicon monoxide film 34 that is positioned at its both sides in bending avoids silicon monoxide film 34 to ftracture.
Conductive layer 50 is formed at and mixes resilient coating 30 surfaces.The material of conductive layer 50 is conductive oxide or metal.Conductive oxide is selected from least one in indium tin oxide (ITO), indium-zinc oxide (IZO), aluminium zinc oxide (AZO) and gallium zinc oxide (GZO).Metal is selected from least one in aluminium (Al), silver (Ag) and gold (Au).The thickness of conductive layer 50 is 70nm～200nm.
Above-mentioned compliant conductive electrode 100, at the bottom of stainless steel lining 10 and conductive layer 50 between arrange mix resilient coating 30, mix the silicon monoxide film 34 that resilient coating 30 comprises polyimide film 32 and is formed at polyimide film 32 surfaces, silicon monoxide film 34 can smooth stainless steel lining at the bottom of 10, reduce surface roughness, polyimide film 32 can absorb the two-layer stress producing in bending being in contact with it, thereby avoid silicon monoxide film 34 to ftracture, and then avoid the conductive layer 50 that is formed on silicon monoxide film 34 surfaces to produce the defects such as pin hole, thereby the stability of this compliant conductive electrode 100 is better.
Please refer to Fig. 2, the preparation method of the compliant conductive electrode 100 of an execution mode, comprises the following steps:
Step S110, in vacuum coating system, by pyromellitic acid anhydride (PMDA) and 4,4 ' diaminodiphenyl ether (ODA) is placed in respectively two crucibles, make pyromellitic acid anhydride and 4,4 ' ratio of the evaporation rate of diaminodiphenyl ether is 1:0.8～1.2, at stainless steel lining basal surface deposition polyimide prepolymer film.
At the bottom of stainless steel lining, 10 material is American Standard AISI304, the conventional stainless steel in the industry such as AISI303 type.At the bottom of stainless steel lining, 10 thickness is 0.05mm～0.2mm.Preferably, at the bottom of stainless steel lining, 10 surface roughness (Ra) is less than 0.6 μ m.
In present embodiment, at the bottom of stainless steel lining, 10 first carry out pre-treatment before use, and pre-treatment comprises: by 10 being placed in the deionized water that contains washing agent and carrying out ultrasonic cleaning at the bottom of stainless steel lining, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.
In present embodiment, the vacuum degree in vacuum coating system is 1 × 10 -3pa～1 × 10 -5pa.
Preferably, the evaporation rate of pyromellitic acid anhydride is 0.1nm/s～1nm/s.
Preferably, by controlling temperature control pyromellitic acid anhydride and 4, the 4 ' evaporation rate of diaminodiphenyl ether of crucible.
In present embodiment, the thickness of polyimide prepolymer film is 100nm～300nm.
Step S120, under vacuum environment, by the bottom of stainless steel lining 10 and be deposited on the polyimide prepolymer film heating to 120 DEG C on 10 surfaces at the bottom of stainless steel lining～200 DEG C and carry out processed, make polyimide prepolymer film dehydration form polyimide film.
In present embodiment, the time of processed is 1 hour～3 hours.
In present embodiment, processed is carried out in vacuum heater, in step S120, first by the bottom of stainless steel lining 10 and be deposited at the bottom of stainless steel lining the polyimide prepolymer film of 10 surface depositions and transfer to from vacuum coating system and carry out processed in vacuum heater.
Step S130, prepare silicon monoxide film 34 at the surperficial evaporation of polyimide film 32.
In present embodiment, the thickness of silicon monoxide film 34 is 200nm～800nm.
Preferably, silicon monoxide film 34 is prepared by evaporation, and evaporation is 1 × 10 in vacuum degree -3pa～1 × 10 -5under Pa, carry out, evaporation speed is 0.2nm/s～2nm/s.
Silicon monoxide film 34 and polyimide film 32 compositions mix resilient coating 30.Preferably, mixing resilient coating 30 is 2～5, and multiple mixing resilient coatings 30 stack gradually, and forms as PI/SiO/PI/SiO/PI/SiO/ ... the structure of/SiO.Thereby the stress producing in the time that the polyimide film 32 between two silicon monoxide films 34 can absorb the silicon monoxide film 34 that is positioned at its both sides in bending avoids silicon monoxide film 34 to ftracture.Now repeating step S110～step S130.
Step S140, prepare conductive layer 50 on silicon monoxide film 34 surfaces.
In present embodiment, the material of conductive layer 50 is conductive oxide or metal.Conductive oxide is selected from least one in indium tin oxide (ITO), indium-zinc oxide (IZO), aluminium zinc oxide (AZO) and gallium zinc oxide (GZO).Metal is selected from least one in aluminium (Al), silver (Ag) and gold (Au).The thickness of conductive layer 50 is 70nm～200nm.
When the material of conductive layer 50 is conductive oxide, conductive layer 50 is preferably prepared by sputter, and sputtering at vacuum pressure is 1 × 10 -3pa～1 × 10 -5under Pa, carry out, speed is 0.1nm/s～1nm/s.When the material of conductive layer 50 is metal, preferably prepare by evaporation, evaporation is 1 × 10 at vacuum pressure -3pa～1 × 10 -5under Pa, carry out, evaporation speed is 0.2nm/s～2nm/s.
The preparation method of above-mentioned compliant conductive electrode, operates comparatively simple.
Below in conjunction with specific embodiment, the preparation method of compliant conductive electrode provided by the invention is elaborated.
The preparation used of the embodiment of the present invention and comparative example and tester are: filming equipment is high vacuum coating system (scientific instrument development center, Shenyang Co., Ltd), the four point probe resistivity tester (4PP) that sheet resistance test is produced for U.S.'s four-dimension (4D) company.
Embodiment 1
Compliant conductive electrode structure is substrate/PI (200nm)/SiO (800nm)/PI (200nm)/SiO (200nm)/Al(100nm), its making step comprises following:
Step 1, provide at the bottom of stainless steel lining and be placed in the deionized water that contains washing agent and carry out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.Thickness at the bottom of stainless steel lining is 0.05mm, and stainless model is AISI304 type, and surface roughness is 0.2 μ m.
Step 2, be 1 × 10 in vacuum degree -3in Pa vacuum coating system, mix resilient coating by hot evaporation process preparation, comprise the following steps:
1, by pyromellitic acid anhydride (PMDA) and 4,4 ' two kinds of monomer materials of diaminodiphenyl ether (ODA) are placed in respectively two crucibles of Vacuum Deposition chamber, control the temperature of crucible, making PMDA and the ratio of the evaporation rate of ODA is 1:1, prepare polyimide prepolymer film at stainless steel lining basal surface evaporation, making the polyimide prepolymer film thickness forming is 200nm, and wherein the evaporation rate of PMDA is 0.1nm/s;
2, the polyimide prepolymer film of above-mentioned preparation is shifted out to vacuum film coating chamber, be transferred in vacuum heater, be heated to 150 DEG C, processed 2 hours, makes polyamic acid dehydration form polyimide film;
3, by the bottom of stainless steel lining and polyimide film be transferred in vacuum coating system, continue to prepare SiO film at polyimide film surface evaporation, evaporation is 1 × 10 at vacuum pressure -3under Pa, carry out, evaporation speed is 2nm/s, and the thickness of the SiO film obtaining is 800nm.
Step 3, repeating step two, the mixing buffer-layer surface forming in step 2 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 3 forms, the thickness of polyimide film is 200nm, and the thickness of silicon monoxide film is 200nm.
At the bottom of step 4, stainless steel lining prepared by step 3 and mix resilient coating to be transferred in vacuum degree be 1 × 10 -3in the vacuum coating system of Pa, prepare conductive layer at SiO film surface evaporation, material is Al, and evaporation speed is 2nm/s, and thickness is 100nm, forms compliant conductive electrode.
Embodiment 2
Compliant conductive electrode structure is substrate/PI (300nm)/SiO (200nm)/PI (300nm)/SiO (600nm)/PI (300nm)/SiO (300nm)/Ag(70nm), its making step comprises following:
Step 1, stainless steel lining is provided at the bottom of, carry out ultrasonic cleaning by being placed at the bottom of stainless steel lining in the deionized water that contains washing agent, after cleaning up, use successively isopropyl alcohol, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.Thickness at the bottom of stainless steel lining is 0.1mm, and stainless model is AISI303 type, and surface roughness is 0.3 μ m.
Step 2, be 1 × 10 in vacuum degree -5in Pa vacuum coating system, preparation mixes resilient coating, comprises the following steps:
1, by pyromellitic acid anhydride (PMDA) and 4,4 ' two kinds of monomer materials of diaminodiphenyl ether (ODA) are placed in respectively two crucibles of Vacuum Deposition chamber, control the temperature of crucible, making PMDA and the ratio of the evaporation rate of ODA is 1:0.8, prepare polyimide prepolymer film at stainless steel lining basal surface evaporation, making the polyimide prepolymer film thickness forming is 300nm, and wherein the evaporation rate of PMDA is 1nm/s;
2, the polyimide prepolymer film of above-mentioned preparation is shifted out to vacuum film coating chamber, be transferred in vacuum heater, be heated to 120 DEG C, processed 1 hour, makes polyamic acid dehydration form polyimide film;
3, by the bottom of stainless steel lining and polyimide film be transferred in vacuum coating system, continue to prepare SiO film at polyimide film surface evaporation, evaporation is 1 × 10 at vacuum pressure -5under Pa, carry out, evaporation speed is 0.2nm/s, and the thickness of the SiO film obtaining is 200nm.
Step 3, repeating step two, the mixing buffer-layer surface forming in step 2 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 3 forms, the thickness of polyimide film is 300nm, and the thickness of silicon monoxide film is 600nm.
Step 4, repeating step two, the mixing buffer-layer surface forming in step 3 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 4 forms, the thickness of polyimide film is 300nm, and the thickness of silicon monoxide film is 300nm.
At the bottom of step 5, stainless steel lining prepared by step 4 and mix resilient coating to be transferred in vacuum degree be 1 × 10 -5in the vacuum coating system of Pa, prepare conductive layer at SiO film surface evaporation, material is Ag, and evaporation speed is 0.2nm/s, and thickness is 70nm, forms compliant conductive electrode.
Embodiment 3
Compliant conductive electrode structure is substrate/PI (200nm)/SiO (200nm)/PI (200nm)/SiO (600nm)/PI (200nm)/SiO (600nm)/PI (200nm)/SiO (100nm)/ITO(200nm), its making step comprises following:
Step 1, stainless steel lining is provided at the bottom of, carry out ultrasonic cleaning by being placed at the bottom of stainless steel lining in the deionized water that contains washing agent, after cleaning up, use successively isopropyl alcohol, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.The thickness of stainless steel film is 0.1mm, and stainless model is AISI304, and surface roughness is 0.3 μ m.
Step 2, be 1 × 10 in vacuum degree -4in Pa vacuum coating system, preparation mixes resilient coating, comprises the following steps:
1, by pyromellitic acid anhydride (PMDA) and 4,4 ' two kinds of monomer materials of diaminodiphenyl ether (ODA) are placed in respectively two crucibles of Vacuum Deposition chamber, control the temperature of crucible, making PMDA and the ratio of the evaporation rate of ODA is 1:1.2, prepare polyimide prepolymer film at stainless steel lining basal surface evaporation, making the polyimide prepolymer film thickness forming is 200nm, and wherein the evaporation rate of PMDA is 0.5nm/s;
2, the polyimide prepolymer film of above-mentioned preparation is shifted out to vacuum film coating chamber, be transferred in vacuum heater, be heated to 200 DEG C, processed 3 hours, makes polyamic acid dehydration form polyimide film;
3, by the bottom of stainless steel lining and polyimide film be transferred in vacuum coating system, continue the film at polyimide film surface preparation SiO, evaporation is 1 × 10 at vacuum pressure -4under Pa, carry out, evaporation speed is 1nm/s, and the thickness of the SiO film obtaining is 200nm.
Step 3, repeating step two, the mixing buffer-layer surface forming in step 2 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 3 forms, the thickness of polyimide film is 200nm, and the thickness of silicon monoxide film is 600nm.
Step 4, repeating step two, the mixing buffer-layer surface forming in step 3 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 4 forms, the thickness of polyimide film is 200nm, and the thickness of silicon monoxide film is 600nm.
Step 5, repeating step two, the mixing buffer-layer surface forming in step 4 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 5 forms, the thickness of polyimide film is 200nm, and the thickness of silicon monoxide film is 100nm.
At the bottom of step 6, stainless steel lining prepared by step 5 and mix resilient coating to be transferred in vacuum degree be 1 × 10 -4in the vacuum coating system of Pa, prepare conductive layer at SiO film surface by sputtering technology, material is IZO, and sputtering rate is 1nm/s, and thickness is 200nm, forms compliant conductive electrode.
Embodiment 4
Compliant conductive electrode structure is substrate/PI (100nm)/SiO (200nm)/PI (100nm)/SiO (400nm)/PI (100nm)/SiO (400nm)/PI (100nm)/SiO (200nm)/PI (100nm)/SiO (400nm)/GZO(100nm), its making step comprises following:
Step 1, stainless steel lining is provided at the bottom of, substrate is placed in the deionized water that contains washing agent and carries out ultrasonic cleaning, after cleaning up, use successively isopropyl alcohol, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.The thickness of stainless steel film is 0.2mm, and stainless model is AISI303, and surface roughness is 0.2 μ m.
Step 2, be 1 × 10 in vacuum degree -4in Pa vacuum coating system, preparation mixes resilient coating, comprises the following steps:
1, by pyromellitic acid anhydride (PMDA) and 4,4 ' two kinds of monomer materials of diaminodiphenyl ether (ODA) are placed in respectively two crucibles of Vacuum Deposition chamber, control the temperature of crucible, making PMDA and the ratio of the evaporation rate of ODA is 1:1, prepare polyimide prepolymer film at stainless steel lining basal surface evaporation, making the polyimide prepolymer film thickness forming is 100nm, and wherein the evaporation rate of PMDA is 0.5nm/s;
2, the polyimide prepolymer film of above-mentioned preparation is shifted out to vacuum film coating chamber, be transferred in vacuum heater, be heated to 180 DEG C, processed 2 hours, makes polyamic acid dehydration form polyimide film;
3, by the bottom of stainless steel lining and polyimide film be transferred in vacuum coating system, continue to prepare SiO film at polyimide film surface evaporation,, evaporation is 1 × 10 at vacuum pressure -4under Pa, carry out, evaporation speed is 0.5nm/s, and the thickness of the SiO film obtaining is 200nm.
Step 3, repeating step two, the mixing buffer-layer surface forming in step 2 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 3 forms, the thickness of polyimide film is 100nm, and the thickness of silicon monoxide film is 400nm.
Step 4, repeating step two, the mixing buffer-layer surface forming in step 3 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 4 forms, the thickness of polyimide film is 100nm, and the thickness of silicon monoxide film is 400nm.
Step 5, repeating step two, the mixing buffer-layer surface forming in step 4 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 5 forms, the thickness of polyimide film is 100nm, and the thickness of silicon monoxide film is 200nm.
Step 6, repeating step two, the mixing buffer-layer surface forming in step 5 forms one deck mixing resilient coating again, and in the mixing resilient coating that step 5 forms, the thickness of polyimide film is 100nm, and the thickness of silicon monoxide film is 400nm.
At the bottom of step 7, stainless steel lining prepared by step 6 and mix resilient coating to be transferred in vacuum degree be 1 × 10 -4in the vacuum coating system of Pa, prepare conductive layer at SiO film surface by sputtering technology, material is GZO, and sputtering rate is 0.1nm/s, and thickness is 100nm, forms compliant conductive electrode.
Comparative example
Compliant conductive electrode structure is substrate/SiO (1000nm)/Al(100nm), its making step comprises following:
Step 1, provide at the bottom of stainless steel lining and be placed in the deionized water that contains washing agent and carry out ultrasonic cleaning, use successively isopropyl alcohol after cleaning up, acetone is processed 20 minutes in ultrasonic wave, and then dries up with nitrogen.Thickness at the bottom of stainless steel lining is 0.05mm, and stainless model is AISI304 type, and surface roughness is 0.2 μ m.
Step 2, be 1 × 10 in vacuum degree -3in Pa vacuum coating system, prepare SiO film at substrate surface evaporation, evaporation speed is 2nm/s, and the thickness of the SiO film obtaining is 1000nm.
At the bottom of step 3, stainless steel lining prepared by step 2 and SiO resilient coating to be transferred in vacuum degree be 1 × 10 -3in the vacuum coating system of Pa, prepare conductive layer at SiO film surface evaporation, material is Al, and evaporation speed is 2nm/s, and thickness is 100nm, forms compliant conductive electrode.
Table 1
Refer to table 1, table 1 is embodiment 1,2,3,4 preparation compliant conductive electrodes under differently curved number of times, the square resistance recording with four point probe resistivity tester.For relatively, polyimides resilient coating is not set between stainless steel thin slice and Al, the SiO film of condition of equivalent thickness is only set as a comparison case, refer to the preparation process of comparative example.
Refer to Fig. 3, Fig. 3 is the schematic diagram that compliant conductive electrode carries out flexibility test, wherein, and L 0for the air line distance at the compliant conductive electrode two ends before bending, L is the air line distance through the compliant conductive electrode two ends after bending.The process of crooked test is as follows: the conductive electrode that the conductive electrode that embodiment is provided and comparative example provide carries out bending in fixture, and the air line distance (L) that makes the compliant conductive electrode two ends after bending is initial value (L 0) half, repeat repeatedly bending, and calculate repeatedly bending after the surperficial square resistance of compliant conductive electrode.
From table 1, can learn, the compliant conductive electrode of embodiment 1～4 preparation is because polyimides resilient coating can be strengthened the adhesion of two SiO films, offset flexible electrode in the time that deflection operates, the internal stress producing between multiple SiO films, thereby can make SiO film can be good in conjunction with on being attached at the bottom of stainless steel lining, can there is not slight crack, pin hole, the situation such as come off.Therefore through after deflection repeatedly, the conductive layer of the compliant conductive electrode of embodiment 1～4 preparation can keep good integrality, thereby after the test of square resistance, it is not very large before and after its resistance, changing difference, has good stability.And comparative example is not because mix resilient coating, through after deflection repeatedly, a large amount of SiO films is destroyed, slight crack or come off occurs, thereby cause conductive layer to come off from substrate surface, thereby conductive layer on substrate is imperfect, lack continuous conductivity, thereby the square resistance on surface improves a lot.
Refer to Fig. 4, the sheet resistivity change curve that Fig. 4 is the compliant conductive electrode prepared of embodiment 1 and comparative example under deflection repeatedly.As can be seen from Figure 4, compliant conductive electrode prepared by embodiment 1 is after deflection repeatedly, and the variation of square resistance is not obvious, and compliant conductive electrode prepared by comparative example square resistance after deflection repeatedly obviously improves.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.

Claims (10)

1. a compliant conductive electrode, is characterized in that, at the bottom of comprising the stainless steel lining stacking gradually, mix resilient coating and conductive layer, described mixing resilient coating comprises polyimide film and is formed at the silicon monoxide film on described polyimide film surface.
2. compliant conductive electrode according to claim 1, is characterized in that, the thickness at the bottom of described stainless steel lining is 0.05mm～0.2mm.
3. compliant conductive electrode according to claim 1, is characterized in that, the thickness of described polyimide film is 100nm～300nm, and the thickness of described silicon monoxide film is 200nm～800nm.
4. compliant conductive electrode according to claim 1, is characterized in that, the material of described conductive layer is selected from least one in indium tin oxide, indium-zinc oxide, aluminium zinc oxide and gallium zinc oxide.
5. compliant conductive electrode according to claim 1, is characterized in that, the material of described conductive layer is selected from least one in aluminium, silver and gold.
6. compliant conductive electrode according to claim 1, is characterized in that, described mixing resilient coating is 2～5, and multiple mixing resilient coatings stack gradually.
7. a preparation method for compliant conductive electrode, is characterized in that, comprises the following steps:
In vacuum coating system, by pyromellitic acid anhydride and 4,4, ' diaminodiphenyl ether is placed in respectively two crucibles, makes pyromellitic acid anhydride and 4,4 ' ratio of the evaporation rate of diaminodiphenyl ether is 1:0.8～1.2, at stainless steel lining basal surface deposition polyimide prepolymer film;
Under vacuum environment, by the bottom of described stainless steel lining and be deposited on the polyimide prepolymer film heating to 120 DEG C of described stainless steel lining basal surface～200 DEG C and carry out processed, make polyimide prepolymer film dehydration form polyimide film;
Surperficial evaporation at described polyimide film is prepared silicon monoxide film; And
Prepare conductive layer at described silicon monoxide film surface.
8. the preparation method of compliant conductive electrode according to claim 7, is characterized in that: the thickness of described polyimide film is 100nm～300nm, and the thickness of described silicon monoxide film is 200nm～800nm.
9. the preparation method of compliant conductive electrode according to claim 7, is characterized in that: described mixing resilient coating is 2～5, and multiple mixing resilient coatings stack gradually.
10. the preparation method of compliant conductive electrode according to claim 7, is characterized in that: the thickness at the bottom of described stainless steel lining is 0.05mm～0.2mm.
CN201310157835.3A 2013-04-28 2013-04-28 Flexible conductive electrode and preparation method thereof Pending CN104124386A (en)

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Application publication date: 20141029