CN108682616A - A kind of preparation method of transparent conductive film for flexible display - Google Patents
A kind of preparation method of transparent conductive film for flexible display Download PDFInfo
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- CN108682616A CN108682616A CN201810436906.6A CN201810436906A CN108682616A CN 108682616 A CN108682616 A CN 108682616A CN 201810436906 A CN201810436906 A CN 201810436906A CN 108682616 A CN108682616 A CN 108682616A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 25
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 150000004985 diamines Chemical class 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 11
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 241000790917 Dioxys <bee> Species 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 10
- NSGXIBWMJZWTPY-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropane Chemical compound FC(F)(F)CC(F)(F)F NSGXIBWMJZWTPY-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- BIXGISJFDUHZEB-UHFFFAOYSA-N 2-[9,9-bis(4-methylphenyl)fluoren-2-yl]-9,9-bis(4-methylphenyl)fluorene Chemical compound C1=CC(C)=CC=C1C1(C=2C=CC(C)=CC=2)C2=CC(C=3C=C4C(C5=CC=CC=C5C4=CC=3)(C=3C=CC(C)=CC=3)C=3C=CC(C)=CC=3)=CC=C2C2=CC=CC=C21 BIXGISJFDUHZEB-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- VGGRCVDNFAQIKO-UHFFFAOYSA-N formic anhydride Chemical compound O=COC=O VGGRCVDNFAQIKO-UHFFFAOYSA-N 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- LGRFSURHDFAFJT-UHFFFAOYSA-N phthalic anhydride Chemical class C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 abstract description 6
- 229910016062 BaRuO Inorganic materials 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004642 Polyimide Substances 0.000 abstract description 4
- 229910021389 graphene Inorganic materials 0.000 abstract description 4
- 229920001721 polyimide Polymers 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- HHLMWQDRYZAENA-UHFFFAOYSA-N 4-[4-[2-[4-(4-aminophenoxy)phenyl]-1,1,1,3,3,3-hexafluoropropan-2-yl]phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC1=CC=C(C(C=2C=CC(OC=3C=CC(N)=CC=3)=CC=2)(C(F)(F)F)C(F)(F)F)C=C1 HHLMWQDRYZAENA-UHFFFAOYSA-N 0.000 abstract 1
- 229910052788 barium Inorganic materials 0.000 abstract 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000011231 conductive filler Substances 0.000 abstract 1
- 239000000428 dust Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 31
- 238000000034 method Methods 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 125000006159 dianhydride group Chemical group 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- -1 metallic mesh Chemical compound 0.000 description 4
- KZVVGZKAVZUACK-BJILWQEISA-N rilpivirine hydrochloride Chemical compound Cl.CC1=CC(\C=C\C#N)=CC(C)=C1NC1=CC=NC(NC=2C=CC(=CC=2)C#N)=N1 KZVVGZKAVZUACK-BJILWQEISA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 2
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical class CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 208000016261 weight loss Diseases 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02697—Forming conducting materials on a substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a kind of transparent and colourless conductive films of flexible display.The preparation method is first with 2,2 bis- [4 (4 aminophenoxy phenyl)] hexafluoropropane) based on diamine monomer and 4,4 ' are obtained by the reaction polyamic acid solution to the dianhydride monomer based on the double phthalic anhydrides of benzene dioxy, then the nanoscale ruthenic acid barium dust by 1700 DEG C or more high temperature sinterings is added, obtain mixed solution, go the film imidization of gained after solvent to get to the water white transparency conductive film for flexible display mixed solution.The conductive film of gained of the invention is using own transparent and colourless flexible polyimide material is matrix, and the BaRuO of high conductivity is added3Powder is obtained, and it is flexible poor to overcome the transparency conducting layers itself such as tradition ITO, nano-silver thread, graphene used in flexible display, and the shortcomings of with flexible substrate poor adhesion.Meanwhile also solving the problems, such as that the transparent poor and conductive effect of gained laminated film is undesirable after conductive filler is added in general polyimide matrix.
Description
Technical field
The present invention relates to flexible display base material fields, the more particularly to preparation of the transparency conducting layer of flexible display
Method.
Technical background
Compared with traditional Rigid displays, flexible display have the advantages that it is more, such as lightly, flexible strong, resistance to punching
It hits, brightness is high and at low cost etc..Therefore, it has more wide application prospect in display field, it has also become novel and intelligent
The important component of electronic product.
Flexible conductive layer is as one of device important in flexible display, presently mainly by the way that ITO, nanometer is added
The materials such as silver, metallic mesh, graphene improve its electric conductivity.Patent [CN 201010162968.6] and patent [CN
201310306194.3] disclose high-transmissivity flexible transparent conductive film and preparation method based on ITO.Gained electrically conducting transparent
Film has good visible transparent and electric conductivity, but since ITO involves great expense, and ITO is unstable on a flexible substrate
Not the features such as resist bending, its application is limited.
Compared to ITO, nano silver and metallic mesh have lower resistivity, therefore can more meet device more low-resistivity
Demand for development.Patent [CN 201410514149.1] and patent [CN 201610857858.9] are reported containing metal nano
Transparent conductive film of silver wire and preparation method thereof.But the transmitance and resistance concrete numerical value of transparent conductive film are not provided, and
It is reported in patent [CN 200610070509.9] and patent [CN 85104006] since the silver of device interfaces can occur
Migration or vulcanization, cause adhesiveness to decline, cause surface wrinkling.In addition, the doping of metal also a degree of can reduce it
Optical transmittance.
Compared to ITO, nano silver and metallic mesh, graphene not only has high transmittance and low-resistance excellent properties,
And its resistance to bend(ing) can be enhanced.Patent [CN 201510247050.4] and patent [CN 201610057005.7] disclose soft
The preparation method of the transparent conductive film of property display.It has flexible well with good transmitance and the transparency
Property.But due to the poor adhesion of graphene and flexible substrate, for a long time using may be peeling-off or even falling off, influencing it makes
Use the service life.
In addition, preparing display conductive film at present mainly by the methods of magnetron sputtering, technique is relatively complicated, and
Display can be caused to deform and cause device fraction defective to increase to a certain degree.Caused by above-mentioned material and preparation method
Shortcomings and limitations, thus seek more particularly suitable conductive material and improve preparation method it is particularly important.
Invention content
The object of the present invention is to provide a kind of flexible display composition of colorless and transparent conductive layer and the sides of preparation
Method..
Realize that the object of the invention technical solution is as follows：
It (1), will [4- (4- aminophenoxy phenyls)] hexafluoros third bis- with 2,2- under the conditions of step 1, room temperature and nitrogen protection
Diamine monomer based on alkane (BDAF) is dissolved in polar non-solute (such as DMAC), waits for that two amine solvents are complete, time segment
It is repeatedly added with 4,4 '-to the dianhydride monomer based on the double phthalic anhydrides (HQDEA) of benzene dioxy, reaction temperature is down to 0 DEG C,
10~20h is reacted, polyamic acid solution is obtained.
(2) step 2, by nano level BaRuO3Powder is sintered 5~10h in 1700 DEG C or more, after being cooled to room temperature, takes
Appropriate be added in polyamic acid solution is uniformly mixed, and forms mixed solution；
(3) step 3, by above-mentioned mixed solution on substrate film, the plank of film is dry in vacuum drying oven, then
Imidization is placed in Muffle furnace to get to the transparent conductive film for flexible display.
Wherein, in above-mentioned steps 1, the mole percent that BDAF accounts for diamine monomer accounts for dianhydride monomer not less than 70%, HQDEA
Mole percent be not less than 60%.
In above-mentioned steps 2, BaRuO3Powder dosage is the total matter of dianhydride and diamine monomer used when prepared by polyamic acid solution
The 3~30% of amount, it is preferable that BaRuO3Powder dosage is dianhydride and diamine monomer gross mass used when prepared by polyamic acid solution
6~11%.
In above-mentioned steps 2, BaRuO3The average particle size range of powder is 10~90nm, preferably average grain diameter be 20~
30nm。
In above-mentioned steps 3, the vacuum degree in vacuum tank is for -0.02~-0.06MPa
In above-mentioned steps 3, in the preparation method of the transparent conductive film, the drying after mixed solution film be
Temperature programming carries out between 80~200 DEG C.Imidization is that temperature programming carries out between 200~400 DEG C.
Compared with the Preparation Method of existing flexible display conductive layer, remarkable advantage is the present invention：
1. thin-film material provided by the invention has colourless characteristic while having the good transparency, improve
The performance of display material.Meet the electric conductivity of conductive layer needed for flexible display again on this basis.
2. conductive film itself has excellent flexibility, overcomes the materials such as ITO, metallic mesh and be attached to flexible liner
Behind bottom, mismatch that when stress caused by the relative brittleness of itself between conductive layer and bending generates.
3. the matrix of conductive film is polyimide material, if dielectric substrate selects unfilled polyimides thin
Film can press the polyamide acid film of the two, common imidization, have between the insulating layer and conductive layer of gained so excellent
Peel strength, overcome the materials such as ITO, metallic mesh on flexible substrates poor adhesive force the shortcomings that, contribute to prepare more high score
The flexible display device of resolution.
Specific implementation mode
Using specific embodiment below, the invention will be further described.The present invention is not limited to scope of embodiments.
Embodiment 1
Under nitrogen protection, bis- [4- (4- the aminophenoxy phenyls)] hexafluoropropane of 2, the 2- of 0.10mol are added three mouthfuls
In flask, add n,N-dimethylacetamide dissolving, at 30 DEG C constant temperature stir, it is to be dissolved completely after, be added 0.080mol
4,4 '-to 3,3 ', 4,4 '-biphenyltetracarboxylic acid dianhydrides of benzene dioxy double phthalic anhydrides and 0.022mol, will reaction temperature
Degree is down to 0 DEG C, reacts 20h, obtains polyamic acid solution.By the BaRuO that average grain diameter is 20nm3Powder is in 1700 DEG C of sintering
5h after being cooled to room temperature, takes appropriate be added in polyamic acid solution to be uniformly mixed, forms mixed solution, during which add N,
N- dimethylacetylamides make the solid content of mixed solution be maintained at 15%, BaRuO3Powder dosage is polyamic acid solution used
The 6% of middle dianhydride and diamine monomer gross mass, by mixed solution, film, control coating thickness will be applied in 0.02mm on substrate
The glass plate of film 80 DEG C in vacuum drying oven, 140 DEG C, 160 DEG C of each dryings 1 hour, then in Muffle furnace 200 DEG C, 240 DEG C and
270 DEG C of each dryings 1 hour are to get to the conductive film of water white transparency.By the use flex endurant degree machine of the film, according to ASTM
After method D in F392 standards is recycled 1000 times, resistivity 0.13*10 is measured-4Ω m (four probe method measures), light transmittance are
87% (ultraviolet-uisible spectrophotometer method measures), tensile strength are 80MPa (electronic tensile machine measures), and heat decomposition temperature is more than
500 DEG C (thermogravimetry measures).
Embodiment 2
Under nitrogen protection, by bis- [4- (4- the aminophenoxy phenyls)] hexafluoropropane of 2, the 2- of 0.08mol and 0.02mol
4,4 '-diaminodiphenyl ethers be added three-necked flask in, add n,N-dimethylacetamide dissolving, constant temperature stirs at 30 DEG C
Mix, it is to be dissolved completely after, be added the 4 of 0.102mol, reaction temperature to the double phthalic anhydrides of benzene dioxy, is down to 0 DEG C by 4 '-,
15h is reacted, polyamic acid solution is obtained.By the BaRuO that average grain diameter is 25nm3Powder is sintered 5h in 1700 DEG C, is cooled to room
Wen Hou takes appropriate be added in polyamic acid solution to be uniformly mixed, forms mixed solution, during which adds N, N- dimethylacetamides
Amine makes the solid content of mixed solution be maintained at 15%, BaRuO3Powder dosage is dianhydride and diamines in polyamic acid solution used
The 10% of monomer gross mass, by mixed solution, film, control coating thickness exist the glass plate of film in 0.02mm on substrate
80 DEG C in vacuum drying oven, 120 DEG C, 150 DEG C of each dryings 1 hour, then 210 DEG C, 240 DEG C, 270 DEG C and 300 DEG C in Muffle furnace
Each drying 1 hour is to get to the conductive film of water white transparency.By the use flex endurant degree machine of the film, marked according to ASTM F392
After method D in standard is recycled 1000 times, resistivity 0.67*10 is measured-5Ω m (four probe method measures), light transmittance are 85% (ultraviolet
Visible spectrophotometer method measures), tensile strength is 70MPa (electronic tensile machine measures), and heat decomposition temperature is more than 480 DEG C of (heat
Weight-loss method measures).
Embodiment 3
Under nitrogen protection, bis- [4- (4- the aminophenoxy phenyls)] hexafluoropropane of 2, the 2- of 0.10mol are added three mouthfuls
In flask, add n,N-dimethylacetamide dissolving, at 30 DEG C constant temperature stir, it is to be dissolved completely after, be added 0.070mol
4,4 '-to 4,4 '-biphenyl ether dianhydrides of benzene dioxy double phthalic anhydrides and 0.032mol, reaction temperature is down to 0 DEG C, instead
18h is answered, polyamic acid solution is obtained.By the BaRuO that average grain diameter is 20nm3Powder is sintered 5h in 1700 DEG C, is cooled to room temperature
Afterwards, it takes appropriate be added in polyamic acid solution to be uniformly mixed, forms mixed solution, during which add N, N- dimethylacetamides
Amine makes the solid content of mixed solution be maintained at 15%, BaRuO3Powder dosage is dianhydride and diamines in polyamic acid solution used
The 8% of monomer gross mass, by mixed solution, film, control coating thickness exist the glass plate of film in 0.02 mm on substrate
80 DEG C in vacuum drying oven, 150 DEG C, 180 DEG C of each dryings 1 hour, then 220 DEG C in Muffle furnace, 240 DEG C, 280 DEG C of each dryings 1
Hour to get to the conductive film of water white transparency.By the use flex endurant degree machine of the film, according in ASTM F392 standards
After method D is recycled 1000 times, resistivity 0.87*10 is measured-5Ω m (four probe method measures), light transmittance are 88% (UV, visible light
Spectrophotometer method measures), tensile strength is 75MPa (electronic tensile machine measures), and heat decomposition temperature is more than 490 DEG C of (thermal weight losses
Method measures).
Embodiment 4
Under nitrogen protection, bis- [4- (4- the aminophenoxy phenyls)] hexafluoropropane of 2, the 2- of 0.10mol are added three mouthfuls
In flask, add n,N-dimethylacetamide dissolving, at 30 DEG C constant temperature stir, it is to be dissolved completely after, be added 0.080mol
4,4 '-to the hexafluorodianhydride (6FDA)s of benzene dioxy double phthalic anhydrides and 0.022mol, reaction temperature is down to 0 DEG C, reacts 20h,
Obtain polyamic acid solution.By the BaRuO that average grain diameter is 25nm3Powder is sintered 5h in 1700 DEG C, after being cooled to room temperature, takes suitable
Amount is added in polyamic acid solution and is uniformly mixed, and forms mixed solution, during which adds N, and N- dimethylacetylamides to mix
The solid content for closing solution is maintained at 15%, BaRuO3Powder dosage is dianhydride and the total matter of diamine monomer in polyamic acid solution used
The 11% of amount, by mixed solution, film, control coating thickness are dried in 0.02 mm, by the glass plate of film in vacuum on substrate
80 DEG C and 150 DEG C of each dryings 1 hour in case, then 210 DEG C, 240 DEG C, 270 DEG C and 300 DEG C each dryings 1 are small in Muffle furnace
When to get to the conductive film of water white transparency.By the use flex endurant degree machine of the film, according to the side in ASTM F392 standards
After method D is recycled 1000 times, resistivity 0.25*10 is measured-5Ω m (four probe method measures), light transmittance are 90% (UV, visible light point
Light photometer measuring method measures), tensile strength is 60MPa (electronic tensile machine measures), and heat decomposition temperature is more than 480 DEG C of (thermogravimetries
It measures).
Claims (8)
1. a kind of preparation method of transparent conductive film for flexible display, which is characterized in that be made of following steps:1)
By based on bis- [4- (4- the aminophenoxy phenyls)] hexafluoropropane of 2,2- diamine monomer and with 4,4 '-adjacent benzene double to benzene dioxy two
Dianhydride monomer based on formic anhydride is reacted in polar non-solute, obtains polyamic acid solution；It 2) will be nano level
BaRuO3Powder is sintered 5~10h in 1700 DEG C or more, after being cooled to room temperature, is added into polyamic acid solution and is stirred
It is even, form mixed solution；3) by mixed solution on substrate film, the plank of film is subjected to vacuum at 80~200 DEG C and is done
It is dry, it is subsequently placed in and imidization is heated and carried out in Muffle furnace to get to the transparent conductive film for flexible display.
2. the preparation method of polyamic acid solution as described in claim 1, which is characterized in that BDAF accounts for mole of diamine monomer
The mole percent that percentage accounts for dianhydride monomer not less than 70%, HQDEA is not less than 60%.
3. the preparation method of mixed solution as described in claim 1, which is characterized in that BaRuO3Powder dosage is polyamic acid
The 3~30% of dianhydride and diamine monomer gross mass used when prepared by solution.
4. the preparation method of mixed solution as claimed in claim 3, which is characterized in that BaRuO3Powder dosage is polyamic acid
The 6~11% of dianhydride and diamine monomer gross mass used when prepared by solution.
5. the preparation method for the transparent conductive film of flexible display as described in claim 1, which is characterized in that vacuum
Dry vacuum degree is for -0.02~-0.06MPa.
6. the preparation method for the transparent conductive film of flexible display as described in claim 1, which is characterized in that described
BaRuO3Its average particle size range of powder is 10~90nm.
7. the preparation method for the transparent conductive film of flexible display as claimed in claim 6, which is characterized in that described
BaRuO3Its average particle size range of powder is 20~30nm.
8. the preparation method for the transparent conductive film of flexible display as described in claim 1, which is characterized in that mixing
Drying after solution coating is that temperature programming carries out between 80~200 DEG C, and imidization is the temperature programming between 200~400 DEG C
It carries out.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060087029A1 (en) * | 2004-10-22 | 2006-04-27 | Fujitsu Limited | Semiconductor device and method of producing the same |
| CN102807675A (en) * | 2012-08-19 | 2012-12-05 | 南京依麦德光电材料科技有限公司 | Flexible transparent polyimide film material and preparation method thereof |
| CN103788650A (en) * | 2013-12-31 | 2014-05-14 | 杭州福斯特光伏材料股份有限公司 | Colorless and transparent polyimide film and preparation method thereof |
-
2018
- 2018-05-09 CN CN201810436906.6A patent/CN108682616B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060087029A1 (en) * | 2004-10-22 | 2006-04-27 | Fujitsu Limited | Semiconductor device and method of producing the same |
| CN102807675A (en) * | 2012-08-19 | 2012-12-05 | 南京依麦德光电材料科技有限公司 | Flexible transparent polyimide film material and preparation method thereof |
| CN103788650A (en) * | 2013-12-31 | 2014-05-14 | 杭州福斯特光伏材料股份有限公司 | Colorless and transparent polyimide film and preparation method thereof |
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