CN107195386A - A kind of preparation method of transparent flexible conductive material - Google Patents

A kind of preparation method of transparent flexible conductive material Download PDF

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Publication number
CN107195386A
CN107195386A CN201710357816.3A CN201710357816A CN107195386A CN 107195386 A CN107195386 A CN 107195386A CN 201710357816 A CN201710357816 A CN 201710357816A CN 107195386 A CN107195386 A CN 107195386A
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China
Prior art keywords
conductive material
transparent flexible
pdms
flexible conductive
preparation
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CN201710357816.3A
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Chinese (zh)
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孙晶
郎明非
杨海波
周文慧
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Dalian University
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Dalian University
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Priority to CN201710357816.3A priority Critical patent/CN107195386A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal

Abstract

The invention belongs to conductive material field, and in particular to a kind of preparation method of transparent flexible conductive material.Present invention polyvinyl alcohol and glycerine modify the hydrophilic layer of PDMS substrates, by nano silver wire spin coating, spraying or are coated on acquisition transparent flexible conductive material in the PDMS substrates through hydrophilic layer modified.Flexible and transparent nano silver wire conductive material prepared by the inventive method, with high transparency, low-resistance feature, transmitance scope:80%~93%;Resistance range:2Ωsq‑1~28 Ω sq‑1, and the optimal result that the inventive method is reached is to reach 2.09 Ω sq in resistance‑1While transmitance up to 91.4%.The performance of transparent flexible conductive material prepared by the inventive method is in a leading position level in the same industry, electronic component miniaturization and it is integrated in there is good application prospect.

Description

A kind of preparation method of transparent flexible conductive material
Technical field
The invention belongs to conductive material field, and in particular to a kind of preparation method of transparent flexible conductive material.
Background technology
Transparent conductive film refers to that wavelength has preferable transmitance, resistivity in 380nm~780nm visible-range Less than 10-3Ω cm thin-film material.Transparent conductive film is attached to the conduction that flexible and transparent is made in flexible clear materials Material, it is flexible, lightweight, non-breakable.In recent years, flexible and transparent conductive material is more and more extensive as main composition material Ground is applied in electronics and optoelectronic device, such as the display of organic solar batteries, Organic Light Emitting Diode, and electronic equipment Screen.It is for representative with indium oxide tin film (Indium Tin Oxide, ITO) that most nesa coatings is applied on Vehicles Collected from Market The characteristics of metal conductive oxide film, this film is that fragility is larger, after multiple bending fold, be also easy to produce crackle or Peeled off from flexible substrate, and indium tin, as rare earth resources in short supply, the expensive amount of valency is few.Miniaturization and collection with electronic component Cheng Hua, such conductive film is increasingly difficult to meet the demand of society.Therefore, it is miscellaneous to there is mechanical flexibility and good The mixing of the conductive film material of transmitance, such as CNT, nano silver wire, conductive polymer, graphene, and these materials Property material, is progressively replacing traditional tin indium oxide conductive film.In these conductive materials, nano silver wire is superior due to its Electric conductivity and have been a great concern.Nano silver wire is layered on a kind of high molecular polymer surface by Junpeng Li etc., is obtained Transmitance and resistance to flexible conducting material are respectively 86.4% and 25 Ω sq-1;Yeongun Ko etc. by nano silver wire anyhow Alternate is layered on plastic substrate surface, obtains transmitance and resistance is respectively:85% and 10 Ω sq-1;Weiwei Xiong etc. are ground The transparent flexible conductive material resistance and transmitance studied carefully are respectively reached:8.4Ωsq-1With 86%.Due to by between nano silver wire The influence of high contact resistance, the resistivity for making conductive material by nano silver wire is very poor, is not appropriate for application.It is contemplated that gram Influence of the high contact resistance to nano silver wire conductive material resistivity is taken, produces that resistance is low, the high transparent flexible of transmitance is led Electric material.
The content of the invention
To make up the deficiencies in the prior art, high transmission is produced using nano silver wire it is an object of the invention to provide one kind Rate, the method for the transparent flexible conductive material of low-resistivity.
The present invention is achieved by the following technical programs:A kind of preparation method of transparent flexible conductive material, including with Lower step:
S1 presses dimethyl silicone polymer (Polydimethylsiloxane, PDMS) A liquid (monomer) and B liquid (primosome) (1-20):1 mass ratio is prepared into PDMS substrates;
S2 is modified with polyvinyl alcohol (Polyvinyl alcohol, PVA) and glycerine (Glycerol, Gly) mixed solution The hydrophilic layer of PDMS substrates;
S3 is by nano silver wire (AgNW) spin coating, spraying or is coated in the PDMS substrates through hydrophilic layer modified.
Further, the step S2 is specially:The dust on PDMS surfaces is first removed with 3M glue, with ozone clean, then In the mixed solution that PDMS substrates are placed in PVA and Gly, wherein PVA mass concentration is 0.1%-10%, and Gly quality is dense Spend for 0.1%-10%.
Further, in the step S3, AgNW concentration is 0.01-10mg/ml, and the rotating speed of AgNW spin coatings is 100- 5000rpm。
Preferably, in the step S2, in PVA and Gly mixed solutions, PVA concentration is that 2%, Gly concentration is 5%.
Preferably, in the step S3, the concentration of AgNW solution is 1mg/ml, and rotating speed used in spin coating is 3000rpm.
Flexible and transparent nano silver wire conductive material prepared by the inventive method, with high transparency, low-resistance feature, is passed through Rate scope:80%~93%;Resistance range:2Ωsq-1~28 Ω sq-1, and the optimal result that is reached of the inventive method be Resistance reaches 2.09 Ω sq-1While transmitance up to 91.4%.Transparent flexible conductive material prepared by the inventive method Performance is in a leading position level in the same industry, electronic component miniaturization and it is integrated in there is good application prospect.
Brief description of the drawings
Fig. 1 is the nano silver wire concentration of the embodiment of the present invention 1 and spin coating rotating speed to resistance and 550nm wavelength light penetrations Influence;
Fig. 2 is the conductive material of the embodiment of the present invention 1 resistance change curves after multiple positive and negative bending.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with Any mode limits the present invention.In following embodiments unless otherwise specified, the experimental method used is conventional method, used Material, reagent etc. chemically company can be bought.
Embodiment 1
(1) PDMS monomers and primosome are pressed 10:1 mass ratio is poured into beaker, is poured into after being stirred 5 minutes with glass bar In culture dish equipped with silicon chip.
(2) culture dish is put in concentrate drying device, is evacuated 1.5 hours to remove the gas in PDMS with vacuum diaphragm pump Bubble, is then placed on solidification 1 hour in 80 DEG C of vacuum drying chamber.
(3) after gently peeling off PDMS from silicon chip template after its natural cooling, it is cut into small pieces with cutting machine, in case experiment Use.
(4) dust of PDMS surface attachments is removed with 3M glue, is subsequently placed in UV ozone cleaning machine and uses ozone clean 20min。
(5) PVA concentration 2%, Gly concentration 5% prepare PVA and Gly mixed solution by weight percent.
(6) PDMS is soaked into 20min in PVA and Gly mixed solutions, taking-up siphons away many extraction raffinates on PDMS surfaces with filter paper Body, and put it into dry 2h in 60 DEG C of vacuum drying oven.
(7) step (6) is repeated once, heating is taken out after terminating, nano silver wire face will not be spread with adhesive tape and is glued totally, Then PDMS is put into heat fixation 20min in 100 DEG C of vacuum drying oven, and naturally cools to room temperature in an oven.
(8) step (6), step (7) are repeated once.
(9) configuration nano silver wire (AgNW) ethanol solution 5mg/ml.
(10) the μ L drops of AgNW solution 50 are drawn in the PDMS substrate surfaces of modified, and in spin coating under 3000rpm rotating speeds 1min。
(11) repeat step (10) twice, obtains transparent flexible conductive material, and it is surveyed with four probe resistance instrument through repeatedly curved Sheet resistance after folding, is shown in Fig. 2.
After tested, conductive material performance produced by the present invention is as shown in table 1.
Table 1:
Embodiment 2
(1) PDMS monomers and primosome are pressed 10:1 mass ratio is poured into beaker, is poured into after being stirred 5 minutes with glass bar In culture dish equipped with silicon chip.
(2) culture dish is put in concentrate drying device, is evacuated 1.5 hours to remove the gas in PDMS with vacuum diaphragm pump Bubble, is then placed on solidification 1 hour in 80 DEG C of vacuum drying chamber.
(3) after gently peeling off PDMS from silicon chip template after its natural cooling, it is cut into small pieces with cutting machine, in case experiment Use.
(4) dust of PDMS surface attachments is removed with 3M glue, is subsequently placed in UV ozone cleaning machine and uses ozone clean 20min。
(5) PVA concentration 5%, Gly concentration 10% prepare PVA and Gly mixed solution by weight percent.
(6) PDMS is soaked into 20min in PVA and Gly mixed solutions, taking-up siphons away many extraction raffinates on PDMS surfaces with filter paper Body, and put it into dry 2h in 60 DEG C of vacuum drying oven.
(7) step (6) is repeated once, heating is taken out after terminating, nano silver wire face will not be spread with adhesive tape and is glued totally, Then PDMS is put into heat fixation 20min in 100 DEG C of vacuum drying oven, and naturally cools to room temperature in an oven.
(8) step (6), step (7) are repeated once.
(9) configuration nano silver wire (AgNW) ethanol solution 1mg/ml.
(10) the μ L drops of AgNW solution 50 are drawn in the PDMS substrate surfaces of modified, and in spin coating under 1500rpm rotating speeds 1min。
(11) repeat step (10) twice, obtains transparent flexible conductive material.
Gained transparent flexible conductive material transmitance scope of the invention:80%~93%;Resistance range:2Ωsq-1~28 Ω sq-1, and the optimal result that this method is reached is to reach 2.09 Ω sq in resistance-1While, transmitance is 91.4%.
Described above not limitation of the present invention, the present invention is also not limited to the example above.The art it is common Technical staff is in the essential scope of the present invention, the variations, modifications, additions or substitutions made, and should also belong to the protection of the present invention Scope, protection scope of the present invention is defined by claims.

Claims (5)

1. a kind of preparation method of transparent flexible conductive material, it is characterised in that comprise the following steps:
PDMS monomers and primosome are pressed (1-20) by S1:1 mass ratio is prepared into PDMS substrates;
S2 modifies PDMS substrates with PVA and Gly mixed solutions, and hydrophilic layer is formed on PDMS surfaces;
S3 is by AgNW spin coatings, spraying or is coated in the PDMS substrates through hydrophilic layer modified.
2. a kind of preparation method of transparent flexible conductive material according to claim 1, it is characterised in that the step S2 Specially:The dust on PDMS surfaces is first removed with 3M glue, with ozone clean, then PDMS substrates are placed in PVA and Gly mixing In solution, wherein PVA mass concentration is 0.1%-10%, and Gly mass concentration is 0.1%-10%.
3. a kind of preparation method of transparent flexible conductive material according to claim 1, it is characterised in that the step S3 In, AgNW concentration is 0.01-10mg/ml, and the rotating speed of AgNW spin coatings is 100-5000rpm.
4. a kind of preparation method of transparent flexible conductive material according to claim 2, it is characterised in that the step S2 In, in PVA and Gly mixed solutions, PVA concentration is that 2%, Gly concentration is 5%.
5. a kind of preparation method of transparent flexible conductive material according to claim 3, it is characterised in that the step S3 In, the concentration of AgNW solution is 1mg/ml, and rotating speed used in spin coating is 3000rpm.
CN201710357816.3A 2017-05-19 2017-05-19 A kind of preparation method of transparent flexible conductive material Pending CN107195386A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107863538A (en) * 2017-11-03 2018-03-30 大连大学 A kind of electrode and its application for alcohol catalysis
CN107991372A (en) * 2017-11-22 2018-05-04 大连大学 A kind of method for lead ion detection
CN108152348A (en) * 2017-12-22 2018-06-12 大连大学 A kind of preparation method and application that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS
CN108181364A (en) * 2017-12-22 2018-06-19 大连大学 A kind of preparation method and application of the Ag/AgCl microelectrode encapsulated membranes based on PDMS
CN108195911A (en) * 2017-12-22 2018-06-22 大连大学 A kind of preparation method and application that can be used repeatedly the Ag/AgCl microelectrodes based on PDMS
CN108717074A (en) * 2018-05-23 2018-10-30 大连大学 A kind of nano-silver thread/N doping multi-walled carbon nanotube combination electrode preparation and the method using the determination of electrode glucose
CN108899278A (en) * 2018-06-30 2018-11-27 昆山国显光电有限公司 The manufacturing method of patterned nano-silver thread film and touch panel
CN109298043A (en) * 2018-10-23 2019-02-01 大连大学 A kind of method of flexible silver nanowires of the application based on PDMS/nanogold combination electrode detection nitrite
CN107843633B (en) * 2017-11-03 2020-05-19 大连大学 Flexible electrode for copper ion determination and determination method thereof

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CN106268355A (en) * 2016-08-31 2017-01-04 浙江大学 A kind of asymmetric super parent/hydrophobic pair of property polymeric film and preparation method thereof

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107863538A (en) * 2017-11-03 2018-03-30 大连大学 A kind of electrode and its application for alcohol catalysis
CN107863538B (en) * 2017-11-03 2020-09-04 大连大学 Electrode for ethanol catalysis and application thereof
CN107843633B (en) * 2017-11-03 2020-05-19 大连大学 Flexible electrode for copper ion determination and determination method thereof
CN107991372A (en) * 2017-11-22 2018-05-04 大连大学 A kind of method for lead ion detection
CN108181364B (en) * 2017-12-22 2020-05-19 大连大学 Preparation method and application of Ag/AgCl microelectrode encapsulating film based on PDMS
CN108152348B (en) * 2017-12-22 2020-05-19 大连大学 Preparation method and application of PDMS-based micro soft Ag/AgCl electrode capable of being used repeatedly
CN108195911A (en) * 2017-12-22 2018-06-22 大连大学 A kind of preparation method and application that can be used repeatedly the Ag/AgCl microelectrodes based on PDMS
CN108195911B (en) * 2017-12-22 2020-05-19 大连大学 Preparation method and application of Ag/AgCl microelectrode based on PDMS in repeatable use
CN108181364A (en) * 2017-12-22 2018-06-19 大连大学 A kind of preparation method and application of the Ag/AgCl microelectrode encapsulated membranes based on PDMS
CN108152348A (en) * 2017-12-22 2018-06-12 大连大学 A kind of preparation method and application that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS
CN108717074A (en) * 2018-05-23 2018-10-30 大连大学 A kind of nano-silver thread/N doping multi-walled carbon nanotube combination electrode preparation and the method using the determination of electrode glucose
CN108899278A (en) * 2018-06-30 2018-11-27 昆山国显光电有限公司 The manufacturing method of patterned nano-silver thread film and touch panel
CN109298043A (en) * 2018-10-23 2019-02-01 大连大学 A kind of method of flexible silver nanowires of the application based on PDMS/nanogold combination electrode detection nitrite

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Application publication date: 20170922

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