CN106298071B - The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating - Google Patents
The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating Download PDFInfo
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- CN106298071B CN106298071B CN201610753188.6A CN201610753188A CN106298071B CN 106298071 B CN106298071 B CN 106298071B CN 201610753188 A CN201610753188 A CN 201610753188A CN 106298071 B CN106298071 B CN 106298071B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The present invention relates to flexible transparent conductive film technical field, the preparation method of the PET base material based on hydrophilic modifying/nano-silver thread nesa coating is specifically disclosed, including：From the optical grade plated film PET base material handled through two-sided hardened layer, cleaned and cleaned using ethanol/acetone mixed solvent；Hydrophilically modified to PET base material progress using low temperature argon/oxygen mixing plasma technology after drying, plasma discharge power is 10 150W, the 900s of processing time 6；Use the accurate mode being coated with that nano-silver thread alcohol dispersion liquid even compact that concentration is 0.01 10mg/ml is coated on into the PET base material surface through hydrophilic modifying, transparent conductive film is prepared after 60 200 DEG C of 10 120min of baking.The nano-silver thread transparent conductive film transmitance of PET base material surface hydrophilic modification of the present invention is high, and electric conductivity is strong, and adhesive force is good, while resistance to deflection is good, has great application prospect.
Description
Technical field
The present invention relates to flexible transparent conductive film technical field, and in particular to and a kind of PET base material based on hydrophilic modifying/
The preparation method of nano-silver thread nesa coating.
Background technology
Transparent conductive film is a kind of both conductive, has the film of high light transmittance again, is widely used in liquid crystal
Show, the electronic component field such as contact panel and solar cell.With following mobile terminal, wearable device and intelligent appliance
Deng the popularization of product, contact panel is in large size, low priceization.Traditional ITO (tin indium oxide) transparent conductive films are dilute because of raw material
Lack, it is expensive and poisonous in itself；Higher using magnetron sputtering technique production cost, impedance variations are larger, and ITO materials compared with
Crisp, the conducting film of preparation can not bend use, graphene, metal grill, nano-silver thread phase with signifying following printing technology
Than, cost price difference up to 50%.
So far, graphene also has a segment distance still in development away from volume production.And in a variety of new materials, again
It is more ripe with the development of nano-silver thread and metal grill.Although metal grill and nano-silver thread all have than ITO electric conductivity more
Advantage good, price is lower, but so far, metal grill still suffers from light tight, high reflection, Mo Rui interferes, folding property is relative
It is weaker, the urgent problem to be solved such as mould costliness.Therefore no matter nano-silver thread technology is come from the flexibility or light transmittance of material
See, be all not available for metalolic network.
Nano-silver thread technology is that nano-silver thread is prepared nano-silver thread conductive film by coating process, and metal grill
Then need by making mould, film is extruded lines, then the filling of micron-sized Argent grain is entered.Micron-sized Argent grain ratio
Nano level silver wire is thicker, and electric conductivity is no doubt more preferable, but shortcoming is also very prominent, and Argent grain is larger, visual stronger, in light
With particle can be seen under strong light, it is more crisp easily broken in addition, material is micron order, be not easy to be used as flexible screen.Due to Nano Silver
The transparent conductive film with Nano grade silver wire conductive network pattern, the line of nano-silver thread is made using radium-shine photoetching technique in line
Wide diameter is very small, about 50nm, much smaller than 1 μm, thus the problem of in the absence of not auspicious interference, can apply various sizes of
On display screen.Compared to metal grill, because line width is smaller, nano-silver thread conductive film has higher light transmittance, simultaneously
With less bending radius, resistance change rate is smaller during bending, can apply to flexible curved surface display device, is most possible
Substitute traditional ITO materials.But in the prior art, deficiency is still suffered from, as nano-silver thread is distributed not in transparent conductive film
Uniformly, pet sheet face hydrophobicity and antistatic behaviour be not strong, causes the electric conductivity of nano-silver thread film and adhesive force poor.
The content of the invention
In view of this, it is necessary in view of the above-mentioned problems, it is saturating to provide a kind of PET base material/nano-silver thread based on hydrophilic modifying
The preparation method of bright conducting film.
To achieve the above object, the present invention takes following technical scheme：
The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating of the invention, including following step
Suddenly：
The preparation of PET base material surface hydrophilic modification and nano-silver thread nesa coating；
The PET base material surface hydrophilic modification includes：From the optical grade plated film PET base material handled through two-sided hardened layer,
Cleaned and cleaned using ethanol/acetone mixed solvent；Using low temperature argon/oxygen mixing plasma technology to the PET base material after drying
Carry out hydrophilically modified, plasma discharge power is 10-150W, processing time 6-900s；
The preparation of the nano-silver thread nesa coating includes：Use the accurate mode being coated with by concentration for 0.01-10mg/
The PET base material surface through hydrophilic modifying is coated on, through 60-200 DEG C of baking ml nano-silver thread alcohol dispersion liquid even compact
Transparent conductive film is prepared after 10-120min.
As preferable, the plasma discharge power is 100W, processing time 6-600s.
As preferable, the nano-silver thread alcohol dispersion liquid concentration is 0.01-5mg/ml.
As preferable, the baking time is 10-90min, temperature is 60-150 DEG C.
It it is 50 μm, 100 μm or 125 μm as preferable, described PET base material thickness.
As preferable, the ethanol/acetone volume ratio is 1.
As preferable, the accurate coating is micro- plate gravure coating method.
The nano-silver thread transparent conductive film thickness that the present invention prepares is 50-600nm, preferably 50-300nm.
Compared with existing nano-silver thread transparent conductive film technology, beneficial effects of the present invention are：
By low temperature argon/oxygen hybrid plasma to PET base material surface carry out it is hydrophilically modified after, PET base material surface production
The oxygen-content active groups such as raw more carboxyl, carbonyl, reduce the contact angle on PET base material surface, and hydrophily obtains very big change
It is kind so that nano-silver thread alcohol dispersion liquid is preferably scattered to be attached in PET base material, is improved between nano-silver thread and PET base material
Adhesive force；
By nano-silver thread homogeneous dispersion, densely precision is coated on PET base material surface by way of micro- intaglio plate coating,
After oven temperature is toasted, alcohol solvent volatilizees completely quickly, the thickness for the nano-silver thread film that whole PET base material region is formed
To spend and into film uniformity all than more uniform, the film of formation is finer and close, and contacting with each other between nano-silver thread is compacter, so as to
Electric conductivity is also improved.
The transmitance for the nano-silver thread transparent conductive film that the present invention is prepared into is high, and electric conductivity is strong, and adhesive force is good, while resistance to
Flexibility is good, has very high application prospect.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical scheme is made further clearly and completely to describe.It should be noted that described embodiment is only the present invention one
Section Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out under the premise of creative work the every other embodiment obtained, belong to the scope of protection of the invention.
Embodiment 1
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 60s；
The preparation of step 2) nano-silver thread nesa coating：By 0.6mg/ml Nano Silver by the way of micro- intaglio plate coating
Line alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 90 DEG C of baking 60min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 50nm thickness.
Embodiment 2
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 180s；
The preparation of step 2) nano-silver thread nesa coating：By 0.6mg/ml Nano Silver by the way of micro- intaglio plate coating
Line alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 90 DEG C of baking 60min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 50nm thickness.
Embodiment 3
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 300s；
The preparation of step 2) nano-silver thread nesa coating：By 0.6mg/ml Nano Silver by the way of micro- intaglio plate coating
Line alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 90 DEG C of baking 60min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 50nm thickness.
Embodiment 4
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 60s；
The preparation of step 2) nano-silver thread nesa coating：By 1mg/ml nano-silver thread by the way of micro- intaglio plate coating
Alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 120 DEG C of baking 30min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 70nm thickness.
Embodiment 5
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 180s；
The preparation of step 2) nano-silver thread nesa coating：By 1mg/ml nano-silver thread by the way of micro- intaglio plate coating
Alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 120 DEG C of baking 30min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 70nm thickness.
Embodiment 6
Step 1) PET base material surface hydrophilic modification：100 μm of optical-grade double-sides with diaphragm are first hardened into PET base material
Cleaned, after 80 DEG C of vacuum dryings with the mixed solvent that ethanol/acetone volume ratio is 1, then using low temperature argon/oxygen hybrid plasma
Discharge process is carried out to PET base material surface, the PET base material of hydrophilic modifying is obtained after discharge power 100W, processing time 300s；
The preparation of step 2) nano-silver thread nesa coating：By 3mg/ml nano-silver thread by the way of micro- intaglio plate coating
Alcohol dispersion liquid precision is coated on the PET base material surface for the hydrophilic modifying that step 1) obtains, after 120 DEG C of baking 30min of temperature
Obtain PET base material/nano-silver thread transparent conductive film of 70nm thickness.
Comparative example 1
Step 1) PET base material surface dust：100 μm of optical-grade double-sides are first hardened into PET base material ethanol/acetone volume ratio
Dedusting is cleaned for 1 mixed solvent, the clean PET base material in surface is obtained after 80 DEG C of vacuum drying；
The preparation of step 2) nano-silver thread nesa coating：Using micro- plate gravure coating method by 0.6mg/ml nano-silver thread
Alcohol dispersion liquid precision is coated on step 1) and obtained in the PET base material of clean surface, is obtained after 90 DEG C of baking 60min of temperature
The nano-silver thread transparent conductive film of 45nm thickness.
Comparative example 2
Step 1) PET base material surface dust：100 μm of optical-grade double-sides are first hardened into PET base material ethanol/acetone volume ratio
Dedusting is cleaned for 1 mixed solvent, the clean PET base material in surface is obtained after 80 DEG C of vacuum drying；
The preparation of step 2) nano-silver thread nesa coating：Using micro- plate gravure coating method by 1mg/ml nano-silver thread second
Alcohol dispersion liquid precision is coated on step 1) and obtained in the PET base material of clean surface, is obtained after 120 DEG C of baking 30min of temperature
The nano-silver thread transparent conductive film of 60nm thickness.
It is the property indices of each embodiment nano-silver thread transparent conductive film of measure in table 1：
The performance of nano-silver thread transparent conductive film in 1 each embodiment of table
It was found from upper table 1, the transmitance of the nano-silver thread transparent conductive film of PET base material hydrophilic modifying of the invention is high,
Electric conductivity is strong, and adhesive force is good, while resistance to deflection is good, has great application prospect.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
- A kind of 1. preparation method of the PET base material based on hydrophilic modifying/nano-silver thread nesa coating, it is characterised in that including Following steps：The preparation of PET base material surface hydrophilic modification and nano-silver thread nesa coating；The PET base material surface hydrophilic modification includes：From the optical grade plated film PET base material handled through two-sided hardened layer, use The cleaning removal of impurities of ethanol/acetone mixed solvent；The PET base material is carried out using low temperature argon/oxygen mixing plasma technology after drying Hydrophilically modified, plasma discharge power is 10-150W, processing time 6-900s；The preparation of the nano-silver thread nesa coating includes：Use the mode of micro- intaglio plate coating by concentration for 0.01-10mg/ml Nano-silver thread alcohol dispersion liquid even compact be coated on the PET base material surface through hydrophilic modifying, through 60-200 DEG C baking 10- Transparent conductive film is prepared after 120min.
- 2. the preparation method of the PET base material based on hydrophilic modifying/nano-silver thread nesa coating according to claim 1, Characterized in that, the plasma discharge power is 100W, processing time 6-600s.
- 3. the preparation method of the PET base material based on hydrophilic modifying/nano-silver thread nesa coating according to claim 1, Characterized in that, the nano-silver thread alcohol dispersion liquid concentration is 0.01-5mg/ml.
- 4. the preparation method of the PET base material based on hydrophilic modifying/nano-silver thread nesa coating according to claim 1, Characterized in that, the baking time is 10-90min, temperature is 60-150 DEG C.
- 5. the PET base material based on hydrophilic modifying/nano-silver thread nesa coating according to claim 1-4 any one Preparation method, it is characterised in that described PET base material thickness is 50 μm, 100 μm or 125 μm.
- 6. the PET base material based on hydrophilic modifying/nano-silver thread nesa coating according to claim 1-4 any one Preparation method, it is characterised in that the ethanol/acetone volume ratio is 1.
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| CN201610753188.6A CN106298071B (en) | 2016-08-29 | 2016-08-29 | The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating |
| PCT/CN2017/098058 WO2018040953A1 (en) | 2016-08-29 | 2017-08-18 | Method for preparing nano silver wire transparent conductive film based on hydrophilically modified pet substrate |
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| CN201610753188.6A CN106298071B (en) | 2016-08-29 | 2016-08-29 | The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating |
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| CN106298071B (en) * | 2016-08-29 | 2017-12-29 | 广东纳路纳米科技有限公司 | The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating |
| CN106648259B (en) * | 2017-01-09 | 2020-07-03 | 京东方科技集团股份有限公司 | Preparation method of touch screen, touch screen and display device |
| CN110181921B (en) * | 2018-02-23 | 2021-03-30 | 农宝企业有限公司 | Nano silver wire structure |
| 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 |
| CN110781600B (en) * | 2019-10-30 | 2023-03-28 | 合肥微晶材料科技有限公司 | Nano-silver wire flexible transparent conductive film easy for electrode patterning and patterning method thereof |
| CN112635103B (en) * | 2020-12-18 | 2022-07-29 | 深圳先进技术研究院 | Conductive pattern, preparation method thereof and flexible electronic device |
| CN113372591B (en) * | 2021-06-17 | 2022-09-02 | 武汉理工大学 | Method for rapidly preparing ultrathin polyimide film |
| CN114496354B (en) * | 2022-01-21 | 2024-04-30 | 深圳市飞墨科技有限公司 | Preparation method and application of transparent conductive film |
| CN116444842A (en) * | 2023-03-20 | 2023-07-18 | 电子科技大学 | Self-assembly-based flexible micro-nano conductive pattern film preparation method and device |
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| US9175183B2 (en) * | 2011-05-23 | 2015-11-03 | Carestream Health, Inc. | Transparent conductive films, methods, and articles |
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| CN106298071B (en) * | 2016-08-29 | 2017-12-29 | 广东纳路纳米科技有限公司 | The preparation method of PET base material based on hydrophilic modifying/nano-silver thread nesa coating |
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| WO2010130986A1 (en) * | 2009-05-14 | 2010-11-18 | Dupont Teijin Films U.S. Limited Partnership | Transparent conductive composite films |
| CN103903817A (en) * | 2014-03-18 | 2014-07-02 | 中科院广州化学有限公司南雄材料生产基地 | Preparing method and application of transparent conducting thin film |
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Inventor after: Duan Xidong Inventor after: Li Xiaofeng Inventor after: Mao Zhihao Inventor before: Duan Xiangfeng Inventor before: Duan Xidong Inventor before: Li Xiaofeng Inventor before: Mao Zhihao |