CN106205788A - A kind of preparation of the PET/ nano-silver thread nesa coating of grafting modification - Google Patents
A kind of preparation of the PET/ nano-silver thread nesa coating of grafting modification Download PDFInfo
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- CN106205788A CN106205788A CN201610761941.6A CN201610761941A CN106205788A CN 106205788 A CN106205788 A CN 106205788A CN 201610761941 A CN201610761941 A CN 201610761941A CN 106205788 A CN106205788 A CN 106205788A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
The present invention relates to flexible transparent conductive film technical field, specifically disclose the preparation of the PET/ nano-silver thread nesa coating of a kind of grafting modification, select the optical grade plated film PET processed through two-sided hardened layer including: PET base material, and use acetone and alcohol mixed solvent that PET base material is processed, clean, drying for standby；0.1 10g coupling agent is joined in the nano-silver thread ethanol solution that concentration is 0.01 10mg/ml, is warming up to 30 150 DEG C of stirring 30 240min and obtains nano-silver thread mixed liquor；PET base material after the remove impurity of surface being immersed in nano-silver thread mixed liquor, reaction temperature controls at 30 120 DEG C, time 30 180min, after reaction terminates, repeatedly rinse through distilled water, then at 60 180 DEG C of oven cooking cycle 30 240min, prepare transparent conductive film.The PET/ nano-silver thread transparent conductive film adhesive force of the present invention is strong, and resistance to deflection is improved, simultaneously mild condition, simple to operate, has the highest using value for flexible electronic field.
Description
Technical field
The present invention relates to flexible transparent conductive film technical field, be specifically related to the PET/ nanometer of a kind of grafting modification
The preparation of silver wire nesa coating.
Background technology
Transparent conductive film is that one had both had electric conductivity, has again the thin film of high light transmittance, is widely used in liquid crystal
Show, the electronic devices and components field such as contact panel and solaode.Following mobile terminal, wearable device, intelligent appliance etc. produce
Product, have solid demand to touch panel, and simultaneously along with contact panel is in large size, low priceization, and tradition ito thin film can not
Being applied to deformable surface, the essential problem such as electric conductivity and light transmittance such as is not easily overcome at the factor, and many manufacturers begin one's study ITO's one after another
Succedaneum, the material such as including nano-silver thread, metal grill, CNT and Graphene.From market reaction, application is new
The proportion shared by film product that material technology produces is improving year by year.At present, Graphene is still in development, from volume production also
There is far distance.CNT industrial volume production technology is the most perfect, and the film product electric conductivity that it is made can't reach
The level of common ito thin film.The product of metal grill fabrication techniques has the most auspicious unsurmountable interference problem, application to be limited
System.To reduce the live width of metal in metal grill, then needing more to change system into technique, cost can increase therewith, and has easily
The problems such as broken string.Nano-silver thread technology is then most possibly close to the new material of volume production.
Nano-silver thread technology is simple because of making technology, and printing process can be used quickly to produce large-area contact panel, with
Time there is less bending radius, and when bending, resistance change rate is less, applies and has the equipment that flexible curved surface shows.Existing
The backing material used in some flexible curved surface equipment mostly is polyethylene terephthalate (PET) thin film, PET macromolecular chain
Compound with regular structure, degree of crystallinity is higher, and without highly polar group in molecule, therefore its surface affinity is poor.The side currently mainly used
Method has surface-coated method, surface oxidation method, plasma method, high-energy radiation, ultraviolet radiation etc., but this all have impact on PET's
Bulk properties or be unable to reach long-term modified effect.Visible, prior art still suffers from bigger defect.
Summary of the invention
In view of this, it is necessary to for the problems referred to above, it is provided that a kind of surface modification that both can reach improves the mesh of adhesive force
, the preparation method of the PET/ nano-silver thread nesa coating of the grafting modification of the bulk properties of base material will not be damaged again.
For achieving the above object, the present invention takes techniques below scheme:
The preparation of the PET/ nano-silver thread nesa coating of the grafting modification of the present invention, including: PET base material surface is removed
Miscellaneous, nano-silver thread mixed liquor is prepared and the preparation of nesa coating；
Described PET base material surface remove impurity includes: PET base material selects the optical grade plated film PET processed through two-sided hardened layer,
And use acetone and alcohol mixed solvent that PET base material is processed, clean, drying for standby；
The preparation of described nano-silver thread mixed liquor includes: it is 0.01-10mg/ml's that 0.1-10g coupling agent joins concentration
In nano-silver thread ethanol solution, the coupling agent obtained-nano-silver thread ethanol solution is warming up to 30-150 DEG C of stirring 30-240min and obtains
To nano-silver thread mixed liquor；
The preparation of nesa coating includes: the PET base material after the remove impurity of surface be immersed in nano-silver thread mixed liquor, instead
Temperature is answered to control at 30-120 DEG C, time 30-180min, after reaction terminates, repeatedly rinses through distilled water, then bakes at 60-180 DEG C
Case baking 30-240min, prepares transparent conductive film.
As preferably, described coupling agent addition is 0.1-5g, and the concentration of nano-silver thread ethanol solution is 0.01-5mg/
ml。
As preferably, described coupling agent-nano-silver thread ethanol solution is warming up to 30-120 DEG C of stirring 30-150min.
As preferably, in the preparation of described nesa coating, reaction temperature controls at 30-100 DEG C, time 30-
150min；Described oven cooking cycle temperature is 60-120 DEG C, and the time is 30-150min.
As preferably, described PET base material thickness is 50um, 100um, 125um, and carries protecting film.
As preferably, described dehydrated alcohol and acetone volume ratio are 1.
As preferably, described coupling agent is mercaptosilane coupling agents KH-580 or mercaptosilane coupling agents KH-590.
Further, described coupling agent is mercaptosilane coupling agents KH-590.
The 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, the invention have the benefit that
The present invention uses nano-silver thread replacement nano-Ag particles to be scattered in ethanol as thin film of conductive material, passes through silver wire
Between contact with each other reach conduct electricity purpose；
Make on nano-silver thread surface chemical modification even by the sulfydryl of silane coupler one end and the coordination of nanometer silver
Connection agent, the siloxy group of the coupling agent other end combines with the hardened layer on pet sheet face simultaneously, will receive with the form of chemical bonding
Rice silver wire is fixedly attached to pet sheet face, makes the adhesive force of the nano-silver thread transparent conductive film of preparation be largely increased.
The transparent conductive film adhesive force of the present invention is strong, and resistance to deflection is improved, simultaneously mild condition, simple to operate,
For flexible electronic field, there is the highest using value.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this
Bright technical scheme is made the most 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 the every other embodiment obtained under creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
Step 1) remove impurity of PET base material surface: the anhydrous second of PET base material that the 50um optical-grade double-side with protecting film is hardened
After alcohol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80 DEG C
The PET base material of clean surface is obtained after vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 0.5g silane coupler KH-590 is joined receiving of 0.08mg/ml
In rice silver wire ethanol solution, the coupling agent obtained-nano-silver thread ethanol solution, after 60 DEG C of magnetic agitation 90min, prepares
Nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 40 DEG C, reaction 150min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then at oven temperature 100 DEG C, toast 60min, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Embodiment 2
Step 1) remove impurity of PET base material surface: the anhydrous second of PET base material that the 50um optical-grade double-side with protecting film is hardened
After alcohol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80 DEG C
The PET base material of clean surface is obtained after vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 1g silane coupler KH-590 is joined the nanometer silver of 0.3mg/ml
In line ethanol solution, after 90 DEG C of magnetic agitation 60min, prepare nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 60 C, reaction 120min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then through the lower 60min of oven temperature 100 DEG C baking, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Embodiment 3
Step 1) remove impurity of PET base material surface: the 100um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 0.5g silane coupler KH-590 is joined receiving of 0.08mg/ml
In rice silver wire ethanol solution, after 60 DEG C of magnetic agitation 90min, prepare nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 40 DEG C, reaction 150min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then at oven temperature 100 DEG C, toast 60min, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Embodiment 4
Step 1) remove impurity of PET base material surface: the 100um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 1g silane coupler KH-590 is joined the nanometer silver of 0.3mg/ml
In line ethanol solution, after 90 DEG C of magnetic agitation 60min, prepare nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 60 C, reaction 120min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then through the lower 60min of oven temperature 100 DEG C baking, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Embodiment 5
Step 1) remove impurity of PET base material surface: the 125um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 0.5g silane coupler KH-590 is joined receiving of 0.08mg/ml
In rice silver wire ethanol solution, after 60 DEG C of magnetic agitation 90min, prepare nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 40 DEG C, reaction 150min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then through the lower 60min of oven temperature 100 DEG C baking, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Embodiment 6
Step 1) remove impurity of PET base material surface: the 125um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread mixed liquor: 3g silane coupler KH-590 is joined the nano-silver thread of 2mg/ml
In ethanol solution, after 90 DEG C of magnetic agitation 60min, prepare nano-silver thread mixed liquor；
Step 3) preparation of nesa coating: by step 1) PET base material of clean surface that obtains is immersed in step 2) system
In standby nano-silver thread mixed liquor, after temperature 90 DEG C, reaction 120min, repeatedly rinse PET base material surface through distilled water and do not connect
The polymer of branch, then through the lower 100min of oven temperature 90 DEG C baking, obtain the PET/ nano-silver thread electrically conducting transparent that thickness is 50nm
Thin film.
Comparative example 1
Step 1) remove impurity of PET base material surface: the anhydrous second of PET base material that the 50um optical-grade double-side with protecting film is hardened
After alcohol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80 DEG C
The PET base material of clean surface is obtained after vacuum drying；
Step 2) preparation of nano-silver thread transparent conductive film: directly by step 1) PET base material of clean surface that obtains
Be immersed in the nano-silver thread ethanol solution of 0.3mg/ml, 60 DEG C dipping 180min, with after distilled water flushing through oven temperature 100
DEG C baking 60min, obtain the nano-silver thread transparent conductive film that thickness is 40nm.
Comparative example 2
Step 1) remove impurity of PET base material surface: the 100um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread transparent conductive film: directly by step 1) PET base material of clean surface that obtains
Be immersed in the nano-silver thread ethanol solution of 0.3mg/ml, 60 DEG C dipping 180min, with after distilled water flushing through oven temperature 100
DEG C baking 60min, obtain the nano-silver thread transparent conductive film that thickness is 40nm.
Comparative example 3
Step 1) remove impurity of PET base material surface: the 125um optical-grade double-side with protecting film is hardened PET base material with anhydrous
After ethanol/acetone volume ratio is the mixed solvent cleaning of 1, then the mixed solvent with distilled water flushing PET base material remained on surface, 80
The PET base material of clean surface is obtained after DEG C vacuum drying；
Step 2) preparation of nano-silver thread transparent conductive film: directly by step 1) PET base material of clean surface that obtains
Be immersed in the nano-silver thread ethanol solution of 0.3mg/ml, 60 DEG C dipping 180min, with after distilled water flushing through oven temperature 100
DEG C baking 60min, obtain the nano-silver thread transparent conductive film that thickness is 40nm.
For measuring each embodiment properties through the PET nano-silver thread transparent conductive film of grafting modification in table 1
Index:
The performance of nano-silver thread transparent conductive film in table 1 the various embodiments described above
As can be known from the above table, the present invention's is strong through grafting modification PET nano-silver thread transparent conductive film adhesive force, resistance to scratches
Song is improved, simultaneously mild condition, simple to operate, has the highest using value for flexible electronic field.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. the preparation of the PET/ nano-silver thread nesa coating of a grafting modification, it is characterised in that including: PET base material
Surface remove impurity, the preparation of nano-silver thread mixed liquor and the preparation of nesa coating；
Described PET base material surface remove impurity includes: PET base material selects the optical grade plated film PET processed through two-sided hardened layer, and adopts
With acetone and alcohol mixed solvent PET base material processed, clean, drying for standby；
The preparation of described nano-silver thread mixed liquor includes: 0.1-10g coupling agent joins the nanometer that concentration is 0.01-10mg/ml
In silver wire ethanol solution, the coupling agent obtained-nano-silver thread ethanol solution is warming up to 30-150 DEG C of stirring 30-240min and is received
Rice silver wire mixed liquor；
The preparation of nesa coating includes: the PET base material after the remove impurity of surface be immersed in nano-silver thread mixed liquor, reaction temperature
Degree controls at 30-120 DEG C, time 30-180min, after reaction terminates, repeatedly rinses through distilled water, then dries at 60-180 DEG C of baking box
Roasting 30-240min, prepares transparent conductive film.
The preparation of the PET/ nano-silver thread nesa coating of grafting modification the most according to claim 1, its feature exists
In, described coupling agent addition is 0.1-5g, and the concentration of nano-silver thread ethanol solution is 0.01-5mg/ml.
The preparation of the PET/ nano-silver thread nesa coating of grafting modification the most according to claim 1, its feature exists
In, described coupling agent-nano-silver thread ethanol solution is warming up to 30-120 DEG C of stirring 30-150min.
The preparation of the PET/ nano-silver thread nesa coating of grafting modification the most according to claim 1, its feature exists
In, in the preparation of described nesa coating, reaction temperature controls at 30-100 DEG C, time 30-150min；Described oven cooking cycle temperature
Degree is for 60-120 DEG C, and the time is 30-150min.
5. according to the system of the PET/ nano-silver thread nesa coating of the grafting modification described in claim 1-4 any one
Standby, it is characterised in that described PET base material thickness is 50um, 100um, 125um, and carries protecting film.
6. according to the system of the PET/ nano-silver thread nesa coating of the grafting modification described in claim 1-4 any one
Standby, it is characterised in that described dehydrated alcohol and acetone volume ratio are 1.
7. according to the system of the PET/ nano-silver thread nesa coating of the grafting modification described in claim 1-4 any one
Standby, it is characterised in that described coupling agent is mercaptosilane coupling agents KH-580 or mercaptosilane coupling agents KH-590.
The preparation of the PET/ nano-silver thread nesa coating of grafting modification the most according to claim 7, its feature exists
In, described coupling agent is mercaptosilane coupling agents KH-590.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610761941.6A CN106205788B (en) | 2016-08-29 | 2016-08-29 | A kind of preparation of the PET/ nano-silver thread nesa coatings of grafting modification |
| PCT/CN2017/098060 WO2018040955A1 (en) | 2016-08-29 | 2017-08-18 | Preparation of chemical grafting-modified pet/nano silver wire transparent conductive film |
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|---|---|---|---|
| CN201610761941.6A CN106205788B (en) | 2016-08-29 | 2016-08-29 | A kind of preparation of the PET/ nano-silver thread nesa coatings of grafting modification |
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| CN106205788B CN106205788B (en) | 2017-10-31 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106648226A (en) * | 2016-12-08 | 2017-05-10 | 上海交通大学 | Transparent pressure sensor and manufacturing method of piezoresistive material thereof |
| WO2018040955A1 (en) * | 2016-08-29 | 2018-03-08 | 广东纳路纳米科技有限公司 | Preparation of chemical grafting-modified pet/nano silver wire transparent conductive film |
| CN109949974A (en) * | 2019-03-15 | 2019-06-28 | 广东格瑞纳思薄膜科技有限公司 | A kind of PET base nano-silver thread graphene composite transparent flexible conductive film of covalent bonding and preparation method thereof |
| CN111180112A (en) * | 2020-01-16 | 2020-05-19 | 南通纺织丝绸产业技术研究院 | Metal nanowire flexible conductive film and preparation method thereof |
| CN111440346A (en) * | 2020-03-12 | 2020-07-24 | 深圳市华科创智技术有限公司 | Nano-silver wire antibacterial layer and nano-silver wire anti-mask |
| CN111796344A (en) * | 2019-04-08 | 2020-10-20 | 超晶维(昆山)光电科技有限公司 | Preparation method of silicon dioxide nano silver wire antireflection film |
| CN113393975A (en) * | 2021-06-09 | 2021-09-14 | 哈尔滨工业大学 | Preparation method of surface-modified silver nanowire flexible transparent conductive film |
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| WO2018040955A1 (en) * | 2016-08-29 | 2018-03-08 | 广东纳路纳米科技有限公司 | Preparation of chemical grafting-modified pet/nano silver wire transparent conductive film |
| CN106648226A (en) * | 2016-12-08 | 2017-05-10 | 上海交通大学 | Transparent pressure sensor and manufacturing method of piezoresistive material thereof |
| CN109949974A (en) * | 2019-03-15 | 2019-06-28 | 广东格瑞纳思薄膜科技有限公司 | A kind of PET base nano-silver thread graphene composite transparent flexible conductive film of covalent bonding and preparation method thereof |
| CN109949974B (en) * | 2019-03-15 | 2020-08-25 | 广东格瑞纳思薄膜科技有限公司 | Covalently bonded PET-based nano silver wire graphene composite transparent flexible conductive film and preparation method thereof |
| CN111796344A (en) * | 2019-04-08 | 2020-10-20 | 超晶维(昆山)光电科技有限公司 | Preparation method of silicon dioxide nano silver wire antireflection film |
| CN111180112A (en) * | 2020-01-16 | 2020-05-19 | 南通纺织丝绸产业技术研究院 | Metal nanowire flexible conductive film and preparation method thereof |
| CN111180112B (en) * | 2020-01-16 | 2021-05-28 | 南通纺织丝绸产业技术研究院 | Metal nanowire flexible conductive film and preparation method thereof |
| CN111440346A (en) * | 2020-03-12 | 2020-07-24 | 深圳市华科创智技术有限公司 | Nano-silver wire antibacterial layer and nano-silver wire anti-mask |
| CN113393975A (en) * | 2021-06-09 | 2021-09-14 | 哈尔滨工业大学 | Preparation method of surface-modified silver nanowire flexible transparent conductive film |
| CN114753142A (en) * | 2022-05-24 | 2022-07-15 | 浙江王金非织造布有限公司 | Spunlaced non-woven fabric capable of achieving lasting antibacterial effect and used for artificial leather and preparation method of spunlaced non-woven fabric |
| CN114753142B (en) * | 2022-05-24 | 2023-11-24 | 浙江王金非织造布有限公司 | Durable antibacterial spunlaced non-woven fabric for artificial leather and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN106205788B (en) | 2017-10-31 |
| WO2018040955A1 (en) | 2018-03-08 |
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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 |