CN108250469A - A kind of production technology of nano-silver thread transparent conductive film - Google Patents
A kind of production technology of nano-silver thread transparent conductive film Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The present invention relates to a kind of production technologies of nano-silver thread transparent conductive film, include the following steps：（1）Base material prepares：The base material of selection is PET sheet base, and ready PET sheet base is carried out cure process；（2）It is coated with the coating nano-silver thread coating fluid being configured and Protection glue coating fluid：The nano-silver thread coating fluid being configured and Protection glue coating fluid are applied to by coating apparatus on PET sheet base respectively；（3）It is dry：Coated film is dried；（4）Winding：The finished product produced is wound.Present invention process can effectively improve the rate of good of nano-silver thread conductive glue slice, accelerate replacement of the nano-silver thread conductive glue slice to ITO.
Description
Technical field
The invention belongs to produce electrically conducting transparent film technologies field, and in particular to a kind of life of nano-silver thread transparent conductive film
Production. art.
Background technology
As domestic capacitance plate shipment area in 2013 is more than 4,000,000 square metres, wherein ITO electro-conductive glass demand is more than
3600000 square metres, ITO PET conductive films demand is more than 1,400,000 square metres.From touch screen industry upstream materials into one's duty
Analysis, ITO materials occupy 40% or so.And with the development of touch screen industry, the demand to ITO materials will be increasing, as
Rare metal indium needed for ITO materials, not only price rises steadily therewith, and will have the danger run out.
Nano-silver thread (SNW, silvernanowire) technology, be by nano-silver thread ink material be applied to PET base material or
On person's glass substrate, then using radium-shine photoetching technique, portray and be made with the transparent of Nano grade silver wire conductive network pattern
Conductive film.Physical mechanism is made since its is special, the diameter of the line width of nano-silver thread is very small, about 50nm, remote small
In 1um, because of the problem of Mo Rui interference may be not present, can apply on the display screen of various sizes.In addition, due to line width compared with
Small, conductive film made of silver wire technology can reach higher light transmittance, example compared to film made of metal grill technology
The film product as made of 3M companies using micro- coining method can reach 89% light transmittance.Again, nano-silver thread film compared to
Metal grill film has smaller bending radius, and in bending, resistance change rate is smaller, applies with curved-surface display
It is more advantageous when equipment, such as smartwatch, bracelet etc. are upper.
At present, a large amount of research has shown that nano silver wire can be used for preparing touch screen, bending Organic Light Emitting Diode
(OLED), performance is still in wearable electronic, electronic skin and the bending transparent electrodes such as solar cell, after bending 1000 times
It is so very stable.In addition, nano-silver thread just possess raw material sources it is extensive, it is cheap, possess excellent crisp toughness, be suitble to big rule
Mould industrialized production.In conclusion nano-silver thread is the ITO substitutes that only one has practical application prospect, become flexible
The leading role of screen.
In addition, according to media report, Apple Inc. attracts star's product iWatch that everybody pays close attention to will be using the nano silver of TPK companies
Line thin film technique, it was demonstrated that nano-silver thread product has the stability of apparent technical advantage and industrial chain really.
In the prior art, the patent document about the preparation of nano-silver thread is very more, as application No. is
" 201510507980.9 ", patent name are " preparation method of nano-silver thread "；" 201510223402.2 ", patent name are
" a kind of nano-silver thread dispersion liquid for being used to prepare conductive film ".But about the patent of nano-silver thread transparent conductive film industrialization
It is considerably less, the industrialized method of the high nano-silver thread transparent conductive film of especially a kind of yields that can produce high quality.
As being " a kind of production method of nano-silver thread transparent conductive film " application No. is " 201410229462.0 ", patent name.From this
A patent can significantly find out, do not have above nano-silver thread coating one layer can be with the protection gel coating of stiffened, that produces receives
Rice silver wire transparent conductive film, either in process of production, in wrapup procedure, during cutting and during use all very
It is easy to cause electrically conducting transparent film and is scratched and apparent disadvantage occur or even draw the nano-silver thread in figure layer to break, influence user
Use；And its nano-silver thread electrically conducting transparent film resistivity produced is more than 50ohm/sq, reduces transparent lead
The scope of application of electrolemma.
Invention content
The object of the present invention is to provide a kind of production technology of nano-silver thread transparent conductive film, which is by that will receive
On the base material that rice silver wire coating solution is crossed to cure process, the photo electric of nano-silver thread electrically conducting transparent film can be effectively improved
Energy：Increase light transmittance, reduce mist degree and increase the mechanical resistance energy of film：Resistance to marring and rub resistance.And it is flowed and squeezed by slope
Extrusion cloth, by primary double-deck extrusion coated technology, disposably by nano-silver thread coating fluid and Protection glue coating solution to PET
Either pass through slope streaming extrusion coated, nick coating, slit type extrusion coated, roller coating or a variety of coating sides of blade coating in chip base
Formula is freely combined, and on nano-silver thread coating fluid and Protection glue coating solution to PET sheet base, can will greatly improve production effect
Rate greatly uses manpower and material resources sparingly, and reduces cost, is advantageously implemented industrialization production, moreover it is possible to which the effective nano-silver thread that improves is led
The rate of good of electric film accelerates replacement of the nano-silver thread conductive glue slice to ITO.
To achieve these goals, the technical solution adopted by the present invention is as follows：
The present invention provides a kind of production technologies of nano-silver thread transparent conductive film, include the following steps：
(1) base material prepares：The base material of selection is PET sheet base, and ready PET sheet base is carried out cure process；
(2) the coating nano-silver thread coating fluid and Protection glue coating fluid that coating has been configured：The nano-silver thread coating fluid that will be configured
It is applied on PET sheet base by coating apparatus respectively with Protection glue coating fluid；
(3) it is dry：Coated film is dried；
(4) it winds：The finished product produced is wound；
(5) packaging is cut：The specification of the finished product wound on demand is carried out cutting packaging.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, cure process is coated with using nick in step (1), item
Seam extrusion coated carries out single side or double spread hardening bath to PET sheet base, carries out cure process.
By weight percentage, the key component composition of above-mentioned hardening bath：Pure acrylic resin 2.5%-7%, ten functional groups
Polyurethane resin 7.5-18%, two functional polyurethane resin 16-26%, reactive diluent 5-10%, photoinitiator 1-4% and
Solvent 45%-55%.
The reactive diluent for lauric acid acrylate, tetrahydrofurfuryl acrylate, tripropylene glycol diacrylate,
One or more of 1,6- hexanediyl ester and 2- hydroxyethyl methacrylate phosphates composition.
The photoinitiator is methyl benzoylformate, bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides of phenyl, 1- hydroxyls-ring
One or more of hexyl-phenyl ketone and 2- hydroxy-2-methyl -1- phenyl -1- acetone composition.
The solvent is that solvent is one or more of butanone, ethylene glycol, acetone, methyl ether composition.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (1), PET sheet base non-nano silver wire applies
Cloth cover need to be coated with hardening coat, and making its hardness, light transmittance increases 0.5- relative to the PET sheet base of non-hardened processing in more than 1H
3%, mist degree relative to non-hardened processing PET sheet base reduce 0.2-0.8%, light transmittance 90%~93%, mist degree≤
0.7%, the thickness of PET sheet base is 25~200 μm, in 150~200 DEG C of temperature, pressure be hot pressing under 5MPa 20~40 seconds, surface
It is flawless.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (2), the nano-silver thread coating fluid is matched
Put method：The nano-silver thread of a diameter of 10~100nm, length≤200 μm are dissolved in solid content to be 0.5~10wt%, put down
In the colloidal sol that equal grain size is 10~100nm so that contain 1~10g of silver in per 1Kg nano-silver thread coating fluids；Nano-silver thread is coated with
Solid content is 0.5~11wt% in liquid, and viscosity is 1~25cps, and nano-silver thread coating coating weight is 10~50mL/m2。
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (2), the Protection glue coating fluid is metal oxygen
Compound colloidal sol, the pH of metal oxide sol are 3~6, and solid content is 0.1~10wt%, protection gel coating coating weight for 10~
50mL/m2。
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (2), the coating method of the coating is
Extrusion coated is flowed on slope, by primary double-deck extrusion coated technology, disposably applies nano-silver thread coating fluid and Protection glue coating fluid
On cloth to PET sheet base.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (2), the coating method of the coating is miniature
Intaglio plate coating, roller coating, slit type extrusion coated or blade coating, but once it is merely able to one layer of coating.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (3), the drying in the drying process
At 20 DEG C or more, drying time is more than 4 minutes temperature.
According to the production technology of above-mentioned nano-silver thread transparent conductive film, in step (4), the finished product：Light transmittance is made
It is 75~92%, mist degree≤3%, surface resistivity is 10~300ohm/sq, 3~5H of hardness, is added through 150~200 DEG C of binding items
Heat binding test 20~30 seconds, surface resistivity no longer changes.
Compared with prior art, beneficial effects of the present invention：
Present invention process is by the base material of crossing nano-silver thread coating solution to cure process, can effectively carry and receive
The photoelectric properties of rice silver wire electrically conducting transparent film：Increase light transmittance, reduce mist degree and increase the mechanical resistance energy of film：Scratch resistance
Property and rub resistance.And pass through slope streaming extrusion coated, nick coating, slit type extrusion coated, roller coating or a variety of paintings of blade coating
Mode for cloth is freely combined, and can greatly improve production efficiency, greatly use manpower and material resources sparingly, reduce cost, be advantageously implemented production
Industry metaplasia is produced, moreover it is possible to which the effective rate of good for improving nano-silver thread conductive glue slice accelerates nano-silver thread conductive glue slice to replace ITO
Generation.
Description of the drawings
Fig. 1 is nano-silver thread electrically conducting transparent film Structure of cross section figure；It is from top to bottom followed successively by Fig. 1：11. protect glue-line；12.
Nano-silver thread layer；3.PET chip bases；14. hardening coat；
Fig. 2 is application angle α when being positive angle slope streaming extrusion coated Structure of cross section figure during i.e. α ＞ 0；1. is flow in Fig. 2 in slit
The Protection glue coating fluid gone out；2. for the nano-silver thread coating fluid flowed out in slit；3. for PET sheet base；It is applied 4. being squeezed for slope streaming
The leftover of bolt of cloth；
Fig. 3 is application angle α slope streaming extrusion coated Structure of cross section figure when being negative angle i.e. α ＜ 0；1. is flow out in Fig. 3 in slit
Protection glue coating fluid；2. for the nano-silver thread coating fluid flowed out in slit；3. for PET sheet base；4. for slope streaming extrusion coated
Head.
Specific embodiment
Below by embodiment, the invention will be further described, but does not therefore limit the present invention to the embodiment
Within the scope of.
Embodiment 1
A kind of production method of nano-silver thread transparent conductive film, includes the following steps：
(1) base material prepares：By on the hardening coating solution to PET sheet base being configured, by weight percentage, hardened layer is coated with
The key component of liquid is：Pure acrylic resin 7%, ten functional polyurethane resins 11%, two functional polyurethane resins 20%,
Lauric acid acrylate 6%, methyl benzoylformate 6%, butanone 50%；Cure process is carried out to chip base；Make PET sheet Ji Feina
Rice silver wire is coated with surface hardness in more than 1H；Light transmittance 92%, mist degree≤0.7%, the thickness of PET sheet base is 100 μm, and coat side reaches
Because of value >=50, through 190 DEG C, 5Mpa hot pressing 30 seconds, surface is flawless；Ready PET sheet base is positioned over feed rack；
(2) nano-silver thread coating fluid and Protection glue coating fluid are coated with：The nano-silver thread coating fluid and Protection glue that have been configured are coated with
Liquid is applied to by coating apparatus on PET sheet base respectively；The nano-silver thread coating fluid configuration method：By a diameter of 10~
100nm, length≤200 μm nano-silver thread be dissolved in that solid content is 0.5~10wt%, average grain diameter is 10~100nm's
In colloidal sol so that contain 1~10g of silver in per 1Kg nano-silver thread coating fluids；In nano-silver thread coating fluid solid content for 0.5~
11wt%, viscosity are 1~25cps, and nano-silver thread coating coating weight is 30mL/m2。
The Protection glue coating fluid is metal oxide sol, and the pH of metal oxide sol is 3~6, solid content for 0.1~
10wt%, protection gel coating coating weight are 30mL/m2；
(3) it is dry：Coated film, which enters in dry road, to be dried.Drying condition is 130 DEG C >=T >=20 DEG C of temperature, when
Between 2min.
(4) it winds：The finished product that will have been produced, is wound by winder.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 1 below：
The transparent conductive film end properties index that 1 embodiment of the present invention 1 of table is produced
Embodiment 2
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 5%, ten functional polyurethane resins 13%, two functional polyurethanes
Resin 26%, tetrahydrofurfuryl acrylate 6%, bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides 3% of phenyl, ethylene glycol
47%；2. the coating weight of nano-silver thread coating is 10mL/m2。
The transparent conductive film end properties index that the present invention produces, it is as shown in table 2 below：
The transparent conductive film end properties index that 2 embodiment of the present invention 2 of table is produced
Embodiment 3
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 5%, ten functional polyurethane resins 18%, two functional polyurethanes
Resin 23%, tripropylene glycol diacrylate 5%, 1- hydroxy-cyclohexyl-phenyls ketone 3%, acetone 46%；2. nano-silver thread
The coating weight of coating is 50mL/m2。
The transparent conductive film end properties index that the present invention produces, it is as shown in table 3 below：
The transparent conductive film end properties index that 3 embodiment of the present invention 3 of table is produced
Embodiment 4
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 6%, ten functional polyurethane resins 15%, two functional polyurethanes
Resin 21%, 2- hydroxyethyl methacrylate phosphate 10%, 2- hydroxy-2-methyl -1- phenyl -1- acetone 3%, methyl ether
45%；2. the coating weight for protecting gel coating is 10mL/m2。
The transparent conductive film end properties index that the present invention produces, it is as shown in table 4 below：
The transparent conductive film end properties index that 4 embodiment of the present invention 4 of table is produced
Embodiment 5
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 4.5%, ten functional polyurethane resins 14%, two function reunion ammonia
Ester resin 24%, lauric acid acrylate 7%, 2- hydroxy-2-methyl -1- phenyl -1- acetone 4%, butanone 46.5%；2. it protects
The coating weight of gel coating is 50mL/m2。
The transparent conductive film end properties index that the present invention produces, it is as shown in table 5 below：
The transparent conductive film end properties index that 5 embodiment of the present invention 5 of table is produced
Embodiment 6
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 2.5%, ten functional polyurethane resins 15%, two function reunion ammonia
Ester resin 26%, tetrahydrofurfuryl acrylate 7%, 1- hydroxy-cyclohexyl-phenyls ketone 3%, ethylene glycol 46.5%；2. it does
Dry temperature is 20 DEG C, and the time is 20 minutes.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 6 below：
The transparent conductive film end properties index that 6 embodiment of the present invention 6 of table is produced
Embodiment 7
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 6%, ten functional polyurethane resins 15%, two functional polyurethanes
Resin 15%, tripropylene glycol diacrylate 5%, bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides 4% of phenyl, methyl ether
55%；2. drying temperature is 70 DEG C, the time is 4 minutes.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 7 below：
The transparent conductive film end properties index that 7 embodiment of the present invention 7 of table is produced
Embodiment 8
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
1. the component of hardened layer coating fluid is：Pure acrylic resin 7%, ten functional polyurethane resins 8%, two functional polyurethane trees
Fat 26%, 1,6- hexanediyl esters 10%, methyl benzoylformate 4%, butanone 45%；2. drying temperature is 130 DEG C,
Time is 4 minutes.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 8 below：
The transparent conductive film end properties index that 8 embodiment of the present invention 8 of table is produced
Embodiment 9
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
The component of hardened layer coating fluid is：Pure acrylic resin 6%, ten functional polyurethane resins 13.5%, two functional polyurethanes
Resin 20%, tetrahydrofurfuryl acrylate 6%, methyl benzoylformate 4%, ethylene glycol 50.5%；2. drying temperature is 70
DEG C, the time is 20 minutes.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 9 below：
The transparent conductive film end properties index that 9 embodiment of the present invention 9 of table is produced
Embodiment 10
The key step and method of the present embodiment are same as Example 1, and narration is not repeated herein, the difference is that
The component of hardened layer coating fluid is：Pure acrylic resin 6%, ten functional polyurethane resins 15%, two functional polyurethane trees
Fat 24%, 2- hydroxyethyl methacrylate phosphate 7.5%, bis- (2,4, the 6- trimethylbenzoyl) phosphine oxides of phenyl
1.5%, acetone 46%；2. drying temperature is 130 DEG C, the time is 20 minutes.
The transparent conductive film end properties index that the present invention produces, it is as shown in table 10 below：
The transparent conductive film end properties index that 10 embodiment of the present invention 10 of table is produced
Comparative example 1
The key step and method of this comparative example are same as Example 5, and narration is not repeated herein, the difference is that
It with embodiment 5 is the same model of same producer but not hardened that the PET base material used, which is,.
The transparent conductive film end properties index that this comparative example is produced, it is as shown in table 11 below：
The transparent conductive film end properties index that 11 comparative example 1 of table is produced
Comparative example 2
The key step and method of this comparative example are same as Example 2, and narration is not repeated herein, the difference is that
It with embodiment 2 is the same model of same producer but not hardened that the PET base material used, which is,.
The transparent conductive film end properties index that this comparative example is produced, it is as shown in table 12 below：
The transparent conductive film end properties index that 12 comparative example 2 of table is produced
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art, not
It is detached under the premise of general idea of the present invention, several changes and improvements can also be made, these should also be considered as the protection of the present invention
Range.
Claims (10)
1. a kind of production technology of nano-silver thread transparent conductive film, it is characterised in that include the following steps：
（1）Base material prepares：The base material of selection is PET sheet base, and ready PET sheet base is carried out cure process；
（2）It is coated with the coating nano-silver thread coating fluid being configured and Protection glue coating fluid：The nano-silver thread coating fluid that will be configured
It is applied on PET sheet base by coating apparatus with Protection glue coating fluid；
（3）It is dry：Coated film is dried；
（4）Winding：The finished product produced is wound.
2. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（1）In it is hard
Change processing is coated with using nick, slit-aperture type extrusion coated, is carried out single side or double spread hardening bath to PET sheet base, is carried out
Cure process.
3. the production technology of nano-silver thread transparent conductive film according to claim 2, it is characterised in that：With weight percent
Meter, the hardening bath key component composition：Pure acrylic resin 2.5%-7%, ten functional polyurethane resin 7.5-18%, two officials
Polyurethane resin 16-26%, reactive diluent 5-10%, photoinitiator 1-4% and solvent 45%-55% can be rolled into a ball.
4. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（1）In,
PET sheet base non-nano silver wire coated face need to be coated with hardening coat, and making its hardness, light transmittance is relative to non-hardened place in more than 1H
The PET sheet base of reason increases 0.5-3%, and mist degree reduces 0.2-0.8% relative to the PET sheet base of non-hardened processing, and light transmittance 90% ~
93%, mist degree≤0.7%, the thickness of PET sheet base is 25 ~ 200 μm, in 150 ~ 200 DEG C of temperature, pressure be hot pressing 20 ~ 40 under 5MPa
Second, surface is flawless.
5. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（2）In, institute
State nano-silver thread coating fluid configuration method：The nano-silver thread of a diameter of 10 ~ 100nm, length≤200 μm is dissolved in solid content
For in 0.5 ~ 10wt%, the colloidal sol that average grain diameter is 10 ~ 100nm so that contain 1 ~ 10g of silver in per 1Kg nano-silver thread coating fluids；
Solid content is 0.5 ~ 11 wt% in nano-silver thread coating fluid, and viscosity is 1 ~ 25cps, and nano-silver thread coating coating weight is 10 ~ 50
mL/m2。
6. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（2）In, institute
Protection glue coating fluid is stated as metal oxide sol, the pH of metal oxide sol is 3 ~ 6, and solid content is 0.1 ~ 10wt%, is protected
Gel coating coating weight is 10 ~ 50 mL/m2。
7. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（2）In, institute
The coating method for stating coating flows extrusion coated for slope, by primary double-deck extrusion coated technology, is disposably coated with nano-silver thread
On liquid and Protection glue coating solution to PET sheet base.
8. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（2）In, institute
The coating method for stating coating is micro gravure coating, roller coating, slit type extrusion coated or blade coating, can only once be coated with one layer,
Need to make two bites at a cherry coating.
9. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（3）In, institute
The drying temperature in drying process is stated at 20 DEG C or more, drying time is more than 4 minutes.
10. the production technology of nano-silver thread transparent conductive film according to claim 1, it is characterised in that：Step（4）In,
The finished product：It is 75 ~ 92% that light transmittance, which is made, mist degree≤3%, and surface resistivity is 10 ~ 300 ohm/sq, 3 ~ 5H of hardness, through 150
~ 200 DEG C of binding item heating bindings are tested 20 ~ 30 seconds, and surface resistivity no longer changes.
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| CN109694663A (en) * | 2018-12-05 | 2019-04-30 | 深圳市摩码科技有限公司 | A kind of high transparency protective film and preparation method thereof |
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