CN103996436A - Conductive film and preparation method thereof - Google Patents
Conductive film and preparation method thereof Download PDFInfo
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- CN103996436A CN103996436A CN201410161739.0A CN201410161739A CN103996436A CN 103996436 A CN103996436 A CN 103996436A CN 201410161739 A CN201410161739 A CN 201410161739A CN 103996436 A CN103996436 A CN 103996436A
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Abstract
The invention relates to the technical field of a conductive film, and especially relates to a conductive film and a preparation method thereof. The conductive film comprises a PET base material layer, the surface of which is subjected to corona treatment. The surface of the PET base material layer is coated with a conductive coating layer. The conductive coating layer comprises raw materials by the following weight percentage: 50-70% absolute ethyl alcohol, 2-5 % terpilenol, 3-8 % dimethylacetamide, 1-3 % acetyl tributyl citrate, 2-8% cementing agent, 1-5 % polyethylene glycol 400, 2-3% Span 85, 1.5-3% ethyl cellulose, 0.5-2% polyimide resin, 0.5-1.5 % polyester resin, 10-18% 150-300 nanometer silver powders, and 3-8% 20-35 nanometer silver powders. The conductive film in the invention is stable in conductivity on the surface of the formed film, low in resistivity, high in light transmittance and strong in adhesive force; and the coating process of the conductive film is simple and mature, convenient to operate, low in cost, and convenient to popularize and apply.
Description
Technical field
The present invention relates to conducting film technical field, relate in particular to a kind of conducting film and preparation method thereof.
Background technology
The transparent conductive film of industry manufacture at present still be take oxide as main, oxidic transparent conductive film is due to its good photoelectric characteristic, as advantages such as the resistivity compared with low, high visible light transmissivities and be widely used in plane demonstration, solar cell, touch-screen, can heated glass window medium as transparency electrode.Current ITO(tin-doped indium oxide) film practical application is the widest, and its preparation of target materials and film-forming process are comparatively ripe.But due to In in ito thin film
20
3expensive, cost is higher, and indium has severe toxicity, can be harmful in preparation and application; In addition, the atomic weight of Sn and In is larger, easily penetrates into base material inside in film forming procedure, poisons base material.
In addition, prepare at present the comparatively ripe method of flexible transparent conducting film and mainly contain magnetron sputtering method, vacuum vapour deposition, ion plating method.But these several preparation methods exist defect separately, equipment as required in sputtering method is complicated, and cost is high, is badly in need of now solving low cost, high membranous, large area quantity-produced contradiction.Existing conducting film is mainly tin indium oxide (Indium-Tin Oxide) transparent conducting film glass, many by ITO electropane production line, in the power house environment of high purification, utilize plane magnetic control technology, sputter tin indium oxide conductive film coating obtaining through the high temperature anneal on ultra-thin glass.Existing technique weak point: 1, energy consumption is large, and cost is high; 2, the surface conductance performance of film is uneven; 3, transparency is low; 4, production yields is low.Along with electronic device, particularly flat-panel monitor is towards the fast development of lightening direction, and flexible transparent conducting film has the corresponding focuses that become research of advantage such as lightweight, flexibility is good because of it.Flexible transparent conductive film research and development is in recent years just towards the future development of high-quality, high efficiency, low cost, environmental protection.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of conducting film and preparation method thereof is provided, it is stable that this conducting film has film formation surface electric conductivity, and resistivity is low, and light transmittance is high, strong adhesion, high temperature resistant and corrosivity, the feature that adhesion strength is good, the preparation technology of this conducting film is simply ripe, easy to utilize, production cost is low.
The present invention is achieved through the following technical solutions.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 50-70%
Terpinol 2-5%
Dimethylacetylamide 3-8%
Tributyl 2-acetylcitrate 1-3%
Cement 2-8%
PEG400 1-5%
85 2-3% of class of department
Ethyl cellulose 1.5-3%
Polyimide resin 0.5-2%
Mylar 0.5-1.5%
20-35 nano-silver powder 3-8%
150-300 nano-silver powder 10-18%.
Wherein, the thickness of the PET base material of described PET substrate layer is 75-250 μ m, and width is below 1500cm, light transmittance >=92%.Preferably, the thickness of the PET base material of described PET substrate layer is 100-180 μ m, and the light transmittance of PET base material is 92-96%.
Wherein, described cement is organic silicone oil, acrylic acid glue or polyurethane glue, and the viscosity of described cement is 1-6cps, and solid content is less than 50%.Preferably, the viscosity of cement is 2-4 cps, and solid content is 30-45.
Wherein, surface is through the described PET substrate layer of corona treatment, surface tension >=50mN/m, coefficient of friction >=0.55.
Wherein, the silver powder of described particle diameter 150-300 nanometer is 6.5-8:1 with the ratio of the particle diameter of the silver powder of described particle diameter 20-35 nanometer.Owing to adding the nano-Ag particles that particle size is different, the nano-Ag particles that during mixing, particle diameter is little can embed between the nano-Ag particles that nano-Ag particles is inner and adjacent two particle diameters are large that particle diameter is large, the silver powder of particle diameter 150-300 nanometer is 6.5-8:1 with the ratio of the particle diameter of the silver powder of described particle diameter 20-35 nanometer, guarantee surrounding and the inner nano-silver powder that is uniformly coated with small particle diameter of the nano-silver powder of large particle diameter, thereby it is tightr that nano-silver conductive particle is connected, improve conductance.
Wherein, described mylar is waterborne polyurethane resin or acrylic resin.
Waterborne polyurethane resin, outward appearance: milky white/micro-opaque/liquid, Gu composition: 22%, PH:6-7, be mainly used in the adherence of promote covering with paint, lacquer, colour wash, etc., there is the ultra-fine film that causes and extend, excellent cold resistance, but can excessively not fill grain.Coordinate polyimide resin to use together and can adjust the soft durometer of filming, guarantee that film coated surface hardness is not less than 2H.Acrylic resin look shallow, water-white is transparent.Film performance is excellent, fast light, weatherability is good, heat-resisting, and resistance to paint baking over, chemical-resistant and the performance such as corrosion-resistant are all fabulous.
Preferably, a kind of conducting film, described electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 55-65%
Terpinol 3-4%
Dimethylacetylamide 4-6%
Tributyl 2-acetylcitrate 1-2%
Cement 3-6%
PEG400 1-3%
85 2-2.5% of class of department
Ethyl cellulose 2-2.5%
Polyimide resin 0.8-1.2%
Mylar 0.5-0.8%
20-35 nano-silver powder 4-6%
150-300 nano-silver powder 12-16%.
Preferably, a kind of conducting film, described electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 60-70%
Terpinol 3-4%
Tributyl 2-acetylcitrate 1-2%
Cement 3-6%
PEG400 1-3%
85 2-2.5% of class of department
Ethyl cellulose 2-2.5%
20-35 nano-silver powder 4-6%
150-300 nano-silver powder 12-16%.
More preferably, a kind of conducting film, described electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 50-65%
Terpinol 3-5%
Tributyl 2-acetylcitrate 1.5-3%
Cement 4-8%
PEG400 3-5%
85 2.5-3% of class of department
Ethyl cellulose 2-3%
20-35 nano-silver powder 5-8%
150-300 nano-silver powder 14-18%.
More preferably, a kind of conducting film, described electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 65-75%
Terpinol 2-3%
Tributyl 2-acetylcitrate 1-1.5%
Cement 2-4%
PEG400 1-3.5%
85 2-2.5% of class of department
Ethyl cellulose 1.5-2%
20-35 nano-silver powder 3-5%
150-300 nano-silver powder 10-15%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the PET base material of light transmittance >=92% of corona treatment;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, above-mentioned nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 20-30 minute; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 10-15min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 15-20min; In said mixture, adding successively particle diameter is the nano-silver powder of 20-35nm, nano-silver powder and the cement that particle diameter is 150-300nm, in blender, with 1000rpm rotating speed, stirs 20-25min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1-2h, obtains particle diameter 200-350nm, and pH value is 6.5-8.5, and solid content is 10%, the water white coating of leading that density is 1.01 ± 0.2g/ml;
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Wherein, described step (3) coating, be specially: PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2-3 μ m, coated PET base material passes bake oven device by live-roller, oven temperature is controlled between 50-200 ℃, oven temperature divides five joints, the temperature of baking oven raises gradually from first segment to the four joints, the 5th joint oven temperature declines, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller.
Wherein, the line number of the oblique anilox roll of described pottery is 80-280, and the temperature of five joint baking ovens are respectively 50-60 ℃, 70-80 ℃, 90-100 ℃, 110-130 ℃, 70-80 ℃, and described material receiving roller tension force is 200-250N, and described emptying roller tension force is 100-150N.
Its principle of the corona treatment of described PET base material is to utilize high-frequency high voltage at processed frosting corona discharge (high-frequency ac voltage is up to 5000-15000V/m2), and generation low temperature plasma, make frosting produce radical reaction and that polymer is occurred is crosslinked. surperficial roughening and increase its to the wetability of polar solvent-these gas ions by shocking by electricity and penetrating into its molecular structure of surface breakdown that is printed body, and then by processed surface molecular oxidation and polarization, ion electric shock erosion surface, so that increase the adhesive ability on stock surface.Corona treatment rearranges stock surface molecule structure, produces more polar fraction, is conducive to adhere to foreign object.Form high glaze transparent membrane, improve the wettability of PET polyester film to ink and adhesive, increase the firmness adhering to.Make oxide-film surface produce chemical group, melt and roughening effect on surface.Make substrate surface tension force >=50mN/m.Coefficient of friction >=0.55.
The present invention utilize the organic carriers such as absolute ethyl alcohol, terpinol, dimethylacetylamide, tributyl 2-acetylcitrate, cement, PEG400, class of department 85, ethyl cellulose, polyimide resin, mylar and nano-silver powder material (nano silver material by particle diameter be respectively the nano-silver powder of 20-35nm, the nano-silver powder grain composition that particle diameter is 150-300nm forms) prepare electrically-conducting paint, the main effect of organic carrier is the effects such as dispersion, thickening, plasticising, levelling, increasing be sliding.
Absolute ethyl alcohol, terpinol are solvent, and ethyl cellulose is thickener, and tributyl 2-acetylcitrate is plasticizer, and its boiling point is also lower, only at 173 ℃, are usually used in coating plasticising.
The viscosity of cement is 1-6cps, and solid content is less than 50%, guarantees that cement and PET film have the system of fine compatibility.Effect lubricated, levelling that organic silicone oil can play, also can improve the wetability of coating.Acrylic acid glue, is called again acrylic acid glue, has ambient temperature curable, a many merits such as easy to operate, adhesive strength is high, quick location, high resiliency, solidfied material are nontoxic.Polyurethane glue is the glue that contains urethano and NCO in strand, due to the isocyanates that contains strong polarity and carbamate groups, there is very high reactivity, can cold curing, thereby the multiple materials such as metal, rubber, glass, pottery, plastics, timber, fabric, leather are had to good glueability.
PEG400 (being called for short PEG-400) can play the effect of froth breaking in the process stirring.
In its structure of terpinol, contain oxygen atom, this can reduce the reunion of nano-Ag particles, uses terpinol can also when coating is dry, control coating evaporation rate as solvent, prevents that coating rete is local because the too fast rete that causes of solvent evaporates shrinks, and produces cracking; And the mixed solvent that ethanol and terpinol are mixed to get can be accelerated coating evaporation rate when evaporation rate is stable.
Dimethylacetylamide (being called for short DMAC), molecular formula CH
3cON (CH
3)
2, molecular weight: 87.12, No. CAS: 127-19-5.Colourless transparent liquid, flammable.Can mix arbitrarily with organic solvents such as water, alcohol, ether, ester, benzene, chloroform and aromatics.
Ethyl cellulose can increase the viscosity of solution as customary thickeners, and this quite positive effect that is suspended with to particle in coating also has facilitation to the film forming of conducting film of the present invention simultaneously.
The class of department 85 that molecular weight is large (anhydrous sorbitol oleic acid three esters), it has good intermiscibility in organic media, and higher light value and molecular weight can, adsorb more granose its suspension that guarantees simultaneously, have facilitation to the stability of coating.
Polyimide resin has high temperature resistant, corrosion-resistant and good electrical property.Polyimides is one of high-molecular organic material of combination property the best, high temperature resistant reaching more than 400 ℃, long-term serviceability temperature scope-200～300 ℃, without sharp melting point, high insulating property, 103 hertz of lower dielectric constants 4.0, dielectric loss only 0.004～0.007, belongs to F to H class F insulating material F.Polyimide resin is dissolved in DMAC, and DMAC can dissolve each other with arbitrary proportion with ethanol, and polyimide resin mixes the conducting resinl making and has high temperature resistant and decay resistance with silver powder.
Mylar has good pliability, good to adhesive force, and the pencil hardness after independent film forming is below 2H, and the electrically-conducting paint pencil hardness making is more than 2H, is conducive to improve the viscosity of coating.Mylar mixes the conducting resinl making with silver powder can improve the adhesion strength of conducting film, and has anti-settling performance.
It is particle diameter 200-350nm that the Nano Silver flexibility that the present invention makes is led coating, and pH value is 6.5-8.5, and solid content is 10%, the colourless transparent liquid that density is 1.01 ± 0.2g/ml.
By the nano-Ag particles of grating after ultrasonic processing and surface coating modification are processed, the nano-silver conductive film making, resistance has reached 100-300 Ω left and right, the adhesive force of coating, hardness, impulsive force etc. are functional.Nano-silver conductive coating of the present invention, for PET film coated, makes PET film obtain good electric conductivity and the conductive layer of mechanical property.
Beneficial effect of the present invention is:
(1) it is stable that conducting film of the present invention has film formation surface electric conductivity, and resistivity is low, and light transmittance is high, strong adhesion, high temperature resistant and corrosivity, the feature that adhesion strength is good, the preparation technology of this conducting film is simply ripe, and coating apparatus is simple, easy to operate, with low cost, easy to utilize.In addition, it is good that the conducting film that the present invention makes also has chemical stability, and the characteristic of antiseptic property excellence, can be used for electromagnetic shielding, antistatic, and the field such as electronic circuit, has extensive use and be worth.
(2) existing ITO is as nano indium tin metal oxide, and its resistivity is between 103-104 Ω/cm, and transmitance reaches 85% left and right.And the present invention uses the coating of anilox roll coating method to have the nano silver particles of conductive capability on insulation PET film, after high polymer solidifies, conducting particles is in contact with one another, form conductive path, make Polymer Surface there is conductive capability, the resistance of the conducting film making can reach 10-100 Ω/cm, transmitance is brought up to more than 90%, case hardness (pencil hardness) >=2H, mist degree≤5.
(3) electrically-conducting paint coating process of the present invention has made great progress aspect industrialization, except possessing ITO, as nano indium tin metal oxide, there is good conductivity and the transparency, can cut off harmful electron radiation, outside ultraviolet ray and far infrared performance, also possess flexible, lightweight, difficult fragmentation, can adopt the continuous mode of production of volume to volume industrialization to be conducive to raise the efficiency, to be convenient to the advantages such as transportation.The relative ITO of conducting film of the present invention possesses flexible, and surface adhesion force is strong, conducts electricity stable feature.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
embodiment 1.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 50%
Terpinol 5%
Dimethylacetylamide 3.5%
Tributyl 2-acetylcitrate 3%
Organic silicone oil 6%
PEG400 4%
Class of department 85 3%
Ethyl cellulose 3%
Polyimide resin 1%
Acrylic resin 1.5%
30 nano-silver powders 4%
200 nano-silver powders 16%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 92%, thickness is the PET base material of 250 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, above-mentioned nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 20 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 10min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 15min; In said mixture, add successively the silver powder of particle diameter 30 nanometers, silver powder and the organic silicone oil of particle diameter 200 nanometers, in blender, with 1000rpm rotating speed, stir 20min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 2h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 250nm, and pH value is 6.5, and solid content is 10%, the colourless transparent liquid that density is 1.01/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 80, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 50 ℃, 70 ℃, 90 ℃, 110 ℃, 70 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 200N, described emptying roller tension force is 100N.
embodiment 2.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 57%
Terpinol 3%
Dimethylacetylamide 5%
Tributyl 2-acetylcitrate 2%
Organic silicone oil 4%
PEG400 2%
Class of department 85 2.5%
Ethyl cellulose 2.5%
Polyimide resin 0.8%
Acrylic resin 1.2%
20 nano-silver powders 6%
150 nano-silver powders 14%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 93%, thickness is the PET base material of 200 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 22 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 10min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 16min; In said mixture, add successively the silver powder of particle diameter 20 nanometers, silver powder and the acrylic acid glue of particle diameter 150 nanometers, in blender, with 1000rpm rotating speed, stir 20min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 2h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 200nm, and pH value is 6.5, and solid content is 10%, the colourless transparent liquid that density is 1.01/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 100, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 55 ℃, 75 ℃, 95 ℃, 115 ℃, 75 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 210N, described emptying roller tension force is 110N.
embodiment 3.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 60%
Terpinol 2%
Dimethylacetylamide 6%
Tributyl 2-acetylcitrate 1%
Organic silicone oil 2%
PEG400 1.5%
Class of department 85 2%
Ethyl cellulose 1.5%
Polyimide resin 1%
Acrylic resin 1%
25 nano-silver powders 4%
200 nano-silver powders 18%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 94%, thickness is the PET base material of 180 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 24 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 11min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 17min; In said mixture, add successively the silver powder of particle diameter 25 nanometers, silver powder and the organic silicone oil of particle diameter 300 nanometers, in blender, with 1000rpm rotating speed, stir 21min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 80min, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 250nm, and pH value is 7, and solid content is 10%, the colourless transparent liquid that density is 0.91g/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 150, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 60 ℃, 80 ℃, 100 ℃, 120 ℃, 80 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 220N, described emptying roller tension force is 120N.
embodiment 4.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 55%
Terpinol 4%
Dimethylacetylamide 5%
Tributyl 2-acetylcitrate 3%
Organic silicone oil 4.5%
PEG400 3.5%
Class of department 85 2.4%
Ethyl cellulose 2.1%
Polyimide resin 1%
Acrylic resin 0.5%
35 nano-silver powders 6%
245 nano-silver powders 13%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 95%, thickness is the PET base material of 150 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 25 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 12min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 18min; In said mixture, add successively the silver powder of particle diameter 40 nanometers, silver powder and the polyurethane glue of particle diameter 450 nanometers, in blender, with 1000rpm rotating speed, stir 22min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1.5h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 300nm, and pH value is 7, and solid content is 10%, the colourless transparent liquid that density is 0.91g/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 180, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2.5 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 50 ℃, 80 ℃, 100 ℃, 130 ℃, 80 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 230N, described emptying roller tension force is 130N.
embodiment 5.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 56%
Terpinol 3.5%
Dimethylacetylamide 4%
Tributyl 2-acetylcitrate 2.5%
Organic silicone oil 4%
PEG400 2.5%
Class of department 85 2.8%
Ethyl cellulose 2.2%
Polyimide resin 1.5%
Waterborne polyurethane resin 0.5%
35 nano-silver powders 6.5%
280 nano-silver powders 14%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 95%, thickness is the PET base material of 120 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 25 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 12min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 19min; In said mixture, add successively the silver powder of particle diameter 40 nanometers, silver powder and the organic silicone oil of particle diameter 300 nanometers, in blender, with 1000rpm rotating speed, stir 23min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1.5h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 350nm, and pH value is 7.5, and solid content is 10%, the colourless transparent liquid that density is 1.11/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 1350, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 60 ℃, 75 ℃, 00 ℃, 120 ℃, 75 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 240N, described emptying roller tension force is 140N.
embodiment 6.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 58%
Terpinol 3.2%
Dimethylacetylamide 7%
Tributyl 2-acetylcitrate 1%
Organic silicone oil 3%
PEG400 2%
Class of department 85 2.3%
Ethyl cellulose 2%
Polyimide resin 2%
Waterborne polyurethane resin 0.5%
30 nano-silver powders 5%
225 nano-silver powders 14%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 94%, thickness is the PET base material of 160 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 26 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 13min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 20min; In said mixture, add successively the silver powder of particle diameter 30 nanometers, silver powder and the acrylic acid glue of particle diameter 250 nanometers, in blender, with 1000rpm rotating speed, stir 24min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 100min, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 300nm, and pH value is 7.5, and solid content is 10%, the colourless transparent liquid that density is 0.81g/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 200, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2.5 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 55 ℃, 80 ℃, 95 ℃, 115 ℃, 75 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 250N, described emptying roller tension force is 150N.
embodiment 7.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 60%
Terpinol 3.4%
Dimethylacetylamide 8%
Tributyl 2-acetylcitrate 2.5%
Organic silicone oil 2%
PEG400 1.5%
Class of department 85 2.1%
Ethyl cellulose 2%
Polyimide resin 1.3%
Waterborne polyurethane resin 0.7%
30 nano-silver powders 4.5%
200 nano-silver powders 12%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 93%, thickness is the PET base material of 100 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 28 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 14min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 15min; In said mixture, add successively the silver powder of particle diameter 30 nanometers, silver powder and the organic silicone oil of particle diameter 200 nanometers, in blender, with 1000rpm rotating speed, stir 25min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 250nm, and pH value is 8, and solid content is 10%, the colourless transparent liquid that density is 1.21g/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 250, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 3 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 50 ℃, 80 ℃, 950 ℃, 130 ℃, 70 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 205N, described emptying roller tension force is 105N.
embodiment 8.
A conducting film, comprises that surface is through the PET substrate layer of corona treatment, and PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 70%
Terpinol 2%
Dimethylacetylamide 3%
Tributyl 2-acetylcitrate 1.5%
Organic silicone oil 3.5%
PEG400 1%
Class of department 85 2%
Ethyl cellulose 2%
Polyimide resin 1.4%
Waterborne polyurethane resin 0.6%
25 nano-silver powders 3%
165 nano-silver powders 10%.
A preparation method for conducting film, comprises following processing step:
(1) draw materials: choose surface through the light transmittance of corona treatment be 96%, thickness is the PET base material of 80 μ m;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 30 minutes; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 15min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 18min; In said mixture, add successively the silver powder of particle diameter 35 nanometers, silver powder and the polyurethane glue of particle diameter 275 nanometers, in blender, with 1000rpm rotating speed, stir 25min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1h, obtains Nano Silver flexible conductive paint.The Nano Silver flexible conductive paint that the present invention makes is particle diameter 210nm, and pH value is 8.5, and solid content is 10%, the colourless transparent liquid that density is 1.11g/ml.
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
Particularly, PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, the pottery tiltedly line number of anilox roll is 280, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 3 μ m, coated PET base material passes bake oven device by live-roller, oven temperature divides five joints, the temperature of five joint baking ovens is respectively 60 ℃, 70 ℃, 90 ℃, 125 ℃, 80 ℃, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller, described material receiving roller tension force is 2250N, described emptying roller tension force is 125N.
Raw material in the formula that the present invention uses all can be from buying and obtain on the market.
Performance to the Nano Silver flexible conductive paint of embodiments of the invention 1-8 is tested, and its physical and chemical index is: particle diameter is 200-350nm, and pH value is 6.5-8.5, and solid content is 10%, and density is 1.01 ± 0.2g/ml, and outward appearance is colourless transparent liquid.
The Nano Silver flexible conductive paint of embodiments of the invention 1-8 is adopted to tiltedly anilox roll coating of pottery, pottery tiltedly anilox roll line number is 80-280, be coated on PET film, obtain conducting film, its performance is as follows: hardness >=2H, adhesive force >=4B, sheet resistance are 100-300 Ω/cm, percent thermal shrinkage MD≤1.0%, TD≤0.8%, light transmittance >=90%, density 1.40 ± 0.5g/ml, mist degree≤5.
The above execution mode, it is better embodiment of the present invention, be not to limit the scope of the present invention, the equivalence of doing according to structure, feature and principle described in the present patent application the scope of the claims therefore all changes or modifies, and all should comprise in patent claim of the present invention.
Claims (10)
1. a conducting film, is characterized in that: comprise that surface is through the PET substrate layer of corona treatment, PET substrate layer surface-coated has electrically-conducting paint layer, and electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 50-70%
Terpinol 2-5%
Dimethylacetylamide 3-8%
Tributyl 2-acetylcitrate 1-3%
Cement 2-8%
PEG400 1-5%
85 2-3% of class of department
Ethyl cellulose 1.5-3%
Polyimide resin 0.5-2%
Mylar 0.5-1.5%
20-35 nano-silver powder 3-8%
150-300 nano-silver powder 10-18%.
2. a kind of conducting film according to claim 1, is characterized in that: the thickness of the PET base material of described PET substrate layer is 75-250 μ m, and width is below 1500cm, light transmittance >=92%.
3. a kind of conducting film according to claim 1, is characterized in that: described cement is organic silicone oil, acrylic acid glue or polyurethane glue, and the viscosity of described cement is 1-6cps, and solid content is less than 50%.
4. a kind of conducting film according to claim 1, is characterized in that: surface is through the described PET substrate layer of corona treatment, surface tension >=50mN/m, coefficient of friction >=0.55.
5. a kind of conducting film according to claim 1, is characterized in that: the silver powder of described particle diameter 150-300 nanometer is 6.5-8:1 with the ratio of the particle diameter of the silver powder of described particle diameter 20-35 nanometer.
6. a kind of conducting film according to claim 1, is characterized in that: described mylar is waterborne polyurethane resin or acrylic resin.
7. a kind of conducting film according to claim 1, is characterized in that: described electrically-conducting paint layer comprises the raw material of following percentage by weight:
Absolute ethyl alcohol 55-65%
Terpinol 3-4%
Dimethylacetylamide 4-6%
Tributyl 2-acetylcitrate 1-2%
Cement 3-6%
PEG400 1-3%
85 2-2.5% of class of department
Ethyl cellulose 2-2.5%
Polyimide resin 0.8-1.2%
Mylar 0.5-0.8%
20-35 nano-silver powder 4-6%
150-300 nano-silver powder 12-16%.
8. the preparation method of a kind of conducting film described in any one in claim 1-7, is characterized in that, comprises following processing step:
(1) draw materials: choose surface through the PET base material of light transmittance >=92% of corona treatment;
(2) modulation electrically-conducting paint: take in proportion the raw material of above-mentioned formula ratio, above-mentioned nano-silver powder is put into respectively to 100 ℃ of baking boxs and place the moisture of removing raw material for 20-30 minute; In container, add load weighted solvent, PEG400, ethyl cellulose, this mixture is put into blender and with 1000rpm rotating speed, stir 10-15min; Then, add load weighted dimethylacetylamide, polyimide resin, mylar, this mixture is put into blender and with 1000rpm rotating speed, stir 15-20min; In said mixture, adding successively particle diameter is the nano-silver powder of 20-35nm, nano-silver powder and the cement that particle diameter is 150-300nm, in blender, with 1000rpm rotating speed, stirs 20-25min; Then add class 85 of department and tributyl 2-acetylcitrate, adopt ultrasonic wave mode to disperse, jitter time is 1-2h, obtains particle diameter 200-350nm, and pH value is 6.5-8.5, and solid content is 10%, the water white coating of leading that density is 1.01 ± 0.2g/ml;
(3) coating: the electrically-conducting paint modulating is put into the coating chute of coating apparatus, coating apparatus is applied to electrically-conducting paint on PET base material, and oven for drying makes to form one deck electrically-conducting paint layer on PET base material, makes conducting film.
9. the preparation method of a kind of conducting film according to claim 8, it is characterized in that: described step (3) coating, be specially: PET base material drives charging by emptying roller by live-roller, and by pressure roller, PET base material is fitted in to the oblique anilox roll upper surface of pottery in coating pond, tiltedly anilox roll rotation direction is contrary with the feedstock direction of PET base material for pottery, pottery tiltedly anilox roll lower surface immerses in the electrically-conducting paint in coating pond, by scraper, the unnecessary electrically-conducting paint of the oblique anilox roll of pottery is scraped off, make to form on PET base material uniform nano-silver conductive dope layer, the coating thickness of electrically-conducting paint layer is 2-3 μ m, coated PET base material passes bake oven device by live-roller, oven temperature is controlled between 50-200 ℃, oven temperature divides five joints, the temperature of baking oven raises gradually from first segment to the four joints, the 5th joint oven temperature declines, electrically-conducting paint layer after oven dry forms conductive layer, after chill roll is cooling, make conducting film, by live-roller transmission rolling on material receiving roller.
10. the preparation method of a kind of conducting film according to claim 9, it is characterized in that: the line number of the oblique anilox roll of described pottery is 80-280, the temperature of five joint baking ovens are respectively 50-60 ℃, 70-80 ℃, 90-100 ℃, 110-130 ℃, 70-80 ℃, described material receiving roller tension force is 200-250N, and described emptying roller tension force is 100-150N.
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| CN110607144A (en) * | 2019-05-10 | 2019-12-24 | 南通康尔乐复合材料有限公司 | Conductive cloth glue for transfer coating and preparation method thereof |
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Effective date of registration: 20201231 Address after: No. 666, Liaohe Road, Xinbei District, Changzhou City, Jiangsu Province Patentee after: Yang Jiawen Address before: 523000 6 HUAYU street, Changlong village, Huang Jiang Town, Dongguan, Guangdong Patentee before: DONGGUAN NALIFILM OPTICAL MATERIAL Co.,Ltd. |