CN110054936A - A kind of mirror-like silver electrically conductive ink and preparation method thereof - Google Patents

A kind of mirror-like silver electrically conductive ink and preparation method thereof Download PDF

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Publication number
CN110054936A
CN110054936A CN201810054334.5A CN201810054334A CN110054936A CN 110054936 A CN110054936 A CN 110054936A CN 201810054334 A CN201810054334 A CN 201810054334A CN 110054936 A CN110054936 A CN 110054936A
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China
Prior art keywords
electrically conductive
mirror
silver
conductive ink
high speed
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Pending
Application number
CN201810054334.5A
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Chinese (zh)
Inventor
江海涵
何利娜
朱庆明
王德龙
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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Priority to CN201810054334.5A priority Critical patent/CN110054936A/en
Publication of CN110054936A publication Critical patent/CN110054936A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/102Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks

Abstract

The present invention relates to a kind of mirror-like silver electrically conductive inks and preparation method thereof, are prepared using the raw material of following components and parts by weight content: nano-scale aluminium flake 50~55;Nanometer silver flakes 15~20;Polyurethane resin 15~20;Butyl acetate 5~8;Propylene glycol methyl ether acetate 5~8;Dibasic ester 5~8;Polyethylene wax 0.5~1.0;Dimethyl siloxane 0.2~0.5.Compared with prior art, the present invention can promote ink fineness and brightness, and mirror effect is good.

Description

A kind of mirror-like silver electrically conductive ink and preparation method thereof
Technical field
The present invention relates to a kind of ink, more particularly, to a kind of mirror-like silver electrically conductive ink and preparation method thereof.
Background technique
Mirror-like silver electrically conductive ink is basic raw material configuration by flake silver powder, flake aluminum, macromolecule resin and solvent It forms.Mirror-like silver electrically conductive ink is usually printed on the transparent materials such as macromolecule membrane, plastic sheet, glass.In these materials After upper printing mirror silver electrically conductive ink, mirror surface or gold stamping imaging effect can be showed.With the rapid hair of intelligent wearable device Exhibition, common mirror surface decorative effect also need the effect of subsidiary conductive path, in the hope of having the function that transmit signal.Common mirror Face silver ink only has the single attribute decorated, the high-intensitive effect stretched and be powered being unable to satisfy on textile fabric.At this stage, Mirror-like silver electrically conductive ink still relies on imported product, domestic not mature and stable product.There are specular brightness for home products not Defects enough, that resistance to settling energy is poor, storage time is short, therefore the research and development of the product are significant.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of mirror-like silver conductive oils Ink and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of mirror-like silver electrically conductive ink, is prepared using the raw material of following components and parts by weight content:
Nano-scale aluminium flake 50~55;Nanometer silver flakes 15~20;Polyurethane resin 15~20;Butyl acetate 5~8; Propylene glycol methyl ether acetate 5~8;Dibasic ester 5~8;Polyethylene wax 0.5~1.0;Dimethyl siloxane 0.2~0.5.
The average grain diameter of the nano-scale aluminium flake is less than 500nm.
The average grain diameter of the Nanometer silver flakes is less than 500nm.
The dibasic ester, propylene glycol methyl ether acetate, butyl acetate constitute mixed solvent component, take into account evaporation rate And the feature of environmental protection.
The preparation method of mirror-like silver electrically conductive ink, using following steps:
(1) it stocks up according to formula;
(2) polyurethane resin and dibasic ester to be poured into dissolution kettle, control mixing speed is controlled in 1000-2000rpm, 5~6h of high-speed stirred;
(3) nano-scale aluminium flake, Nanometer silver flakes, butyl acetate, propylene glycol methyl ether acetate and residue are continuously added Raw material;
(4) high speed dispersion: material barrel is moved on high speed dispersion machine platform after mixing, is then turned on high speed dispersion Machine switch, opens variable frequency switch to 60Hz, and stirring is integrally in silver gray slurry and without silver powder particles to ink;
The grinding of (5) three rollers: the product that step (4) is prepared is rolled three times using grinder, every time after the completion of rolling A high speed dispersion is carried out again, and control discharge fineness is not more than 10 μm;
(6) vacuum filter: stainless steel cavity is connected using vacuum pump, stainless steel material is placed in position in stainless steel cavity Cylinder installs silk screen above stainless steel cavity, opens vacuum pump switch, and the electrically conductive ink that dispersion finishes is toppled on silk screen, and Ink is constantly paved with rubber flap, makes its rapid filtration into built-in stainless steel material barrel;
(7) homogeneous stirs: being stirred, is prepared using the electrically conductive ink that homogenizer obtains step (6) Final products.
Between constantly being controlled by easy stages when being ground three times in step (5) in three-roll grinder between fast roller and central roll Gap, control roller gap in 0.3mm-0.35mm, second of grinding in roller gap is controlled in 0.25-0.3mm when first time grinds, the The control of roller gap is in 0.2-0.25mm when grinding three times.
Silk screen described in step (6) is the stainless (steel) wire of 250-400 mesh, and the vacuum degree that when vacuum filter controls is 1000Pa。
Control vacuum degree is 0.08~0.12Mpa, mixing speed 2500rpm when step (7) carries out homogeneous stirring.
Compared with prior art, the present invention is designed by the formula to ink coating, is screened to different raw material, is multiple Match, prepares novel mirror silver electrically conductive ink.Using nano-scale aluminium flake as primary solids phase, it is reflective that mirror surface mirror surface can be enhanced Property, using Nanometer silver flakes as conductive phase, mirror effect can be enhanced again, the electric conductivity and attachment of electrically conductive ink can be enhanced Power;Using polyurethane as Binder Phase, flexibility can have, and enhance the extensive adaptability to different printed substrates;Ladder Formula Compositional type solvent phase (butyl acetate, propylene glycol methyl ether acetate, dibasic ester), had both met the ring of European Union ROSH and WEEE Guaranteed request, and rapid curing may be implemented, meet the printing technology of client's spray printing or silk-screen;Using polyethylene wax as anti-settling Resistance to settling can be enhanced in depressant prescription, extends the resting period of product, and since it is linear structure, to the impact effect of mirror surface It is smaller;The printing and levelability of mirror-like silver electrically conductive ink can be enhanced in the addition of levelling agent dimethyl siloxane.To mirror-like silver The actual production of electrically conductive ink carries out process optimization, that is, passes through the steps such as high speed dispersion, three roller grindings, vacuum filter, homogeneous stirring It is rapid to obtain the stable practical application product of performance.Wherein vacuum filter is designed, designed, and homogeneous stirring technique can be obvious Ground reaches defoaming effect, and further promotes ink fineness and brightness.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
Examples 1 to 5
A kind of preparation method of mirror-like silver electrically conductive ink, each component and ingredient are as shown in table 1.Wherein nano-silver powder is averaged Partial size is less than 500nm, and nanometer aluminium powder average grain diameter is rained 500nm.Dimethyl silicone polymer is as levelling agent.Polyethylene wax is made For sagging inhibitor.
Table 1
Title material Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Nanometer sheet aluminium powder (kg) 5 5 5 5 5
Nanometer silver powder (kg) on chip 1.5 1.5 1.6 1.7 1.8
Polyurethane resin (kg) 2 2 2 2 2
Butyl acetate (kg) 0.5 0.8 0.5 0.5 0.5
Propylene glycol methyl ether acetate (kg) 0.6 0.6 0.6 0.6 0.6
Dibasic ester (kg) 0.8 0.5 0.7 0.6 0.5
Polyethylene wax (kg) 0.05 0.05 0.05 0.05 0.05
Dimethyl siloxane (kg) 0.05 0.05 0.05 0.05 0.05
Load weighted polyurethane resin and solvent dibasic ester are poured into dissolution kettle according to formula rate, it then will dissolution The mixing speed of kettle is controlled in 1500rpmmin, high-speed stirred 6h.The additive amount of polyurethane resin is 30%.Mei Tele is used The electronic scale of BBA211 model cooperates record component as weighing tool, and the original of corresponding code name is added according to Display panel value Material.The sequence of batch weighing is: addition saturated polyester resin → addition silver powder → addition solvent → addition residue auxiliary agent.Due to The weighing of auxiliary agent uses the electronic scale of JY20002 model.Material barrel is moved on high speed dispersion machine platform after weighing, so High speed disperser switch is opened afterwards, stirring-head is down at barrel bottom 2cm, is opened variable frequency switch to 60Hz, is arranged after timing continuously Stir 3min.It takes up the ball material barrel and moves to three-roll grinder platform, the rolling of three-roll grinder needs three circulations, every to have rolled A time silver paste requires to carry out a high speed dispersion step again.Then the fast roller of three-roll grinder kind is constantly controlled by easy stages Gap between central roll, first pass grind the roller gap of low-temperature conductive silver paste in 0.3mm, second time roller gap in 0.25mm, Third is controlled all over roller gap in 0.2mm.It is up to 10um fineness material barrel below and moves to vacuum filter platform, on filter The stainless (steel) wire of 300 mesh of side's installation is simultaneously complete by ink filter.Complete semi-finished product, which will be filtered, transfers to detection department to detect, and reaches Homogeneous stirring is carried out after company standard, vacuum degree is set as 0.12Mpa, then the silver paste that tinning is finished is put into homogenizer and stirs 3min.The performance of mirror-like silver electrically conductive ink is as shown in table 2.
Table 2
Embodiment 6
A kind of mirror-like silver electrically conductive ink, be prepared using the raw material of following components and parts by weight content: average grain diameter is small In the flake aluminum 50 of 500nm;Average grain diameter is less than the flake silver powder 15 of 500nm;Polyurethane resin 15;Butyl acetate 5;The third two Alcohol methyl ether acetate 5;Dibasic ester 5;Polyethylene wax 0.5;Dimethyl siloxane 0.2, wherein utilizing dibasic ester, propylene glycol first Ether acetate, butyl acetate constitute mixed solvent component, take into account evaporation rate and the feature of environmental protection.
The preparation method of mirror-like silver electrically conductive ink, using following steps:
(1) it stocks up according to formula;
(2) polyurethane resin and dibasic ester are poured into dissolution kettle, the control of control mixing speed is in 1000rpm, high speed Stir 5h;
(3) nano-scale aluminium flake, Nanometer silver flakes, butyl acetate, propylene glycol methyl ether acetate and residue are continuously added Raw material;
(4) high speed dispersion: material barrel is moved on high speed dispersion machine platform after mixing, is then turned on high speed dispersion Machine switch, opens variable frequency switch to 60Hz, and stirring is integrally in silver gray slurry and without silver powder particles to ink;
The grinding of (5) three rollers: rolling three times the product that step (4) is prepared using grinder, continuous when grinding three times The gap in three-roll grinder between fast roller and central roll is controlled by easy stages, roller gap is controlled in 0.3mm when grinding for the first time, The control of roller gap is in 0.25mm when grinding for the second time, and roller gap controls after the completion of 0.2mm is rolled every time again when third time is ground A high speed dispersion is carried out, control discharge fineness is not more than 10 μm;
(6) vacuum filter: stainless steel cavity is connected using vacuum pump, stainless steel material is placed in position in stainless steel cavity Cylinder installs the stainless steel cloth of 250 mesh above stainless steel cavity, opens vacuum pump switch, topples over dispersion on silk screen and finish Electrically conductive ink, blend rubber scraper plate constantly paves ink, makes its rapid filtration into built-in stainless steel material barrel, vacuum filter When the vacuum degree that controls be 1000Pa;
(7) homogeneous stirs: being stirred using the electrically conductive ink that homogenizer obtains step (6), homogeneous stirring When control vacuum degree be 0.08Mpa, final products are prepared in mixing speed 2500rpm, and the product mirror effect is good, And also there is good adhesive force.
Embodiment 7
A kind of mirror-like silver electrically conductive ink, be prepared using the raw material of following components and parts by weight content: average grain diameter is small In the flake aluminum 55 of 500nm;Average grain diameter is less than the flake silver powder 20 of 500nm;Polyurethane resin 20;Butyl acetate 8;The third two Alcohol methyl ether acetate 8;Dibasic ester 8;Polyethylene wax 1;Dimethyl siloxane 0.5, wherein utilizing dibasic ester, propylene glycol monomethyl ether Acetate, butyl acetate constitute mixed solvent component, take into account evaporation rate and the feature of environmental protection.
The preparation method of mirror-like silver electrically conductive ink, using following steps:
(1) it stocks up according to formula;
(2) polyurethane resin and dibasic ester are poured into dissolution kettle, the control of control mixing speed is in 2000rpm, high speed Stir 6h;
(3) nano-scale aluminium flake, Nanometer silver flakes, butyl acetate, propylene glycol methyl ether acetate and residue are continuously added Raw material;
(4) high speed dispersion: material barrel is moved on high speed dispersion machine platform after mixing, is then turned on high speed dispersion Machine switch, opens variable frequency switch to 60Hz, and stirring is integrally in silver gray slurry and without silver powder particles to ink;
The grinding of (5) three rollers: rolling three times the product that step (4) is prepared using grinder, continuous when grinding three times The gap in three-roll grinder between fast roller and central roll is controlled by easy stages, and the control of roller gap exists when grinding for the first time 0.35mm, the control of roller gap is in 0.3mm when grinding for the second time, and roller gap controls and rolled every time in 0.25mm when third time is ground Cheng Houzai carries out a high speed dispersion, and control discharge fineness is not more than 10 μm;
(6) vacuum filter: stainless steel cavity is connected using vacuum pump, stainless steel material is placed in position in stainless steel cavity Cylinder installs the stainless steel cloth of 400 mesh above stainless steel cavity, opens vacuum pump switch, topples over dispersion on silk screen and finish Electrically conductive ink, blend rubber scraper plate constantly paves ink, makes its rapid filtration into built-in stainless steel material barrel, vacuum filter When the vacuum degree that controls be 1000Pa;
(7) homogeneous stirs: being stirred using the electrically conductive ink that homogenizer obtains step (6), homogeneous stirring When control vacuum degree be 0.12Mpa, final products are prepared in mixing speed 2500rpm, and the product mirror effect is good, And also there is good adhesive force.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring substantive content of the invention.

Claims (8)

1. a kind of mirror-like silver electrically conductive ink, which is characterized in that be prepared using the raw material of following components and parts by weight content:
Nano-scale aluminium flake 50~55;Nanometer silver flakes 15~20;Polyurethane resin 15~20;Butyl acetate 5~8;The third two Alcohol methyl ether acetate 5~8;Dibasic ester 5~8;Polyethylene wax 0.5~1.0;Dimethyl siloxane 0.2~0.5.
2. a kind of mirror-like silver electrically conductive ink according to claim 1, which is characterized in that the nano-scale aluminium flake is put down Equal partial size is less than 500nm.
3. a kind of mirror-like silver electrically conductive ink according to claim 1, which is characterized in that the Nanometer silver flakes are put down Equal partial size is less than 500nm.
4. a kind of mirror-like silver electrically conductive ink according to claim 1, which is characterized in that the dibasic ester, propylene glycol Methyl ether acetate, butyl acetate constitute mixed solvent component.
5. a kind of preparation method of mirror-like silver electrically conductive ink as described in claim 1, which is characterized in that this method is using following Step:
(1) it stocks up according to formula;
(2) polyurethane resin and dibasic ester are poured into dissolution kettle, the control of control mixing speed is in 1000-2000rpm, high speed Stir 5~6h;
(3) nano-scale aluminium flake, Nanometer silver flakes, butyl acetate, propylene glycol methyl ether acetate and surplus stock are continuously added;
(4) material barrel: being moved on high speed dispersion machine platform by high speed dispersion after mixing, is then turned on high speed disperser and opens It closes, opens variable frequency switch to 60Hz, stirring is integrally in silver gray slurry and without silver powder particles to ink;
The grinding of (5) three rollers: the product rolling that step (4) is prepared using grinder three times, every time after the completion of rolling again into High speed dispersion of row, control discharge fineness are not more than 10 μm;
(6) vacuum filter: connecting stainless steel cavity using vacuum pump, and stainless steel material barrel is placed in position in stainless steel cavity, Silk screen is installed above stainless steel cavity, opens vacuum pump switch, the electrically conductive ink that dispersion finishes is toppled on silk screen, and use rubber Glue scraper plate constantly paves ink, makes its rapid filtration into built-in stainless steel material barrel;
(7) homogeneous stirs: being stirred, is prepared final using the electrically conductive ink that homogenizer obtains step (6) Product.
6. a kind of preparation method of mirror-like silver electrically conductive ink according to claim 5, which is characterized in that three in step (5) The gap in three-roll grinder between fast roller and central roll, roller gap when grinding for the first time are constantly controlled when secondary grinding by easy stages In 0.3mm-0.35mm, second of grinding, the control of roller gap is in 0.25-0.3mm for control, and roller gap controls when third time is ground In 0.2-0.25mm.
7. a kind of preparation method of mirror-like silver electrically conductive ink according to claim 5, which is characterized in that institute in step (6) The silk screen stated is the stainless (steel) wire of 250-400 mesh, and the vacuum degree that when vacuum filter controls is 1000Pa.
8. a kind of preparation method of mirror-like silver electrically conductive ink according to claim 5, which is characterized in that step (7) carries out Control vacuum degree is 0.08~0.12Mpa, mixing speed 2500rpm when homogeneous stirs.
CN201810054334.5A 2018-01-19 2018-01-19 A kind of mirror-like silver electrically conductive ink and preparation method thereof Pending CN110054936A (en)

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CN111363412A (en) * 2020-02-29 2020-07-03 上海宝银电子材料有限公司 Silver-coated nickel conductive ink for membrane switch and preparation method thereof
CN111383791A (en) * 2020-02-29 2020-07-07 上海宝银电子材料有限公司 High-resolution printing low-temperature conductive silver paste and preparation method thereof
CN111471160A (en) * 2020-04-21 2020-07-31 广州致辉精化股份有限公司 Organic silicon modified polyurethane urea resin and preparation method and application thereof
CN111489847A (en) * 2020-04-21 2020-08-04 上海宝银电子材料有限公司 Low-temperature conductive silver paste for alarm of automobile safety belt and preparation method thereof
CN112961540A (en) * 2021-03-31 2021-06-15 上海宝银电子材料有限公司 Conductive ink for pad printing process and preparation method thereof
CN113527948A (en) * 2020-04-21 2021-10-22 上海宝银电子材料有限公司 Conductive ink for pad printing process and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN111363412A (en) * 2020-02-29 2020-07-03 上海宝银电子材料有限公司 Silver-coated nickel conductive ink for membrane switch and preparation method thereof
CN111383791A (en) * 2020-02-29 2020-07-07 上海宝银电子材料有限公司 High-resolution printing low-temperature conductive silver paste and preparation method thereof
CN111383791B (en) * 2020-02-29 2023-05-23 上海宝银电子材料有限公司 High-resolution printing low-temperature conductive silver paste and preparation method thereof
CN111471160A (en) * 2020-04-21 2020-07-31 广州致辉精化股份有限公司 Organic silicon modified polyurethane urea resin and preparation method and application thereof
CN111489847A (en) * 2020-04-21 2020-08-04 上海宝银电子材料有限公司 Low-temperature conductive silver paste for alarm of automobile safety belt and preparation method thereof
CN113527948A (en) * 2020-04-21 2021-10-22 上海宝银电子材料有限公司 Conductive ink for pad printing process and preparation method thereof
WO2021213190A1 (en) * 2020-04-21 2021-10-28 上海宝银电子材料有限公司 Conductive printing ink for pad printing process and preparation method therefor
CN111471160B (en) * 2020-04-21 2022-01-18 广州致辉精化股份有限公司 Organic silicon modified polyurethane urea resin and preparation method and application thereof
CN112961540A (en) * 2021-03-31 2021-06-15 上海宝银电子材料有限公司 Conductive ink for pad printing process and preparation method thereof

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Application publication date: 20190726

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