CN105006272A - Ultraviolet conductive silver slurry, and preparation method and application thereof - Google Patents
Ultraviolet conductive silver slurry, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an ultraviolet conductive silver slurry, and a preparation method and application thereof. The preparation method comprises the following steps that: an acrylic acid ester oligomer, a proper single uv body, a uv photoinitiator, a proper auxiliary agent, and silver powder are used for preparing an ultraviolet solidified conductive silver slurry containing 50% to 85% of silver; and then grinding is carried out by a three-roller machine to enable the fineness to be less than 5 microns. According to the invention, the prepared ultraviolet solidified conductive silver slurry also can be used for laser etching. The ultraviolet solidified silver slurry has excellent anti-bending and conductive performers; the printability is high; the performances are stable; and the production efficiency is extremely high. The large-scale production requirement of the touch screen conductive silver slurry can be met.
Description
Technical field
The present invention relates to a kind of conductive silver paste, be specifically related to the preparation method of a kind of touch-screen conducting wire production ultraviolet light polymerization silver slurry, belong to electric conducting material field.
Background technology
Utilize the screen printing technique of ultraviolet light polymerization conductive silver paste to produce touch-screen conducting wire industrially also not find application, at present, conductive silver paste still uses the mode of low-temperature setting to come obtained conducting wire, owing to containing a large amount of solvents in low-temperature silver slurry system, be unfavorable for environmental protection, and can baking oven be applied in the process of solidification, shortcoming is energy consumption height very.Low-temperature silver slurry time of toasting in the process of solidification is longer, usually can toast 30 to 50 minutes, production efficiency very low.
Laser-induced thermal etching conductive film layer technique utilizes pulse laser to be the hot spot of 10 microns to 90 microns by laser beam focus by optical focusing system, hot spot after focusing, arrive the place to go energy threshold of material, by the accurate rapid scanning of high-velocity scanning galvanometer system, thus the circuit realizing touch-screen upper conductive film layer makes object, the not visible region of such making is narrower, and practicality is stronger.
Summary of the invention
The object of this invention is to provide a kind of the present invention and aim to provide a kind of ultraviolet light conductive silver paste and preparation method thereof and application.
The invention solves in prior art, silver slurry baking time is long, and energy consumption is high, and efficiency is low, these defects seriously polluted.
The object of the present invention is achieved like this:
A kind of ultraviolet light conductive silver paste, is characterized in that, composed of the following components by mass parts: silver powder 50-85 mass parts, acrylate oligomer 10-20 mass parts, uv monomer 5-10 mass parts, light trigger 7-12 mass parts, additive 1-3 mass parts;
Described additive is made up of dispersant 16 mass parts, defoamer 39 mass parts, levelling agent 39 mass parts and storage stabilizing agent 8 mass parts;
Its preparation method comprises the steps:
(1), in uv monomer, storage stabilizing agent and light trigger is added, with under the high shear of 800-1000R/min in high speed dispersor, temperature controls at 30 DEG C ~ 60 DEG C, until be dissolved into transparent liquid completely, then filter out impurity, obtain initiator solution;
(2), add acrylate oligomer with the shearing force of 500R/min dispersion 30min in the initiator solution of step (1), temperature controls, at 30 DEG C ~ 60 DEG C, then to filter out impurity, obtain resin semi-finished product;
(3), in resin semi-finished product add silver powder, with the Rate Dispersion 2 hours of 500R/min in dispersion machine, on three-roller, be then ground to fineness be less than 5 microns, obtain uv silver slurry.
The present invention can also adopt following technical measures to solve:
Described silver powder is conductive submicron indefinite form silver powder, comprises following production stage:
(1) preparing concentration is respectively the liquor argenti nitratis ophthalmicus of 0.5-1.0mol/L and the sodium carbonate liquor of 0.5-1.0mol/L;
(2) liquor argenti nitratis ophthalmicus step (1) prepared and sodium carbonate liquor mix and blend obtain silver carbonate solution, and keep silver carbonate solution temperature to be 25-60 DEG C;
(3) after mix and blend, silver carbonate solution temperature is set to 60-80 DEG C, reducing agent is poured directly in silver carbonate solution, keep stirring reaction 0.5-2h, obtain silver powder suspension;
(4) the silver powder suspension washed with de-ionized water obtained, washing lotion is to conductivity lower than after 50 μ s/cm, and vacuum filtration is less than 35% to moisture content, obtains silver powder;
(5) prepare by silver powder, surfactant, absolute ethyl alcohol weight ratio 100: 0. 5 ~ 2: 10, first by surfactant and absolute ethyl alcohol mixed preparing ethanolic solution, then ethanolic solution is added sabot after stirring in silver powder, 60 DEG C of dry 15h;
(6) silver powder after drying is pulverized to obtain the indefinite form conductive silver powder of 0.2-4 μm.
Reducing agent is weak reductant, is glucose or glycerol.
Acrylate oligomer be selected from epoxy acrylate, polyester acrylate, urethane acrylate one or more.
Described acrylate oligomer is made up of epoxy acrylate and polyester acrylate, and the mass ratio of epoxy acrylate and polyester acrylate is 1:2.
Uv monomer is selected from 1,6 hexanediyl esters, tripropylene glycol diacrylate, neopentylglycol diacrylate, the third oxidation trimethylolpropane triacrylate, pentaerythritol triacrylate, two-trimethylolpropane triacrylate, 2-phenyl ethoxy acrylate, one or more in ethoxyethoxyethyl acrylate.
Conductive submicron indefinite form silver powder particle diameter is 50nm-2 μm.
Uv light trigger is selected from a, a-dimethoxy-a-phenyl acetophenone, 1-hydroxycyclohexyl phenyl ketone (184), 2-hydroxy-2-methyl-1-phenyl-1-acetone (1173), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (369), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (907), 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide (TPO), 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1-[4-(2-hydroxyl-oxethyl) phenyl]-2-hydroxyl-2 methyl isophthalic acids-propane-1-ketone (2959), one or more in reactive amines.
By uv silver slurry by after the solidification of UV lamp, touch screen circuitry plate obtains silver slurry conductive coating (in fact, before the solidification of UV lamp, need uv silver slurry silk-screen on touch screen circuitry plate, make touch screen circuitry plate to obtain silver slurry conductive coating), and on touch screen circuitry plate, prepare finished product conducting wire by laser etch process, and the live width of conducting wire after preparation on touch screen circuitry plate and line-spacing are 20 μm × 20 μm.
The invention has the beneficial effects as follows:
(1) uv silver slurry of the present invention, not containing volatile solvent (voc), possesses the characteristic of environmental protection.
(2) preparation method of uv silver slurry of the present invention, its production efficiency is high, without the need to operations such as bakings of the prior art, greatly saves preparation time, and the uv silver after preparation is starched after the solidification of uv lamp, by laser-induced thermal etching by conducting wire etch-forming.
(3) in the application of uv silver slurry of the present invention on touch screen circuitry plate, the live width of the conducting wire formed on touch screen circuitry plate by laser-induced thermal etching and line-spacing are 20 μm × 20 μm, adopt screen printer printing compared to existing technology, its live width and line-spacing are generally more than 80 μm, compare existing laser etching technology, its live width and line-spacing are generally all more than 35 μm, greatly improve the fineness of conducting wire, when can carry out more complicated line arrangement or arrange circuit on limited wiring board area, position is more abundant.
(4) uv silver slurry of the present invention, square resistance is low, between 13 ~ 15m Ω/ /mil, even lower, compares common 20 ~ 25m Ω/ /mil low.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
A kind of ultraviolet light conductive silver paste, is characterized in that, composed of the following components by mass parts: silver powder 50-85 mass parts, acrylate oligomer 10-20 mass parts, uv monomer 5-10 mass parts, light trigger 7-12 mass parts, additive 1-3 mass parts;
Described additive is made up of dispersant 16 mass parts, defoamer 39 mass parts, levelling agent 39 mass parts and storage stabilizing agent 8 mass parts;
Its preparation method comprises the steps:
(1), in uv monomer, storage stabilizing agent and light trigger is added, with under the high shear of 800-1000R/min in high speed dispersor, temperature controls at 30 DEG C ~ 60 DEG C, until be dissolved into transparent liquid completely, then filter out impurity, obtain initiator solution;
(2), add acrylate oligomer with the shearing force of 500R/min dispersion 30min in the initiator solution of step (1), temperature controls, at 30 DEG C ~ 60 DEG C, then to filter out impurity, obtain resin semi-finished product;
(3), in resin semi-finished product add silver powder, with the Rate Dispersion 2 hours of 500R/min in dispersion machine, on three-roller, be then ground to fineness be less than 5 microns, obtain uv silver slurry.
The present invention adopts the mass parts of each component of following table embodiment 1 ~ 5 to combine, and carries out classification declaration:
The present invention can also adopt following technical measures to solve:
Described silver powder is conductive submicron indefinite form silver powder, comprises following production stage:
(1) preparing concentration is respectively the liquor argenti nitratis ophthalmicus of 0.5-1.0mol/L and the sodium carbonate liquor of 0.5-1.0mol/L;
(2) liquor argenti nitratis ophthalmicus step (1) prepared and sodium carbonate liquor mix and blend obtain silver carbonate solution, and keep silver carbonate solution temperature to be 25-60 DEG C;
(3) after mix and blend, silver carbonate solution temperature is set to 60-80 DEG C, reducing agent is poured directly in silver carbonate solution, keep stirring reaction 0.5-2h, obtain silver powder suspension;
(4) the silver powder suspension washed with de-ionized water obtained, washing lotion is to conductivity lower than after 50 μ s/cm, and vacuum filtration is less than 35% to moisture content, obtains silver powder;
(5) prepare by silver powder, surfactant, absolute ethyl alcohol weight ratio 100: 0. 5 ~ 2: 10, first by surfactant and absolute ethyl alcohol mixed preparing ethanolic solution, then ethanolic solution is added sabot after stirring in silver powder, 60 DEG C of dry 15h;
(6) silver powder after drying is pulverized to obtain the indefinite form conductive silver powder of 0.2-4 μm.
Reducing agent is weak reductant, is glucose or glycerol.
Acrylate oligomer be selected from epoxy acrylate, polyester acrylate, urethane acrylate one or more.
Described acrylate oligomer is made up of epoxy acrylate and polyester acrylate, and the mass ratio of epoxy acrylate and polyester acrylate is 1:2.
Uv monomer is selected from 1,6 hexanediyl esters, tripropylene glycol diacrylate, neopentylglycol diacrylate, the third oxidation trimethylolpropane triacrylate, pentaerythritol triacrylate, two-trimethylolpropane triacrylate, 2-phenyl ethoxy acrylate, one or more in ethoxyethoxyethyl acrylate.
Conductive submicron indefinite form silver powder particle diameter is 50nm-2 μm.
Uv light trigger is selected from a, a-dimethoxy-a-phenyl acetophenone, 1-hydroxycyclohexyl phenyl ketone (184), 2-hydroxy-2-methyl-1-phenyl-1-acetone (1173), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (369), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (907), 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide (TPO), 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1-[4-(2-hydroxyl-oxethyl) phenyl]-2-hydroxyl-2 methyl isophthalic acids-propane-1-ketone (2959), one or more in reactive amines.
By uv silver slurry by after the solidification of UV lamp, touch screen circuitry plate obtains silver slurry conductive coating (in fact, before the solidification of UV lamp, need uv silver slurry silk-screen on touch screen circuitry plate, make touch screen circuitry plate to obtain silver slurry conductive coating), and on touch screen circuitry plate, prepare finished product conducting wire by laser etch process, and the live width of conducting wire after preparation on touch screen circuitry plate and line-spacing are 20 μm × 20 μm.
The ultraviolet light polymerization conductive silver paste obtained, what select due to acrylate oligomer is epoxy acrylate and polyester acrylate, epoxy acrylate is provide excellent curing rate and chemicals-resistant character in system, and polyester acrylate is that system provides good pigment wettability and excellent printing performance.And polyurethane acrylic resin due to its pigment wettability inadequate, its curing rate of the polyurethane acrylic resin of low functional group is very slow, and its pliability of the urethane acrylate of high functional group is too poor, therefore not as our first-selection.
The initiating system of the ultraviolet light polymerization silver slurry obtained only selects the light trigger of cracking type, and the adding just for we provide resistance to the oxygen inhibiting polymerization of reactive amines.It is not identical for causing principle with specific silver-colored slurry.
Its main performance is tested:
Concrete method of testing:
1: ultraviolet light polymerization conductive silver paste viscosity test: after 1 hour, measure the viscosity of silver-colored slurry samples at 25 DEG C of constant temperature with VT-04F rotation viscometer, 300-700dpa.s is applicable.
2: ultraviolet light polymerization conductive silver paste printability is tested: on manual silk-screen platform, mix 300 orders and 420 object polyester half tones respectively, the square pattern of printing 3 × 3cm in the ito film of shrinking, and the lines of 1 × 10cm.Thickness is 9-11 micron, then crosses the uv machine that dominant wavelength is 365nm.The integrity degree of range estimation lines and pattern and evenness.
3: the adhesive force test of ultraviolet light polymerization silver slurry: mark test hundred lattice with cross-cut tester in square pattern, then use the adhesive tape of 3M810 to test.Do not come off completely.
4: ultraviolet light polymerization conductive silver paste resistance test: by the resistance value at universal instrument testing of printed lines two ends.Then its square resistance of formulae discovery of sheet resistance is used.
Above-described specific embodiment, is only preferred embodiment of the present invention, such as according to the equivalent arrangements that the present patent application the scope of the claims does, all should be technology of the present invention and contained.
Claims (9)
1. a ultraviolet light conductive silver paste, is characterized in that, composed of the following components by mass parts: silver powder 50-85 mass parts, acrylate oligomer 10-20 mass parts, uv monomer 5-10 mass parts, light trigger 7-12 mass parts, additive 1-3 mass parts;
Described additive is made up of dispersant 16 mass parts, defoamer 39 mass parts, levelling agent 39 mass parts and storage stabilizing agent 8 mass parts;
Its preparation method comprises the steps:
(1), in uv monomer, storage stabilizing agent and light trigger is added, with under the high shear of 800-1000R/min in high speed dispersor, temperature controls at 30 DEG C ~ 60 DEG C, until be dissolved into transparent liquid completely, then filter out impurity, obtain initiator solution;
(2), add acrylate oligomer with the shearing force of 500R/min dispersion 30min in the initiator solution of step (1), temperature controls, at 30 DEG C ~ 60 DEG C, then to filter out impurity, obtain resin semi-finished product;
(3), in resin semi-finished product add silver powder, with the Rate Dispersion 2 hours of 500R/min in dispersion machine, on three-roller, be then ground to fineness be less than 5 microns, obtain uv silver slurry.
2. ultraviolet light conductive silver paste according to claim 1, is characterized in that, silver powder is conductive submicron indefinite form silver powder, comprises following production stage:
(1) preparing concentration is respectively the liquor argenti nitratis ophthalmicus of 0.5-1.0mol/L and the sodium carbonate liquor of 0.5-1.0mol/L;
(2) liquor argenti nitratis ophthalmicus step (1) prepared and sodium carbonate liquor mix and blend obtain silver carbonate solution, and keep silver carbonate solution temperature to be 25-60 DEG C;
(3) after mix and blend, silver carbonate solution temperature is set to 60-80 DEG C, reducing agent is poured directly in silver carbonate solution, keep stirring reaction 0.5-2h, obtain silver powder suspension;
(4) the silver powder suspension washed with de-ionized water obtained, washing lotion is to conductivity lower than after 50 μ s/cm, and vacuum filtration is less than 35% to moisture content, obtains silver powder;
(5) prepare by silver powder, surfactant, absolute ethyl alcohol weight ratio 100: 0. 5 ~ 2: 10, first by surfactant and absolute ethyl alcohol mixed preparing ethanolic solution, then ethanolic solution is added sabot after stirring in silver powder, 60 DEG C of dry 15h;
(6) silver powder after drying is pulverized to obtain the indefinite form conductive silver powder of 0.2-4 μm.
3. ultraviolet light conductive silver paste according to claim 2, is characterized in that, reducing agent is weak reductant, is glucose or glycerol.
4. ultraviolet light conductive silver paste according to claim 1, is characterized in that, acrylate oligomer be selected from epoxy acrylate, polyester acrylate, urethane acrylate one or more.
5. ultraviolet light conductive silver paste according to claim 1, is characterized in that, described acrylate oligomer is made up of epoxy acrylate and polyester acrylate, and the mass ratio of epoxy acrylate and polyester acrylate is 1:2.
6. ultraviolet light conductive silver paste according to claim 1, it is characterized in that, uv monomer is selected from 1,6 hexanediyl esters, tripropylene glycol diacrylate, neopentylglycol diacrylate, the third oxidation trimethylolpropane triacrylate, pentaerythritol triacrylate, two-trimethylolpropane triacrylate, 2-phenyl ethoxy acrylate, one or more in ethoxyethoxyethyl acrylate.
7. ultraviolet light conductive silver paste according to claim 2, is characterized in that, conductive submicron indefinite form silver powder particle diameter is 50nm-2 μm.
8. ultraviolet light conductive silver paste according to claim 1, it is characterized in that, uv light trigger is selected from a, a-dimethoxy-a-phenyl acetophenone, 1-hydroxycyclohexyl phenyl ketone (184), 2-hydroxy-2-methyl-1-phenyl-1-acetone (1173), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (369), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (907), 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide (TPO), 2-hydroxyl-4'-(2-hydroxy ethoxy)-2-methyl phenyl ketone, 1-[4-(2-hydroxyl-oxethyl) phenyl]-2-hydroxyl-2 methyl isophthalic acids-propane-1-ketone (2959), one or more in reactive amines.
9. ultraviolet light conductive silver paste according to claim 1 application on the touchscreen, it is characterized in that, by uv silver slurry by after the solidification of UV lamp, touch screen circuitry plate obtains silver slurry conductive coating, and on touch screen circuitry plate, prepare finished product conducting wire by laser etch process, and the live width of conducting wire after preparation on touch screen circuitry plate and line-spacing are 20 μm × 20 μm.
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Cited By (6)
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| CN106205775A (en) * | 2016-07-23 | 2016-12-07 | 佛山市中彩科技有限公司 | A kind of UV conductive silver paste formula and preparation method thereof |
| CN106531285A (en) * | 2016-11-03 | 2017-03-22 | 广州市尤特新材料有限公司 | Ultraviolet curing conductive silver slurry, and preparation method and application thereof |
| CN106833353A (en) * | 2016-12-21 | 2017-06-13 | 华南理工大学 | A kind of touch-screen UV curing nano silver wire slurries and preparation method thereof |
| CN107068242A (en) * | 2017-04-12 | 2017-08-18 | 佛山市顺德区百锐新电子材料有限公司 | A kind of preparation method of aqueous uv conductive silver pastes |
| CN107236099A (en) * | 2017-06-01 | 2017-10-10 | 长兴化学工业(中国)有限公司 | Acrylate urethane copolymer resins and the conductive silver paste containing the resin |
| CN111702166A (en) * | 2020-06-23 | 2020-09-25 | 西安汇创贵金属新材料研究院有限公司 | Metal composite material and preparation method thereof |
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| CN106205775A (en) * | 2016-07-23 | 2016-12-07 | 佛山市中彩科技有限公司 | A kind of UV conductive silver paste formula and preparation method thereof |
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| CN107236099B (en) * | 2017-06-01 | 2020-09-15 | 长兴化学工业(中国)有限公司 | Acrylate-polyurethane copolymer resin and conductive silver paste containing same |
| CN111702166A (en) * | 2020-06-23 | 2020-09-25 | 西安汇创贵金属新材料研究院有限公司 | Metal composite material and preparation method thereof |
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