CN104130628A - UV conductive ink and preparation method thereof - Google Patents
UV conductive ink and preparation method thereof Download PDFInfo
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- CN104130628A CN104130628A CN201410351189.9A CN201410351189A CN104130628A CN 104130628 A CN104130628 A CN 104130628A CN 201410351189 A CN201410351189 A CN 201410351189A CN 104130628 A CN104130628 A CN 104130628A
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Abstract
The invention discloses a UV conductive ink and a preparation method thereof. The UV conductive ink comprises, by mass 20-70 parts of a conductive slurry, 10-40 parts of a film forming resin, 10-30 parts of a monomer and 1-10 parts of a photoinitiator. The conductive slurry comprises, by mass, 20-50 parts of a conductive material, 10-30 parts of the a prepolymer, 2-40 parts of a monomer and 1-15 parts of a dispersant. The preparation method comprises the following steps: mixing the conductive material with the prepolymer, the monomer and the dispersant, stirring the above obtained mixture for 30min for pre-dispersion, and grinding by a high-speed grinding machine at a grinding speed of 1800r/min for 3h to make the above obtained material fully wetted and dispersed in order to obtain the conductive slurry; and mixing the conductive slurry with the film forming resin, the monomer and the photoinitiator, putting the newly obtained mixture into a vessel, arranging the vessel on an HJ-6A type digital thermostat long magnetic stirrer, and carrying out thermostatic stirring at 40DEG C for 0.5h until uniformity to obtain the ink. The production process of the UV conductive ink has little pollution to the environment.
Description
Technical field
The invention belongs to technical field of ink, relate to a kind of UV electrically conductive ink and preparation method thereof.
Background technology
According to the analysis of NanoMarkets market researchy corporation, electrically conductive ink market will be developed into a very large industry in the near future, and by 2015, electrically conductive ink market capitalisation will be current 3 times, reached 2,400,000,000 dollars.UV electrically conductive ink is a kind of functional ink, can in UV ink, add conductive carrier, makes ink have electroconductibility.UV electrically conductive ink is as a kind of environmental type functional ink, and the application prospect in flexographic printing is subject to extensive concern.Along with the development need of printing new technology, UV flexo electrically conductive ink is become better and better in the application prospect in printed electronic field.
A good UV electrically conductive ink formula, requires to have good printability, and the China ink layer after printing has the features such as strong adhesion, resistivity is low, solidification value is low, conductivity is stable.And in use there are a large amount of organic solvent volatilizations in existing UV electrically conductive ink at present, environment is caused to larger pollution, cost is high simultaneously, and specific conductivity also awaits improving.
Summary of the invention
The object of this invention is to provide a kind of UV electrically conductive ink.Solved the problem that in existing UV electrically conductive ink making processes, environment is caused larger pollution.
Another object of the present invention is to provide the making method of UV electrically conductive ink.
The technical solution used in the present invention is UV electrically conductive ink, and the mass fraction of its moiety is as follows: conductive paste 20-70 part, film-forming resin 10-40 part, monomer 10-30 part, light trigger 1-10 part.
Further, the mass fraction of the moiety of described conductive paste is electro-conductive material 20-50 part, prepolymer 10-30 part, monomer 2-40 part, dispersion agent 1-15 part.
Further, described electro-conductive material adopts the difform silver-colored particle of silver-colored particle, same particle size of identical shaped different-grain diameter or one or more mixtures of combined silver particle.
Further, described film-forming resin is one or more mixtures of epoxy acrylic resin, polyurethane acrylic resin, polyester acrylic resin, vinyl chloride-vinyl acetate resin.
Further, described prepolymer is one or more mixtures of epoxy acrylic resin, polyurethane acrylic resin, polyester acrylic resin, vinyl chloride-vinyl acetate resin.
Further, described monomer is one or more mixtures of vinylformic acid 2-ethoxy ethoxy ethyl ester, hexanediyl ester, phthalic acid di-alcohol diacrylate, neopentylglycol diacrylate, Triethylene glycol diacrylate, trimethylolpropene triacrylate.
Further, the olefin(e) acid segmented copolymer of the modified propylene hydrochlorate segmented copolymer of the disperbyk series of described dispersion agent WeiBYK company, the EFKA series of BASF AG, the CH series of Shanghai San Zheng company with one or more mixtures in the hyper-dispersant of anchor formula group.
Further; described light trigger is 2; 4; 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-cyclohexyl-phenyl ketone, 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone, phenyl two (2; 4,6-trimethylbenzoyl) one or more mixtures of phosphine oxide, 2-isopropyl thioxanthone.
The preparation method of above-mentioned UV electrically conductive ink, carries out according to following steps:
Step 1: the preparation of conductive paste:
By electro-conductive material, prepolymer, monomer and dispersant, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, add ready grinding bead, use high-speed grinder to grind 3 hours, grinding rate is 1800r/min, makes the fully wetting dispersion of material, obtains conductive paste.
Step 2: the preparation of ink:
Ground conductive paste, film-forming resin, monomer and light trigger are mixed, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, obtain ink to be prepared after stirring.
The production process environmental pollution that the invention has the beneficial effects as follows UV electrically conductive ink is little.
Accompanying drawing explanation
Fig. 1 is the UV electrically conductive ink experiment flow schematic diagram of the present invention to preparation;
Fig. 2 is that solid content of the present invention affects schematic diagram to ink conductivity;
Fig. 3 is laboratory sample Electronic Speculum figure of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be described:
A kind of UV electrically conductive ink of the present invention, the mass fraction of its moiety is as follows: conductive paste 20-70 part, film-forming resin 10-40 part, monomer 10-30 part, light trigger 1-10 part;
Wherein, the mass fraction of the moiety of conductive paste is electro-conductive material 20-50 part, prepolymer 10-30 part, monomer 2-40 part, dispersion agent 1-15 part.
Electro-conductive material in the present invention adopts one or more mixtures of the difform silver-colored particle of silver-colored particle, the same particle size of identical shaped different-grain diameter and combined silver particle.
Described prepolymer and film-forming resin are all one or more mixtures of epoxy acrylic resin, polyurethane acrylic resin, polyester acrylic resin, vinyl chloride-vinyl acetate resin.
Described monomer is one or more mixtures of vinylformic acid 2-ethoxy ethoxy ethyl ester, hexanediyl ester, phthalic acid di-alcohol diacrylate, neopentylglycol diacrylate, Triethylene glycol diacrylate, trimethylolpropene triacrylate.
The olefin(e) acid segmented copolymer of the modified propylene hydrochlorate segmented copolymer of the disperbyk series of described dispersion agent WeiBYK company, the EFKA series of BASF AG, the CH series of Shanghai San Zheng company with one or more mixtures in the hyper-dispersant of anchor formula group.
Described light trigger is 2; 4; 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-cyclohexyl-phenyl ketone, 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone, phenyl two (2; 4,6-trimethylbenzoyl) one or more mixtures of phosphine oxide, 2-isopropyl thioxanthone.
Preparation method according to the UV electrically conductive ink of mentioned component is:
The preparation of UV flexo electrically conductive ink adopts dispersion method.Dispersion method refer to utilize various machinery by grinding, pulverizing means become the particle of big particle into micropartical, are a kind of physical methods.
1, the preparation of conductive paste:
By electro-conductive material, prepolymer, monomer and dispersant, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, add ready grinding bead, use high-speed grinder to grind 3 hours, grinding rate is 1800r/min, makes the fully wetting dispersion of material, obtains conductive paste.
2, the preparation of ink
Ground conductive paste, film-forming resin, monomer and light trigger are mixed, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, obtain ink to be prepared after stirring.
Prepare electrically conductive ink, its required electro-conductive material plays vital effect to the electroconductibility of ink, for conductive silver paste, its electro-conductive material particle diameter used is less, dispersiveness is poorer, because metallic substance particle diameter is less, metallic particles is more active, surfactivity is higher, and " gathering of uniting " phenomenon is more obvious.Because electro-conductive material particle diameter used is nano level, its particle is less, and performance is more active, is exposed to very easily oxidation in air, and at particle surface, forms the oxidizing substance of one deck high-insulation.For this reason, before this ink of preparation, must first to electro-conductive material, remove zone of oxidation and process.Secondly, for difform conductive silver particle, there is larger difference in its conductivity, the electro-conductive material that this UV electrically conductive ink adopts is the mixed system of sheet and spherical silver powder, while causing contacting due to flake silver powder out-of-shape, there is gap, so fill the spherical conductive silver particle filling chink of appropriate ratio, the contact of conductive silver material is more stable like this, contact area is larger, electroconductibility and dispersed better, electroconductibility and the dispersing property of the electrically conductive ink preparing are better, and resistance is less and stable.Finally, sintering temperature has direct impact to the electroconductibility of UV flexo electrically conductive ink, obtain the good UV flexo of conductivity electrically conductive ink printed matter, sintering temperature must be controlled in optimum range, both guarantee the electroconductibility of UV flexo electrically conductive ink printed matter, guaranteed again the ink adhesion of UV flexo electrically conductive ink printed matter.The present invention show that the sintering temperature of conductive paste is controlled at 160-200 ℃ and is advisable after deliberation, and the sintering temperature of electrically conductive ink is controlled at 300 ℃ and is advisable.
The present invention will be described to enumerate specific embodiment below, and the proportioning in the embodiment of the present invention is by weight.
Embodiment 1: by 30 parts of electro-conductive materials, 25 parts of prepolymers, 40 parts of monomers, 5 parts of mixing of dispersion agent, wherein to select product designation be the spherical silver powder of MSP-07 to electro-conductive material, prepolymer is polyester acrylic resin, be selected from the CN series of SATORMAR company, monomer is commercially available vinylformic acid 2-ethylhexyl, the mixture of tri (propylene glycol) diacrylate and neopentylglycol diacrylate, ratio is vinylformic acid 2-ethylhexyl: tri (propylene glycol) diacrylate: neopentylglycol diacrylate=8:4:3 (weight ratio), dispersion agent is with the hyper-dispersant of anchor formula group, to be selected from the CH series of Shanghai San Zheng company, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, use high-speed grinder to grind 3 hours, obtain conductive paste.By 20 parts of conductive paste, 30 parts of monomers, 40 parts of film-forming resins, light trigger 10 parts (comprising hydrogen donor) mixes, monomer is commercially available vinylformic acid 2-ethylhexyl, the mixture of tri (propylene glycol) diacrylate and neopentylglycol diacrylate, ratio is vinylformic acid 2-ethylhexyl: tri (propylene glycol) diacrylate: neopentylglycol diacrylate=8:4:3 (weight ratio), film-forming resin is the VIAJET series that hyperbranched polyester acrylic resin is selected from UCB. S.A. (BE) Bruxelles Belgium, light trigger is 2, 4, the mixture of 6-trimethylbenzoyl-diphenyl phosphine oxide and 2-hydroxy-2-methyl-1-phenyl-1-acetone, ratio is 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide: 2-hydroxy-2-methyl-1-phenyl-1-acetone=2:1 (weight ratio), pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, after stirring, obtain ink to be prepared.
Embodiment 2: by 20 parts of electro-conductive materials, 30 parts of prepolymers, 45 parts of monomers, 5 parts of mixing of dispersion agent, wherein to select product designation be the spherical silver powder of MSP-01 to electro-conductive material, prepolymer is commercially available vinyl chloride-vinyl acetate resin, monomer is commercially available vinylformic acid 2-ethoxy ethoxy ethyl ester, the mixture of the Viscoat 295 of hexanediyl ester and ethoxylation, ratio is vinylformic acid 2-ethoxy ethoxy ethyl ester: hexanediyl ester: the Viscoat 295=10:6:1 of ethoxylation (weight ratio), dispersion agent is the byk-9077 that modified propylene hydrochlorate segmented copolymer is selected from BYK company, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, use high-speed grinder to grind 3 hours, obtain conductive paste.By 25 parts of conductive paste, 25 parts of monomers, 49 parts of film-forming resins, light trigger 1 part (comprising hydrogen donor) mixes, monomer is commercially available vinylformic acid 2-ethoxy ethoxy ethyl ester, the mixture of the Viscoat 295 of hexanediyl ester and ethoxylation, ratio is vinylformic acid 2-ethoxy ethoxy ethyl ester: hexanediyl ester: the Viscoat 295=10:6:1 of ethoxylation (weight ratio), film-forming resin is the VIAJET series that hyperbranched polyester acrylic resin is selected from UCB. S.A. (BE) Bruxelles Belgium, light trigger is 1-hydroxyl-cyclohexyl-phenyl ketone and phenyl two (2, 4, 6-trimethylbenzoyl) mixture of phosphine oxide, ratio is 1-hydroxyl-cyclohexyl-phenyl ketone: phenyl two (2, 4, 6-trimethylbenzoyl) phosphine oxide=4:3 (weight ratio), pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, after stirring, obtain ink to be prepared.
Embodiment 3: by 15 parts of electro-conductive materials, 30 parts of prepolymers, 40 parts of monomers, 15 parts of mixing of dispersion agent, wherein to select product designation be the flake silver powder of SF-05 to electro-conductive material, prepolymer is commercially available epoxy acrylic resin, monomer is commercially available isobornyl acrylate and the mixture of neopentylglycol diacrylate, ratio is isobornyl acrylate and neopentylglycol diacrylate=5:4 (weight ratio), dispersion agent is with the hyper-dispersant of anchor formula group, to be selected from the CH series of Shanghai San Zheng company, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, use high-speed grinder to grind 3 hours, obtain conductive paste.By 30 parts of conductive paste, 25 parts of monomers, 38 parts of film-forming resins, light trigger 7 parts (comprising hydrogen donor) mixes, monomer is commercially available isobornyl acrylate and the mixture of neopentylglycol diacrylate, ratio is isobornyl acrylate and neopentylglycol diacrylate=5:4 (weight ratio), film-forming resin is polyester acrylic resin, be selected from the CN series of SATORMAR company, light trigger is 1-hydroxyl-cyclohexyl-phenyl ketone, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, after stirring, obtain UV electrically conductive ink to be prepared.
Embodiment 4: by 15 parts of electro-conductive materials, 25 parts of prepolymers, 55 parts of monomers, 5 parts of mixing of dispersion agent, wherein to select product designation be the flake silver powder of SF-01 to electro-conductive material, prepolymer is the VIAJET series that hyperbranched polyester acrylic resin is selected from UCB. S.A. (BE) Bruxelles Belgium, monomer is commercially available neopentylglycol diacrylate and the mixture of tri (propylene glycol) diacrylate, ratio is neopentylglycol diacrylate: tri (propylene glycol) diacrylate=8:9 (weight ratio), dispersion agent is the EFKA series that olefin(e) acid segmented copolymer is selected from BASF AG, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, use high-speed grinder to grind 3 hours, obtain conductive paste.By 30 parts of conductive paste, 30 parts of monomers, 30 parts of film-forming resins, light trigger 10 parts (comprising hydrogen donor) mixes, monomer is commercially available neopentylglycol diacrylate and the mixture of tri (propylene glycol) diacrylate, ratio is neopentylglycol diacrylate: tri (propylene glycol) diacrylate=8:9 (weight ratio), film-forming resin is polyester acrylic resin, be selected from the CN series of SATORMAR company, light trigger is the mixture of 2-isopropyl thioxanthone and 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone, ratio is 2-isopropyl thioxanthone: 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone=1:3, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, after stirring, obtain UV electrically conductive ink to be prepared.
Embodiment 5: by 15 parts of electro-conductive materials, 40 parts of prepolymers, 40 parts of monomers, 5 parts of mixing of dispersion agent, wherein to select product designation be the spherical silver powder of MSP-02H to electro-conductive material, prepolymer is the VIAJET series that hyperbranched polyester acrylic resin is selected from UCB. S.A. (BE) Bruxelles Belgium, monomer is commercially available isobornyl acrylate, the mixture of two contracting propylene glycol double methacrylates and Viscoat 295, ratio is isobornyl acrylate: two contracting propylene glycol double methacrylate: Viscoat 295=5:3:2 (weight ratio), dispersion agent is the byk-2001 that modified propylene hydrochlorate segmented copolymer is selected from BYK company, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, use high-speed grinder to grind 3 hours, obtain conductive paste.By 20 parts of conductive paste, 25 parts of monomers, 50 parts of film-forming resins, light trigger 5 parts (comprising hydrogen donor) mixes, monomer is commercially available isobornyl acrylate, the mixture of two contracting propylene glycol double methacrylates and Viscoat 295, ratio is isobornyl acrylate: two contracting propylene glycol double methacrylate: Viscoat 295=5:3:2 (weight ratio), film-forming resin is the VIAJET series that hyperbranched polyester acrylic resin is selected from UCB. S.A. (BE) Bruxelles Belgium, light trigger is 2, 4, the mixture of 6-trimethylbenzoyl-diphenyl phosphine oxide and 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone, ratio is 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide and 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone=1:1, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, after stirring, obtain UV electrically conductive ink to be prepared.
Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition, various changes or modification that those skilled in the art make the present invention, these equivalent form of values fall within the application's scope required for protection equally.
UV electrically conductive ink of the present invention is carried out to experimental verification below:
Be illustrated in figure 1 the schematic flow sheet of experiment; Experiment material is in Table 1.
Table 1 experiment material
Experimental instrument and equipment:
1, GJ-2S type high-speed stirring decollator;
2, HJ-6A type digital display constant temperature bull magnetic stirring apparatus;
3, AR2000ex rheometer;
4, Hegman grind gage;
5, retort furnace;
6, Multi-functional general-service becomes;
7, FusionUV solidifies machine;
8, " 0 " number hardened coating silk rod;
Experimental technique: by research electro-conductive material shape and grain diameter, prepare optimum conductive paste; By changing conductive paste and prepolymer ratio, control electro-conductive material content, thus the impact of research electro-conductive material content on ink electroconductibility; By changing light trigger kind, control ink solidification speed, thus the impact of research curing speed on ink electroconductibility; By changing sintering temperature, the impact of research sintering temperature on ink electroconductibility, as shown in Figure 1.The performance test methods of UV flexo electrically conductive ink: the salient features of UV flexo electrically conductive ink comprises dispersiveness, curing speed, viscosity, electroconductibility and sintering temperature etc.
Distributes ink testing method: use Hegman grind gage to carry out dispersiveness test to the conductive paste of having ground.Testing method is as follows: the conductive paste that grinding is completed is poured vessel into, use dropper to draw 5-10 gram on sheet glass, add the alcohol of equal in quality to dilute the conductive paste of extracting, separately get a new dropper conductive paste being diluted is extracted on Hegman grind gage, with scraper plate equipment, extracted conductive paste is at the uniform velocity coated with and observe phenomena.Even particle distribution and more position are exactly the average particle size distribution of particle, read corresponding data, analyze dispersed.
Ink viscosity testing method: use AR2000ex rheometer test ink rheology row, obtain ink viscosity curve and it is analyzed.Start preheating AR2000ex rheometer, the aluminum Peltier board that installation diameter is 60mm, connects waters and prepares calibration.After having calibrated, ink to be measured is extracted to operating table surface with dropper, extract 10-15g and ink is covered to Peltier board completely and be as the criterion, start operation, the viscograph that after completing, automatic generation contains 13 coordinate point, preserves and does Viscosity Analysis.
Ink solidification testing method: use FusionUV to solidify machine to ink solidification.Testing method is as follows: the pre-thermofixation machine of starting shooting, after machine is stable, can test.By on same sample coated thin film, be then separately fixed on several card fixtures, then allow these samples be cured under identical curing power (100W) and different curing speed, observe phenomena record.
Ink electroconductibility testing method: use Multi-functional digital display volt ohm-milliammeter to carry out conducting performance test, measure the resistance value of electrically conductive ink printed matter.To use the printing of electrically conductive ink printing to carry out last sintering processes, sintering processes finishes rear use multi-function multimeter and measures its resistance value, and record data also carry out analyzing and processing, and the conductivity of electrically conductive ink is proved in contrast.
Ink sintering temperature testing method: use retort furnace to carry out sintering processes to the sample printing.1, the product that uses conductive paste to print is put into retort furnace and carry out sintering processes, time is 3min, temperature is decided to be respectively 140 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 215 ℃, after sintering processes, take out sample, when temperature is down to room temperature, its resistance is measured, recorded and contrast the conductivity of proving conductive paste.2, the product that uses electrically conductive ink to print is first put into retort furnace after the curing machine of UV solidifies again and carry out sintering processes, time is decided to be respectively 3min, 5min, temperature is decided to be 300 ℃, after sintering processes, take out sample, when temperature is down to room temperature, its resistance is measured, recorded and contrast the conductivity of proving electrically conductive ink.
Method for making sample: use flexographic printing, manual evenly coating.The electrically conductive ink that configuration is completed takes out 5-10g with suction pipe and drips on sheet glass, use " 0 " number silk rod to be evenly coated with electrically conductive ink, flexographic printing plates is rolled across gently to the sheet glass that is evenly coated with electrically conductive ink, again the upper forme of crossing electrically conductive ink is rolled across to slide glass gently, after hand-printing completes, can carry out next step photocuring operation.
Experimental result and analysis: different electro-conductive material analyzing conductivities.Prepare the required electro-conductive material of electrically conductive ink the electroconductibility of ink is played to vital effect, for this reason, this problem selects four kinds of electro-conductive materials to test, and therefrom selects the material of conductivity optimum to prepare electrically conductive ink, and experimental performance is to such as table 2:
The comparison of table 2 electro-conductive material conductivity
By table 2, can find out, because electro-conductive material particle diameter used is nano level, its particle is less, and performance is more active, is exposed to very easily oxidation in air, and at particle surface, forms the oxidizing substance of one deck high-insulation.For this reason, before preparing ink, must first to electro-conductive material, remove zone of oxidation and process.And silver powder is with respect to above-mentioned other three kinds of metal powders, its chemical property is comparatively stable, and oxidation rate is slower, removes zone of oxidation method comparatively simple, optimum because of its conductivity again, and the preparation that consolidates problem ink adopts silver powder to carry out.
The research of conductive silver paste conductivity: silver-colored particle shape, the impact of particle diameter on silver slurry electroconductibility; Select the silver powder of four kinds of different shapes different-grain diameters, keep its content constant, securing unit and prepolymer contamination, prepare conductive silver paste.Sintering temperature is 200 ℃, and sintering time is 3min, the resistance of testing conductive silver slurry, and result is as shown in table 3:
The different silver-colored particle shapes of table 3, the prepared electricity slurry of particle diameter resistance
By table 3, can find out, for the conductive silver material of sheet and spherical particle, the larger conductivity of particle diameter is better and more stable, and this is because particle diameter is larger, and conductive silver particle contact is better, and point of contact is more, and contact area is larger.When configuration electrically conductive ink, the electroconductibility of electro-conductive material directly affects the conductivity of electrically conductive ink.For difform conductive silver particle, the electroconductibility of sheet conductive silver particle is better than spherical conductive silver particle, and this is because spherical conductive silver particle is mainly with tangent contact, is a contact, and contact area is narrow and small, contacts unstable; And sheet conductive silver particle is mainly with being affixed contact, be face contact, contact area is larger, and contact stabilization is more conducive to prepare electrically conductive ink so sheet conductive silver particle is compared spherical conductive silver particle.
Silver particle shape, particle diameter are starched dispersed impact to silver: select the silver powder of four kinds of different shapes different-grain diameters, keep its content constant, securing unit and prepolymer contamination, prepare conductive silver paste, the particle diameter of test silver slurry, and result is as shown in table 4:
Table 4 silver slurry is dispersed
By table 4, can find out, for conductive silver paste, its electro-conductive material particle diameter used is less, and dispersiveness is poorer, because metallic substance particle diameter is less, metallic particles is more active, and surfactivity is higher, and " gathering of uniting " phenomenon is more obvious.
In sum, in order to control dispersiveness and the electroconductibility of ink, this problem determines to use SF-05 and two kinds of model silver powder of MSP-02H to wait mass mixing slurrying, sintering temperature is 200 ℃, sintering time is 3min, tests its electroconductibility and dispersiveness, and result is as shown in table 5:
Table 5 mixture plasma performance
By table 5, can find out, silver slurry particle diameter and resistance prepared by mixing SF-05 and two kinds of model silver powder of MSP-02H are all less and stable, this is to have gap while causing contacting due to flake silver powder out-of-shape, so can fill the spherical conductive silver particle filling chink of appropriate ratio, the contact of conductive silver material is more stable like this, contact area is larger, electroconductibility and dispersed better, and electroconductibility and the dispersing property of the electrically conductive ink preparing are better.
The impact of sintering temperature on conductive paste conductivity: select the silver powder of four kinds of different shapes different-grain diameters, keep its content constant, securing unit and prepolymer contamination, prepare conductive silver paste.Sintering time is 3min, the sintering temperature of testing conductive silver slurry, and result is as shown in table 6:
Table 6 conductive silver paste sintering temperature and resistance corresponding relation
By table 6, can find out, the temperature variant variation of electroconductibility of conductive paste there is no evident regularity, and optimal sintering temperature is at 160 ℃-200 ℃.The too low conductive paste printing sample surface macromolecular material that causes of temperature is trapped in sample surfaces, forms the film of one deck high-insulation, thereby affects the conductivity of conductive paste; Excess Temperature can cause macromolecular material in conductive paste to evaporate too much, thereby causes that the printing sample of conductive silver paste ruptures, and then causes the experiment of silver slurry conducting performance test cannot proceed (occurring resistance ∞ phenomenon).
The research of UV flexo electrically conductive ink conductivity: the impact of solid content on ink electroconductibility, fixedly prepolymer and monomeric species and content, change light trigger kind, is mixed with electrically conductive ink by conductive paste and the UV system of preparation.Change the blending ratio of conductive silver paste and UV system, changed the solid content of ink, the conductivity of research ink, result as shown in Figure 2, by Fig. 2 (a), (c) can find out, the lower electrically conductive ink conductivity of conductive silver content is better, and Fig. 2 (b) can find out, the higher electrically conductive ink conductivity of conductive silver content is better.Therefore, the conductivity of electrically conductive ink is tight relevant with the content of electro-conductive material, also relevant with other component of electrically conductive ink, and when content one timing, the component that the conductivity of electrically conductive ink depends primarily on electrically conductive ink itself forms.For this reason, during preparation electrically conductive ink, must carry out the research of electrically conductive ink self component property, thereby filter out, be more suitable for developing the required various constituent materialss of electrically conductive ink.
The impact of curing speed on ink electroconductibility: fixedly prepolymer and monomeric species and content, be mixed with electrically conductive ink by conductive paste and the UV system of preparation.Change light trigger contamination, changed the curing speed of ink, the conductivity of research ink, sintering time is 5min, and curing power is 100w, and result is as shown in table 7:
Table 7 curing speed and conductivity reduced parameter
By table 7, can find out, the ultraviolet light polymerization speed of electrically conductive ink is faster, and the conductivity of ink is poorer and unstable.Get above-mentioned front 3 kinds of electrically conductive inks, use " 0 " number hardened coating silk rod to be evenly coated with, make respectively two samples, be labeled as 1-1,1-2,2-1,2-2,3-1,3-2.Wherein after 3 kinds of sample 1 hardened coatings all without other operations, 2, all the other 3 kinds of samples carry out ultraviolet light polymerization after hardened coating, after solidifying, these 6 kinds of samples are carried out to electron microscopic observation, thereby the ultraviolet light polymerization speed of analyzing electrically conductive ink is faster, poorer and the unsettled reason of conductivity of ink, Electronic Speculum figure as shown in Figure 3.(a) being sample 1-1 Electronic Speculum figure, is (b) sample 1-2 Electronic Speculum figure, is (c) sample 2-1 Electronic Speculum figure, is (d) sample 2-2 Electronic Speculum figure, (e) is sample 3-1 Electronic Speculum figure, is (f) sample 3-2 Electronic Speculum figure.As seen in Figure 3, morphological differences before sample solidifies and after solidifying is larger, before solidifying, conductive silver material contact in sample is good, after solidifying, the conductive silver material contact in sample is unstable, between conductive silver material, occurs gap, the material of filling this gap is other mixture paste while preparing electrically conductive ink, and its main component is photo-curing material.Therefore can indirectly infer, sample after ultraviolet light polymerization, photo-curing material in its electrically conductive ink is shown in light generation crosslinking reaction, the longer polymkeric substance of " C " chain is opened and be reassembled as to " C=C " two keys, thereby cause occurring between conductive silver material expendable gap, and then cause the conductivity of electrically conductive ink sample to decline and unstable.Electron microscopy observation further shows, ultraviolet light polymerization ability is stronger, and photocuring efficiency is higher, and " becoming wall to intercept " phenomenon between this polymkeric substance is more obvious, and the conductivity of electrically conductive ink is poorer and more unstable.
The impact of sintering temperature on ink electroconductibility: fixedly prepolymer, monomer and light trigger contamination, be mixed with electrically conductive ink by conductive paste and the UV system of preparation.Adopt two kinds of ink data to carry out lateral comparison, be respectively light trigger ITX, 907,184 and the ink of light trigger ITX, 184 preparations, change sintering temperature, the conductivity of research ink, sintering time is 5min, result is as shown in table 8:
Table 8 sintering temperature is to ink Conductivity
By table 8, can find out, regularly, sintering temperature is higher for sintering time one, electrically conductive ink conductivity is better, and optimal sintering temperature is 300 ℃ of left and right, and excess Temperature can cause electrically conductive ink printed matter surface macromolecule resin to volatilize in a large number, ink surface layer ruptures, and conductivity cannot be measured.
Experiment conclusion: show that by experiment concrete conclusion is as follows:
1, electro-conductive material contamination has a great impact the conductivity of UV flexo electrically conductive ink.Make electrically conductive ink conductivity reach best, need to select to there is the electro-conductive material of satisfactory electrical conductivity, and select suitable electro-conductive material content, make ink reach suitable conductivity.The conductivity of material of the present invention is best.
2, light trigger contamination has important impact to UV flexo electrically conductive ink curing speed, adopts composite photoinitiator can obtain the good ink of over-all properties.Meanwhile, the curing speed of ink has affected indirectly its electroconductibility, the electrically conductive ink of light trigger preparation of the present invention, and its conductivity is optimum and the most stable.
3, sintering temperature has direct impact to the electroconductibility of UV flexo electrically conductive ink, obtain the good UV flexo of conductivity electrically conductive ink printed matter, sintering temperature must be controlled in optimum range, both guarantee the electroconductibility of UV flexo electrically conductive ink printed matter, guaranteed again the ink adhesion of UV flexo electrically conductive ink printed matter.This experimental result shows, the sintering temperature of conductive paste is controlled at 160-200 ℃ and is advisable, and the sintering temperature of electrically conductive ink is controlled at 300 ℃ and is advisable.
Claims (9)
1. a UV electrically conductive ink, the mass fraction of its moiety is as follows: conductive paste 20-70 part, film-forming resin 10-40 part, monomer 10-30 part, light trigger 1-10 part.
2. according to a kind of UV electrically conductive ink described in claim 1, it is characterized in that: the mass fraction of the moiety of described conductive paste is electro-conductive material 20-50 part prepolymer 10-30 part, monomer 2-40 part, dispersion agent 1-15 part.
3. according to a kind of UV electrically conductive ink described in claim 2, it is characterized in that: described electro-conductive material adopts one or more mixtures of the difform silver-colored particle of silver-colored particle, the same particle size of identical shaped different-grain diameter or combined silver particle.
4. according to a kind of UV electrically conductive ink described in claim 1, it is characterized in that: described film-forming resin is one or more mixtures of epoxy acrylic resin, polyurethane acrylic resin, polyester acrylic resin, vinyl chloride-vinyl acetate resin.
5. according to a kind of UV electrically conductive ink described in claim 2, it is characterized in that: described prepolymer is one or more mixtures of epoxy acrylic resin, polyurethane acrylic resin, polyester acrylic resin, vinyl chloride-vinyl acetate resin.
6. according to a kind of UV electrically conductive ink described in claim 1 or 2, it is characterized in that: described monomer is one or more mixtures of vinylformic acid 2-ethoxy ethoxy ethyl ester, hexanediyl ester, phthalic acid di-alcohol diacrylate, neopentylglycol diacrylate, Triethylene glycol diacrylate, trimethylolpropene triacrylate.
7. according to a kind of UV electrically conductive ink described in claim 2, it is characterized in that: the olefin(e) acid segmented copolymer of the modified propylene hydrochlorate segmented copolymer of the disperbyk series of described dispersion agent WeiBYK company, the EFKA series of BASF AG, the CH series of Shanghai San Zheng company with one or more mixtures in the hyper-dispersant of anchor formula group.
8. according to a kind of UV electrically conductive ink described in claim 1; it is characterized in that: described light trigger is 2; 4; 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-cyclohexyl-phenyl ketone, 2-methyl isophthalic acid-[4-methylthio group phenyl]-2-morpholinyl-1-acetone, phenyl two (2; 4,6-trimethylbenzoyl) one or more mixtures of phosphine oxide, 2-isopropyl thioxanthone.
9. according to the preparation method of a kind of UV electrically conductive ink described in claim 1, it is characterized in that carrying out according to following steps:
Step 1: the preparation of conductive paste:
By electro-conductive material, prepolymer, monomer and dispersant, use agitator by mixture stir within 30 minutes, carry out pre-dispersed after, add ready grinding bead, use high-speed grinder to grind 3 hours, grinding rate is 1800r/min, makes the fully wetting dispersion of material, obtains conductive paste;
Step 2: the preparation of ink:
Ground conductive paste, film-forming resin, monomer and light trigger are mixed, pack in vessel and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 40 degree constant temperature stir half an hour, obtain ink to be prepared after stirring.
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Application publication date: 20141105 |