CN105632591A - Conductive slurry and preparation thereof and application thereof - Google Patents
Conductive slurry and preparation thereof and application thereof Download PDFInfo
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- CN105632591A CN105632591A CN201610195292.8A CN201610195292A CN105632591A CN 105632591 A CN105632591 A CN 105632591A CN 201610195292 A CN201610195292 A CN 201610195292A CN 105632591 A CN105632591 A CN 105632591A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The present invention discloses conductive slurry and preparation thereof and application thereof. The conductive slurry comprises the following raw materials, by mass ratio, 1 part of photo-thermal dual-curing resin, 1.5 to 4 parts of diluent, and 0.5 to 11 parts of silver flour; the photo-thermal dual-curing resin is resin containing acrylic group; the boiling point of the diluent is from 80 DEG C to 180 DEG C, the viscosity of the diluent is from 1mPa.s to 2mPa.s, the surface tension of the diluent is from 20mN/m to 30 mN/m, and the diluent is volatile; and the particle size of the silver flour is from 0.1 to 1[Mu]m. The conductive slurry selects photo-thermal dual-curing resin to take as a curing matrix, and is able to make up the not enough depth solidification caused by light scattering, refraction and absorption of filling materials through thermocuring. Besides, the diluent/thixotropic agent mutual regulation method is adopted to allow the slurry to ensure the requirement of 3D ink-jet injection and have good stability.
Description
(1) technical field
The present invention relates to a kind of electrocondution slurry and preparation and application thereof.
(2) background technology
3D inkjet technology is a kind of increasing material manufacture (AdditiveManufacturing) technology, is a kind of emerging rapid shaping technique of informationization technology, intelligent manufacturing and novel material combination of sciences. 3D spray ink Printing does not need mould and following process, is considered to likely change the future of production, thus more and more causes the concern of national governments and industrial community. The position precision of 3D spray ink Printing and dimensional precision are the highest in various rapid shaping technique, by adopting multiple shower nozzle can conveniently realize the printing of many materials, are thus best suited for the target compound manufacturing high precision, many materials and complex construction.
For surface-mounted integrated circuit (pcb board), nowadays pcb board is all manufacture in the way of thick film screen printing and film printing. They respectively have the strengths and weaknesses place of oneself: film printing manufactures pcb board by subtraction indirect processes, especially wastewater problem is serious for " three wastes " problem, and prepared by individual layer, chemical corrosion is responsive, cost height, but make precision is far superior to thick film screen printing and uniform in material good; Thick film screen printing is with the direct manufacture technics pcb board of additive process, and cost is low, " three wastes " do not give prominence to, and severe rugged environment is stablized, and prepared by multilayer, but precision is low, and lines fineness is poor, and uniform in material is poor by problem. And if carry out the manufacture of pcb board by the mode of 3D spray ink Printing, be possible not only to the advantage of comprehensive both sides, it is also possible to weaken both sides' inferior position place. But also undeniable, its cost still can improve relative to film printing, performance is also weaker than the thick film screen printing technology of sintering process.
The precondition that the 3D utilizing 3D inkjet technology to realize multiple material prints is the uniform sizing material system being had the various materials that may be used for 3D spray ink Printing, print the target compound with electric function, it is necessary to have the electric slurry being applicable to 3D spray ink Printing to print the various electronic devices and components such as wire, resistance, electric capacity, inductance, semi-conductor. The research of this respect is also very rare in the world at present.
For the research of the electric slurry class for spray ink Printing in prior art, the especially research of electrocondution slurry, or of common occurrence. As patent CN101560349A has published the preparation method of a kind of jet conductive ink, patent CN101547980A has published the preparation method etc. of a kind of high electrical resistivity ink jet ink composition. But these invention be all aimed at film printing exploitation, really for 3D spray ink Printing electric slurry research very rare.
(3) summary of the invention
The present invention seeks to for the 3D ink-jet printing material not making conducting element in prior art, it provides a kind of can be used for 3D spray ink Printing high solids content electrocondution slurry and its preparation method and application.
The technical solution used in the present invention is:
The present invention provides a kind of electrocondution slurry, and described electrocondution slurry is made up of the raw material of following mass ratio: photo-thermal dual curable resin 1 part, thinner 1.5��4 parts, 0.5��11 part, silver powder; Described photo-thermal dual curable resin is the resin containing propylene acidic group; Described thinner boiling point 80 DEG C��180 DEG C, viscosity 1mPa s��2mPa s, surface tension 20mN/m��30mN/m, easily volatilize; Described silver powder particle diameter is 0.1��1 ��m.
Described photo-thermal dual curable resin is preferably epoxy acrylic resin, polyester acrylate, polyether acrylate or aliphatic epoxy resin. Photo-thermal dual curable resin refers to and both can carry out separately photocuring, can carry out separately again the resin of thermofixation. Here select this resinoid as cured matrix be because silver powder add the propagation that membership affects light, such internal layer is difficult to cured portion and just can make up with thermofixation. Thinner is the good solvent of selected photo-thermal dual curable resin, and acting as dissolving resin and resin is fully disperseed in the slurry, makes slurry have a suitable viscosity to reach the rheological requirement of 3D spray ink Printing. Thinner performance requriements is: boiling point 80 DEG C��180 DEG C, viscosity 1mPa s��2mPa s, and surface tension 20mN/m��30mN/m, more easily volatilizees, it is preferable that thinner is dehydrated alcohol, 1-Methoxy-2-propyl acetate or Virahol. Adding of silver powder is to allow slurry have conductivity, such that it is able to make the element printed have conductivity, expand the range of application of 3D spray ink Printing, it is desired to the particle diameter of silver powder is between 0.1��1 ��m, and the size of electric conductivity is regulated by the ratio of silver powder and resin.
Further, described electrocondution slurry also comprises 0.03-0.09 part thixotropic agent, and described thixotropic agent is thixotropic agent MT6900-20X (polyamide compound, Taiyuan Mei Te Xiang Science and Technology Ltd.). Thixotropic agent is after a kind of dispersion in the solution, the auxiliary agent of space three-dimensional reticulated structure is set up by non-bondings such as hydrogen bond/Intermolecular Forcess, its effect is for slurry provides stability depositing in process, due to its space structure and non-bonding set up, under certain external force effect, slurry meets 3D spray ink Printing requirement to ensure still can to reply viscosity. Its performance requriements is: have good consistency with selected thinner, it is possible to set up three-dimensional structure fast, obvious by its viscosity B coefficent after power effect.
Further, described electrocondution slurry also comprises light-initiated dose of 0.008-0.025 part, and described light-initiated dose is 2,4,6-trimethylbenzoy-dipheny phosphine oxide (chemical symbol TPO). Light-initiated dose for become free radical by absorbing the Energy Decomposition of certain optical wavelength, then free radical cause the monomer in component, performed polymer, functional group carry out polyreaction. Here light-initiated dose is in order to the resin in slurry carries out cross-linking and curing reaction further under ultraviolet lighting. Light-initiated dose of requirement is: optimum absorb wavelength is at 400nm��300nm.
Further, described electrocondution slurry is made up of the raw material of following quality proportioning: photo-thermal dual curable resin 1 part, thinner 1.5��4 parts, 0.5��11 part, silver powder, thixotropic agent is 0.03-0.09 part, light-initiated dose is 0.008-0.025 part, preferred electrocondution slurry is made up of the raw material of following quality proportioning: photo-thermal dual curable resin 1 part, thinner 2��3 parts, 2��11 parts, silver powder, thixotropic agent is 0.02-0.08 part, and light-initiated dose is 0.006-0.024 part.
The present invention provides the preparation method of a kind of described electrocondution slurry, and described method is: each component mixed by formula ratio, ultrasonic disperse, stir evenly, obtain described electrocondution slurry, it is preferable that join in thinner by photo-thermal dual curable resin, fully it is stirred to dissolve completely, in solution, adds silver powder, after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, sealing preserves, and obtains product.
If suitable interpolation thixotropic agent will be conducive to the stable of slurry, concrete making step is as follows: by formula ratio, photo-thermal dual curable resin is joined in thinner, fully stirring makes it dissolve completely, add thixotropic agent (mechanical stirring better effects if can be used if desired) again, it is stirred well in solution and can't see obvious particulate matter, leave standstill till forming an equal colloidal sol, stir evenly, then add silver powder, after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, stir evenly, obtain electrocondution slurry.
If light-initiated dose of suitable interpolation will be conducive to slurry to carry out photocuring faster, concrete making step is as follows: by formula ratio, photo-thermal dual curable resin is joined in thinner, fully stirring makes it dissolve completely, then light-initiated dose is added, fully stirring makes it dissolve completely, add thixotropic agent again, it is stirred well in solution and can't see obvious particulate matter (mechanical stirring better effects if can be used if desired), leave standstill till forming an equal colloidal sol, stir evenly, add silver powder again, after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, stir evenly, obtain electrocondution slurry.
In addition, the present invention also provides the application of a kind of described electrocondution slurry in 3D spray ink Printing conducting element.
Compared with prior art, the useful effect of the present invention is mainly reflected in:
Electrocondution slurry of the present invention selects photo-thermal dual curable resin as cured matrix, it is possible to thermofixation make up because of filler to scattering of light, refraction, absorption and cause can not deeply-curing. Meanwhile, the way mutually regulated with thinner/thixotropic agent, has again satisfactory stability while making this slurry ensure 3D spray ink Printing eject request.
The present invention adopts the mode of 3D spray ink Printing to make conducting element, the precision of conducting element can be promoted and realize the diversification of the creative making of conducting element, food, medical science, industry field are widened by field of food, medical field in the field printed by 3D, and the applicability that 3D is printed increases further. In addition, the way that this kind of thinner/thixotropic agent regulates jointly, it is possible to greatly improve the solid content of silver powder in final part, thus reduce and print part and tradition manufacture parts difference functionally.
Circuit to print on pcb board: film printing is owing to being individual layer manufacture, and thickness (general wet film layer is no more than 10 microns) in certain scope, cause needing with the conduction raw material of high-quality and by adding thick line width, resistance to be dropped to reduce heating loss in certain scope, but do like this and wiring board area can be made significantly to increase; Thick film screen printing precision is lower, and the circuit causing fineness higher is unstable. But, it is equipped with the mode of 3D printing with the electrocondution slurry of the present invention, multilayer printing can be carried out, print targeted strong, tolerance range height.
(4) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment of the present invention silver powder used is purchased from white sijna rice Science and Technology Ltd., and the equal footpath of powder grain is 0.8 micron. Described epoxy acrylic resin is purchased from Jiangsu Miki Chemical Co., Ltd.
Ultrasonication described in the embodiment of the present invention adopts ultrasonic disruption machine (JY99-IIDN, Xin Zhi bio tech ltd, Ningbo, instrument frequency: 19.5��20.5KHz) to carry out.
Embodiment 1
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined in 10g thinner (surface tension 22.32mN/m, easily volatilizees for dehydrated alcohol: viscosity 1.06mPa s, boiling point 78.4 DEG C), fully it is stirred to dissolve completely. 11g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 26g. Each performance test is in table 1.
Embodiment 2
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined in 15g thinner (surface tension 22.32mN/m, easily volatilizees for dehydrated alcohol: viscosity 1.06mPa s, boiling point 78.4 DEG C), fully it is stirred to dissolve completely. 11g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 31g. Each performance test is in table 1.
Embodiment 3
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 10g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 11g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 26g. Each performance test is in table 1.
Embodiment 4
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 15g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 11g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 31g. Each performance test is in table 1.
Embodiment 5
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 10g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 37g. Each performance test is in table 1.
Embodiment 6
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 10g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 33g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 48g. Each performance test is in table 1.
Embodiment 7
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 10g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 44g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 59g. Each performance test is in table 1.
Embodiment 8
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 10g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 55g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 70g. Each performance test is in table 1.
Embodiment 9
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.5g. Each performance test is in table 1.
Embodiment 10
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 15g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 42g. Each performance test is in table 1.
Embodiment 11
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 33g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 50.5g. Each performance test is in table 1.
Embodiment 12
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. (dimethylbenzene Peng of polymeric amide is moisted all things on earth to add 0.1g thixotropic agent MT6900-20X in solution, Taiyuan Mei Te Xiang Science and Technology Ltd.), fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.6g. Each performance test is in table 1.
Embodiment 13
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.7g. Each performance test is in table 1.
Embodiment 14
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. 0.4g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.9g. Each performance test is in table 1.
Embodiment 15
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.03g light-initiated dose of TPO (2,4,6-trimethylbenzoy-dipheny phosphine oxide), fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X (dimethylbenzene Peng of polymeric amide is moisted all things on earth) is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.73g. Each performance test is in table 1.
Embodiment 16
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.06g light-initiated dose of TPO, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.76g. Each performance test is in table 1.
Embodiment 17
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.09g light-initiated dose of TPO, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. 22g silver powder (white sijna rice Science and Technology Ltd. is added in solution, the equal footpath of powder grain is 0.8 micron), after fully stirring, ultrasonication 5 minutes, make the abundant wetting and dispersing of silver powder, supplement the thinner lost because of volatilization by mass conservation method, stir evenly, namely obtain product electrocondution slurry 39.79g. Each performance test is in table 1.
Embodiment 18
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.12g light-initiated dose of TPO, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. Adding 22g silver powder in solution, after fully stirring, ultrasonication 5 minutes, makes the abundant wetting and dispersing of silver powder, supplements the thinner lost because of volatilization by mass conservation method, stirs evenly, namely obtains product electrocondution slurry 39.82g. Each performance test is in table 1.
Embodiment 19
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.06g light-initiated dose of TPO, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. Adding 33g silver powder in solution, after fully stirring, ultrasonication 5 minutes, makes the abundant wetting and dispersing of silver powder, supplements the thinner lost because of volatilization by mass conservation method, stirs evenly, namely obtains product electrocondution slurry 50.76g. Each performance test is in table 1.
Table 1
Note: viscosity test: with rotational rheometer test, testing standard temperature: 25 DEG C, shearing rate: 8000s-1��
Stability of Slurry is tested: test according to GB/T6753.3-1986. But only carry out two tests of skinning, sedimentation degree here. All slurries all keep in Dark Place.
Photocuring time test: paint the film of 20��80 microns with slurry after, the time shutter required for surface drying is the photocuring time. Table is dry to be judged: be not stained with cotton-wool after photocuring.
Cured film powder dispersion state: pass judgment on the SEM figure of cured film cross section.
Cured film surface topography: directly visual inspection.
Cured film hardness: measure according to GB/T6739-2006.
Sticking power: test according to GB/T9286-98.
Embodiment 20
5g photo-thermal dual curable resin (epoxy acrylic resin) is joined 12.5g thinner (1-Methoxy-2-propyl acetate: viscosity 1.10mPa s, boiling point 146 DEG C, surface tension 28.9mN/m, more easily volatilizees) in, fully it is stirred to dissolve completely. In solution, add 0.06g light-initiated dose of TPO, fully it is stirred to dissolve completely. 0.2g thixotropic agent MT6900-20X is added in solution, fully stir (mechanical stirring better effects if can be used if desired), obvious particulate matter is can't see to solution, an equal colloidal sol leave standstill till within 5 minutes, can be formed, supplement the thinner lost because of volatilization by mass conservation method, stir evenly. Adding 11g silver powder in solution, after fully stirring, ultrasonication 5 minutes, makes the abundant wetting and dispersing of silver powder, supplements the thinner lost because of volatilization by mass conservation method, stirs evenly, namely obtains electrocondution slurry 28.76g. By electrocondution slurry automatic spray instrument (AFA-2, general Shen, Shanghai chemical industry apparatus company limited) paint after the coating of 20��80 ��m with UV curing (ID-UVI, Baoding Rong Da Electronics Equipment Co., Ltd) ultraviolet light polymerization 6��10 second, repeat after this step to overall thickness reaches about 0.1cm, being cut into the slice of 50mm*1mm, its resistivity and density are in table 2.
Embodiment 21
Operation is with embodiment 20, and silver powder consumption changes 22g into, and its electric conductivity and density are in table 2.
Embodiment 22
Operation is with embodiment 20, and silver powder consumption changes 33g into, and its electric conductivity and density are in table 2.
Embodiment 23
Operation is with embodiment 20, and silver powder consumption changes 44g into, and its electric conductivity and density are in table 2.
Embodiment 24
Operation is with embodiment 20, and silver powder consumption changes 55g into, and its electric conductivity and density are in table 2.
Table 2
Resistivity measurement method: measure volumetric resistivity value with DJ44 type direct-flow double bridge, then calculates resistivity with formula ��=RS/L. Wherein R is measured volume resistance, and S is slice sectional area, and L is strand length.
Density measurement: Archimedes's drainage is tested. The tap density of former silver powder is 9.4g/cm3��
Embodiment 25
The electrocondution slurry of embodiment 16 is adopted to print electrode and wire, coordinate by 1 part of epoxy acrylate, 2.5 parts of thinners, 4 parts of barium titanate powders, 0.05 part of thixotropic agent, the dielectric slurry print media of 0.008 part light-initiated dose composition, by the many shower nozzles ink jet type ultraviolet light polymerization printer produced by Canon Inc. of Japan3500SD/HD prints electrical condenser. Electrical condenser width 1.0mm after solidification, thick 0.5mm, electrode area 0.5mm2, dielectric thickness 1.0mm. With the accurate LCR tester test of Anji human relations E4980A, capacitance is 0.149F.
Claims (10)
1. an electrocondution slurry, it is characterised in that described electrocondution slurry is made up of the raw material of following mass ratio: photo-thermal dual curable resin 1 part, thinner 1.5��4 parts, 0.5��11 part, silver powder; Described photo-thermal dual curable resin is the resin containing propylene acidic group; Described thinner boiling point 80 DEG C��180 DEG C, viscosity 1mPa s��2mPa s, surface tension 20mN/m��30mN/m, easily volatilize; Described silver powder particle diameter is 0.1��1 ��m.
2. electrocondution slurry as claimed in claim 1, it is characterised in that described thinner is dehydrated alcohol, 1-Methoxy-2-propyl acetate or Virahol.
3. electrocondution slurry as claimed in claim 1, it is characterised in that described photo-thermal dual curable resin is epoxy acrylic resin, polyester acrylate, polyether acrylate or aliphatic epoxy resin.
4. electrocondution slurry as claimed in claim 1, it is characterised in that described electrocondution slurry also comprises 0.03-0.09 part thixotropic agent, and described thixotropic agent is thixotropic agent MT6900-20X.
5. electrocondution slurry as claimed in claim 4, it is characterised in that described electrocondution slurry also comprises light-initiated dose of 0.008-0.025 part, and described light-initiated dose is 2,4,6-trimethylbenzoy-dipheny phosphine oxide.
6. electrocondution slurry as described in one of claim 1-5, it is characterized in that described electrocondution slurry is made up of the raw material of following quality proportioning: photo-thermal dual curable resin 1 part, thinner 1.5��4 parts, 0.5��11 part, silver powder, thixotropic agent 0.03-0.09 part, light-initiated dose of 0.008-0.025 part.
7. the described electrocondution slurry of one of claim 1-6, it is characterized in that described electrocondution slurry is made up of the raw material of following quality proportioning: photo-thermal dual curable resin 1 part, thinner 2��3 parts, 2��11 parts, silver powder, thixotropic agent 0.02-0.08 part, light-initiated dose of 0.006-0.024 part.
8. electrocondution slurry as claimed in claim 4, it is characterised in that the preparation method of described electrocondution slurry is: by formula ratio, joins in thinner by photo-thermal dual curable resin, fully stirring makes it dissolve completely, then adds thixotropic agent, is stirred well in solution and can't see obvious particulate matter, leave standstill till forming an equal colloidal sol, stir evenly, then add silver powder, after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, stir evenly, obtain electrocondution slurry.
9. electrocondution slurry as claimed in claim 5, it is characterized in that the preparation method of described electrocondution slurry is: by formula ratio, photo-thermal dual curable resin is joined in thinner, fully stirring makes it dissolve completely, then light-initiated dose is added, fully stirring makes it dissolve completely, then adds thixotropic agent, is stirred well in solution and can't see obvious particulate matter, leave standstill till forming an equal colloidal sol, stir evenly, then add silver powder, after fully stirring, ultrasonic 5 minutes, make the abundant wetting and dispersing of silver powder, stir evenly, obtain electrocondution slurry.
10. the application of electrocondution slurry described in a claim 1 in 3D spray ink Printing conducting element.
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| CN116254016A (en) * | 2023-03-22 | 2023-06-13 | 哈尔滨工业大学重庆研究院 | Photo-curing printing ink, preparation method thereof and printing method |
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