CN105702380A - Method for forming conductive layer by employing ink composition - Google Patents
Method for forming conductive layer by employing ink composition Download PDFInfo
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- CN105702380A CN105702380A CN201410705954.2A CN201410705954A CN105702380A CN 105702380 A CN105702380 A CN 105702380A CN 201410705954 A CN201410705954 A CN 201410705954A CN 105702380 A CN105702380 A CN 105702380A
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Abstract
The invention discloses a method for forming a conductive layer by employing ink composition. The method includes: mixing each component of the ink composition with a solvent, and forming an ink mixture; coating a treating agent on the surface of an insulating substrate, and forming a treating agent layer; coating the ink mixture on the treating agent layer, and forming an ink layer; after the drying of the ink layer, performing rotation centrifugation of the insulating substrate equipped with the ink layer, depositing conductive materials in the ink layer, and forming an ink deposition layer; soaking the insulating substrate equipped with the ink deposition layer into the solvent, removing a part or all of connecting materials in the ink deposition layer, and forming a pre-conductive layer; and taking out the insulating substrate equipped with the pre-conductive layer, removing the solvent in the pre-conductive layer, and forming the conductive layer via curing. According to the method, the insulating substrate equipped with the ink deposition layer is soaked into the solvent, and all or a part of the connecting materials can be removed so that the thickness of the conductive layer is reduced, and the conductive layer is more applicable to the thinning trend of electronic devices.
Description
Technical field
The present invention relates to ink printing field, in particular it relates to a kind of method that ink application compositions forms conductive layer。
Background technology
Form conductive layer at surfaces of polymeric articles, as the path of electromagnetic signal conduction, be widely used in the fields such as automobile, industry, computer, communication。Being formed selectively conductive layer at surfaces of polymeric articles is the core link that such polymer product manufactures。
Electrically conductive ink (is primarily referred to as mixed type conduction compound oil ink), and, as the raw material forming conductive layer, its conductive material being made by being dispersed in ink carrier is to conduct electric current。
Conventional conductive ink mostly is solvent-borne type, and this solvent-borne type electrically conductive ink is in the process forming conductive layer, for the ease of coating printing ink, by adding binder (binding agent) in ink。And binding agent electric conductivity conventional at present is relatively low, for reaching conduction demand, it has to improve the coating thickness of ink。In this case, not only increase cost of material, but also be unfavorable for ensureing the ruggedness of conductive layer self。Thick conductive layer certainly will affect the assembling of miscellaneous part, and then is difficult to meet the thinning trend of electronic installation。
Summary of the invention
It is an object of the invention to overcome existing middle because of binder electric conductivity relatively low, cause the technical problem that the coating thickness of ink is thicker, it is provided that a kind of ink application compositions forms the method for conductive layer。
To achieve these goals, the invention provides a kind of method that ink application compositions forms conductive layer, wherein ink composite contains at least one conductive material and at least one binder, and ink application compositions forms the method for conductive layer and comprises the following steps:
Each component in above-mentioned ink composite is mixed with solvent, forms ink mixture；
In insulating properties substrate surface coating processing agent, formation processes oxidant layer；
Ink mixture is coated in process oxidant layer, forms ink layer；
After ink layer surface drying, the insulating properties base material being formed with ink layer is rotated centrifugal, make the conductive material in ink layer deposit, form ink deposition layer；
Will be formed with the insulating properties base material of ink deposition layer and be impregnated in solvent, remove all or part of binder in ink deposition layer, form pre-conductive layer；
Take out the insulating properties base material being formed with pre-conductive layer, remove solvent cures in pre-conductive layer and form conductive layer。
Its method forming conductive layer of above-mentioned ink application compositions provided by the present invention, by the mode of rotating centrifugal, the conductive material formation of deposits in ink layer is made to precipitate, conductive material deposition is made to come together on the surface of insulating properties base material, the bottom of ink layer, and then while making conductive material and binder layering, conductive material is combined with inorganic agent；Utilize binder can be dissolved in the characteristic of solvent, will be formed with the insulating properties base material of ink deposition layer and be impregnated in solvent, all or part of binder in ink deposition layer can be removed, reduce the impact of the electric conductivity of the binder conductive layer on being formed, and reduce the thickness of conductive layer, and then make to be more suitable for the thinning trend of electronic installation by its prepared conductive layer。
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently。
Detailed description of the invention
It is described in detail below in conjunction with the specific embodiment of the present invention。It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention。
In the present invention, term " solidification " refers to when uniform temperature, makes the method that pre-conductive layer desolvation (being similar to dehydration) forms solid (film)。
Introduce as background section, exist in the prior art because binder electric conductivity is relatively low, cause the technical problem that the coating thickness of ink is thicker。In order to solve this technical problem。Provide a kind of method that ink application compositions forms conductive layer in the present invention, wherein ink composite contains at least one conductive material and at least one binder, ink application compositions forms the method for conductive layer and comprises the following steps: each component in above-mentioned ink composite mixed with solvent, forms ink mixture；In insulating properties substrate surface coating processing agent, formation processes oxidant layer；Ink mixture is coated in process oxidant layer, forms ink layer；After ink layer surface drying, the insulating properties base material being formed with ink layer is rotated centrifugal, make the conductive material in ink layer deposit, form ink deposition layer；Will be formed with the insulating properties base material of ink deposition layer and be impregnated in solvent, remove all or part of binder in ink deposition layer, form pre-conductive layer；Take out the insulating properties base material being formed with pre-conductive layer, remove solvent cures in pre-conductive layer and form conductive layer。
Said method provided by the present invention, by the mode of rotating centrifugal, the conductive material formation of deposits in ink layer is made to precipitate, conductive material deposition is made to come together on the surface of insulating properties base material, the bottom of ink layer, and then while making conductive material and binder layering, conductive material is combined with inorganic agent；Utilize binder can be dissolved in the characteristic of solvent, will be formed with the insulating properties base material of ink deposition layer and be impregnated in solvent, all or part of binder in ink deposition layer can be removed, reduce the impact of the electric conductivity of the binder conductive layer on being formed, and reduce the thickness of conductive layer, and then make to be more suitable for the thinning trend of electronic installation by its prepared conductive layer。
Operable inorganic agent preferably includes, but is not limited to vinyl trichlorosilane in the present invention, VTES, vinyl three (beta-methoxy ethyoxyl) silane, γ-glycidylpropyl-trimethoxy silane, γ-methacryloxypropyl-trimethoxy silane, N-(β-aminoethyl)-γ-aminopropyl-trimethoxy silane, N-(β-aminoethyl)-γ-aminopropyl-Methyl-trimethoxy silane, γ-chloropropyl-trimethoxy silane, the at least one of γ-mercapto propyl-trimethoxysilane and γ-aminopropyl-trimethoxy silane。Such as, the inorganic agent used is be KH550, KH560, KH-570 commercially available from being polymerized to the trade mark of million industry organosilicon materials company limiteies, or commercially available from DowCorning, the trade mark is one or more in the inorganic agent of Z6020 or Z6040。In use, by above-mentioned inorganic agent and alcohol by volume than coating after mixing for 1:100 (such as spraying) on insulating properties substrate surface。
By adopting said method provided by the present invention, utilize binder can be dissolved in the characteristic of solvent, will be formed with the insulating properties base material of ink deposition layer and be impregnated in solvent, it is possible to remove all or part of binder in ink deposition layer。Wherein, it is impregnated in the process of solvent at the insulating properties base material that will be formed with ink deposition layer, as long as having binder to be dissolved in solvent just can play the impact of electric conductivity reducing the binder conductive layer on being formed and the effect of the thickness of reduction conductive layer。As a preferred embodiment of the present invention, so that the conductive layer prepared by the present invention is more suitable for the thinning trend of electronic installation, preferably remove the binder (when wherein binder 100% is removed, conductive material with inorganic agent combined fixed) of 30-100% in ink deposition layer in the present invention。In order to realize this effect of optimization, invention further provides following preferred version。
In the method for above-mentioned formation conductive layer, each component in ink composite is dissolved in solvent, is mixed to form in the step of ink mixture, as long as each component in ink composite is mixed to form solution morphology。But, guaranteeing that metallic compound can be homogeneously dispersed in binder and under the premise uniformly forming rete of insulating properties base material, from the angle reducing solvent load, in the preferred embodiment of the present invention, 0.4-2 times that makes consumption be the above-mentioned ink composite weight of the present invention of solvent。
In the method for above-mentioned formation conductive layer, ink mixture being coated in insulating properties substrate surface, is formed in the step of ink layer, the mode of coating includes but not limited to the modes such as brushing and spraying, in the preferred embodiment of the present invention, print process is adopted to form above-mentioned ink layer。
In the preferred embodiment of the present invention, in said method, the insulating properties base material being formed with ink layer being rotated centrifugal step, the rotating speed of rotating centrifugal is 10000-25000r/min, and the time is 10-20min。In said method of the present invention, rotating centrifugal rotating speed is not limited to, in above-mentioned scope, be limited in above-mentioned scope, is conducive to, while ensureing ink layer integrity, being deposited to by conductive material on insulating properties substrate surface。
In the preferred embodiment of the present invention, said method will be formed with the step that the insulating properties base material of ink deposition layer is impregnated in solvent, and dipping temperature is 0 DEG C-90 DEG C, and dip time is 5-30min。Dipping temperature and dip time are not limited to above-mentioned scope in the present invention, if can dissolution to remove part binder。Preferred dipping temperature is 20 DEG C-70 DEG C, and dip time is 10-20min。
In the preferred embodiment of the present invention, in said method in the step of desolvation, the insulating properties base material being formed with pre-conductive layer is rotated centrifugal, dry drying and processing and be formed with the insulating properties base material of pre-conductive layer。The step of desolvation is not limited to above-mentioned rotating centrifugal and drying and processing in the present invention, in the present invention by adopting rotating centrifugal and drying to be jointly processed by, be conducive to while fast eliminating solvent on the one hand so that pre-conductive material is better fixed on insulating properties substrate surface。On the other hand, by first rotating centrifugal, then the step dried also reduces the impact dried the pre-conductive layer formed of heating。Preferably, the rotating speed of rotating centrifugal is 500-1500r/min, and the time is 30-60min。The temperature dried is 50-80 DEG C, and the time is 10-60min。
In the preferred embodiment of the present invention, said method also includes before the step forming ink layer: clean the step of insulating properties substrate surface。By adopting the step cleaned to be conducive to the adhesion between enhancement process agent and insulating properties base material。
In the preferred embodiment of the present invention, in said method, also include after the step forming conductive layer: the surface printing at conductive layer protects ink, and dries the step of protection ink。Conductive layer can be protected by the ink of printing protection in the present invention, to avoid conductive layer directly to contact with external environment, advantageously reduces the pollution to conductive layer, extends the service life of conductive layer。Operable protection ink preferably includes, but is not limited to commercially available from the trade mark of NSK company be INQ-000 or MIB-001 model gloss oil in the present invention, or the trade mark commercially available from company of kingdom is at least one in MIB-001 or INQ-000 model gloss oil。
Formed in the step of ink mixture at said method of the present invention, by component mix homogeneously each in above-mentioned for present invention ink composite。In the preferred embodiment of the present invention, the step of above-mentioned formation ink mixture includes: first binder and solvent are mixed, and after soaking 1-5h, stirs 10-60min, obtains mixture A；Optional wetting agent is added to mixture A, stirs 5-30min, obtain mixture B；Conductive material and other optional auxiliary agents are joined in mixture B, stirs 10-40min, obtain required ink mixture。
On identical surfaces of polymeric articles, adopt the above-mentioned ink composite of the present invention and the thickness of conductive layer that said method of the present invention is formed, hence it is evident that lower than the thickness adopting existing ink composite and the conductive layer prepared by existing method。Adopt the above-mentioned ink composite of the present invention, and the thickness of conductive layer that said method of the present invention is formed lower than 7 μm, can reach the scope of 3-7 μm。
In the preferred embodiment of the present invention, said method does not have special requirement for the consumption of raw material each in ink composite。As one preferred embodiment, above-mentioned ink composite contains by weight: the conductive material of 16-30 part and the binder of 15-40 part。The proportioning of above-mentioned each raw material being limited to this scope inherence improve on the basis of ink viscosity, what be conducive to all or part of binder in follow-up making conductive layer process is dissolved in removal of solvents。
Preferably, said method does not have special requirement for binder in ink composite, as long as this binder can be dissolved in solvent。Solvent pointed herein includes but not limited to water, C1-C12Alcohol, C3-C12Ketone, C6-C12Aromatic hydrocarbons, C1-C12Halogenated alkane and C2-C12Alkenyl halide in one or more。Specifically, above-mentioned solvent can be water, methanol, ethanol, normal propyl alcohol, isopropanol, n-butyl alcohol, the tert-butyl alcohol, n-amyl alcohol, hexanol, n-heptanol, n-octyl alcohol, acetone, the positive pentanone of 2-, the positive butanone of 2-, 3-methyl-2 pentanone, 2,3-diacetyl, 2,3-pentanedione, 2,5-acetyl butyryl, 1, one or more in hydroresorcinol, toluene, dimethylbenzene and trichloro ethylene。
Preferably, in the above-mentioned ink composite of the present invention, it is possible to use binder include but not limited in chitosan, polyvinyl alcohol (preferred Weight-average molecular is 120000-220000), fructose, thermoplastic acrylic resin, thermoplastic polyurethane one or more。More preferably, in order to avoid operator and the healthy of user are worked the mischief by solvent volatilization, and to environment, in the preferred embodiment of the present invention, preferred solvent is water, preferably employ the binder being dissolved in water, one or more in chitosan, what fructose of polyvinyl alcohol。
Wherein, operable chitosan, polyvinyl alcohol, fructose, thermoplastic acrylic resin and thermoplastic polyurethane select conventional commercial product, such as commercially available from the chitosan that He Te is international, such as commercially available from the fructose of the capable biological Engineering Co., Ltd of dimension, such as it is purchased the polyvinyl alcohol that the trade mark is PVA-1788 or PVA-2488 of Anhui Wanwei New High-tech Materials Co., Ltd, or it is the polyvinyl alcohol of BP-05, BP-17 or BP-24 commercially available from Changchun, the Taiwan trade mark, or is PVA-217, PVA-224 or PVA-205 polyvinyl alcohol commercially available from the Kuraray trade mark。Such as commercially available from plastic propene's acid esters that the trade mark of Mitsubishi is BR-116, BR113, MB2660, MB2952 or DSMB-731, or it is full of, commercially available from three, plastic propene's acid esters that the trade mark is AC1250A。It is such as the thermoplastic polyurethane of AH-0201D commercially available from Anhui Anda-Huatai New Material Co., Ltd.'s trade mark, or commercially available from the thermoplastic polyurethane that the Yantai ten thousand China trade mark is 6320 or 6520, or it is the thermoplastic polyurethane of TPU5715, TPU58213, TPU5702, TPU5703 or TPU5778 commercially available from the Lu Borun trade mark。
Preferably, said method does not have particular/special requirement for conductive material in ink composite。In the preferred embodiment of the present invention, above-mentioned conductive material is the conductive material of energy formation of deposits precipitation under centrifugal action。Adopt this conductive material of energy formation of deposits precipitation under centrifugal action, be conducive to adopting ink composite to be formed in the process of conductive layer, by the ink layer that centrifugal treating is formed by ink composite, conductive material deposition is come together in the bottom of ink layer, on the surface of product to be coated, and then make conductive material and binder layering, consequently facilitating follow-up solvent impregnated process is removed the process of all or part of binder, to form more densely cross-linked conductive layer surface。Preferably, above-mentioned conductive material is at least one in metal material, composite conducting material, carbon or graphite material。
As above-mentioned conductive material, it is possible to use metal material preferably include, but is not limited to as any one in gold, palladium, platinum, silver, copper, nickel, magnesium, aluminum, manganese, cobalt, zinc, ferrum, titanium, tungsten, stannum and molybdenum or multiple；The form of preferred above-mentioned metal material be in metallic particles, metal dust, sheet metal or metallic fiber any one or multiple；The particle diameter of preferred above-mentioned metallic particles is 1-1000nm, and the length of metallic fiber is 5-2000nm, diameter 1-1000nm, and the draw ratio of metallic fiber is 2-2000:1。
As above-mentioned conductive material, it is possible to use composite conducting material be complex conductive particle or composite conducting fiber；Above-mentioned composite conducting material preferably includes, but is not limited to as having at least one in the thermometal-powder of nucleocapsid structure, bimetal leaf, bimetallic fiber, metallized glass ball, metallized glass fiber, plating ceramic powders, plating ceramic fibre, metal coated carbon fiber, plating conductive black, plating graphite micro nano structure, the oxide powder of plating and the oxide fibre of plating。
As above-mentioned conductive material, it is possible to use carbon or graphite material be carbon or graphite micro-nano granules or carbon or graphite micro nanometer fiber。The particle diameter of preferred carbon or graphite micro-nano granules is 1-10000nm；Preferred carbon or graphite material are at least one in nano-graphite ball, Graphene, nano graphite flakes, carbon fiber, CNT and conductive black。
In the preferred embodiment of the present invention, said method is according to its concrete application scenario present invention, and ink composite can also contain the various auxiliary agents that ink area is conventional, the specific performance of ink composite to give the present invention or function。Preferably, it is possible to the auxiliary agent of employing preferably includes, but is not limited at least one in dispersant, wetting agent, defoamer, levelling agent and viscosity modifier。The consumption of the auxiliary agent used can be the conventional selection of this area。Preferably, the above-mentioned ink composite of the present invention contains the auxiliary agent of 0.1-10 part by weight。
Said method uses dispersant be mainly used for shortening the time being dispersed in binder and solvent by conductive material, and improve conductive material dispersion stabilization in binder and solvent。Operable dispersant is the various materials being capable of above-mentioned functions commonly used in the art。Such as, the dispersant used can be organic dispersing agent commonly used in the art, for instance: aliphatic amine system dispersant, hydramine system dispersant, ring-type unsaturated amine system dispersant, fatty acid series dispersant, aliphatic amide system dispersant, ester system dispersant, paraffin series dispersant, phosphate ester system dispersant, polymer-based dispersing agents (such as: polyacrylate system dispersant and Polyester dispersant) and organic phosphine system dispersant etc.。
Preferably, the dispersant used in said method can be the various dispersants that can be commercially available commonly used in the art。Specifically, the dispersant used can be one or more in following dispersant: the trade mark commercially available from BYK company of Germany is ANTI-TERRA-U, ANTI-TERRA-U80, ANTI-TERRA-U100, DISPERBYK-101, DISPERBYK-130, BYK-220S, LACTIMON, LACTIMON-WS, BYK-W966, DISPERBYK, BYK-154, BYK-9076, DISPERBYK-108, DISPERBYK-109, DISPERBYK-110, DISPERBYK-102, DISPERBYK-111, DISPERBYK-180, DISPERBYK-106, DISPERBYK-187, DISPERBYK-181, DISPERBYK-140, DISPERBYK-142, DISPERBYK-145, DISPERBYK-115, DISPERBYK-160, DISPERBYK-161, DISPERBYK-162, DISPERBYK-163, DISPERBYK-164, DISPERBYK-165, DISPERBYK-166, DISPERBYK-167, DISPERBYK-182, DISPERBYK-183, DISPERBYK-184, DISPERBYK-185, DISPERBYK-168, DISPERBYK-169, DISPERBYK-170, DISPERBYK-171, DISPERBYK-174, DISPERBYK-190, DISPERBYK-2150, BYK-9077, DISPERBYK-112, DISPERBYK-116, DISPERBYK-191, DISPERBYK-192, DISPERBYK-2000, DISPERBYK-2001, DISPERBYK-2010, DISPERBYK-2020, DISPERBYK-2025, the dispersant of DISPERBYK-2050 and DISPERBYK-2070；The dispersant that the trade mark is PHOSPHOLANPS-236 commercially available from AkzoNobel company of Holland；The dispersant that the trade mark is PS-21A commercially available from Witco chemical company of the U.S.；HypermerKD Series Dispersant and ZephrymPD Series Dispersant commercially available from Croda company of Britain；The dispersant that the trade mark is Dispers-655, Dispers-670, Dispers-163 commercially available from TEGO company。
Preferably, the consumption of the dispersant used in said method can be the conventional amount used of this area。Such as, in ink composite, the dispersant of 0-10 part is contained by weight, it is preferable that containing the dispersant of 1.5-7 part。
Using wetting agent to be mainly used for making solid material be more easy to by solvent-soaked in said method, it is by reducing its surface tension or interfacial tension, makes solvent can be deployed on solid material surface, or penetrates its surface, and solid material moistening。Operable wetting agent is the various materials being capable of above-mentioned functions commonly used in the art。The materials such as such as sulfonated oil, soap, soybean lecithin, thio-alcohol, hydrazides class and mercaptan acetals。In the above-mentioned ink composite of the present invention, the wetting agent used can be the various wetting agent that can be commercially available commonly used in the art。Specifically, the wetting agent used can be one or more in following wetting agent: is available commercially from the TEGOWet250 of TEGO company, TEGOWet265, TEGOWet270, TEGOWet280, TEGOWet500, TEGOWet505, TEGOWet510, TEGOWet520, TEGOWetKL245, or it is available commercially from the DISPERBYK-180DISPERBYK-182 of BYK company, DISPERBYK-184, DISPERBYK-190, DISPERBYK-192, DISPERBYK-194, DISPERBYK, DISPERBYK-102, LACTIMON-WS, DISPERBYK-181 or DISPERBYK-187。
Preferably, the wetting agent used in said method can be the various wetting agent that can be commercially available commonly used in the art。Specifically, the wetting agent used can be one or more in following wetting agent: commercially available from one or more in the wetting agent that the trade mark is Wet-250, Wet-260, Wet-270 of TEGO company of Germany。
Preferably, the consumption of the wetting agent used in said method can be the conventional amount used of this area。Such as, in ink composite, the wetting agent of 0-3 part is contained by weight, it is preferable that containing the wetting agent of 0.1-2.5 part。
Said method use defoamer be mainly used for suppressing formation of foam, destroying the foam formed or the material deviate from from system by the foam of formation。Operable defoamer is the various materials being capable of above-mentioned functions commonly used in the art。Such as, the defoamer used can be organopolysiloxane system defoamer, polyethers system defoamer and higher alcohol system defoamer。Preferably, the defoamer used is organopolysiloxane system defoamer。
The defoamer that said method uses can be the various defoamer that can be commercially available commonly used in the art。Specifically, the defoamer used can be one or more in the defoamer that the trade mark is BYK-020, BYK-080A, BYK-021, BYK-022, BYK-023, BYK-024, BYK-025, BYK-028, BYK-045 and BYK-094, BYK-1650, BYK-1660, BYK-044, BYK-1610, BYK-1615, BYK-1770, BYK-012, BYK-016, BYK-011 commercially available from BYK company of Germany。
Preferably, the consumption of the defoamer used in said method can be the conventional amount used of this area。Such as, in ink composite, contain the defoamer of 0-0.3 part in parts by weight。
The levelling agent that said method uses is mainly used in promoting ink to form more smooth, a smooth and uniform rete in drying and forming-film process。The kind of the present invention levelling agent for using is not particularly limited, and it can for the commonly used in the art material being capable of above-mentioned functions。Such as, the levelling agent used can be one or more in polyacrylate system levelling agent, polydimethylsiloxane system levelling agent, PSI system levelling agent and fluorine-containing surfactant。
The levelling agent that said method uses can be the various levelling agents that can be commercially available commonly used in the art。Such as, described levelling agent can be one or more in the levelling agent that the trade mark is BYK-333, BYK-306, BYK-358N, BYK-310, BYK-354 and BYK-356 commercially available from BYK company of Germany。
Preferably, the consumption of the levelling agent used in said method can be the conventional amount used of this area。Such as, in ink composite, contain the levelling agent of 0-4 part by weight。
The viscous regulator that said method uses is for regulating the viscosity of ink composite。The kind of the present invention viscous regulator for using is not particularly limited, it is possible to for the conventional selection of this area。Such as, the viscous regulator used can be one or more in aerosil, polyamide wax, organobentonite, castor oil hydrogenated, metallic soap, hydroxy alkyl cellulose and derivant, polyvinyl alcohol and polyacrylate。
Preferably, in said method, the consumption of viscous regulator can be the conventional amount used of this area。Such as, in ink composite, contain the viscous regulator of 0-3 part by weight。
Below by specific embodiment, exemplarily the present invention is described in further detail。
One, the raw material adopted in following each embodiment and producer。
The raw material adopted in each embodiment of table 1. and producer
Two, the device adopted in following each embodiment and producer thereof。
In the step of printing-ink, adopting 300 orders, thickness is the screen printing plate of 30 μm, buys from Hua En printing apparatus Science and Technology Ltd.；
In the step of rotating centrifugal, adopt horizontal sediment separator, buy from Shanghai chemical machinery Co., Ltd., Factory。
Three, specific embodiment
Embodiment 1
The composition of ink composite: chitosan 38g, argentum powder 30g, Wet-2500.5g, Dispers-6551.5g。
Ink application compositions forms the method for conductive layer:
(1) by the mixing of ink composite Yu solvent: add chitosan in 30g water, stir 30min under the speed of 1000r/min with dispersion machine after soaking two hours；Add Wet-250, under the speed of 1000r/min, stir 10min with dispersion machine；Adding nanometer silver powder and Dispers-655, dispersion machine stirs 20min under the speed of 200r/min, obtains ink mixture；
(2). cleaning insulating properties substrate surface, insulating properties substrate surface after cleaning sprays inorganic agent (KH550 and alcohol by volume than for 1:100 mixture)；
(3). adopt aforementioned screen printing plate that ink mixture is coated in insulating properties substrate surface, form ink layer；
(4). after ink layer surface drying, the insulating properties base material being formed with ink layer is rotated centrifugal (rotating speed 12000r/min, time 20min), make conductive material deposition in ink layer, form ink deposition layer；
(5). will be formed with being impregnated in water 15min under the insulating properties base material room temperature of ink deposition layer, remove part binder in ink deposition layer, form pre-conductive layer；
(6). the insulating properties base material being formed with pre-conductive layer is rotated centrifugal (rotating speed 1000r/min, time 45min), drying dehydration post-drying (70 DEG C, 30min) processes the insulating properties base material being formed with pre-conductive layer, makes pre-conductive layer solidify to form conductive layer；
(7). the surface printing at conductive layer protects ink, and dries protection ink。
Embodiment 2
The composition of ink composite: fructose 15g, argentum powder 16g, Wet-2601g, Dispers-6703g。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(1) by the mixing of ink composite Yu solvent: add chitosan in 65g water, stir 60min under the speed of 1000r/min with dispersion machine after soaking one hour；Add Wet-260, under the speed of 1000r/min, stir 30min with dispersion machine；Adding nanometer silver powder and Dispers-670, dispersion machine stirs 40min under the speed of 200r/min, obtains electrically conductive ink；
(4). when ink layer is half-dried, the insulating properties base material being formed with ink layer is rotated centrifugal (rotating speed 18000r/min, time 15min), make conductive material deposition in ink layer, form ink deposition layer；
(5). will be formed with the insulating properties base material of ink deposition layer and be impregnated into 30min in the water of 20 DEG C, remove part binder in ink deposition layer, form pre-conductive layer；
(6). the insulating properties base material being formed with pre-conductive layer is rotated centrifugal (rotating speed 800r/min, 60min), drying dehydration post-drying (60 DEG C, 40min) processes the insulating properties base material being formed with pre-conductive layer, makes pre-conductive layer solidify to form conductive layer。
Embodiment 3
The composition of ink composite: polyvinyl alcohol 25g, argentum powder 20g, Wet-2700.1g, DISPERBYK-1631.8g。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(1) by the mixing of ink composite Yu 53.1g water；(4). when ink layer is half-dried, the insulating properties base material being formed with ink layer is rotated centrifugal (rotating speed 23000r/min, time 10min), make conductive material deposition in ink layer, form ink deposition layer；
(5). will be formed with the insulating properties base material of ink deposition layer and be impregnated into 5min in the water of 90 DEG C, remove part binder in ink deposition layer, form conductive layer；
(6). the insulating properties base material being formed with pre-conductive layer is rotated centrifugal (rotating speed 1500r/min, 30min), drying dehydration post-drying (80 DEG C, 15min) processes the insulating properties base material being formed with pre-conductive layer, makes pre-conductive layer solidify to form conductive layer。
Embodiment 4
The composition of ink composite: with embodiment 1。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(6). the insulating properties base material being formed with pre-conductive layer is rotated centrifugal (rotating speed 1600r/min, 25min), drying dehydration post-drying (100 DEG C, 60min) processes the insulating properties base material being formed with pre-conductive layer, makes pre-conductive layer solidify to form conductive layer。
Embodiment 5
The composition of ink composite: with embodiment 1。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(5). will be formed with the insulating properties base material of ink deposition layer and be impregnated into 60min in the water of 0 DEG C, remove part binder in ink deposition layer, form conductive layer。
Embodiment 6
The composition of ink composite: thermoplastic acrylic 38g, argentum powder 30g, Wet-2500.5g, Dispers-6551.5g。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(1) by the mixing of ink composite Yu solvent: first take 5 grams of n-butyl alcohol preparation mixed solvents of 25g butyl acetate, and stir 10min under the speed of 300r/min with dispersion machine；Then add thermoplastic propene's acid esters wherein, after soaking two hours, under the speed of 1000r/min, stir 30min with dispersion machine；Add Wet-250, under the speed of 1000r/min, stir 10min with dispersion machine；Adding nanometer silver powder and Dispers-655, dispersion machine stirs 20min under the speed of 200r/min, obtains ink mixture；
Embodiment 7
The composition of ink composite: thermoplastic polyurethane 20g, argentum powder 40g, Wet-2500.5g, Dispers-6551.5g。
Ink application compositions forms the method for conductive layer: with reference to embodiment 6, the difference is that:
(1) by the mixing of ink composite Yu 51g solvent, wherein solvent is butyl acetate: n-butyl alcohol is the mixed solvent of 5:1；
Embodiment 8
The composition of ink composite: chitosan 25g, argentum powder 22g。
Ink application compositions forms the method for conductive layer: with reference to embodiment 1, the difference is that:
(1) by the mixing of ink composite Yu 55g solvent。
Comparative example 1
The composition of ink composite: acrylic resin 38g, argentum powder 30g, Wet-2500.5g, Dispers-6551.5g。
Ink application compositions forms the method for conductive layer:
(1) by the mixing of ink composite Yu solvent: add chitosan in 30g water, stir 30min under the speed of 1000r/min with dispersion machine after soaking two hours；Add Wet-250, under the speed of 1000r/min, stir 10min with dispersion machine；Adding nanometer silver powder and Dispers-655, dispersion machine stirs 20min under the speed of 200r/min, obtains ink mixture；
(2). cleaning insulating properties substrate surface, insulating properties substrate surface after cleaning sprays inorganic agent (KH550 and alcohol by volume are than the mixture for 1:100)；
(3). adopt aforementioned screen printing plate that ink mixture is coated in insulating properties substrate surface, form ink layer；
(4) under .70 DEG C of temperature conditions, solidify the ink layer 15min of insulating properties substrate surface, form cured layer, obtain conductive layer。
Four, test
Conductive layer prepared by example 1 to 8 performed as described above and comparative example 1 is tested。
4.1 method of testings:
The measuring method of ink layer state (surface drying, half-dried, absolutely dry): surface drying: put a rayon balls on coating surface gently, with mouth from cotton balls 10-15 centimetre, featheriness cotton balls in the horizontal direction, if blowing away, face does not leave staple；Half-dried: mobile phone touches coating surface, and applies pressure, and coating surface is without fingerprint；Absolutely dry: to cut on model with blade and scrape paint film or putty membrane, and observe in its bottom and film all without adherent phenomenon。
The measuring method of cured layer thickness and conductive layer thickness: method of section, adopts diamond cutter to be blocked together with thickness by ground, then section is placed in microscopy and measures thickness。
The measuring method of conductive layer degree of compaction: first testing conductive layer porosity, then according to " degree of compaction+porosity=1, is converted into degree of compaction。Porosity adopts porosity test instrunment (purchased from scientific and technological (Beijing) company limited of Bei Shide instrument)。
The measuring method of conduction sheet resistance: adopt sheet resistance tester (four-point probe device: purchased from Guangzhou Kunder Science & Technology Co., Ltd.'s KDY-1 type four probe resistance rate/sheet resistance tester), test instrunment middle probe adopts carbon tungsten tipped probe, the spacing of four end of probes is equal, and four probes are connected on sheet resistance tester by four lead-in wires。Test condition is: temperature: 23 DEG C；Relative humidity: 65% without stronger electric jamming, and isolated from power filters, without intense direct illumination。
4.2 test results。
Test result: as shown in table 2, wherein:
" thickness of ink layer " refers to the thickness by the formed film of printing-ink mixture, its thickness depends on the screen printing plate used, and what above-described embodiment and contrast all adopted for example is 300 orders, and thickness is the screen printing plate of 30 μm, therefore the thickness of ink layer is identical, is 30 μm。
The thickness of the film (conductive layer) that " thickness of conductive layer " refers to ink layer rotated centrifugal (making conductive material deposit), impregnates (removing all or part of binder), cured is formed。
Table 2.
From data in table 2: compared with comparative example 1, the conductive layer that the embodiment of the present invention 1 to 8 is formed all can remove more than 30% binder, and this thickness allowing for conductive layer is lower, and conduction sheet resistance is lower。As can be seen here, the present invention by adding the binder being dissolved in solvent in ink composite, increasing on the basis of viscosity of ink composite, utilize binder can be dissolved in the feature of solvent, the rotated centrifugal ink deposition layer obtained of impregnation process, to remove all or part of binder contained in ink deposition layer, so just can reduce the impact of the electric conductivity of the binder conductive layer on being formed, reduce the thickness of conductive layer, and then make to be more suitable for by its prepared conductive layer the thinning trend of electronic installation。
The preferred embodiment of the present invention described in detail above; but, the present invention is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention; technical scheme can being carried out multiple simple variant, these simple variant belong to protection scope of the present invention。
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, it is possible to be combined by any suitable mode, in order to avoid unnecessary repetition, various possible compound modes are no longer illustrated by the present invention separately。
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally。
Claims (10)
1. the method that an ink application compositions forms conductive layer, it is characterised in that described ink composite contains at least one conductive material and at least one binder, and described ink application compositions forms the method for conductive layer and comprises the following steps:
Each component in described ink composite is mixed with solvent, forms ink mixture；
In insulating properties substrate surface coating processing agent, formation processes oxidant layer；
Described ink mixture is coated in described process oxidant layer, forms ink layer；
After described ink layer surface drying, the insulating properties base material being formed with described ink layer is rotated centrifugal, make the conductive material in described ink layer deposit, form ink deposition layer；
Will be formed with the insulating properties base material of described ink deposition layer and be impregnated in solvent, remove all or part of binder in described ink deposition layer, form described pre-conductive layer；
Taking out the insulating properties base material being formed with described pre-conductive layer, desolvation makes described pre-conductive layer solidify to form described conductive layer。
2. method according to claim 1, wherein, the described insulating properties base material to being formed with ink layer rotates centrifugal step, and the rotating speed of rotating centrifugal is 10000-25000r/min, time 10-20min。
3. method according to claim 1, wherein, described in will be formed with the insulating properties base material step that is impregnated in solvent of ink deposition layer, dipping temperature is 0 DEG C-90 DEG C, and dip time is 5-30min。
4. method according to claim 1, wherein, in the step of described desolvation, rotates centrifuge dripping to the insulating properties base material being formed with described pre-conductive layer, dries the insulating properties base material being formed with described pre-conductive layer described in post-drying process。
5. method according to claim 4, wherein, in the step of described desolvation, the rotating speed of rotating centrifugal is 500-1500r/min, and the time is 30-60min, and the temperature of described drying and processing is 50-80 DEG C, and the time is 10-60min。
6. method according to claim 1, wherein,
Also include before the step forming described process oxidant layer: clean the step of described insulating properties substrate surface；
Also include after the step forming described conductive layer: the surface printing at described conductive layer protects ink, and dries the step of described protection ink。
7. method according to any one of claim 1 to 6, wherein, described ink composite contains by weight: the described conductive material of 16-30 part and the described binder of 15-40 part。
8. method according to any one of claim 1 to 6, wherein, described binder is one or more in chitosan, polyvinyl alcohol, fructose, thermoplastic acrylic resin and thermoplastic polyurethane。
9. method according to any one of claim 1 to 6, wherein, described conductive material is the conductive material of energy formation of deposits precipitation under centrifugal action, it is preferable that described conductive material is at least one in metal material, composite conducting material, carbon or graphite material, more preferably
Described metal material be in gold, palladium, platinum, silver, copper, nickel, magnesium, aluminum, manganese, cobalt, zinc, ferrum, titanium, tungsten, stannum and molybdenum any one or multiple；The form of preferred described metal material be in metallic particles, metal dust, sheet metal or metallic fiber any one or multiple；The particle diameter of preferred described metallic particles is 1-1000nm, and the length of described metallic fiber is 5-2000nm, diameter 1-1000nm, and the draw ratio of described metallic fiber is 2-2000:1；
Described composite conducting material is complex conductive particle or composite conducting fiber；Preferred described composite conducting material is have at least one in the thermometal-powder of nucleocapsid structure, bimetal leaf, bimetallic fiber, metallized glass ball, metallized glass fiber, plating ceramic powders, plating ceramic fibre, metal coated carbon fiber, plating conductive black, plating graphite micro nano structure, the oxide powder of plating and the oxide fibre of plating；
Described carbon or graphite material are carbon or graphite micro-nano granules or carbon or graphite micro nanometer fiber, and the particle diameter of described carbon or graphite micro-nano granules is 1-10000nm；Preferred described carbon or graphite material are at least one in nano-graphite ball, Graphene, nano graphite flakes, carbon fiber, CNT and conductive black。
10. method according to any one of claim 1 to 6, wherein, described ink composite is by weight possibly together with the auxiliary agent of 0.1-10 part, and described auxiliary agent is at least one in dispersant, wetting agent, defoamer, levelling agent and viscosity modifier。
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| CN111839903A (en) * | 2019-04-24 | 2020-10-30 | 沃黛普物联网科技(上海)有限公司 | Intelligent sanitary nursing product and preparation method thereof |
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