CN105722254A - Photo-curable resistance paste for flexible electrothermal film and preparation method of photo-curable resistance paste - Google Patents

Photo-curable resistance paste for flexible electrothermal film and preparation method of photo-curable resistance paste Download PDF

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Publication number
CN105722254A
CN105722254A CN201610099552.1A CN201610099552A CN105722254A CN 105722254 A CN105722254 A CN 105722254A CN 201610099552 A CN201610099552 A CN 201610099552A CN 105722254 A CN105722254 A CN 105722254A
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Prior art keywords
light
powder
silver powder
solid phase
resistance slurry
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CN201610099552.1A
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Chinese (zh)
Inventor
苏冠贤
蒋国辉
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Dongguan Corehelm Electronic Material Technology Co Ltd
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Dongguan Corehelm Electronic Material Technology Co Ltd
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Priority to CN201610099552.1A priority Critical patent/CN105722254A/en
Publication of CN105722254A publication Critical patent/CN105722254A/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material

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  • Conductive Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses photo-curable resistance paste for a flexible electrothermal film and a preparation method of the photo-curable resistance paste. The resistance paste comprises the following constituents by weight: 40-80% of solid phase and 20-60% of organic binding agent, wherein the solid phase comprises 80-100% of silver powder and 0-20% of oxide by weight, the silver powder comprises 30-90% of sheet-shaped silver powder and 10-70% of linear silver powder by weight, the organic binding agent comprises 65-90% of photo-curable resin, 5-30% of photo active monomer, 0.5-5% of photo initiator, 0.1-1% of defoaming agent and 0.5-2% of dispersing agent by weight. By the resistance paste, photo-curable formation can be adopted, the resistance adjustment range can be expanded, and the effect of building a conductive path in the sheet-shaped silver powder by the linear silver powder can be fully utilized. The preparation method comprises the three steps of solid phase preparation, organic binding agent preparation and resistance paste preparation, and can be used for effectively producing the photo-curable resistance paste for the flexible electrothermal film.

Description

A kind of flexible electrothermal membrane light-cured type resistance slurry and preparation method thereof
Technical field
The present invention relates to technical field of electronic materials, particularly relate to a kind of flexible electrothermal membrane light-cured type resistance slurry and Its preparation method.
Background technology
Flexible electrothermal membrane belongs to a kind of low-temperature heating new material in heated by electrothermal film technology, and its likeness in form paper tape and softness are light Thin, there is higher hot strength, folding resistance good (10,000 times), and in planar heating, the thermal efficiency is high, applied voltage wide ranges (2.4-380 volt), watt level can set on demand, any cutting forming, and the energy conversion being easily achieved under low-voltage. Based on These characteristics, flexible electrothermal membrane has a wide range of applications at domestic and industrial aspect;For domestic aspect, flexible electrical Hotting mask is usually used in safety electric heating wearing article, electric heating articles for use, direct-heating bathing device, electric kettle etc.;For industrial aspect For, flexible electrothermal membrane is usually used in information terminal large screen display, cockpit light guide plate, de-electrifying lamp for automatic copier, oil pipeline Heat preservation, electric heating, the antifreeze frost etc. of equipment;According to the range of application of flexible electrothermal membrane, flexible electrothermal membrane has higher Researching value.
Resistant heat generating layer is as one of flexible electrothermal membrane core component, and on the one hand electric energy is turned by it as energy conversion unit Chemical conversion heat energy, is on the other hand transferred to base material as energy transport vehicle by heat energy, in order to realize the uniform biography of planar heat producing body Heat;Therefore, resistant heat generating layer plays extremely important effect to the performance of flexible electrothermal membrane combination property.
Need to be explained further, noble metal and rare earth element have good electric heating and convert and capacity of heat transmission, generally with electricity Sub-slurry form and be applied in Electric radiant Heating Film, such as Patent No.: 201010158934.X, entitled: based on stainless steel substrate The Chinese invention patent of YBCO thick-film resistor paste and preparation method thereof and Patent No. 200610036715.8, title For: rare earth thick film circuit rare earth base metal resistor slurry based on metal basal board and the Chinese invention patent of preparation technology thereof, Resistance slurry disclosed in above-mentioned two Chinese invention patent is all that metal powder is prepared as electric slurry, then passes through screen printing System and high temperature sintering form resistant heat generating layer, and sintering temperature is generally more than 500 DEG C, but the highest bearing temperature of flexible parent metal About 400 DEG C, this to a certain degree on limit sintering process application on flexible parent metal;Therefore, seeking gentle curing process is The Basic Ways that in flexible electrothermal membrane prepared by resistant heat generating layer.
It should further be noted that Application No.: 201510183663.6, entitled: the manufacture method of a kind of flexible electrothermal membrane Chinese invention patent, it discloses resistant heat generating layer preparation relate to magnetron sputtering plating, pad pasting, expose, the process such as etching, have Effect avoid high-sintering process, during additionally use ferrum nickel manganese evanohm replace noble metal, this reduces to a certain extent Material cost, but also bring some new problems: 1, ferrum nickel manganese evanohm replacement noble metal reduces electrothermal layer stability and electricity Thermal transition ability;2, to prepare link more for electrothermal layer, adds somewhat to the complexity of technique;3, etching can produce in a large number Waste liquid, is unfavorable for environmental protection.Therefore seek that a kind of technique is simple, the development to flexible electrothermal membrane of the low-temperature setting technique of energy-conserving and environment-protective Significant.
Summary of the invention
Present invention aims to the deficiencies in the prior art and a kind of flexible electrothermal membrane light-cured type resistance is provided Slurry, this flexible electrothermal membrane light-cured type resistance slurry has the advantage that 1, can use ultraviolet curing process molding, molding Energy saving technology, environmental protection, low cost, process is simple and is prone to large-scale production;2, mixing argentum powder is used to mix the solid of oxide again Powder, as function phase, has effectively widened resistance adjustment scope, it is provided that more resistive arrangement selects;3, flake silver powder and wire Being used in mixed way of argentum powder, can make full use of wire argentum powder and set up the effect of conductive path between flake silver powder, it is achieved less argentum powder The possibility of more conductive path, same electric conductivity is provided to use less argentum powder, thus effectively reduce resistance slurry Cost of material.
Another object of the present invention is to provide the preparation method of a kind of flexible electrothermal membrane light-cured type resistance slurry, should Preparation method operatively production can prepare flexible electrothermal membrane light-cured type resistance slurry.
For reaching above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of flexible electrothermal membrane light-cured type resistance slurry, includes the material of following weight portion, particularly as follows:
Solid phase 40%-80%
Organic binder bond 20%-60%;
Wherein, solid phase includes the material of following weight portion, particularly as follows:
Argentum powder 80%-100%
Oxide 0%-20%;
Argentum powder is mixed by flake silver powder, wire argentum powder, and flake silver powder, the weight portion of two kinds of materials of wire argentum powder are followed successively by: 30%-90%、10%-70%;
Organic binder bond includes the material of following weight portion, particularly as follows:
Light-cured resin 65%-90%
Photoactive monomer 5%-30%
Light trigger 0.5%-5%
Defoamer 0.1%-1%
Dispersant 0.5%-2%.
Wherein, the median particle diameter of described argentum powder is 1 μm-2 μm.
Wherein, described oxide is SnO2、SiO2、TiO2、Al2O3In one or more mixture formed.
Wherein, the median particle diameter of described oxide is 1 μm-2 μm.
Wherein, described light-cured resin is o-cresol formaldehyde epoxy acrylic resin, bisphenol-A epoxy acrylic resin, polyamides One or more mixture formed in imine modified epoxy acrylic resin.
Wherein, described photoactive monomer is double pentaerythritol methacrylate, ethoxyquin trimethylolpropane tris acrylic acid One or more mixture formed in ester, trimethylolpropane trimethacrylate.
Wherein, described light trigger is 2-isopropyl thioxanthone, 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1- One or more mixture formed in acetone, 2,4,6-trimethylbenzoy-dipheny phosphine oxides.
Wherein, described defoamer is dimethicone.
Wherein, described dispersant is BYK-AT204.
The preparation method of a kind of flexible electrothermal membrane light-cured type resistance slurry, includes following processing step, particularly as follows:
Prepared by a, solid phase: flake silver powder uniformly mixes to prepare combined silver powder, the sheet in combined silver powder with wire argentum powder Shape argentum powder, the weight portion of wire argentum powder are followed successively by 30%-90%, 10%-70%, after prepared by argentum powder material to be mixed, toward combined silver Adding oxide in powder, combined silver powder, the weight portion of two kinds of materials of oxide are followed successively by 80%-100%, 0%-20%, mixing The mixture that argentum powder material and oxide are formed is ground, to obtain solid phase;
Prepared by b, organic binder bond: light-cured resin, photoactive monomer, light trigger, defoamer, dispersant are placed in container Mixing and stirring, to obtain organic binder bond, wherein, light-cured resin, photoactive monomer, light trigger, defoamer, dispersion The weight portion of five kinds of materials of agent is followed successively by 65%-90%, 5%-30%, 0.5%-5%, 0.1%-1%, 0.5%-2%;
Prepared by c, resistance slurry: carry out three-roll rolling, solid phase, organic binder bond two after solid phase, organic binder bond mixing dispersion The weight portion planting material is followed successively by 40%-80%, 20%-60%, obtains resistance slurry after rolling.
The invention have the benefit that a kind of flexible electrothermal membrane light-cured type resistance slurry of the present invention, its bag Include the material of following weight portion: solid phase 40%-80%, organic binder bond 20%-60%;Wherein, solid phase includes following weight portion Material: argentum powder 80%-100%, oxide 0%-20%;Argentum powder is mixed by flake silver powder, wire argentum powder, flake silver powder, wire The weight portion of two kinds of materials of argentum powder is followed successively by: 30%-90%, 10%-70%;Organic binder bond includes the material of following weight portion: Light-cured resin 65%-90%, photoactive monomer 5%-30%, light trigger 0.5%-5%, defoamer 0.1%-1%, dispersant 0.5%- 2%.By above-mentioned material proportion, the flexible electrothermal membrane light-cured type resistance slurry of the present invention has the advantage that 1, can adopt Using ultraviolet curing process molding, moulding process energy-saving and environmental protection, low cost, process is simple and is prone to large-scale production;2, mixing is used Argentum powder is mixed the solid powder again of oxide and, as function phase, has effectively been widened resistance adjustment scope, it is provided that more resistive arrangement Select;3, being used in mixed way of flake silver powder and wire argentum powder, can making full use of wire argentum powder, to set up conduction between flake silver powder logical The effect on road, it is achieved less argentum powder provides the possibility of more conductive paths, same electric conductivity to use less argentum powder, thus Effectively reduce the cost of material of resistance slurry.
Another of the present invention has the beneficial effect that a kind of flexible electrothermal membrane light-cured type resistance slurry of the present invention Preparation method, it comprises the following steps that: prepared by a, solid phase: uniformly mix to prepare mixing with wire argentum powder by flake silver powder Argentum powder material, the flake silver powder in combined silver powder, the weight portion of wire argentum powder are followed successively by 30%-90%, 10%-70%, silver to be mixed After prepared by powder, in combined silver powder add oxide, combined silver powder, two kinds of materials of oxide weight portion successively For 80%-100%, 0%-20%, the mixture that combined silver powder and oxide are formed is ground, to obtain solid phase;B, organic Prepared by binding agent: by light-cured resin, photoactive monomer, light trigger, defoamer, that dispersant is placed in mix and blend in container is equal Even, to obtain organic binder bond, wherein, light-cured resin, photoactive monomer, light trigger, defoamer, five kinds of materials of dispersant Weight portion be followed successively by 65%-90%, 5%-30%, 0.5%-5%, 0.1%-1%, 0.5%-2%;Prepared by c, resistance slurry: by solid phase, have Machine binding agent mixing dispersion after carry out three-roll rolling, solid phase, the weight portion of two kinds of materials of organic binder bond be followed successively by 40%-80%, 20%-60%, obtains resistance slurry after rolling.This preparation method production can prepare flexible electrothermal membrane light-cured type electricity effectively Resistance paste.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described.
Embodiment one, a kind of flexible electrothermal membrane light-cured type resistance slurry, include the material of following weight, specifically For:
Solid phase 75g
Organic binder bond 25g;
Wherein, solid phase is mixed by argentum powder, oxide, wherein, containing flake silver powder 70g in 100g solid phase, and wire argentum powder 25g, stannum oxide 5g;
Organic binder bond is formed by light-cured resin, photoactive monomer, light trigger, defoamer, dispersant, wherein, Containing (light-cured resin) bisphenol-A epoxy acrylic resin 70g, (photoactive monomer) Bis(pentaerythritol) in 100g organic binder bond Six acrylate 25.5g, (light trigger) 2-isopropyl thioxanthone 3g, (defoamer) dimethicone 0.5g, (dispersant) BYK-AT204 1g。
For the flexible electrothermal membrane light-cured type resistance slurry of the present embodiment one, the present embodiment one can use following soft The preparation method of property Electric radiant Heating Film light-cured type resistance slurry is prepared, concrete:
A kind of preparation method of flexible electrothermal membrane light-cured type resistance slurry, it includes following processing step, particularly as follows:
Prepared by a, solid phase: flake silver powder uniformly mixes to prepare combined silver powder, the sheet in combined silver powder with wire argentum powder Shape argentum powder, the weight of wire argentum powder are followed successively by 70g, 25g, after prepared by argentum powder material to be mixed, add in combined silver powder Oxide, combined silver powder, the weight of two kinds of materials of oxide are followed successively by what 95g, 5g, combined silver powder and oxide were formed Mixture is ground, to obtain solid phase;
Prepared by b, organic binder bond: light-cured resin, photoactive monomer, light trigger, defoamer, dispersant are placed in container Mixing and stirring, to obtain organic binder bond, wherein, light-cured resin, photoactive monomer, light trigger, defoamer, dispersion The weight of five kinds of materials of agent is followed successively by 70g, 25.5g, 3g, 0.5g, 1g;
Prepared by c, resistance slurry: carry out three-roll rolling after 75g solid phase, the mixing dispersion of 25g organic binder bond, obtain electricity after rolling Resistance paste, the viscosity 120Pas-180 Pas of resistance slurry, fineness < 8 μm.
The flexible electrothermal membrane light-cured type resistance slurry prepared by above-mentioned formula and processing step is had the following advantages, Particularly as follows: 1, can use ultraviolet curing process molding, moulding process energy-saving and environmental protection, low cost, process is simple and is prone to scale Produce;2, the solid powder again using mixing argentum powder to mix oxide, as function phase, has effectively widened resistance adjustment scope, it is provided that More resistive arrangement selects;3, being used in mixed way of flake silver powder and wire argentum powder, can make full use of wire argentum powder at lamellar silver The effect of conductive path is set up, it is achieved less argentum powder provides the possibility of more conductive paths, same electric conductivity to use between powder Less argentum powder, thus effectively reduce the cost of material of resistance slurry.
Embodiment two, a kind of flexible electrothermal membrane light-cured type resistance slurry, include the material of following weight, particularly as follows:
Solid phase 65g
Organic binder bond 35g;
Wherein, solid phase is mixed by argentum powder, oxide, wherein, containing aluminium oxide 5g in 100g solid phase, and flake silver powder 80g, line Shape argentum powder 15g;
Organic binder bond is formed by light-cured resin, photoactive monomer, light trigger, defoamer, dispersant, wherein, Containing (light-cured resin) polyimide modified epoxy acrylic resin 80g, (photoactive monomer) ethoxy in 100g organic binder bond Change trimethylolpropane trimethacrylate 15.5g, (light trigger) 2-isopropyl thioxanthone 3g, (defoamer) dimethicone 0.5g, (dispersant) BYK-AT204 1g.
For the flexible electrothermal membrane light-cured type resistance slurry of the present embodiment two, the present embodiment two can use following soft The preparation method of property Electric radiant Heating Film light-cured type resistance slurry is prepared, concrete:
A kind of preparation method of flexible electrothermal membrane light-cured type resistance slurry, it includes following processing step, particularly as follows:
Prepared by a, solid phase: flake silver powder uniformly mixes to prepare combined silver powder, the sheet in combined silver powder with wire argentum powder Shape argentum powder, the weight of wire argentum powder are followed successively by 80g, 15g, after prepared by argentum powder material to be mixed, add in combined silver powder Oxide, combined silver powder, the weight of two kinds of materials of oxide are followed successively by what 95g, 5g, combined silver powder and oxide were formed Mixture is ground, to obtain solid phase;
Prepared by b, organic binder bond: light-cured resin, photoactive monomer, light trigger, defoamer, dispersant are placed in container Mixing and stirring, to obtain organic binder bond, wherein, light-cured resin, photoactive monomer, light trigger, defoamer, dispersion The weight of five kinds of materials of agent is followed successively by 80g, 15.5g, 3g, 0.5g, 1g;
Prepared by c, resistance slurry: carry out three-roll rolling after 65g solid phase, the mixing dispersion of 35g organic binder bond, obtain electricity after rolling Resistance paste, the viscosity 120Pas-180 Pas of resistance slurry, fineness < 8 μm.
The flexible electrothermal membrane light-cured type resistance slurry prepared by above-mentioned formula and processing step is had the following advantages, Particularly as follows: 1, can use ultraviolet curing process molding, moulding process energy-saving and environmental protection, low cost, process is simple and is prone to scale Produce;2, the solid powder again using mixing argentum powder to mix oxide, as function phase, has effectively widened resistance adjustment scope, it is provided that More resistive arrangement selects;3, being used in mixed way of flake silver powder and wire argentum powder, can make full use of wire argentum powder at lamellar silver The effect of conductive path is set up, it is achieved less argentum powder provides the possibility of more conductive paths, same electric conductivity to use between powder Less argentum powder, thus effectively reduce the cost of material of resistance slurry.
Above content is only presently preferred embodiments of the present invention, for those of ordinary skill in the art, according to the present invention's Thought, the most all will change, and this specification content should not be construed as the present invention Restriction.

Claims (8)

1. a flexible electrothermal membrane light-cured type resistance slurry, it is characterised in that include the material of following weight portion, specifically For:
Solid phase 40%-80%
Organic binder bond 20%-60%;
Wherein, solid phase includes the material of following weight portion, particularly as follows:
Argentum powder 80%-100%
Oxide 0%-20%;
Argentum powder is mixed by flake silver powder, wire argentum powder, and median particle diameter is 1 μm-2 μm, flake silver powder, two kinds of things of wire argentum powder The weight portion of material is followed successively by: 30%-90%, 10%-70%;
Organic binder bond includes the material of following weight portion, particularly as follows:
Light-cured resin 65%-90%
Photoactive monomer 5%-30%
Light trigger 0.5%-5%
Defoamer 0.1%-1%
Dispersant 0.5%-2%.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described oxidation Thing is SnO2、SiO2、TiO2、Al2O3In one or more mixture formed, oxide median particle diameter is 1 μm-2 μm.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described light is solid Changing resin is o-cresol formaldehyde epoxy acrylic resin, bisphenol-A epoxy acrylic resin, polyimide modified epoxy acrylic resin In one or more mixture formed.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described light is lived Property monomer is double pentaerythritol methacrylate, ethoxyquin trimethylolpropane trimethacrylate, trimethylolpropane tris propylene One or more mixture formed in acid esters.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described light draws Sending out agent is 2-isopropyl thioxanthone, 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone, 2,4,6-trimethylbenzene first One or more mixture formed in acyl group-diphenyl phosphine oxide.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described froth breaking Agent is dimethicone.
A kind of flexible electrothermal membrane light-cured type resistance slurry the most according to claim 1, it is characterised in that: described dispersion Agent is BYK-AT204.
8. the flexible electrothermal membrane preparation method of light-cured type resistance slurry, it is characterised in that include following technique step Suddenly, particularly as follows:
Prepared by a, solid phase: flake silver powder uniformly mixes to prepare combined silver powder, the sheet in combined silver powder with wire argentum powder Shape argentum powder, the weight portion of wire argentum powder are followed successively by 30%-90%, 10%-70%, after prepared by argentum powder material to be mixed, toward combined silver Adding oxide in powder, combined silver powder, the weight portion of two kinds of materials of oxide are followed successively by 80%-100%, 0%-20%, mixing The mixture that argentum powder material and oxide are formed is ground, to obtain solid phase;
Prepared by b, organic binder bond: light-cured resin, photoactive monomer, light trigger, defoamer, dispersant are placed in container Mixing and stirring, to obtain organic binder bond, wherein, light-cured resin, photoactive monomer, light trigger, defoamer, dispersion The weight portion of five kinds of materials of agent is followed successively by 65%-90%, 5%-30%, 0.5%-5%, 0.1%-1%, 0.5%-2%;
Prepared by c, resistance slurry: carry out three-roll rolling, solid phase, organic binder bond two after solid phase, organic binder bond mixing dispersion The weight portion planting material is followed successively by 40%-80%, 20%-60%, obtains resistance slurry after rolling.
CN201610099552.1A 2016-02-24 2016-02-24 Photo-curable resistance paste for flexible electrothermal film and preparation method of photo-curable resistance paste Pending CN105722254A (en)

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WO2018103164A1 (en) * 2016-12-09 2018-06-14 东莞珂洛赫慕电子材料科技有限公司 Medium-temperature sintered all-silver electrode paste for thick film circuit for use in aluminum alloy substrate

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Publication number Priority date Publication date Assignee Title
WO2018103164A1 (en) * 2016-12-09 2018-06-14 东莞珂洛赫慕电子材料科技有限公司 Medium-temperature sintered all-silver electrode paste for thick film circuit for use in aluminum alloy substrate
CN106753144A (en) * 2017-01-12 2017-05-31 东莞珂洛赫慕电子材料科技有限公司 A kind of light-cured type high heat conduction packaging plastic with infrared window characteristic and preparation method thereof

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Application publication date: 20160629