WO2021213190A1 - 一种移印工艺用导电油墨其制备方法 - Google Patents

一种移印工艺用导电油墨其制备方法 Download PDF

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Publication number
WO2021213190A1
WO2021213190A1 PCT/CN2021/086305 CN2021086305W WO2021213190A1 WO 2021213190 A1 WO2021213190 A1 WO 2021213190A1 CN 2021086305 W CN2021086305 W CN 2021086305W WO 2021213190 A1 WO2021213190 A1 WO 2021213190A1
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Prior art keywords
printing process
stirring
conductive ink
pad printing
silver powder
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PCT/CN2021/086305
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English (en)
French (fr)
Inventor
江海涵
朱庆明
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上海宝银电子材料有限公司
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Publication of WO2021213190A1 publication Critical patent/WO2021213190A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0042—Degasification of liquids modifying the liquid flow
    • B01D19/0052—Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/02—Foam dispersion or prevention
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C09D11/104—Polyesters
    • 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

Definitions

  • the invention belongs to the technical field of electronic materials, and in particular relates to a conductive ink used in a pad printing process and a preparation method thereof.
  • Conductive inks are widely used in printed circuits, semiconductor packaging, solar cells and other fields. Conductive silver paste and conductive carbon paste are the most widely used series of conductive inks. These products are usually printed on a flat substrate by screen printing and then dried to form a conductive path. With the development of the electronics industry, the traditional screen printing process cannot be printed on special-shaped objects, so the pad printing process has been developed. Pad printing is one of the special printing methods. It can print graphics and images on the surface of irregular and special-shaped objects through colloidal transfer, and it is now becoming an important special printing. For example, the surface electronic circuit printing of many electronic products, such as mobile phone antennas, PCB board connectors, instrumentation, smart wearables, etc., is completed by pad printing.
  • the substrate After transferring the conductive ink in these application areas, the substrate will have excellent conductivity. Unlike screen printing conductive inks, pad printing conductive inks dry faster, which is also the most prominent feature of pad printing conductive inks. At the same time, pad printing conductive inks are susceptible to factors such as temperature, humidity and static electricity. Therefore, weather resistance needs to be considered when designing conductive inks for pad printing. The ink degumming rate of the conductive ink used in the pad printing process needs to reach 98% or more, and the printing accuracy diffusion rate should be controlled within 10%. In addition, since the printed substrate has a low thermal deformation temperature, it needs to be cured at a low temperature ( ⁇ 120°C).
  • the conductive ink After the conductive ink is transferred, it needs to have excellent conductivity, friction resistance and weather resistance. In addition to meeting the above-mentioned weather resistance conditions, the environmental protection requirements for products are getting higher and higher. Now ordinary low-temperature conductive inks only have the requirements for conductivity and adhesion, and cannot meet the full degumming rate and friction resistance. At this stage, the conductive ink used in the pad printing process still has the defects of poor ink degumming rate, substandard friction resistance, and poor electrical conductivity, so the research and development of this product is of great significance.
  • the purpose of the present invention is to overcome the above-mentioned defects in the prior art and provide a method for preparing conductive ink for pad printing process with good degumming head rate, good wear resistance and good conductivity.
  • a conductive ink for pad printing process including the following components by weight:
  • the average particle size of the flake silver powder is 4-6 ⁇ m, its shape is flake, it has good dispersibility in the ink system and excellent electrical conductivity.
  • the powder has good hardness and is low in cost. It is more expensive than pure silver powder. The cost is about 50% lower;
  • Nano-silver powder has a low bulk ratio, good fluidity, has a good leveling effect, and further promotes conductivity.
  • the saturated polyester resin is a high molecular weight linear saturated copolyester, with a molecular weight of 20000g/mol, a glass transition temperature of 65-70°C, a softening temperature of 155°C, and a density of 1.25g/cm3; the hardness of the polymer resin , Flexibility is very good, strong adhesion to the substrate.
  • thermoplastic polycarbonate resin The density of the thermoplastic polycarbonate resin is 1.18-1.22g/cm3, the linear expansion rate is 3.8 ⁇ 10-5cm/°C, and the heat distortion temperature is 135°C; the polycarbonate is colorless, transparent, heat-resistant, and impact-resistant. Flame-retardant BI grade, with good mechanical properties at ordinary use temperature. Compared with performance close to polymethyl methacrylate, polycarbonate has good impact resistance, high refractive index, and good processing performance. It does not require additives. It has UL94V-0 flame retardant performance.
  • the dibasic acid ester is high-purity MDBE, which is a mixture of dimethyl succinate, dimethyl glutarate, and dimethyl adipate; its content is greater than 99%, and its moisture content is less than 0.1%.
  • This solvent is an environmentally friendly high-boiling solvent with a boiling range of 196-225°C, an average molecular weight of 159, and a freezing point of -20°C.
  • the dibasic acid ester has excellent solubility, and can promote the ink to have good leveling and improve gloss. .
  • the molecular formula of the propylene glycol methyl ether acetate is C6H12O3, a colorless and hygroscopic liquid with a special odor. It is a non-polluted solvent with multifunctional groups, a molecular weight of 132.16, a melting point of -87°C, a boiling point of 146°C, a density of 0.96, colorless and transparent Liquid can improve the strength of the coating film.
  • the polyethylene wax has a density of 0.93-0.98, a molecular weight of 3500, and a melting point of 100°C. It has good compatibility with polyethylene, polypropylene, polyvinyl wax, ethylene propylene rubber, and butyl rubber, and can improve polyethylene and poly The fluidity of propylene and ABS and the release properties of polymethyl methacrylate and polycarbonate. Compared to PVC and other external lubricants, polyethylene wax has a stronger internal lubricating effect.
  • the working principle is as follows: Polyethylene wax is dissolved in the solvent at high temperature (about 100-140°C), and precipitates when cooled to normal temperature. It exists in the paint in the form of microcrystals.
  • the dimethylsiloxane molecular formula is C2H8Si, the melting point is -150°C, the boiling point is -20°C, and the defoaming agent with excellent performance can make the spreading performance of the ink surface more excellent and form a firm film layer.
  • the said fumed silica has an average particle size of 30nm, a specific surface area of 180-220m2/g, a purity of >99.8%, and an apparent density of 30-60g/L, and is used as a hydrophobic fumed silica for non-aqueous inks.
  • the average particle size of the flake graphite is 30-50nm, the purity is more than 99.9%, the specific surface area is 180m2/g-200m2/g, the tap density is 2-2.5g/cm3, and the flake black powder. After the surface of the powder is treated, it can have good dispersibility and increase a certain degree of conductivity and friction resistance in the ink coating.
  • a preparation method of conductive ink for pad printing process includes the steps of carrier configuration, ingredients, high-speed dispersion, three-roller grinding, filtering, finished product inspection, homogenous stirring, canning, etc. The specific steps are as follows:
  • an electronic scale of the Mettler BBA211 model is used as a weighing tool, and in conjunction with the recording component, the operator can add the raw material of the corresponding code according to the value displayed on the panel, and the accuracy is controlled at one ten thousandth.
  • the solvent here is the remaining dibasic acid ester and propylene glycol methyl ether acetate);
  • Step (3) The mixing head of the high-speed mixer is lowered to 2cm at the bottom of the material barrel, the frequency of the high-speed dispersing mixer is 75Hz, and the mixing time is 10-15min; the way to determine the uniform dispersion of the material is to observe that the ink is silver-gray paste and there is no silver powder. The particles are evenly dispersed.
  • Step (3) The number of cycles of dispersion grinding is three times, and the roller gap between the fast roller and the middle roller in the three-roll mill is continuously controlled step by step.
  • the roller gap is controlled at 0.3mm-0.35mm.
  • the roller gap is controlled at 0.25-0.3mm
  • the roller gap is controlled at 0.2-0.25mm.
  • the equipment used for the vacuum filtration in step (4) includes a vacuum pump and a stainless steel material cylinder connected to it.
  • a 250-400 mesh stainless steel mesh is installed above the stainless steel material cylinder.
  • When using first turn on the vacuum pump switch, and then continuously dump and disperse on the stainless steel mesh.
  • the finished conductive silver paste is continuously flattened with a rubber scraper to quickly filter it into the built-in stainless steel material cylinder.
  • Step (5) The function of homogenization and stirring is mainly to defoam and prevent the sedimentation of silver powder.
  • the conductive ink after homogenization will be very fine and uniform.
  • set the vacuum degree to 0.08 ⁇ 0.12Mpa, and then put the filled ink into Stir in the homogenizer for 3 to 5 minutes.
  • the conductive ink used in the pad printing process after homogenization and mixing can be directly filled out of the warehouse.
  • the present invention uses flaky silver powder (average particle size 4-6 ⁇ m) as the main solid phase, which can have excellent conductivity after curing into a film, and nano-spherical silver powder (average particle size about 250nm) as the solid filling phase, which can be further filled
  • flaky silver powder average particle size 4-6 ⁇ m
  • nano-spherical silver powder average particle size about 250nm
  • the gap between the nano silver powder film formation enhances the conductivity and adhesion of the conductive ink
  • the saturated polyester resin is used as the main binding phase, which can have strong adhesion and flexibility, and enhance the wide range of different substrates.
  • thermoplastic polycarbonate resin as the auxiliary binder phase, which can have strong wear resistance
  • stepped compound solvent phase dibasic acid ester, propylene glycol methyl ether acetate
  • the environmental protection requirements of WEEE can also achieve rapid curing to prevent local expansion of the graphics after printing
  • the use of polyethylene wax as an anti-settling agent can enhance the anti-settling performance and extend the storage time of the product. Because of its linear structure, The effect of conductive performance is small; using conductive graphite as a lubricant after film formation can effectively increase the lubricity and hardness of the film after the conductive ink is formed.
  • the self-made vacuum filter can effectively simulate the screen printing effect of the client and filter out the impurities produced in the conductive ink; the homogeneous mixer can effectively defoam the conductive ink and further fully mix the raw materials. Achieve higher fineness and uniformity.
  • the present invention has the following advantages:
  • the screening and compounding of different raw materials are carried out to prepare conductive inks for the pad printing process.
  • flake silver powder (average particle size 4-6 ⁇ m) as the main solid phase, it can have excellent conductivity after curing into a film, and nano-spherical silver powder (average particle size about 250nm) as the solid filling phase can be further filled with nano silver powder
  • the gap after film formation enhances the conductivity and adhesion of the conductive ink; the saturated polyester resin is used as the main binder phase, which can have strong adhesion and flexibility, and enhance the wide adaptability to different substrates.
  • thermoplastic polycarbonate resin as the auxiliary binder phase, which can have strong wear resistance
  • stepped compound solvent phase dibasic acid ester, propylene glycol methyl ether acetate
  • EU ROSH and WEEE Environmental protection requirements can achieve rapid curing to prevent local expansion of the graphics after printing
  • using polyethylene wax as an anti-settling agent can enhance the anti-settling performance and prolong the storage time of the product. Because of its linear structure, it is conductive The effect of the conductive ink is small; the use of conductive graphite as a lubricant after film formation can effectively increase the lubricity and hardness of the film after the conductive ink is formed.
  • the self-made vacuum filter can effectively simulate the screen printing effect of the client and filter out the impurities produced in the conductive ink; the homogeneous mixer can effectively defoam the conductive ink and further fully mix the raw materials. Achieve higher fineness and uniformity.
  • the degumming rate of the obtained conductive ink can reach 100%, the friction resistance can reach more than 600 times, and the conductivity is good, so the research and development of the product is of great significance.
  • a preparation method of conductive ink for pad printing process, each component and composition are shown in Table 1.
  • the saturated polyester resin and the thermoplastic polycarbonate resin are used as the binder phase.
  • the formula is: first add the saturated polyester resin and the thermoplastic polycarbonate resin into the reactor, and gradually increase the temperature to 50°C, and then add the dibasic acid ester , Propylene glycol methyl ether acetate is made by dripping in a ratio of 5:1 and then heating and melting; the nano spherical silver powder used is an ultrafine powder with an average particle size of 300-500nm.
  • an electronic scale of the Mettler BBA211 model is used as a weighing tool, and in conjunction with the recording component, the operator can add the raw material of the corresponding code according to the value displayed on the panel, and the accuracy is controlled at one ten thousandth.
  • the order of ingredient weighing is: adding saturated polyester resin and polycarbonate resin composite carrier ⁇ adding polyethylene wax, dimethylsiloxane, silane coupling agent, fumed silica ⁇ adding nano spherical silver powder and flake silver powder Mixture ⁇ add solvent.
  • the material bucket After the weighing is completed, move the material bucket to the high-speed disperser platform, then turn on the high-speed disperser switch, lower the stirring head to 2cm at the bottom of the bucket, turn on the frequency conversion switch to 60Hz, and set the timing to continue stirring for 3 minutes.
  • the material barrel is moved to the three-roll mill platform.
  • the rolling of the three-roll mill requires four cycles. Each time the silver paste is rolled, a high-speed dispersion step is required again. Then the gap between the fast roll and the middle roll of the three-roll mill is continuously controlled.
  • the roll gap for the first pass of low-temperature conductive silver paste is 0.3mm
  • the second pass is 0.25mm
  • the third pass At 0.2mm.
  • Example 6 Example 7
  • Example 8 Example 9
  • Saturated polyester resin 1.0 1.0 1.5 1.0
  • Thermoplastic polycarbonate resin 0.5 0.5 0.7 0.7 1.0
  • Dibasic acid ester 1 1.22 1
  • Propylene Glycol Methyl Ether Acetate 0.5 0.2 0.2 0.2 0.4
  • Polyethylene wax 0.05 0.02 0.02 0.02 0.02 Dimethicone 0.05 0.02 0.02 0.02 0.02 0.02 0.02 0.02
  • a silane coupling agent 0.005 0.01 0.01 0.01 0.01 0.01 Fumed silica 0.05 0.02 0.02 0.02 0.02 Flake graphite 0.05 0.01 0.03 0.03 0.03
  • an electronic scale of the Mettler BBA211 model is used as a weighing tool, and in conjunction with a recording component, the operator can add the raw material of the corresponding code according to the value displayed on the panel, and the accuracy is controlled at one ten thousandth.
  • the solvent here is the remaining dibasic acid ester and propylene glycol methyl ether acetate);
  • the mixing head of the high-speed mixer is lowered to 2cm at the bottom of the material bucket, the frequency of the high-speed dispersing mixer is 75Hz, and the mixing time is 10-15min, so that the material is stirred evenly at high speed, and finally observe that the ink is silver-grey paste. If there is no silver powder particles, the dispersion is even, and then it is added to the three-roll mill for circular grinding, the number of cycles is three, and the roll gap between the fast roll and the middle roll in the three-roll mill is continuously controlled step by step.
  • the first grinding is When the roll gap is controlled at 0.3mm-0.35mm, in the second grinding pass, the roll gap is controlled at 0.25-0.3mm, and during the third grinding pass, the roll gap is controlled at 0.2-0.25mm. Need to perform high-speed stirring again; multiple cycles until the fineness of the material is less than or equal to 10 ⁇ m;
  • the equipment used in vacuum filtration includes a vacuum pump and a stainless steel material cylinder connected to it.
  • the stainless steel material cylinder is installed with 250 -400 mesh stainless steel mesh, first turn on the vacuum pump switch when using, then continuously pour the dispersed conductive silver paste on the stainless steel mesh, and use a rubber scraper to continuously flatten the silver paste to quickly filter it into the built-in stainless steel material cylinder.
  • the function of homogenization and stirring is mainly to defoam and prevent the sedimentation of silver powder.
  • the conductive ink after homogenization will be very fine and uniform.
  • set the vacuum degree to 0.08 ⁇ 0.12Mpa, and then put the filled ink into the homogenizer Stir for 3 to 5 minutes.
  • the conductive ink used in the pad printing process after homogenization and mixing can be directly discharged from the warehouse for filling.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
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  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

一种移印工艺用导电油墨，包括的组分为片状银粉、纳米球状银粉、饱和聚酯树脂、热塑性聚碳酸酯树脂、二价酸酯、丙二醇甲醚醋酸酯、聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅和片状石墨。该导电油墨的制备方法为将饱和聚酯树脂、热塑性聚碳酸酯树脂、二价酸酯、丙二醇甲醚醋酸酯倒入溶解釜中，将溶解釜的搅拌速度控制在1500-2500rpm/min，高速搅拌5-6h，升温至70℃，加入片状石墨，反应3h后趁热出料，得到复合载体；依次在物料桶中加入配置的复合载体、聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅、纳米球状银粉与片状银粉的混合物、溶剂；将物料桶移至高速搅拌机搅拌均匀，加入三辊研磨机进行循环研磨，真空过滤后的物料装罐，置于均质机中搅拌3-5min即可。

Description

一种移印工艺用导电油墨其制备方法 技术领域
本发明属于电子材料技术领域，尤其是涉及一种移印工艺用导电油墨及其制备方法。
背景技术
导电油墨被广泛应用于印刷电路、半导体封装、太阳能电池等领域。导电银浆、导电碳浆是导电油墨中应用最广的系列产品，这些产品通常使用丝网印刷的方式印刷在平面基材上然后经过烘干形成导电通路。随着电子工业的发展，传统的丝网印刷工艺由于不能印刷在异形件物体上，所以发展出移印工艺。移印工艺属于特种印刷方式之一。它能够通过胶体转印在不规则异形对象表面上印刷图形和图象，现在正成为一种重要的特种印刷。例如，手机天线、PCB板连接件、仪器仪表、智能穿戴等很多电子产品的表面电子线路印刷都以移印完成。在这些应用领域上转印完导电油墨后，会使基材具备优异的导电性能。与丝印导电油墨不同，移印导电油墨干燥速度要快一些，这也是移印导电油墨最突出的特点。与此同时，移印导电油墨很容易受到一些因素例如温度、湿度和静电的影响。所以设计移印用导电油墨时还需要考虑耐候性。移印工艺用导电油墨的油墨脱胶头率需要达到98％以上，且印刷精度扩散率要控制在10％以内。另外由于印刷的基材热变形温度较低，所以需要在低温下完成固化(≤120℃)。转印完导电油墨后，还需要具备优异的导电性、耐摩擦性以及耐候性。除了满足上述的耐候性条件外，对产品的环保要求越来越高，现在普通的低温导电油墨只有导电性能和附着力的要求，无法满足全部脱胶率以及耐摩擦性。现阶段，移印工艺用导电油墨仍存在油墨脱胶头率差、耐摩擦性不达标、导电性能较差的缺陷，故该产品的研发意义重大。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种脱胶头率好、耐磨性、导电性佳的移印工艺用导电油墨其制备方法。
本发明的目的可以通过以下技术方案来实现：一种移印工艺用导电油墨，包括以下重量份含量的组分：
Figure PCTCN2021086305-appb-000001
所述的片状银粉的平均粒径在4～6μm，其形状为片状、在油墨体系中分散性良好且导电性能优异，该粉末具备良好的硬度，且成本低廉，较纯银粉配置的油墨成本低50％左右；
所述的纳米球状银粉的平均粒径在200-300nm，纯度＞99.95％，其形状为球状，比表面积25m2/g-40m2/g，体积密度0.8-1.0g/cm3。纳米银粉低松比，流动性好，拥有良好的填平效果，进一步促进导电性。
所述的饱和聚酯树脂为高分子量线型饱和共聚聚酯，其分子量为20000g/mol，玻璃化温度为65-70℃，软化温度155℃，密度1.25g/cm3；该高分子树脂的硬度、柔韧性都很好，对基材的附着力很强。
所述的热塑性聚碳酸酯树脂的密度为1.18-1.22g/cm3，线膨胀率为3.8×10-5cm/℃，热变形温度为135℃；聚碳酸酯无色透明，耐热，抗冲击，阻燃BI级，在普通使用温度内都有良好的机械性能，同性能接近聚甲基丙烯酸甲酯相比，聚碳酸酯的耐冲击性能好，折射率高，加工性能好，不需要添加剂就具有UL94V-0级阻燃性能。
所述的二价酸酯为高纯度MDBE，是丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯的混合物；其含量＞99％，其水分含量＜0.1％，该种溶剂是环保型高 沸点溶剂，沸程在196-225℃，平均分子量159，凝固点-20℃，二价酸酯具备极好的溶解性，并能够促进油墨具备良好的流平性，提高光泽。
所述的丙二醇甲醚醋酸酯分子式为C6H12O3，无色吸湿液体，有特殊气味，是一种具有多官能团的非公害溶剂，分子量132.16，熔点-87℃，沸点146℃，密度0.96，无色透明液体，能够提高涂膜强度。
所述的聚乙烯蜡的密度0.93-0.98，分子量为3500，熔点100℃，能够与聚乙烯、聚丙烯、聚蜡酸乙烯、乙丙橡胶、丁基橡胶相溶性好，能改善聚乙烯、聚丙烯、ABS的流动性和聚甲基丙烯酸甲酯、聚碳酸酯的脱模性，对于PVC和其它的外部润滑剂相比，聚乙烯蜡具有更强的内部润滑作用。其作用原理是这样的：聚乙烯蜡在高温中(约100-140℃)溶解于溶剂中，而在冷却至常温时析出，以微晶形式存在于涂料中，因其触变性有利于涂料的贮存，而在涂料施工应用之后，在溶剂挥发过程中能迁移到涂膜表层，最终与涂料其他组分形成一个“蜡化”的表层。
所述的二甲基硅氧烷分子式为C2H8Si，熔点-150℃，沸点-20℃，具备优异性能的消泡剂，能使油墨表面的铺展性能更加优异，形成坚固的膜层。
所述的气相二氧化硅平均粒径为30nm，比表面积180-220m2/g，纯度＞99.8％，表观密度30-60g/L，用于非水性油墨的疏水性气相二氧化硅。
所述的片状石墨的平均粒径为30-50nm，纯度＞99.9％，比表面积180m2/g-200m2/g，振实密度2-2.5g/cm3，片状黑色粉体。该粉体表面经过处理，可以具备良好的分散性，在油墨涂层中增加一定的导电性和耐摩擦性。
一种移印工艺用导电油墨的制备方法，包括载体配置、配料、高速分散、三辊研磨、过滤、成品检测、匀质搅拌、装罐等步骤，具体步骤如下：
(1)载体配置
将饱和聚酯树脂、热塑性聚碳酸酯树脂和作为溶剂的二价酸酯、丙二醇甲醚醋酸酯(此处二价酸酯、丙二醇甲醚醋酸酯的质量比为5:1)倒入溶解釜中，随后将溶解釜的搅拌速度控制在1500-2500rpm/min，高速搅拌5～6h，将反应釜升温至70℃，加入片状石墨，反应3h后趁热出料，得到复合载体；最后检测载体，若溶解完全则取出，若仍有未溶解的粉末颗粒可适当增加分散时间。待溶解完毕后通过250目的不锈钢网过滤出最终载体。
(2)配料
配料的步骤使用了梅特勒BBA211型号的电子秤作为称量工具，并配合记录组件，操作员可以根据面板显示值添加对应代号的原材料，精度控制在万分之一。按质量百分比依次在物料桶中添加步骤(1)配置的复合载体、聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅、纳米球状银粉与片状银粉的混合物、溶剂(此处溶剂为剩余二价酸酯和丙二醇甲醚醋酸酯)；
(3)分散、研磨
将物料桶移至高速搅拌机，使物料高速搅拌均匀，然后加入三辊研磨机进行循环研磨，每轧制完一遍银浆都需要再次进行高速搅拌；多次循环，至物料细度小于等于10μm；
(4)真空过滤
采用250-400目的不锈钢网进行真空过滤，其主要作用是为了分离研磨过程中产生的大颗粒杂质；
(5)均质搅拌
将真空过滤后的物料装罐，并置于均质机中搅拌3～5min即可。
步骤(3)高速搅拌机的搅拌头降至物料桶底2cm处，高速分散搅拌机的频率为75Hz，搅拌时间为10～15min；物料分散均匀的判定方式为观察油墨整体呈银灰色浆体且无银粉颗粒，则分散均匀。
步骤(3)分散研磨的循环次数为三次，且不断循序渐进地控制三辊研磨机中快辊和中辊之间的辊间隙，第一遍研磨时，辊间隙控制在0.3mm-0.35mm，第二遍研磨时，辊间隙控制在0.25-0.3mm，第三遍研磨时，辊间隙控制在0.2-0.25mm。
步骤(4)所述真空过滤采用的设备包括真空泵、以及与其连接的不锈钢物料筒，该不锈钢物料筒上方安装有250-400目的不锈钢网，使用时先打开真空泵开关，随后在不锈钢网上不断倾倒分散完毕的导电银浆，并用橡胶刮板不断铺平银浆，使其迅速过滤到内置不锈钢物料筒中去。
步骤(5)均质搅拌的作用主要是脱泡和防止银粉沉降，均质后的导电油墨会非常细腻均匀，使用时将真空度设为0.08～0.12Mpa，再将装罐完毕的油墨放入均质机中搅拌3～5min即可。均质搅拌后的移印工艺用导电油墨可以直接出 库灌装。
本发明采用片状银粉(平均粒径4～6μm)为主要固体相，可以在固化成膜后具备优异的导电性，以纳米球状银粉(平均粒径250nm左右)作为固体填充相，可以进一步填充纳米银粉成膜后的缝隙，增强导电油墨的导电性和附着力；采用饱和聚酯树脂树脂作为主要粘结相，可以具有很强的附着力和柔韧性，并增强对不同承印基材的广泛适应性；采用热塑性聚碳酸酯树脂作为辅助粘结相，可以具有很强的耐磨性；采用阶梯式复配型溶剂相(二价酸酯、丙二醇甲醚醋酸酯)，既满足欧盟ROSH以及WEEE的环保要求，又可以实现快速固化，防止出现印刷后的图形局部膨胀现象；采用聚乙烯蜡作为防沉降剂，可以增强抗沉降性，延长产品的存放时间，并由于其是线性结构，对导电性能的影响效果较小；采用导电石墨作为成膜后的润滑剂，可以有效增加导电油墨成膜后的润滑性增强膜层硬度。采用自制的真空过滤器，可以有效模拟客户端的丝网印刷效果，过滤掉导电油墨制成中产生的杂质；采用均质搅拌机，可以有效地使导电油墨脱泡、并使原材料进一步地充分混合，达到更高的细度和均匀度。
与现有技术相比，本发明具有以下优点：
通过对油墨涂层的配方设计，对不同原材料进行筛选、复配，制备移印工艺用导电油墨。采用片状银粉(平均粒径4～6μm)为主要固体相，可以在固化成膜后具备优异的导电性，以纳米球状银粉(平均粒径250nm左右)作为固体填充相，可以进一步填充纳米银粉成膜后的缝隙，增强导电油墨的导电性和附着力；采用饱和聚酯树脂树脂作为主要粘结相，可以具有很强的附着力和柔韧性，并增强对不同承印基材的广泛适应性；采用热塑性聚碳酸酯树脂作为辅助粘结相，可以具有很强的耐磨性；采用阶梯式复配型溶剂相(二价酸酯、丙二醇甲醚醋酸酯)，既满足欧盟ROSH以及WEEE的环保要求，又可以实现快速固化，防止出现印刷后的图形局部膨胀现象；采用聚乙烯蜡作为防沉降剂，可以增强抗沉降性，延长产品的存放时间，并由于其是线性结构，对导电性能的影响效果较小；采用导电石墨作为成膜后的润滑剂，可以有效增加导电油墨成膜后的润滑性增强膜层硬度。采用自制的真空过滤器，可以有效模拟客户端的丝网印刷效果，过滤掉导电油墨制成中产生的杂质；采用均质搅拌机，可以有效地使导电油墨脱泡、并使原材料进一步地充分混合，达到更高的细度和均 匀度。
所得导电油墨的脱胶头率可达100％、耐摩擦性可达600次以上、导电性能良好，故该产品的研发意义重大。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1～5
一种移印工艺用导电油墨的制备方法，各组分及成分如表1所示。其中饱和聚酯树脂和热塑性聚碳酸酯树脂作为粘结相，其配方为：先将饱和聚酯树脂和热塑性聚碳酸酯树脂加入反应釜中，并逐渐升温至50℃，随后将二价酸酯、丙二醇甲醚醋酸酯按比例5:1的比例滴加后加热融化制成；使用的纳米球状银粉为超细粉末，平均粒径在300～500nm。
表1
Figure PCTCN2021086305-appb-000002
按照配方比例将饱和聚酯树脂和聚碳酸树脂加入反应釜中，并逐渐升温至50℃，随后将二价酸酯、丙二醇甲醚醋酸酯、按照5:1的以滴加的方式加入反应釜，滴加时间为1.5h，滴加完成后继续反映3h。接着，将反应釜升温至70℃，将片状石墨加入反应釜，反应3h后趁热出料，得到聚氨酯树脂和聚碳酸树脂复 合载体，避光保存。配料的步骤使用了梅特勒BBA211型号的电子秤作为称量工具，并配合记录组件，操作员可以根据面板显示值添加对应代号的原材料，精度控制在万分之一。配料称量的顺序是：添加饱和聚酯树脂和聚碳酸树脂复合载体→加入聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅→添加纳米球状银粉与片状银粉的混合物→添加溶剂。
称量完毕后将物料桶移动至高速分散机平台上，然后开启高速分散机开关，将搅拌头降至桶底2cm处，开启变频开关至60Hz，设置定时后连续搅拌3min。接着讲物料桶移至三辊研磨机平台，三辊研磨机的轧制需要四个循环，每轧制完一遍银浆都需要再次进行一遍高速分散步骤。然后不断循序渐进地控制三辊研磨机种快辊和中辊之间的间隙，第一遍研磨低温导电银浆的辊间隙在0.3mm，第二遍辊间隙在0.25mm，第三遍辊间隙控制在0.2mm。将达到10um细度以下的物料桶移至真空过滤平台，在过滤机上方安装400目的不锈钢网并将油墨过滤完全。将过滤完全的半成品交由检测部门检测，达到企业标准后进行均质搅拌，将真空度设为为0.12Mpa，再将装罐完毕的银浆放入均质机中搅拌3min即可。移印工艺用导电油墨的性能如表2所示。
表2
Figure PCTCN2021086305-appb-000003
Figure PCTCN2021086305-appb-000004
实施例6～10
下面各实施例所述移印工艺用导电油墨的配方组分及含量(wt％)见表3：
表3
材料名称 实施例6 实施例7 实施例8 实施例9 实施例10
片状银粉 5 5 5 5 5
纳米球状银粉 1.795 2 1.5 1.5 1.5
饱和聚酯树脂 1.0 1.0 1.5 1.0 1.0
热塑性聚碳酸酯树脂 0.5 0.5 0.7 0.7 1.0
二价酸酯 1 1.22 1 1.5 1
丙二醇甲醚醋酸酯 0.5 0.2 0.2 0.2 0.4
聚乙烯蜡 0.05 0.02 0.02 0.02 0.02
二甲基硅氧烷 0.05 0.02 0.02 0.02 0.02
硅烷偶联剂 0.005 0.01 0.01 0.01 0.01
气相二氧化硅 0.05 0.02 0.02 0.02 0.02
片状石墨 0.05 0.01 0.03 0.03 0.03
上述各实施例中移印工艺用导电油墨通过以下方法制得：
(1)载体配置
将饱和聚酯树脂、热塑性聚碳酸酯树脂和作为溶剂的二价酸酯、丙二醇甲醚醋酸酯(此处二价酸酯、丙二醇甲醚醋酸酯的质量比为5:1)倒入溶解釜中，随后将溶解釜的搅拌速度控制在1500-2500rpm/min，高速搅拌5～6h，将反应釜升温至70℃，加入片状石墨，反应3h后趁热出料，得到复合载体；最后检测载体，若溶解完全则取出，若仍有未溶解的粉末颗粒可适当增加分散时间。待溶解完毕后通过250目的不锈钢网过滤出最终载体。
(2)配料
配料的步骤使用了梅特勒BBA211型号的电子秤作为称量工具，并配合记 录组件，操作员可以根据面板显示值添加对应代号的原材料，精度控制在万分之一。按质量百分比依次在物料桶中添加步骤(1)配置的复合载体、聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅、纳米球状银粉与片状银粉的混合物、溶剂(此处溶剂为剩余二价酸酯和丙二醇甲醚醋酸酯)；
(3)分散、研磨
将物料桶移至高速搅拌机，高速搅拌机的搅拌头降至物料桶底2cm处，高速分散搅拌机的频率为75Hz，搅拌时间为10～15min，使物料高速搅拌均匀，最后观察油墨整体呈银灰色浆体且无银粉颗粒，则分散均匀，然后加入三辊研磨机进行循环研磨，循环次数为三次，且不断循序渐进地控制三辊研磨机中快辊和中辊之间的辊间隙，第一遍研磨时，辊间隙控制在0.3mm-0.35mm，第二遍研磨时，辊间隙控制在0.25-0.3mm，第三遍研磨时，辊间隙控制在0.2-0.25mm，每轧制完一遍银浆都需要再次进行高速搅拌；多次循环，至物料细度小于等于10μm；
(4)真空过滤
采用250-400目的不锈钢网进行真空过滤，其主要作用是为了分离研磨过程中产生的大颗粒杂质；真空过滤采用的设备包括真空泵、以及与其连接的不锈钢物料筒，该不锈钢物料筒上方安装有250-400目的不锈钢网，使用时先打开真空泵开关，随后在不锈钢网上不断倾倒分散完毕的导电银浆，并用橡胶刮板不断铺平银浆，使其迅速过滤到内置不锈钢物料筒中去。
(5)均质搅拌
将真空过滤后的物料装罐，并置于均质机中搅拌3～5min即可。均质搅拌的作用主要是脱泡和防止银粉沉降，均质后的导电油墨会非常细腻均匀，使用时将真空度设为0.08～0.12Mpa，再将装罐完毕的油墨放入均质机中搅拌3～5min即可。均质搅拌后的移印工艺用导电油墨可以直接出库灌装。
表4
Figure PCTCN2021086305-appb-000005
Figure PCTCN2021086305-appb-000006

Claims (10)

  1. 一种移印工艺用导电油墨，其特征在于，包括以下重量份含量的组分：
    Figure PCTCN2021086305-appb-100001
  2. 根据权利要求1所述的移印工艺用导电油墨，其特征在于，所述的片状银粉的平均粒径在4～6μm；
    所述的纳米球状银粉的平均粒径在200-300nm，纯度＞99.95％，其形状为球状，比表面积25m 2/g-40m 2/g，体积密度0.8-1.0g/cm 3。
  3. 根据权利要求1所述的移印工艺用导电油墨，其特征在于，所述的饱和聚酯树脂为高分子量线型饱和共聚聚酯，其分子量为20000g/mol，玻璃化温度为65-70℃，软化温度155℃，密度1.25g/cm 3；
    所述的热塑性聚碳酸酯树脂的密度为1.18-1.22g/cm 3，线膨胀率为3.8×10-5cm/℃，热变形温度为135℃；
    所述的二价酸酯为高纯度MDBE，是丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯的混合物；
    所述的丙二醇甲醚醋酸酯分子式为C 6H 12O 3，无色吸湿液体，有特殊气味，是一种具有多官能团的非公害溶剂。
  4. 根据权利要求1所述的移印工艺用导电油墨，其特征在于，所述的聚乙 烯蜡的密度0.93-0.98，分子量为3500，熔点100℃；
    所述的二甲基硅氧烷分子式为C2H8Si，熔点-150℃，沸点-20℃；
    所述的气相二氧化硅平均粒径为30nm，比表面积180-220m 2/g，纯度＞99.8％，表观密度30-60g/L。
  5. 根据权利要求1所述的移印工艺用导电油墨，其特征在于，所述的片状石墨的平均粒径为30-50nm，纯度＞99.9％，比表面积180m2/g-200m 2/g，振实密度2-2.5g/cm 3，片状黑色粉体。
  6. 一种如权利要求1～5中任一所述的移印工艺用导电油墨的制备方法，其特征在于，包括以下步骤：
    (1)载体配置
    将饱和聚酯树脂、热塑性聚碳酸酯树脂和二价酸酯、丙二醇甲醚醋酸酯倒入溶解釜中，随后将溶解釜的搅拌速度控制在1500-2500rpm/min，高速搅拌5～6h，将反应釜升温至70℃，加入片状石墨，反应3h后趁热出料，得到复合载体；
    (2)配料
    按质量百分比依次在物料桶中添加步骤(1)配置的复合载体、聚乙烯蜡、二甲基硅氧烷、硅烷偶联剂、气相二氧化硅、纳米球状银粉与片状银粉的混合物、溶剂；
    (3)分散、研磨
    将物料桶移至高速搅拌机，使物料高速搅拌均匀，然后加入三辊研磨机进行循环研磨，每轧制完一遍银浆都需要再次进行高速搅拌；多次循环，至物料细度小于等于10μm；
    (4)真空过滤
    采用250-400目的不锈钢网进行真空过滤；
    (5)均质搅拌
    将真空过滤后的物料装罐，并置于均质机中搅拌3～5min即可。
  7. 根据权利要求1所述的移印工艺用导电油墨的制备方法，其特征在于，步骤(3)高速搅拌机的搅拌头降至物料桶底2cm处，高速分散搅拌机的频率为75Hz，搅拌时间为10～15min；物料分散均匀的判定方式为观察油墨整体呈 银灰色浆体且无银粉颗粒，则分散均匀。
  8. 根据权利要求1所述的移印工艺用导电油墨的制备方法，其特征在于，步骤(3)分散研磨的循环次数为三次，且不断循序渐进地控制三辊研磨机中快辊和中辊之间的辊间隙，第一遍研磨时，辊间隙控制在0.3mm-0.35mm，第二遍研磨时，辊间隙控制在0.25-0.3mm，第三遍研磨时，辊间隙控制在0.2-0.25mm。
  9. 根据权利要求1所述的移印工艺用导电油墨的制备方法，其特征在于，步骤(4)所述真空过滤采用的设备包括真空泵、以及与其连接的不锈钢物料筒，该不锈钢物料筒上方安装有250-400目的不锈钢网，使用时先打开真空泵开关，随后在不锈钢网上不断倾倒分散完毕的导电银浆，并用橡胶刮板不断铺平银浆，使其迅速过滤到内置不锈钢物料筒中去。
  10. 根据权利要求1所述的移印工艺用导电油墨的制备方法，其特征在于，步骤(5)均质搅拌前物料罐中的真空度为0.08～0.12Mpa。
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