WO2020143273A1 - Encre conductrice à base de nanoparticules d'ag-cu à structure cœur-enveloppe, son procédé de préparation et son utilisation - Google Patents

Encre conductrice à base de nanoparticules d'ag-cu à structure cœur-enveloppe, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2020143273A1
WO2020143273A1 PCT/CN2019/112849 CN2019112849W WO2020143273A1 WO 2020143273 A1 WO2020143273 A1 WO 2020143273A1 CN 2019112849 W CN2019112849 W CN 2019112849W WO 2020143273 A1 WO2020143273 A1 WO 2020143273A1
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core
shell structure
conductive ink
precursor solution
source precursor
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PCT/CN2019/112849
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English (en)
Chinese (zh)
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魏昂
郑泽军
位威
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南京邮电大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/02—Layer formed of wires, e.g. mesh
    • 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
    • C09D11/52—Electrically conductive inks

Definitions

  • the invention belongs to the field of metal conductive nanoparticles, and particularly relates to a core-shell structure Ag@Cu nanoparticle conductive ink for inkjet printing on a flexible substrate and a preparation method thereof.
  • Conductive materials used in printing inks have been continuously developed. Because of their huge potential, they have been widely developed and used in various electronic devices, such as radio frequency identification (RFID), photovoltaic cells, conductive circuits, sensors, and displays. Materials such as carbon nanotubes, conductive polymers and graphene have been used in conductive printing inks, but these inks tend to have low conductivity and poor chemical properties, and the adhesion of these inks on flexible substrates is poor The effect of inkjet printing is not very fine, and the application of metal nanoparticles in printing inks will effectively solve the above problems.
  • RFID radio frequency identification
  • Silver nanoparticles have been widely used in conductive inks, which have high conductivity and good oxidation stability.
  • the high price of silver nanoparticles and its severe electromigration that is, the migration of metal ions under the action of an electric field, when the device works, a certain current passes through the metal interconnection line, and the metal ions will be transported along the conductor.
  • voids or whiskers may be generated in certain parts of the conductor, which hinders its application in printing inks.
  • copper Compared with precious metals (gold, silver), copper has excellent equivalent conductivity (only 6% lower than silver) and a lower price, so copper nanoparticles are considered as a substitute for silver nanoparticles used in printing inks
  • copper nanoparticles are easily oxidized under air conditions, and their oxides will have a serious impact on electrical conductivity.
  • Ag@Cu core-shell nanoparticles are very suitable as a substitute for printing inks.
  • the application of copper not only reduces the cost, but also reduces the possibility of electromigration.
  • the outer silver shell can passivate the inner copper core to avoid its oxidation.
  • the current methods for preparing Ag@Cu core-shell nanoparticles mainly include magnetic field preparation method, high temperature hot extrusion method, chemical dealloying method, electroplating method, etc.
  • the equipment required by magnetic field preparation method and high temperature extrusion method is expensive. Experimental conditions such as chemical dealloying and electroplating are more demanding.
  • Chinese patent CN101088670A discloses a method for preparing Cu-Ag core-shell composite metal powder, which uses direct plating to pre-plat copper particles followed by two glucose baths to coat a layer of silver, but the required reagents are not environmentally friendly , The steps are complicated and the prepared particles are in the micron level.
  • Chinese patent CN102950282A discloses a method for preparing silver-copper coated powder, which uses ultrasonic agitation reduction method, but the reaction involves strong acid solvents such as nitric acid and sulfuric acid, and the shape of the prepared powder is not uniform, spherical and flake exist at the same time .
  • the purpose of the present invention is to provide a core-shell structure Ag@Cu nanoparticle conductive ink and its preparation method and use in view of the above problems of the core-shell structure Ag@Cu nanoparticle conductive ink.
  • the preparation method is simple and easy to operate.
  • a core-shell structure Ag@Cu nanoparticle conductive ink which is formed by spherical nanoparticles dispersed in a liquid, the spherical nanoparticles are Ag@Cu nanoparticles coated with a silver core coated with a copper core, and the liquid is deionized water ,
  • a mixture of ethylene glycol and glycerin; the solid content of the spherical nanoparticles is 10 to 30% by weight.
  • a method for preparing a core-shell structure Ag@Cu nanoparticle conductive ink includes the following steps:
  • reducing agent and dispersing agent adding sodium hypophosphite monohydrate (NaH 2 PO 2 ⁇ H 2 O) as reducing agent and poly as dispersing agent to the copper source precursor solution obtained in step (1) Vinylpyrrolidone (PVP-K30);
  • Oil bath treatment Transfer the reaction vessel containing the copper source precursor solution, reducing agent and dispersant solution obtained in step (2) to an oil bath pot, stir the oil bath, and perform the reaction;
  • Oil bath treatment Place the dried product in step (4) in a reaction vessel, add ethylene glycol, stir, and then drop the silver source precursor solution obtained in step (5) to perform the reaction under an oil bath ;
  • Step (7) The powder obtained in step (7) is dissolved in a mixed solution of deionized water, ethylene glycol, and glycerin, and is ultrasonically dispersed to obtain the core-shell structure Ag@Cu nanoparticle conductive ink.
  • the concentration of the copper source precursor solution is 0.01M-0.05M; in the step (2), the mass ratio of the reducing agent to copper sulfate is 1:1.6, and the mass of the dispersant and copper sulfate The ratio is 2:1.6.
  • the temperature of the oil bath is 60-80° C., and the reaction time is 10-30 min.
  • the concentration of the silver source precursor solution is 0.01-0.05M.
  • the ratio of the deionized water, ethylene glycol and glycerin is changed so that the viscosity of the prepared ink is 8 to 12 cps.
  • the core-shell structure Ag@Cu nanoparticle conductive ink of the present invention can be used in flexible printing, and the specific method is:
  • Step a processing the substrate: performing plasma treatment on the flexible substrate;
  • Step b Printing ink: inkjet printing the core-shell structure Ag@Cu nanoparticle conductive ink on the flexible substrate processed in step a to obtain a flexible substrate with a conductive pattern attached;
  • Step c sintering treatment: the flexible substrate with conductive pattern attached obtained in step b is placed in a vacuum oven for sintering.
  • the flexible substrate is PET or photo paper, and the plasma treatment time is 1 to 20 minutes; in the step c, the sintering temperature is 100 to 200°C.
  • the contact angle between the core-shell structure Ag@Cu nanoparticle conductive ink and the flexible substrate is 48-100°.
  • the core-shell structure Ag@Cu nanoparticle conductive ink of the present invention is formed by dispersing spherical nanoparticles in a liquid.
  • the nanoparticles have the characteristics of a silver shell covering the copper core, which not only benefits the improvement of copper oxidation stability, but also Can improve its resistance to electromigration. Therefore, the conductive ink prepared by the nanoparticles has good stability, and the conductive pattern printed on the flexible substrate exhibits good conductivity and adhesion.
  • the ink-printed conductive film based on the present invention has the characteristics of being flexible and bendable, and has good conductivity under bending conditions.
  • the conductive ink of the present invention is suitable for inkjet printing, is firmly compounded with a flexible substrate, and has good film conductivity.
  • the preparation method of the invention adopts the method of liquid-phase alcohol thermal reduction, with PVP-K30 as the dispersant, NaH 2 PO 2 ⁇ H 2 O as the reducing agent, the reaction temperature is 60 ⁇ 80°C, and the reaction is 10 ⁇ 30min to prepare copper nanoparticles .
  • the silver particles were coated on the washed copper particles, and reacted at 60-80°C for 10-30 minutes.
  • the prepared core-shell structure Ag@Cu nanoparticles are spherical particles with a particle size of about 50 nm, and the conductive ink can be applied to flexible printing after adding a corresponding proportion of solvent.
  • the method is simple, the reaction raw materials are easily available, the reaction conditions are mild and easy to operate, and it is suitable for large-scale industrial production.
  • Example 1 is a scanning electron microscope (SEM) image of the core-shell structure Ag@Cu nanoparticles prepared in Example 1;
  • EDS energy spectrum
  • Example 3 is an X-ray diffraction (XRD) pattern of the core-shell structure Ag@Cu nanoparticles prepared in Example 1;
  • Example 4 is a scanning electron microscope element mapping diagram of the core-shell structure Ag@Cu nanoparticles prepared in Example 1;
  • FIG. 5 is a schematic diagram of the contact angle of the core-shell structure Ag@Cu nanoparticle conductive ink prepared in Example 2 on PET;
  • Example 6 is a physical diagram of a small light bulb bent and lighted after the core-shell structure Ag@Cu nanoparticle conductive ink prepared in Example 2 is printed on PET.
  • a core-shell structure Ag@Cu nanoparticle conductive ink of the present invention is formed by spherical nanoparticles dispersed in a liquid; wherein:
  • Spherical nanoparticles are Ag@Cu nanoparticles with silver shells covering the copper core, and their particle size is about 50nm.
  • the nanoparticles have a core-shell structure, which not only helps the silver shell protect the copper core from oxidation, but also reduces electromigration
  • the possibility that the nanoparticles are formulated with ink has better stability and conductivity;
  • the liquid is a mixture of deionized water, ethylene glycol and glycerin;
  • the solid content of the spherical nanoparticles is 10-30% by weight.
  • a method for preparing a core-shell structure Ag@Cu nanoparticle conductive ink includes the following steps:
  • reducing agent and dispersing agent adding sodium hypophosphite monohydrate (NaH 2 PO 2 ⁇ H 2 O) as reducing agent and poly as dispersing agent to the copper source precursor solution obtained in step (1) Vinylpyrrolidone (PVP-K30); wherein, the mass ratio of reducing agent to copper sulfate is 1:1.6, and the mass ratio of dispersant to copper sulfate is 2:1.6;
  • Oil bath treatment transfer the reaction vessel containing the copper source precursor solution, the reducing agent and the dispersant solution obtained in step (2) to an oil bath pot, stir the oil bath, and perform the reaction; wherein, the oil bath temperature is 60 ⁇ 80°C, reaction time is 10 ⁇ 30min;
  • silver nitrate AgNO 3
  • ethylene glycol ethylene glycol
  • magnetic stirring is uniformly prepared into a silver source precursor solution; wherein, the concentration of the silver source precursor solution is 0.01 ⁇ 0.05M;
  • Oil bath treatment Place the dried product in step (4) in a reaction vessel, add ethylene glycol, stir, and then drop the silver source precursor solution obtained in step (5) to perform the reaction under an oil bath ;
  • the oil bath temperature is 60 ⁇ 80 °C
  • the reaction time is 10 ⁇ 30min;
  • Formulating ink dissolve the powder obtained in step (7) in a mixed solution of deionized water, ethylene glycol and glycerin, and disperse ultrasonically to obtain the core-shell structure Ag@Cu nanoparticle conductive ink; wherein , By changing the ratio of deionized water, ethylene glycol and glycerol, so that the viscosity of the prepared ink is 8 ⁇ 12cps.
  • the core-shell structure Ag@Cu nanoparticle conductive ink of the present invention can be used in flexible printing, and the specific method is:
  • Step a processing the substrate: performing plasma treatment on the flexible substrate; wherein, the flexible substrate is PET, and the plasma treatment time is 1-20 min;
  • Step b Printing ink: inkjet printing the core-shell structure Ag@Cu nanoparticle conductive ink on the flexible substrate processed in step a to obtain a flexible substrate with a conductive pattern attached;
  • Step c sintering treatment: the flexible substrate with the conductive pattern attached obtained in step b is placed in a vacuum oven for sintering; wherein, the sintering temperature is 100-200°C.
  • the contact angle of the core-shell structure Ag@Cu nanoparticle conductive ink and the flexible substrate is 48-100°.
  • the conductive pattern on the flexible substrate obtained by the above method still maintains good conductivity under the bending condition after thermal sintering, and the resistivity is 18-27 ⁇ cm.
  • Step 1 Prepare the copper source precursor solution: Weigh 1.6g of copper sulfate (CuSO 4 ) in a round bottom flask, add 100mL of ethylene glycol (EG), and stir to prepare a copper source precursor solution;
  • CuSO 4 copper sulfate
  • EG ethylene glycol
  • Step 2 Add reducing agent and dispersing agent: add 1g of reducing agent sodium hypophosphite monohydrate (NaH 2 PO 2 ⁇ H 2 O) and 2g of dispersing agent polyvinylpyrrolidone to the copper source precursor solution obtained in step 1. (PVP-K30);
  • Step 3 Oil bath treatment: Transfer the round bottom flask containing the copper source precursor solution, reducing agent and dispersant solution obtained in Step 2 to an oil bath, and stir the oil bath at 70°C for 15 min;
  • Step 4 centrifugal washing: the product obtained in step 3 was washed three times with deionized water and three times with absolute ethanol, the centrifuge speed was 6000 rpm, the centrifugation time was 6 min, and then it was dried in a vacuum oven;
  • Step 5 Preparation of silver source precursor: Weigh 0.85g of silver nitrate (AgNO 3 ) in a beaker, add 50mL of ethylene glycol, magnetically stir to a clear solution, and prepare a silver source precursor solution;
  • Step 6 oil bath treatment: place the product obtained in step 4 in a round bottom flask, add 50 mL of ethylene glycol, vigorously stir at 70°C, and then drop the silver source precursor solution in step 5 in 5 minutes at 70 Carry out the reaction in an oil bath at °C for 15 min;
  • Step 7 centrifugal drying: the product obtained in step 6 was washed three times with deionized water and three times with absolute ethanol, the centrifuge speed was 6000 rpm, the centrifugation time was 6 min, and then it was dried in a vacuum oven to obtain the core-shell structure Ag@Cu Nanoparticles.
  • the morphology of the core-shell structure Ag@Cu nanoparticles prepared in Example 1 was analyzed.
  • the scanning electron microscope (SEM) image is shown in FIG.
  • the core-shell structure Ag@Cu nanoparticles prepared in Example 1 were subjected to energy spectrum analysis. As shown in FIG. 2, it can be clearly seen that there are only peaks of silver and copper in the nanoparticles, indicating that the prepared nanoparticles are almost There are no remaining impurity elements.
  • the core-shell structure Ag@Cu nanoparticles prepared in Example 1 were subjected to X-ray diffraction analysis. As shown in FIG. 3, the prepared nanoparticles were indeed silver-copper alloys.
  • the application of the core-shell structure Ag@Cu nanoparticle conductive ink in flexible printing includes the following steps:
  • Step 1 Substrate cleaning: PET is used as a flexible substrate, and ultrasonic cleaning is performed in acetone, absolute ethanol, and deionized water respectively for 30 minutes to remove impurities on the surface. After washing, it is naturally dried, and after 15 minutes and 2 minutes of plasma treatment, it is ready for use ;
  • Step 2 Prepare the ink: mix the core-shell structure Ag@Cu nanoparticles obtained in Example 1 with deionized water, ethylene glycol and glycerin at a mass ratio of 2:8:1:1 and ultrasonic for 20 min;
  • Step 3 Printing ink: Inkjet printing the ink prepared in Step 2 on the flexible substrate processed in Step 1, to obtain a flexible substrate with a conductive pattern attached;
  • Step 10 Sintering process: Place the flexible substrate with conductive patterns on it in a vacuum oven for thermal sintering.
  • the thermal sintering temperature is 150°C and the sintering time is 60 minutes.
  • Example 2 was tested for contact angle. As shown in FIG. 5, after 15 minutes of plasma treatment, the contact angle of the ink with the substrate was 48°, and after 2 minutes of plasma treatment, the contact angle of the ink with the substrate was 100°. The degree of wetting of the ink and the base has a certain influence on the fineness of the circuit after subsequent sintering.
  • the bending test of Example 2 shows that the conductive pattern will not fall off under bending and has good adhesion to the substrate, as shown in FIG. 6. And it can still light the small light bulb even when it is bent, as shown in Figure 6, which shows good conductivity and application value.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

La présente invention concerne une encre conductrice à base de nanoparticules d'Ag-Cu à structure cœur-enveloppe. L'encre est formée par dispersion des nanoparticules sphériques dans un liquide, les nanoparticules sphériques étant des nanoparticules d'Ag-Cu formées par revêtement d'un noyau de cuivre avec une enveloppe d'argent, et le liquide étant une solution mixte d'eau désionisée, d'éthylène glycol et de glycérine ; et la teneur en solides des nanoparticules sphériques étant de 10 à 30 % en poids. L'encre conductrice peut être imprimée par jet d'encre sur un substrat souple.
PCT/CN2019/112849 2019-01-08 2019-10-23 Encre conductrice à base de nanoparticules d'ag-cu à structure cœur-enveloppe, son procédé de préparation et son utilisation WO2020143273A1 (fr)

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CN201910015697.2A CN109852146A (zh) 2019-01-08 2019-01-08 一种核壳结构Ag@Cu纳米颗粒导电墨水及其制备方法和用途

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CN114122433A (zh) * 2021-11-12 2022-03-01 北京化工大学 一种银铜锰核壳结构纳米线氧还原催化剂
CN114534721A (zh) * 2022-02-24 2022-05-27 河南科技大学 水相中Au@Pd核壳结构超长纳米线的制备方法及应用
CN114799195A (zh) * 2022-03-10 2022-07-29 昆明理工大学 一种自组装微纳结构Cu-Ag纳米颗粒的制备方法
CN114905038A (zh) * 2022-04-02 2022-08-16 刘勤华 一种纳米多面球体结构银包铜复合粉及其制备方法
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CN109852146A (zh) * 2019-01-08 2019-06-07 南京邮电大学 一种核壳结构Ag@Cu纳米颗粒导电墨水及其制备方法和用途
KR102051321B1 (ko) * 2019-07-15 2019-12-03 파워팩 주식회사 습식공정을 이용한 코어-쉘 구조의 은-구리 혼합분말의 제조 방법
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Publication number Priority date Publication date Assignee Title
CN113523649A (zh) * 2021-07-21 2021-10-22 北京工业大学 一种复合焊膏的制备方法
CN114122433A (zh) * 2021-11-12 2022-03-01 北京化工大学 一种银铜锰核壳结构纳米线氧还原催化剂
CN114122433B (zh) * 2021-11-12 2024-03-26 北京化工大学 一种银铜锰核壳结构纳米线氧还原催化剂
CN114534721A (zh) * 2022-02-24 2022-05-27 河南科技大学 水相中Au@Pd核壳结构超长纳米线的制备方法及应用
CN114534721B (zh) * 2022-02-24 2023-10-17 河南科技大学 水相中Au@Pd核壳结构超长纳米线的制备方法及应用
CN114799195A (zh) * 2022-03-10 2022-07-29 昆明理工大学 一种自组装微纳结构Cu-Ag纳米颗粒的制备方法
CN114905038A (zh) * 2022-04-02 2022-08-16 刘勤华 一种纳米多面球体结构银包铜复合粉及其制备方法
CN114905038B (zh) * 2022-04-02 2024-01-05 刘勤华 一种纳米多面球体结构银包铜复合粉及其制备方法
CN115889768A (zh) * 2023-01-06 2023-04-04 合肥迈微新材料技术有限公司 一种铜@镍核壳结构颗粒的制备方法及其应用

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