CN110527468B - Preparation and application of force-induced conductive adhesive based on one-dimensional and two-dimensional materials - Google Patents
Preparation and application of force-induced conductive adhesive based on one-dimensional and two-dimensional materials Download PDFInfo
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- CN110527468B CN110527468B CN201910752700.9A CN201910752700A CN110527468B CN 110527468 B CN110527468 B CN 110527468B CN 201910752700 A CN201910752700 A CN 201910752700A CN 110527468 B CN110527468 B CN 110527468B
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
Abstract
The invention discloses a preparation and application of a force-induced conductive adhesive based on a one-dimensional and two-dimensional material, wherein a liquid metal layer is coated on the surface of the one-dimensional and two-dimensional material to serve as a force-induced response conductive film of a conductive filler to form the force-induced conductive material. The conductive adhesive is applied to (1) force sensing parts of various devices, such as flexible touch screens, intelligent cloth, touch interaction parts of robots and the like. (2) As a conductive adhesive for various circuits.
Description
Technical Field
The invention relates to preparation and application of a force-induced conductive adhesive based on a one-dimensional and two-dimensional material, belonging to the technical field of preparation of force-induced conductive materials.
Background
The force-induced electric response flexible packaging material is widely applied to the fields of biomedical engineering, robots, flexible electronic devices, conductive 3D printing materials and the like. Most conductive flexible materials are conductive from conductive fillers and flexible from adhesives. Under the condition of external force, the flexibility of the adhesive can realize the movement of the internal conductive filler, so that the conductive performance is changed, and the force-induced electric response is realized. The conductivity, size and shape of the conductive filler and the strength and flexibility of the adhesive greatly influence the conductivity and mechanical strength of the force-induced electric response flexible material.
The rising trend of the electronic packaging industry is obvious day by day, and products such as displays, sensors and the like are already in the market from a laboratory, so that the development of a novel easily-processed high-performance force-induced electrical response packaging material has great significance.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of a force-induced conductive packaging material (adhesive) based on a one-dimensional and two-dimensional material. Another object is a method for applying force-induced conductive encapsulating material (glue) based on one-dimensional, two-dimensional materials. The thickness of the liquid metal layer can be controlled by adjusting the proportion of the liquid metal to the one-dimensional and two-dimensional materials, and the conductivity of the conductive material caused by force can be further controlled.
The technical scheme is as follows: the invention relates to a preparation method of a force-induced conductive adhesive based on a one-dimensional and two-dimensional material, which is characterized in that a liquid metal layer is coated on the surface of the one-dimensional and two-dimensional material to serve as a force-induced response conductive film of a conductive filler to form the force-induced conductive material.
The preparation method comprises the following steps of coating a liquid metal layer on the surface of a one-dimensional and two-dimensional material to serve as a force-induced response conductive film of a conductive filler to form a force-induced conductive material: coating the liquid metal on the surface of the substrate of the one-dimensional and two-dimensional material by a mechanical stirring or infiltration mode, namely mixing the conductive filler into the adhesive by a mechanical stirring method, heating and curing at high temperature, chemically initiating, and volatilizing the solvent to coat the liquid metal on the surface of the substrate of the one-dimensional and two-dimensional material.
The mixture of the conductive filler and the adhesive is flatly paved on the surface of one circuit substrate, then the other circuit substrate with an electrode is placed on the mixture, and the upper layer substrate and the lower layer substrate need to be aligned to form a sandwich structure; the upper and lower substrates of the force-induced conductive adhesive are bonded by hot pressing and chemical-induced curing, and the mixture film of the conductive filler and the adhesive has good conductivity between the upper and lower electrodes and is in an insulating state in the horizontal direction.
The liquid metal layer is made of simple substance gallium and eutectic low-melting-point alloy containing indium, zinc, bismuth, cadmium, tin, lead, dysprosium or indium as auxiliary components, and the melting points of the eutectic low-melting-point alloy are lower than 150 ℃.
The one-dimensional and two-dimensional material comprises polymer fibers, inorganic materials and oxide nanowires; the material morphology comprises nanorods, nanotubes, nanowires, nanofibers or nanofilms of different sizes.
The material of the high polymer fiber comprises nylon, polyurethane, polycarbonate, polypropylene and polyethylene; the inorganic material comprises a graphene sheet layer, a carbon nano tube, silicon, a silicon dioxide nano wire, a metal nano wire or a nano sheet; the oxide nanowire material comprises copper oxide, zinc oxide and calcium oxide.
The adhesive consists of a main agent and an auxiliary agent; the main agent of the adhesive comprises:
thermosetting adhesive: epoxy resin adhesives, phenol resin adhesives, unsaturated polyester adhesives, polyurethane adhesives, polyimide adhesives, allyl resin adhesives, alkyd resin adhesives;
thermoplastic adhesive: polyethylene adhesives, polypropylene adhesives, polyvinyl chloride adhesives, acrylic resin adhesives, and polycarbonate adhesives;
modified multi-component adhesive: phenol-epoxy type adhesives, phenol-polyurethane type adhesives, phenol-butadiene-acrylonitrile rubber type adhesives, phenol-polyvinyl acetal type adhesives, epoxy-polyamide type adhesives;
the auxiliary agent of the adhesive is a curing agent, an initiator, a catalyst, an accelerator, a cross-linking agent, a diluent, a plasticizer, a flexibilizer, a thickening agent or a stabilizing agent.
The application of the force-induced conductive adhesive based on the one-dimensional and two-dimensional materials prepared by the method is as follows: the force-induced conductive adhesive is used for force-sensing parts of various devices.
The force sensing component comprises a flexible touch screen, intelligent cloth and a touch interactive component of a robot.
The force sensing component induces the external force of the conductive path of the material of the force sensing component, including pressure, shearing force or bending force, under the action of the external force, the resistance of the material in the direction of the force is sharply reduced, and the circuit is conducted.
The one-dimensional and two-dimensional material matrixes with the liquid metal layers coated on the surfaces are used as conductive fillers to be combined with adhesive raw materials to prepare the force-induced conductive material, and the conductivity of the stressed part of the prepared material can be changed under the action of external force.
Has the advantages that:
compared with the traditional force-induced conductive adhesive containing conductive filler, the invention has the following advantages:
(1) the conductive filler disclosed in the patent is a one-dimensional and two-dimensional material with the surface coated with liquid metal, and the thickness of the liquid metal layer can be controlled by adjusting the proportion of the liquid metal to the one-dimensional and two-dimensional material, so that the conductivity of the conductive material is controlled.
(2) The conductive filler stated in the patent is a particle coated with a liquid metal layer on the surface, wherein the liquid metal layer is a eutectic low-melting-point alloy containing elemental gallium and elements such as indium, zinc, bismuth, cadmium, tin, lead, dysprosium, indium and the like as auxiliary components, the melting points of the eutectic low-melting-point alloy are all lower than 150 ℃, and the eutectic low-melting-point alloy has stronger fluidity compared with the solid conductive filler.
(3) The conductive filler disclosed in the patent is a one-dimensional or two-dimensional material with a liquid metal layer coated on the surface, and the size of a matrix can be controlled by mechanical cutting or chemical corrosion and other modes.
(4) The matrix stated in the patent is materials such as nano-rods, nano-tubes, nano-wires, nano-fibers and nano-sheets, and has good dispersion effect on liquid metal which has high density and is easy to gather, so that the material can not have the condition of conductive filler deposition after processing, and the conductive performance is uniform and stable.
(5) The resistance range of the force-induced conductive film based on the fact that the liquid metal layer is coated on the surface of one-dimensional and two-dimensional materials such as nano rods, nano tubes, nano wires, nano fibers and nano films to serve as conductive fillers is large, and the resistance of the conductive film in the direction of external force can be reduced from tens of mega ohms to less than 1 ohm by increasing the external force.
(6) The electric response of the force-induced conductive film to an external force in the patent is applicable to various forces, such as pressure, shearing force, bending force and the like, and the resistance sharply drops in the force-bearing direction to conduct a circuit.
Drawings
Figure 1 is a polyester fiber that is not coated with a liquid metal layer,
fig. 2 is a polyester fiber coated with a liquid metal layer.
Detailed Description
The invention can be realized by the following technical scheme:
the preparation and application of the force-induced conductive adhesive based on one-dimensional and two-dimensional materials comprise the following steps:
preparing a force-induced conductive material based on a one-dimensional and two-dimensional material surface coated with a liquid metal layer as a conductive filler: dispersing liquid metal in a volatile solvent in an ultrasonic mode, spraying a liquid metal droplet suspension on the surface of a one-dimensional and two-dimensional matrix (the one-dimensional and two-dimensional matrix comprises nanorods, nanotubes, nanowires, nanofibers, nano films and the like with different sizes), or coating the liquid metal on the surface of the one-dimensional and two-dimensional matrix in a mechanical stirring and infiltration mode, mixing a conductive filler coated with the liquid metal on the surface into an adhesive by a mechanical stirring method, heating and curing at high temperature, chemically initiating, volatilizing the solvent and the like to form the material, and storing for later use;
the use method of the force-induced conductive adhesive based on the one-dimensional and two-dimensional material surface coated with the liquid metal layer as the conductive filler comprises the following steps: the force-induced conductive material is arranged on a force sensing part of various devices, such as a flexible touch screen, intelligent cloth, a touch interactive part of a robot and the like, and is connected with a circuit and a data receiver, so that an electric signal generated by an external force can be collected, wherein the external force can comprise pressure, shearing force, bending force and the like. In addition, the mixture of the conductive filler and the adhesive is paved on the surface of the circuit substrate, and the other substrate with the electrode is arranged on the upper layer and the lower layer of the mixture to be aligned to form a sandwich structure. The upper and lower substrates are bonded by thermally pressing, chemically curing, etc. with the thin film having good conductivity between the upper and lower electrodes and being horizontally insulated.
In order to better illustrate the present invention, the following examples are further illustrated, but the present invention is not limited to the following examples.
Example of production Process (taking polyethylene terephthalate fiber as a substrate for conductive Filler)
Step (1) preparing the polyester fiber with the surface coated with the liquid metal layer as the conductive filler of the force-induced conductive film
Coating a certain amount of liquid metal on the polyester fiber in a spraying, mechanical stirring or solvent volatilization mode to obtain a skin-core structure with the polyester fiber as a core and the liquid metal coating as a skin, and storing at room temperature for later use.
Step (2) preparing a mixture of polyester fibers and epoxy resin with the surface coated with a liquid metal layer
And adding a certain amount of polyester fiber with the surface coated with the liquid metal layer into a certain amount of epoxy resin, mechanically stirring to obtain a uniform mixture of the polyester fiber with the surface coated with the liquid metal layer and the epoxy resin, and storing at room temperature for later use.
Step (3) preparing a force-induced conductive film with the polyester fiber surface coated with a liquid metal layer as a conductive filler
And heating and curing the mixture of the polyester fiber and the epoxy resin with the surface coated with the liquid metal layer at high temperature, and cooling to room temperature for later use. The resistance in the z-axis direction can be reduced from 50M Ω to 50M Ω or less as the magnitude of the applied force increases, while all directions perpendicular to the external force are always kept in an insulating state.
Examples of applications (use of a conductive material comprising polyester fibers as a conductive filler, for example)
The method comprises the steps of coating a mixture of polyester fibers coated with liquid metal and an adhesive on the surface of a substrate with an electrode, and then placing the other substrate with the electrode on the mixture (the upper and lower substrates need to be accurately aligned to ensure that the electrodes of the upper and lower substrates can be accurately aligned to ensure the anisotropy of a conductive adhesive), so as to form a sandwich structure. And (5) performing high-temperature curing molding, and cooling to room temperature for later use. And setting the processing temperature according to the glass transition temperature of the adhesive (the temperature is generally higher than the glass transition temperature by 30 ℃), applying pressure perpendicular to the direction of the sample to the sample under the temperature environment, and cooling to return to room temperature under the condition of keeping the pressure to obtain the anisotropic conductive adhesive. At this time, the conductive paste has good conductivity in the direction along the external force, and is kept in an insulating state (on resistance value is lower than 100m Ω) in all directions perpendicular to the external force.
In addition, the force-induced conductive adhesive with different response sensitivity to mechanics can be prepared by combining the adhesive with different mechanical properties, for example, conductive filler and silicon rubber are mixed and heated and pressurized at high temperature for curing, the cured conductive material is soft and elastic, and can be used as a touch sensor of a robot.
Although the present invention has been described in detail in the foregoing general description and specific examples, the present invention can be implemented by taking the values of the upper and lower limits and intervals of the listed raw materials and reaction parameters based on the present invention, and thus, additional details are not described herein.
And (3) performance testing:
and (3) testing tensile property: the test is carried out according to CB/T1040.3-2006, a computer controlled electronic universal tester SANS E42.503 is adopted for testing at room temperature, the stretching speed is 5mm/min, each sample needs to be tested with 5 sample strips, and the results are averaged. Tensile toughness can be obtained by integrating the tensile stress-strain curve.
And (3) testing the compression performance: the test is carried out according to CB/T1040.3-2006, a computer controlled electronic universal tester SANS E42.503 is adopted for testing at room temperature, the compression rate is 1mm/min, each sample needs to be tested by 5 sample strips, and the results are averaged.
Impact strength: and testing by using an impact tester according to GB/T1843-2008, and selecting a simple beam mode, wherein the testing temperature is room temperature.
And (3) hardness performance analysis: the test temperature is room temperature by using a Shore durometer.
Differential scanning calorimeter: the test was carried out using a DSC25TA differential scanning calorimeter. The sample is tested under the protection of nitrogen, the heating rate is 5 ℃/min, and the temperature scanning range is 20-300 ℃.
Dynamic thermomechanical property test: the test is carried out by using a Q800 type dynamic thermodynamic analyzer, the test mode is double cantilevers, the sample size is 80mm multiplied by 10mm multiplied by 4mm, the heating rate is 3 ℃/min, the frequency is 1Hz, and the test temperature range is 0-200 ℃.
Thermogravimetric analysis: and testing by using a TG 209F1 thermogravimetric analyzer, wherein the sample is tested under the protection of nitrogen, the heating rate is 10 ℃/min, and the temperature scanning range is 25-800 ℃.
Characterization by a scanning electron microscope: the surface topography of the fracture surface of the sample in the tensile test can be tested by a FEI Nova Nano SEM450 scanning electron microscope.
And (3) conductivity test: keysight 34461A monitored the resistance over time at room temperature in a two-wire mode. The Number of Power Line Cycles (NPLC) and the measurement range is 0.02 and auto mode, while the measurement option is a resistance of 2W. Wires connect both sides of the rectangular sample to Keysight 34461A. In the above process, all the wires are firmly fixed by the insulating tape.
Claims (7)
1. A preparation method of a force-induced conductive adhesive based on one-dimensional and two-dimensional materials is characterized in that a liquid metal layer is coated on the surface of the one-dimensional and two-dimensional materials to serve as a force-induced response conductive film of conductive fillers, and the force-induced conductive materials are integrally formed; or coating the liquid metal on the surface of the substrate of the one-dimensional and two-dimensional materials in a mechanical stirring or infiltration mode, and coating the liquid metal on the surface of the substrate of the one-dimensional and two-dimensional materials by using a method of high-temperature heating curing, chemical initiation and solvent volatilization to prepare the force-induced conductive material based on the conductive filler which is formed by coating the liquid metal layer on the surface of the one-dimensional and two-dimensional materials; the force-induced conductive material is mixed with an adhesive to prepare the force-induced conductive adhesive; the one-dimensional and two-dimensional material comprises polymer fibers and inorganic materials; the material appearance comprises nano rods, nano tubes, nano wires, nano fibers or nano films with different sizes; the material of the high polymer fiber comprises nylon, polyurethane, polycarbonate, polypropylene and polyethylene; the inorganic material comprises silicon, silicon dioxide nanowires, copper oxide, zinc oxide and calcium oxide.
2. The method for preparing the force-induced conductive adhesive based on the one-dimensional and two-dimensional materials as claimed in claim 1, wherein the mixture of the force-induced conductive material and the adhesive is laid on the surface of a circuit substrate, and then another circuit substrate with an electrode is placed on the mixture, and the upper and lower layers of the circuit substrate need to be aligned to form a sandwich structure; the upper and lower substrates of force-induced conductive material are bonded by hot pressing and chemical-induced curing, and the mixture film of force-induced conductive material and adhesive has good conductivity between the upper and lower electrodes and is in an insulating state in the horizontal direction.
3. The method for preparing the force-induced conductive adhesive based on the one-dimensional and two-dimensional materials as claimed in claim 1 or 2, wherein the liquid metal layer is made of elemental gallium and eutectic low-melting-point alloy containing indium, zinc, bismuth, cadmium, tin, lead and dysprosium, and the melting points of the eutectic low-melting-point alloy are lower than 150 ℃.
4. The method for preparing the force-induced conductive adhesive based on the one-dimensional and two-dimensional materials as claimed in claim 1 or 2, wherein the adhesive is composed of a main agent and an auxiliary agent; the main agent of the adhesive comprises: epoxy resin adhesives, phenol resin adhesives, unsaturated polyester adhesives, polyurethane adhesives, polyimide adhesives, allyl resin adhesives, alkyd resin adhesives; polyethylene adhesives, polypropylene adhesives, polyvinyl chloride adhesives, acrylic resin adhesives, and polycarbonate adhesives; phenol-epoxy type adhesives, phenol-polyurethane type adhesives, phenol-nitrile rubber type adhesives, phenol-polyvinyl acetal type adhesives, epoxy-polyamide type adhesives; the auxiliary agent of the adhesive is a curing agent, an initiator, a catalyst, an accelerator, a cross-linking agent, a diluent, a plasticizer, a flexibilizer, a thickening agent or a stabilizing agent.
5. Use of a force-induced conductive adhesive based on a one-dimensional, two-dimensional material prepared by the method of claim 1 or 2, wherein: the force-induced conductive adhesive is used for force-sensing parts of various devices.
6. Use of a force conducting glue based on one-dimensional, two-dimensional material according to claim 5, characterised in that: the force sensing component comprises a flexible touch screen, intelligent cloth and a touch interactive component of a robot.
7. Use of a force conducting glue based on one-dimensional, two-dimensional material according to claim 5, characterised in that: the force sensing component induces the external force of the conductive path of the material of the force sensing component, including pressure, shearing force or bending force, under the action of the external force, the resistance of the material in the direction of the force is sharply reduced, and the circuit is conducted.
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| CN113235294A (en) * | 2020-11-19 | 2021-08-10 | 嘉兴立一新材料有限公司 | Durable electromagnetic shielding fabric and preparation method thereof |
| CN114752332B (en) * | 2022-04-08 | 2023-07-14 | 宁波曦晗科技有限公司 | Wide-temperature-zone anisotropic conductive adhesive based on liquid metal and preparation method thereof |
| CN115558432A (en) * | 2022-10-14 | 2023-01-03 | 江苏富勤电子材料有限公司 | Directional conductive film based on liquid metal, and preparation and use methods thereof |
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| CN107541072B (en) * | 2017-08-22 | 2019-10-18 | 华南理工大学 | High temperature circulation drawing force causes the silicon rubber composite material and preparation method thereof of electric conductivity enhancing |
| CN108389645B (en) * | 2018-03-02 | 2020-08-18 | 华南理工大学 | Preparation method of liquid metal conductive filler based on liquid-solid two-phase structure |
| CN108447592A (en) * | 2018-03-02 | 2018-08-24 | 华南理工大学 | A kind of stretchable flexibility function conductor and preparation method thereof based on liquid metal |
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| CN109852281B (en) * | 2019-02-01 | 2020-07-28 | 扬州富威尔复合材料有限公司 | Preparation method of anisotropic conductive adhesive based on liquid metal |
| CN110343484B (en) * | 2019-06-21 | 2020-07-10 | 扬州富威尔复合材料有限公司 | Anisotropic conductive adhesive based on particle matrix coated with liquid metal and preparation method |
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