CN109852281B - Preparation method of anisotropic conductive adhesive based on liquid metal - Google Patents
Preparation method of anisotropic conductive adhesive based on liquid metal Download PDFInfo
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- CN109852281B CN109852281B CN201910103418.8A CN201910103418A CN109852281B CN 109852281 B CN109852281 B CN 109852281B CN 201910103418 A CN201910103418 A CN 201910103418A CN 109852281 B CN109852281 B CN 109852281B
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Abstract
The invention discloses a preparation method of anisotropic conductive adhesive based on liquid metal, which is characterized in that the anisotropic conductive adhesive prepared by combining low-melting-point liquid metal and an adhesive is easy to process and form and has good conductive anisotropy and excellent adhesion. The preparation method comprises the following steps: (1) preparing liquid metal anisotropic conductive adhesive: dispersing liquid metal in the adhesive to obtain a mixture of liquid metal particles and the adhesive, removing bubbles, and storing for later use; (2) the use method of the liquid metal anisotropic conductive adhesive comprises the following steps: and coating the mixture of the liquid metal particles and the adhesive, which is subjected to bubble removal, on a substrate, then placing the other substrate on the mixture, and curing and forming to obtain the liquid metal conductive adhesive. The temperature is set according to the glass transition temperature of the conductive adhesive, and the conductive adhesive is applied with force at the temperature and is restored to the room temperature, and at the moment, the conductive adhesive has excellent conductivity along the direction of the force and is in an insulating state in the direction vertical to the force.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of an anisotropic conductive adhesive based on liquid metal.
Background
Anisotropic conductive adhesives (ACAs for short) have a unique conductive anisotropy, i.e., the electrical conductivity (or resistivity) varies in three dimensions (x, y and z). With the advent of the electronic information age, ACAs have been developed because of their combination with the unique advantages of light weight of polymers, easy processing and molding, and excellent electricity of conductive fillers. Physical characteristics such as thermal characteristics are favored, and they are widely used in the fields of package links, electronic components, optical components, displays, and the like. By accurately controlling the distribution of the conductive filler in the adhesive matrix, the conductive and bonding in the z-axis direction is achieved, and good insulation is formed in the x and y directions. When heated and pressed, the conductive particles form a continuous conduction in the z-direction between the die bumps and the substrate pads. The region between the substrate pads, the polymer matrix and the remaining particles act as an insulator to prevent current flow in any other direction.
At present, the anisotropic conductive adhesive consists of a polymer resin matrix, conductive fillers and other auxiliary agents. Bisphenol a epoxy resins are one of the thermoplastic resins widely used in polymer resin matrices. The bisphenol A epoxy resin conductive adhesive has good conductivity but poor mechanical property. On one hand, the bisphenol A epoxy resin is used as the epoxy resin conductive adhesive of the matrix due to the high crosslinking density and rigidity of the bisphenol A epoxy resin, and has the defects of great brittleness, poor flexibility and the like; on the other hand, in order to achieve the expected conductivity, a large amount of traditional conductive fillers such as silver, copper and the like must be filled in the epoxy resin group, which can cause the mechanical property of the cured product to be greatly reduced, and limits the application of the cured product in the fields of flexible electronic appliances, aerospace and the like. The development of a novel high-performance anisotropic conductive adhesive for replacing the traditional bisphenol A epoxy resin conductive adhesive is significant in the electronic packaging industry.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of an anisotropic conductive adhesive based on liquid metal, in particular to a preparation method of an anisotropic conductive adhesive based on liquid metal (simple substance gallium, or alloy containing one or more elements of gallium, bismuth, cadmium, tin, lead, dysprosium and indium, the melting point of the alloy is lower than 100 ℃).
The technical scheme is as follows: the preparation method of the anisotropic conductive adhesive based on the liquid metal comprises the following steps:
step 1, preparing a mixture of liquid metal particles and an adhesive: the used adhesive is divided into a single-component adhesive and a multi-component adhesive, liquid metal is dispersed in the adhesive to obtain a mixture of liquid metal particles and the adhesive, bubbles are removed, and the mixture is stored for later use;
step 2, preparing the liquid metal anisotropic conductive adhesive: coating a mixture of the liquid metal particles and the adhesive, from which bubbles are removed in the step 1, on a substrate, then placing the other substrate on the mixture, and curing and forming to obtain the liquid metal conductive adhesive; and setting the temperature according to the glass transition temperature of the conductive adhesive, applying force to the conductive adhesive at the temperature, and recovering to room temperature, wherein the conductive adhesive has good conductivity along the direction of the force and is in an insulating state perpendicular to the direction of the force, so that the anisotropic conductive adhesive based on the liquid metal is obtained.
Wherein the content of the first and second substances,
the liquid metal is simple substance gallium or an alloy containing one or more elements of gallium, bismuth, cadmium, tin, lead, dysprosium and indium, and the melting point of the liquid metal is lower than 100 ℃.
The substrate is an electrically conductive substrate for an electrical device or apparatus, such as a conventional circuit board or a flexible circuit board.
The kind of the force applied to the conductive paste includes, but is not limited to, a compressive force, a bending force, or a tensile force.
The core component of the adhesive is a high molecular polymer or prepolymer, including but not limited to cyanoacrylate, ethyl acrylate, epoxy acrylate, polyurethane, polyester, polyacrylic acid and esters thereof, polymethacrylic acid and esters thereof, epoxy resin, silicon-containing polymer or polyvinyl alcohol and the like.
The high molecular material in the single-component adhesive is a high molecular polymer or prepolymer, and comprises cyanoacrylate, ethyl acrylate, epoxy acrylate, polyurethanes, polyesters, polyacrylic acids, methacrylic acids, epoxy resins, polyvinyl alcohols, silicon-containing polymers and the like.
The multi-component adhesive is composed of two or more components.
The multi-component adhesive is prepared by selectively combining a plurality of components in a polymer or a prepolymer, a curing agent and a modifier:
classes of adhesive polymer resins include, but are not limited to: epoxy resins, cyanoacrylates, ethacrylates, epoxy acrylates, polyurethanes, polyesters, polyacrylic acid and esters thereof, polymethacrylic acid and esters thereof, polyvinyl alcohols, silicon-containing polymers, and the like;
types of adhesive curing agents include, but are not limited to: a latent epoxy resin curing agent, a catalytic epoxy resin curing agent, a polyetheramine type epoxy resin curing agent, and a radical initiator;
classes of adhesive modifiers include, but are not limited to: polysulfide rubber, polyamide resin, nitrile rubber, phenolic resin, polyester resin and silicone resin.
Has the advantages that: compared with the traditional anisotropic conductive adhesive of low-melting-point metal (the melting point is more than 150 ℃), the melting point of the liquid metal in the invention is lower than 100 ℃.
By controlling the force applied to the conductive adhesive, the conductive adhesive can be conducted in the force direction, the insulation in the direction perpendicular to the force direction is kept, and the magnitude of the on-resistance of the conductive adhesive can be lower than 100m omega.
Compared with the traditional anisotropic conductive adhesive of low-melting-point metal (the melting point is more than 150 ℃), the anisotropic conductive adhesive of liquid metal can be firstly cured, and then force is applied near room temperature to conduct a circuit (under the condition of selecting proper liquid metal); the conducting circuit temperature of the conventional low melting point metal (melting point is more than 150 ℃) anisotropic conductive adhesive operation must be performed at a high temperature (more than 150 ℃), and the curing and conducting circuit must be performed simultaneously.
After the liquid metal conductive adhesive is solidified, the conductive range in the stress direction can be controlled by selecting a proper force and a proper force range, and the effect of selectively conducting a circuit can be achieved.
The liquid metal anisotropic conductive adhesive is applicable to the application range (such as circuit board gluing and the like) of the traditional low-melting-point metal (the melting point is more than 150 ℃) anisotropic conductive adhesive; the conductive adhesive is also suitable for conductive connection between flexible circuits, and the application range of the anisotropic conductive adhesive is expanded.
The liquid metal anisotropic conductive adhesive can conduct a circuit under pressure, and can conduct the circuit in the parallel direction of force under the action of other forces (including but not limited to pulling force, bending force and the like) while keeping insulation in the direction perpendicular to the force.
Detailed Description
The preparation method of the anisotropic conductive adhesive based on the liquid metal can be realized by the following technical scheme:
step (1) preparing liquid metal anisotropic conductive adhesive: the adhesive used in the invention can be divided into single-component adhesive and multi-component adhesive, liquid metal is dispersed in the adhesive (solvent can be used or not) to obtain a mixture of liquid metal particles and the adhesive, bubbles are removed, and the mixture is stored for later use;
the use method of the liquid metal anisotropic conductive adhesive in the step (2) comprises the following steps: the mixture of liquid metal particles and adhesive is applied to a substrate (e.g., a conventional circuit board, a flexible circuit board, etc.) and another substrate is placed on the mixture to form a sandwich structure. And curing and forming to obtain the liquid metal conductive adhesive. The temperature is set according to the glass transition temperature of the conductive adhesive, at which the conductive adhesive is applied with force (including but not limited to pressure, bending force, pulling force, etc.), and the conductive adhesive is cooled to room temperature, and then the conductive adhesive has good conductivity along the direction of the force and is in an insulating state perpendicular to the direction of the pressure.
Examples (multi-component adhesives, in which the multi-component adhesive consists of three components of adhesive A, B, C; the present invention is not limited to the following examples)
Step (1) preparation of a mixture of liquid metal particles and component A (polymer resin) of the adhesive
Adding a certain amount of liquid metal gallium into the component A of the adhesive, dispersing to obtain a mixture of liquid metal particles and the component A of the adhesive, and storing at room temperature for later use.
Step (2) preparing a mixture of liquid metal particles, an adhesive A component (polymer resin), a B component (curing agent) and a C component (modifier)
Adding a certain amount of the component B and the component C of the adhesive into the mixture of the liquid metal particles and the component A of the adhesive, stirring the mixture for 5min at 1000rpm, then removing bubbles for standby by using an ultrasonic cleaner for 30min by ultrasonic cleaning, and storing at low temperature for standby.
Application method of liquid metal anisotropic conductive adhesive in step (3)
Coating the mixture of the bubble-removed metal particles and the adhesive A component, the B component and the C component on a substrate, and then placing another substrate on the mixture to form a sandwich structure. Curing at 80 ℃ for 2h, curing at 120 ℃ for 2h, curing at 150 ℃ for 2h and curing at 180 ℃ for 2h in a forced air drying oven, and cooling to room temperature for later use. And setting the temperature according to the glass transition temperature of the sample (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 liquid metal anisotropic conductive adhesive. The conductive paste has good conductivity in the force direction (resistance value lower than 100m omega) and is in an insulating state perpendicular to the pressure direction.
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.
In the above embodiment, the liquid metal anisotropic conductive adhesive with different properties is obtained by changing the composition and the ratio of the three components of the adhesive A, B, C, and the content of each component is shown in table 1:
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.
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-50-250 ℃.
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 ℃.
And (3) dynamic thermal mechanical property testing, namely testing by using a Q800 type dynamic thermodynamic analyzer in a double-cantilever mode, wherein the size of a sample is 80mm × 10mm × 4mm, the temperature rise rate is 3 ℃/min, the frequency is 1Hz, and the testing temperature range is 0-200 ℃.
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.
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.
Conductivity test Keysight 34461A monitors the resistance over time at room temperature using a two wire mode the number of cycles of the power line (NP L C) and the measurement range is 0.02 and automatic mode, while the measurement option is resistance 2W. wires connect both sides of the rectangular sample to Keysight 34461A. during the above process, all wires are firmly fixed by an insulating tape.
Compared with the traditional anisotropic conductive adhesive of low-melting-point metal (the melting point is more than 150 ℃), the invention has the following advantages:
(1) the liquid metal in the invention is simple substance gallium or alloy containing one or more elements of gallium, bismuth, cadmium, tin, lead, dysprosium and indium, and the melting point of the liquid metal is lower than 100 ℃.
(2) By controlling the force applied to the conductive adhesive, the conductive adhesive can be conducted in the force direction, the insulation in the direction perpendicular to the force direction is kept, and the magnitude of the on-resistance of the conductive adhesive can be lower than 100m omega.
(3) The liquid metal anisotropic conductive adhesive can be cured firstly, and then force is applied near room temperature to conduct a circuit (under the condition of selecting proper liquid metal); the conducting circuit temperature of the conventional low melting point metal (melting point is more than 150 ℃) anisotropic conductive adhesive operation must be performed at a high temperature (more than 150 ℃), and the curing and conducting circuit must be performed simultaneously.
(4) The liquid metal conductive adhesive can select proper force and force range to control the conductive range in the stress direction after being solidified, and the effect of selectively conducting a circuit can be achieved.
(5) The liquid metal anisotropic conductive adhesive is applicable to the application range (such as circuit board gluing and the like) of the traditional low-melting-point metal (the melting point is more than 150 ℃) anisotropic conductive adhesive; the conductive adhesive is also suitable for conductive connection between flexible circuits, and the application range of the anisotropic conductive adhesive is expanded.
(6) The liquid metal anisotropic conductive adhesive can conduct a circuit under pressure, and can conduct the circuit in a direction parallel to a force under the action of other forces (including but not limited to a pulling force, a bending force and the like).
Claims (8)
1. A preparation method of anisotropic conductive adhesive based on liquid metal is characterized by comprising the following steps:
step 1, preparing a mixture of liquid metal particles and an adhesive: the used adhesive is divided into single-component adhesive and multi-component adhesive, liquid metal is dispersed in the adhesive to obtain a mixture of liquid metal particles and the adhesive, bubbles are removed, and the mixture is stored for later use;
step 2, preparing the liquid metal anisotropic conductive adhesive: coating a mixture of the liquid metal particles and the adhesive, from which bubbles are removed in the step 1, on a substrate, then placing the other substrate on the mixture, and curing and forming to obtain the liquid metal conductive adhesive; setting the glass transition temperature of the conductive adhesive to be higher than 30 ℃ of the glass transition temperature, applying force to the conductive adhesive at the temperature, and recovering to room temperature, wherein the conductive adhesive has good conductivity along the direction of force and is in an insulating state perpendicular to the direction of force, so that the anisotropic conductive adhesive based on liquid metal is obtained;
in the step 1, the liquid metal is elemental gallium or an alloy containing one or more elements of gallium, bismuth, cadmium, tin, lead, dysprosium, and indium, the melting point of the liquid metal is lower than 100 ℃, and the volume content of the liquid metal is 30-50%.
2. The method for preparing an anisotropic conductive adhesive based on liquid metal according to claim 1, wherein in the step 2, the substrate is a circuit substrate for electrical equipment.
3. The method for preparing anisotropic conductive adhesive based on liquid metal according to claim 1, wherein in the step 2, the force applied to the conductive adhesive comprises a compressive force, a bending force or a tensile force.
4. The method for preparing anisotropic conductive adhesive based on liquid metal according to claim 1, wherein in step 1, the core component of the adhesive is a high molecular polymer or prepolymer, including but not limited to cyanoacrylate, epoxy acrylate, polyurethane, polyester, polyacrylic, polymethacrylic, epoxy resin, silicon-containing polymer or polyvinyl alcohol.
5. The method for preparing an anisotropic conductive adhesive based on liquid metal according to claim 1, wherein in the step 1, the high molecular material in the single-component adhesive is a high molecular polymer or a prepolymer.
6. The method for preparing an anisotropic conductive adhesive based on liquid metal according to claim 5, wherein the high molecular polymer or prepolymer includes, but is not limited to, cyanoacrylate, epoxy acrylate, polyurethane, polyester, polyacrylic acid and its esters, polymethacrylic acid and its esters, epoxy resin, polyvinyl alcohol, and silicon-containing polymer.
7. The method for preparing an anisotropic conductive adhesive based on liquid metal according to claim 1, wherein in the step 1, the multi-component adhesive is composed of two or more components.
8. The method for preparing anisotropic conductive adhesive according to claim 7, wherein the multi-component adhesive is prepared by selectively combining a polymer or a prepolymer, a curing agent and a modifier, wherein the polymer or the prepolymer comprises:
classes of adhesive polymers or prepolymers include, but are not limited to: epoxy resins, cyanoacrylates, epoxy acrylates, polyurethanes, polyesters, polyacrylics, polymethacrylics, polyvinyl alcohols, silicon-containing polymers;
types of adhesive curing agents include, but are not limited to: a latent epoxy resin curing agent, a catalytic epoxy resin curing agent, a polyetheramine type epoxy resin curing agent, and a radical initiator;
classes of adhesive modifiers include, but are not limited to: polysulfide rubber, polyamide resin, nitrile rubber, phenolic resin, polyester resin and silicone resin.
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| 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 |
| CN110527468B (en) * | 2019-08-15 | 2020-10-16 | 江苏富威尔电子材料科技有限公司 | Preparation and application of force-induced conductive adhesive based on one-dimensional and two-dimensional materials |
| CN114231227A (en) * | 2020-09-09 | 2022-03-25 | 深圳斯巴达光电有限公司 | Epoxy resin composition and production method thereof |
| CN114539946A (en) * | 2022-01-28 | 2022-05-27 | 深圳市世椿运控技术有限公司 | High-heat-conductivity liquid gold sizing method |
| 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 |
| CN116190337B (en) * | 2023-04-23 | 2023-07-14 | 深圳平创半导体有限公司 | Electronic device and method for manufacturing the same |
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| US5328087A (en) * | 1993-03-29 | 1994-07-12 | Microelectronics And Computer Technology Corporation | Thermally and electrically conductive adhesive material and method of bonding with same |
| CN106486183A (en) * | 2015-08-31 | 2017-03-08 | 三星电子株式会社 | Anisotropic conductive material and the electronic installation including it |
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