CN110223798A - A kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles - Google Patents
A kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles Download PDFInfo
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- CN110223798A CN110223798A CN201910595036.1A CN201910595036A CN110223798A CN 110223798 A CN110223798 A CN 110223798A CN 201910595036 A CN201910595036 A CN 201910595036A CN 110223798 A CN110223798 A CN 110223798A
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- 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
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- 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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a kind of preparation methods of " core-shell structure copolymer " structural functionality conducting particles to obtain micro-and nano-particles precursor liquid comprising steps of gallium base liquid metal is carried out thermostatic ultrasonic dispersion under surfactant solution effect by (1)；(2) silver-colored source and reducing agent are added in precursor liquid and carry out heating stirring, obtain " core-shell structure copolymer " structural conductive particle.The initial conductivity and resistance to acid and alkali of gallium base fluid state metal micro-nano particle greatly improved due to the effect of silver-colored shell in " core-shell structure copolymer " structural conductive particle prepared by the present invention；And liquid metal core can overflow the electric conductivity for keeping prepared conducing composite material when being destroyed by external force, with important application prospects in conducing composite material.
Description
Technical field
The present invention relates to conductive material fields, more particularly to a kind of preparation side of " core-shell structure copolymer " structural functionality conducting particles
Method.
Background technique
Conducing composite material is widely used in fields such as printed circuit, flexible electrode, chip testing encapsulation, usually by gathering
It closes object matrix and conductive filler forms.Traditional soft conductive filler with rigid conductor for example graphene, carbon nanotube, conductive black,
Nano silver etc., although the relative maturity in manufacture craft, the electric conductivity of circuit is good, with circuit for material can
Requirement of the deformability as being bent, folding is higher and higher, and traditional rigid conductor is no longer satisfied demand, and low modulus liquid
The research of metal flexible circuit also has certain limitation.Low modulus liquid metal micro-nano granules are in printed circuit processing than it
Block state have can directly print, can be compound etc. advantages.But the material prepared due to oxidation film presence and show
Insulating properties needs further progress machinery to be sintered.
In conclusion preparing one kind " core-shell structure copolymer " structural functionality conductive filler by silver cladding liquid metal watch to solve
The above problem is of great significance in conducing composite material field.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of " core-shell structure copolymer " structural functionality conducting particles
Preparation method.Rigidity, the mobility of electric conductivity and liquid metal of the present invention using silver, are prepared by simple and effective technique
Out it is highly conductive and realize circuit can selfreparing conducting particles.The conducting particles passes through silver-colored shell and assigns initial conductivity and acidproof
Alkalinity realizes that circuit keeps the connection of conductive network under external force destruction by the spilling of liquid metal core.It is led in composite material
Domain is with important application prospects.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles, comprising steps of
(1) gallium base liquid metal is subjected to thermostatic ultrasonic dispersion under surfactant solution effect, obtains the micro-nano grain of rice
Sub- precursor liquid；
(2) silver-colored source and reducing agent are added in precursor liquid and carry out heating stirring, obtain " core-shell structure copolymer " structural conductive particle.
Preferably, the gallium base liquid metal is gallium indium or gallium-indium-tin alloy.
Preferably, the surfactant solution is polyvinylpyrrolidone, neopelex or positive 12
The aqueous solution of alkyl hydrosulfide.
Preferably, the mass ratio of the gallium base liquid metal and surfactant is 2:1~1:5.
Preferably, in the thermostatic ultrasonic dispersion process, thermostat temperature is 15 DEG C, and ultrasonic power is 100W~500W, is surpassed
The sound time is 20~120 minutes.
Preferably, the silver-colored source is the one of which of silver ammino solution, silver acetate solution or silver fluoride solution.
Preferably, the mass ratio of the silver-colored source and gallium base liquid metal is 1:5~5:1.
Preferably, the reducing agent is the one of which in glucose, ascorbic acid or acetaldehyde.
Preferably, the reducing agent dosage and silver-colored source mass ratio are 2:1.
Preferably, during the heating stirring, heating temperature is 25~90 DEG C, and speed of agitator is 200~2000rpm,
The heating stirring time is 15~60 minutes.
Present invention simultaneously provides a kind of " core-shell structure copolymer " structural functionality conducting particles, are prepared by above-mentioned method.
The present invention compared to the prior art, have it is below the utility model has the advantages that
1, " core-shell structure copolymer " structural functionality conducting particles that the present invention is prepared is safe and non-toxic, and resistance can be according to addition
Silver content regulation, modification scope are 0.5 Ω -1k Ω/sq, and can overflow keep conductive network connection under external force, make to make
Standby circuit has certain self-repair function, has in fields such as printed circuit, flexible electrode and chip testing encapsulation wide
Application prospect.
2, simple process of the invention efficiently, material source be easy to get, can be steady compared to pure liquid metal particle acid-fast alkali-proof
It is fixed to save.
Detailed description of the invention
Fig. 1 be in the preparation method of embodiment 1 silver-colored source additive amount to the schematic diagram of particle surface Resistance Influence.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of preparation of " core-shell structure copolymer " structural functionality conducting particles, the specific steps are as follows:
(1) 1.0g liquid metal (gallium: indium=3:2, g/g) is weighed at room temperature in 500mL beaker, while being weighed and being added
Enter 0.5g polyvinylpyrrolidone, adds 100mL deionized water and sufficiently dissolve.Mixed liquor is placed in ultrasound point in Ultrasound Instrument
It dissipates, 15 DEG C of constant temperature, ultrasonic power 100W, the time 120 minutes obtain precursor liquid.
(2) silver ammino solution of 50mL 4.0g/L and 0.4g glucose are added and preparation in (1) is dissolved and be added in beaker
In precursor liquid, is reacted 60 minutes under conditions of 25 DEG C of thermostat temperature, revolving speed 200rpm, " core-is then obtained by centrifuge washing
Shell " structural functionality conducting particles.
Preparing " core-shell structure copolymer " structural functionality conducting particles sheet resistance is 1k Ω/sq.It is as shown in Figure 1 silver in the present embodiment
Schematic diagram of the source additive amount to particle surface Resistance Influence.
Embodiment 2
A kind of preparation of " core-shell structure copolymer " structural functionality conducting particles, the specific steps are as follows:
(1) 1.0g liquid metal (gallium: indium: tin=6:3:1, g/g/g) is weighed at room temperature in 500mL beaker, simultaneously
1.0g neopelex is weighed and be added, 100mL deionized water is added and sufficiently dissolves.Mixed liquor is placed in Ultrasound Instrument
Middle ultrasonic disperse, 15 DEG C of constant temperature, ultrasonic power 200W, the time 40 minutes obtain precursor liquid.
(2) the silver acetate solution of 50mL 20.0g/L and 2.0g acetaldehyde are added in the precursor liquid prepared in (1), in constant temperature
It is reacted 30 minutes under conditions of 90 DEG C of temperature, revolving speed 1000rpm, " core-shell structure copolymer " structural functionality is then obtained by centrifuge washing
Conducting particles.
Preparing " core-shell structure copolymer " structural functionality conducting particles sheet resistance is 200 Ω/sq.
Embodiment 3
A kind of preparation of " core-shell structure copolymer " structural functionality conducting particles, the specific steps are as follows:
(1) 1.0g liquid metal (gallium: indium=7:3, g/g) is weighed at room temperature in 500mL beaker, while being weighed and being added
Enter 5.0g lauryl mercaptan, adds 100mL deionized water and sufficiently dissolve.Mixed liquor is placed in ultrasonic disperse in Ultrasound Instrument,
Obtain precursor liquid for 15 DEG C of constant temperature, ultrasonic power 500W, the time 15 minutes.
(2) the silver fluoride solution of 50mL 50.0g/L and 5.0g ascorbic acid are added in the precursor liquid prepared in (1),
It is reacted 15 minutes under conditions of 60 DEG C of thermostat temperature, revolving speed 2000rpm, " core-shell structure copolymer " structure function is then obtained by centrifuge washing
It can property conducting particles.
Preparing " core-shell structure copolymer " structural functionality conducting particles sheet resistance is 0.5 Ω/sq.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles, which is characterized in that comprising steps of
(1) gallium base liquid metal is subjected to thermostatic ultrasonic dispersion under surfactant solution effect, before obtaining micro-and nano-particles
Drive liquid；
(2) silver-colored source and reducing agent are added in precursor liquid and carry out heating stirring, obtain " core-shell structure copolymer " structural conductive particle.
2. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The gallium base liquid metal is gallium indium or gallium-indium-tin alloy.
3. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The surfactant solution is the water-soluble of polyvinylpyrrolidone, neopelex or n-dodecyl mercaptan
Liquid.
4. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The mass ratio of the gallium base liquid metal and surfactant is 2:1~1:5.
5. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
In the thermostatic ultrasonic dispersion process, thermostat temperature is 15 DEG C, and ultrasonic power is 100W~500W, and ultrasonic time is 20~120
Minute.
6. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The silver source is the one of which of silver ammino solution, silver acetate solution or silver fluoride solution.
7. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The mass ratio of the silver source and gallium base liquid metal is 1:5~5:1.
8. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The reducing agent is the one of which in glucose, ascorbic acid or acetaldehyde.
9. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
The reducing agent dosage and silver-colored source mass ratio are 2:1.
10. the preparation method of one kind " core-shell structure copolymer " structural functionality conducting particles according to claim 1, which is characterized in that
During the heating stirring, heating temperature is 25~90 DEG C, and speed of agitator is 200~2000rpm, and the heating stirring time is 15
~60 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910595036.1A CN110223798A (en) | 2019-07-03 | 2019-07-03 | A kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles |
| PCT/CN2019/111353 WO2021000451A1 (en) | 2019-07-03 | 2019-10-16 | "core-shell" structure functional conductive particle preparation method |
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| CN201910595036.1A CN110223798A (en) | 2019-07-03 | 2019-07-03 | A kind of preparation method of " core-shell structure copolymer " structural functionality conducting particles |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021000451A1 (en) * | 2019-07-03 | 2021-01-07 | 华南理工大学 | "core-shell" structure functional conductive particle preparation method |
| CN114752332A (en) * | 2022-04-08 | 2022-07-15 | 宁波曦晗科技有限公司 | Wide-temperature-range anisotropic conductive adhesive based on liquid metal and preparation method thereof |
| CN115181453A (en) * | 2022-06-24 | 2022-10-14 | 温州大学新材料与产业技术研究院 | Gallium-containing metal conductive ink and preparation method and application thereof |
| CN116313218A (en) * | 2023-02-20 | 2023-06-23 | 北京梦之墨科技有限公司 | Ultralow-temperature-cured wear-resistant conductive paste and preparation method and application thereof |
| CN116435005A (en) * | 2023-03-15 | 2023-07-14 | 深圳先进电子材料国际创新研究院 | Preparation method of conductive metal particles and conductive metal particles |
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| WO2021000451A1 (en) * | 2019-07-03 | 2021-01-07 | 华南理工大学 | "core-shell" structure functional conductive particle preparation method |
| CN114752332A (en) * | 2022-04-08 | 2022-07-15 | 宁波曦晗科技有限公司 | Wide-temperature-range anisotropic conductive adhesive based on liquid metal 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 |
| CN115181453A (en) * | 2022-06-24 | 2022-10-14 | 温州大学新材料与产业技术研究院 | Gallium-containing metal conductive ink and preparation method and application thereof |
| CN116313218A (en) * | 2023-02-20 | 2023-06-23 | 北京梦之墨科技有限公司 | Ultralow-temperature-cured wear-resistant conductive paste and preparation method and application thereof |
| CN116435005A (en) * | 2023-03-15 | 2023-07-14 | 深圳先进电子材料国际创新研究院 | Preparation method of conductive metal particles and conductive metal particles |
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| WO2021000451A1 (en) | 2021-01-07 |
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