CN106180749A - The preparation method of the Graphene of a kind of big L/D ratio nano-silver thread that adulterates and the application in terms of preparing conducting resinl thereof - Google Patents
The preparation method of the Graphene of a kind of big L/D ratio nano-silver thread that adulterates and the application in terms of preparing conducting resinl thereof Download PDFInfo
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- CN106180749A CN106180749A CN201610587418.6A CN201610587418A CN106180749A CN 106180749 A CN106180749 A CN 106180749A CN 201610587418 A CN201610587418 A CN 201610587418A CN 106180749 A CN106180749 A CN 106180749A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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 belongs to the preparation and application field of graphene composite material, particularly to the preparation method of Graphene of a kind of big L/D ratio nano-silver thread that adulterates and application in terms of preparing conducting resinl thereof.First Graphene, silver presoma, curing accelerator are ground in mortar and stir, the mixture stirred is placed in microwave reactor reaction and obtains the Graphene of doping big L/D ratio nano-silver thread；Again the Graphene ultrasonic agitation of epoxy resin, firming agent, defoamer and above-mentioned doping big L/D ratio nano-silver thread uniformly and is solidified, obtain Graphene doping big L/D ratio nano-silver thread conducting resinl.
Description
Technical field
The invention belongs to the preparation and application field of graphene composite material, particularly to one doping big L/D ratio nanometer
The preparation method of the Graphene of silver wire and the application in terms of preparing conducting resinl thereof.
Background technology
Along with the development of electronic science and technology, electronic devices and components present miniaturization, miniaturization and printed circuit board (PCB) and present
High density words and Highgrade integration trend.Conducting resinl is as a kind of multifunctional novel composite, more and more wider by people
General concern, conventional conductive glue is mainly filled conductive glue, with resin material as matrix, relies on interpolation conductive filler to make glue carry
Liquid has electric action.
Metal current nanoparticle, with some material with carbon elements including gold, silver, palladium, platinum etc., such as the hydridization material formed between carbon pipe
Material shows the most excellent characteristic at numerous areas.Graphene compares other material with carbon elements, by SP2Hydbridized carbon atoms forms
Two-dimensional hexagonal honeycomb crystal structure, has bigger specific surface area (2.630m2.g-1), higher Young's modulus
(1.0TPa) and heat conductivity (5000w.m-1.k-1), the P track pi-electron of the most each carbon atom contribution can be put down at crystal
Move freely in face so that Graphene has the electric conductivity of excellence.
Predominantly gold, silver, palladium, the platinum etc. common with the particle of Graphene hydridization, Graphene and nano silver wire hybridization compounding
After there is synergistic enhancing effect, present all lower than independent component nano silver wire or Graphene sheet resistance, and silver wire
Itself having one-dimensional special construction, show the performance of uniqueness in terms of flexibility and electric conductivity, Graphene serves as close limit
Conductor, and silver wire serves as the conductor of long scope.But currently available technology also cannot prepare receiving of big L/D ratio by in-situ method
Rice silver wire and composite thereof.
Summary of the invention
The problem that the present invention is directed to mention in above-mentioned background technology, it is provided that the stone of a kind of big L/D ratio nano-silver thread that adulterates
The preparation method of ink alkene:
Graphene, silver presoma, curing accelerator are ground in mortar and stir, the mixture stirred is put
In microwave reactor, reaction obtains the Graphene of doping big L/D ratio nano-silver thread, and in Graphene, the draw ratio of nano-silver thread is high
Reach 50:1～100:1,
Wherein, the number of plies of Graphene between 1～10, silver presoma be the silver salt such as silver nitrate or silver acetate, Graphene with
The mass ratio of silver presoma is 20:1～10:1,
Curing accelerator is imidazoles accelerator, such as 2-methylimidazole, 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 2-
Isopropylimdazole, 2-undecyl imidazole, 2-heptadecyl imidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole or 2-benzyl
Base-4-methylimidazole etc., curing accelerator is 5:1～2:1 with the mol ratio of silver presoma,
The power setting of microwave reactor is 300～500w, and the response time is 2～5min,
The present invention passes through above-mentioned steps, under conditions of without additional protective agent and reducing agent, first passes through ground and mixed and makes
Silver presoma and curing accelerator form complex, degrade this complex then at microwave situ, and this original position is preparation technology obtain
The silver wire simple substance that structure is the most regular, the most also imparts the length that silver wire is enough, and this is favorably improved this silver wire composite wood
The flexibility of material and electric conductivity,
Meanwhile, above-mentioned original position preparation technology is also obtained the coordination compound of imidazoles, in follow-up solidification, and the coordination compound of imidazoles
May also participate in the solidification of epoxy resin, eliminate routine " conductive filler fabricated in situ washs the most afterwards, remove surface
Have neither part nor lot in the material of reaction " post-processing step, and play quickening thermosetting resin and firming agent reaction rate, reduce solidification
Temperature, shorten hardening time, reduce hardener dose, improve the effect such as the physical and mechanical properties of thermosetting resin, chemical property,
Chemical reaction mechanism is approximately as (as a example by 2-ethyl-4-methylimidazole):
The first step:
Present invention also offers the Graphene of a kind of above-mentioned doping big L/D ratio nano-silver thread in terms of preparing conducting resinl
Application, particularly as follows:
By epoxy resin, firming agent, defoamer and the graphite of the above-mentioned doping big L/D ratio nano-silver thread prepared
Alkene ultrasonic agitation uniformly and solidifies, and obtains Graphene doping big L/D ratio nano-silver thread conducting resinl,
Wherein, the weight ratio of the Graphene of epoxy resin, firming agent, defoamer, doping big L/D ratio nano-silver thread is
100:10～20:0.1～1:5～10,
Epoxy resin is diglycidyl ether type epoxy resin, mainly includes bisphenol A type epoxy resin, bisphenol S type epoxy tree
Fat, bisphenol f type epoxy resin, such as 609, E-06, E-03, E-20, E-12, E-51 or E-44 etc.,
Firming agent be dicyandiamide, adipic dihydrazide, phthalic anhydride, trimellitic anhydride, pyromellitic acid anhydride,
Benzophenone hydroxy acid three acid anhydride, maleic anhydride, 070 anhydride or 647 anhydride etc.,
Defoamer is a kind of modified silicone complex, it is possible to well froth breaking, suds, base material had wetting action, be difficult to
Produce flake, the surface tension bubble factor low, the most broken is disperseed in system, and specially emulsified silicone oil, higher alcohols fatty acid ester are again
Compound, polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxy propanol amidogen ether, polypropylene glycerol aether and polyoxypropylene
Polyoxyethylene glycerol ether, polydimethylsiloxane etc.,
Solidification temperature is 120～150 DEG C, and hardening time is 3～4h.
The beneficial effects of the present invention is:
Electric conductivity that specific surface area that Graphene is bigger and excellent chemical property, adulterated silver wire are good and good
Processability so that Graphene-silver composite material has advantages such as low noise, low resistance, low friction, gives conducting resinl good
Heat conduction, electric conductivity.Doping big L/D ratio silver wire covered by Graphene in the layer structure of Graphene so that silver be difficult to by
Oxidation, electric conductivity and the heat conductivility stability of material are higher；
Use the Graphene doping big L/D ratio nano-silver thread conducting resinl that this in-situ method prepares, compared to traditional system
The method of standby filled conductive glue, solves the post processing problem in conductive filler preparation process and produces during processing
The problem of product loss.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the Graphene of the doping big L/D ratio nano-silver thread prepared by the embodiment of the present invention 3.
Fig. 2 is the XRD figure of the Graphene of the doping big L/D ratio nano-silver thread prepared by the embodiment of the present invention 3.
Detailed description of the invention
Embodiment 1
(1) by Graphene, silver nitrate, curing accelerator 2-undecyl imidazole, (Graphene with the mass ratio of silver nitrate is
20:1；Curing accelerator is 5:1 with the mol ratio of silver nitrate) grind in mortar and stir, the mixture that will stir
It is placed in 300w in microwave reactor and reacts 5min, obtain the Graphene of doping big L/D ratio nano-silver thread；
(2) by the firming agent phthalic anhydride of epoxy resin 609,10 mass parts of 100 mass parts, 0.1 mass parts
The doping big L/D ratio nanometer obtained in the step (1) of defoamer polyoxyethylene polyoxypropylene tetramethylolmethane ether and 5 mass parts
The Graphene thickness complex ultrasonic agitation of silver wire the most also 120 DEG C of solidification 3h, obtain Graphene doping big L/D ratio nanometer silver
Line conducting resinl.
Embodiment 2
(1) by Graphene, silver acetate, curing accelerator 2-phenylimidazole, (Graphene is 15:1 with the mass ratio of silver acetate；
Curing accelerator is 4:1 with the mol ratio of silver acetate) grind in mortar and stir, the mixture stirred is placed in micro-
In ripple reactor, 400w reacts 4min, obtains the Graphene of doping big L/D ratio nano-silver thread；
(2) by the epoxy resin E-06 of 100 mass parts, firming agent Benzophenone hydroxy acid three acid anhydride of 15 mass parts, 0.5 mass parts
Defoamer polyoxyethylene polyoxy propanol amidogen ether and 8 mass parts step (1) in the doping big L/D ratio nano-silver thread that obtains
Graphene thickness complex ultrasonic agitation uniformly and 130 DEG C of solidification 4h, obtain Graphene doping big L/D ratio nano-silver thread and lead
Electricity glue.
Embodiment 3
(1) by Graphene, silver nitrate, curing accelerator 2-phenyl-4-methylimidazole (Graphene and the mass ratio of silver nitrate
For 10:1；Curing accelerator is 2:1 with the mol ratio of silver nitrate) grind in mortar and stir, the mixing that will stir
Thing is placed in microwave reactor 500w and reacts 5min, and (SEM schemes such as accompanying drawing 1 Graphene of the big L/D ratio nano-silver thread that obtains adulterating
Shown in, XRD figure is as shown in Figure 2)；
(2) by the epoxy resin E51 of 100 mass parts, the firming agent phthalic anhydride of 20 mass parts, the disappearing of 1 mass parts
The Graphene of the doping big L/D ratio nano-silver thread obtained in the step (1) of infusion polypropylene glycerol aether and 10 mass parts glues
Thick complex ultrasonic agitation the most also 140 DEG C of solidification 3.5h, obtain Graphene doping big L/D ratio nano-silver thread conducting resinl.
Embodiment 4
(1) by Graphene, silver acetate, curing accelerator 2-ethyl imidazol(e), (Graphene is 10:1 with the mass ratio of silver acetate；
Curing accelerator is 3:1 with the mol ratio of silver acetate) grind in mortar and stir, the mixture stirred is placed in micro-
In ripple reactor, 450w reacts 3min, obtains the Graphene of doping big L/D ratio nano-silver thread；
(2) by the epoxy resin E-44 of 100 mass parts, firming agent 647 anhydride of 20 mass parts, the froth breaking of 0.6 mass parts
The Graphene thickness of the doping big L/D ratio nano-silver thread obtained in the step (1) of agent polydimethylsiloxane and 10 mass parts
Complex ultrasonic agitation the most also 150 DEG C of solidification 4h, obtain Graphene doping big L/D ratio nano-silver thread conducting resinl.
The shear strength of conducting resinl is carried out according to standard ASTM1002-01, first will be used for the Copper base material acetic acid second of test
Ester carries out scouring and deoils, and uncured conducting resinl is applied to need the surface of bonding, is closed up by two panels copper sheet, use metal holder
It is fixed and is placed in curing oven solidification；
The resistivity measurement of conducting resinl is carried out according to standard GB/T 12966-91, by the conductive glue for preparing in one
Length of a film 50mm, wide 20mm glass plate on, be placed in curing oven solidification, after completion of cure, be cooled to room temperature, use four resistance
Instrument carries out sheet resistance test.
The shear strength of conducting resinl that specific embodiment 1～4 prepares, the test result of specific insulation are listed in table 1:
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Specific insulation/Ω cm | 1.2×10-5 | 1.0×10-5 | 0.9×10-5 | 1.3×10-5 |
| Shear strength/Mpa | 26.4 | 27 | 27.5 | 26.5 |
Claims (10)
1. the preparation method of the Graphene of the big L/D ratio nano-silver thread that adulterates, it is characterised in that: described preparation method is,
Graphene, silver presoma, curing accelerator are ground in mortar and stir, the mixture stirred is placed in micro-
In ripple reactor, reaction obtains the Graphene of doping big L/D ratio nano-silver thread.
2. the preparation method of the Graphene of doping big L/D ratio nano-silver thread as claimed in claim 1, it is characterised in that: described
Silver-colored presoma be silver nitrate or silver acetate.
3. the preparation method of the Graphene of doping big L/D ratio nano-silver thread as claimed in claim 1, it is characterised in that: described
Curing accelerator be 2-methylimidazole, 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, 2 isopropyl imidazole, 2-undecyl
Imidazoles, 2-heptadecyl imidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole or 2-benzyl-4-methylimidazole.
4. the preparation method of the Graphene of doping big L/D ratio nano-silver thread as claimed in claim 1, it is characterised in that: solidification
Accelerator is 5:1～2:1 with the mol ratio of silver presoma.
5. the preparation method of the Graphene of doping big L/D ratio nano-silver thread as claimed in claim 1, it is characterised in that: microwave
The power setting of reactor is 300～500w, and the response time is 2～5min.
6. the Graphene of the doping big L/D ratio nano-silver thread that prepared by a method as described in any one of claim 1 to 5 is in system
Application in terms of standby conducting resinl, it is characterised in that:
The graphite of the doping big L/D ratio nano-silver thread that epoxy resin, firming agent, defoamer and described preparation method are obtained
Alkene ultrasonic agitation uniformly and solidifies, and obtains Graphene doping big L/D ratio nano-silver thread conducting resinl.
Apply the most as claimed in claim 6, it is characterised in that: epoxy resin, firming agent, defoamer, doping big L/D ratio are received
Weight ratio between the Graphene of rice silver wire is 100:10～20:0.1～1:5～10.
Apply the most as claimed in claim 6, it is characterised in that: described epoxy resin is 609, E-06, E-03, E-20, E-
12, E-51 or E-44.
Apply the most as claimed in claim 6, it is characterised in that: described firming agent is dicyandiamide, adipic dihydrazide, adjacent benzene
Dicarboxylic acid anhydride, trimellitic anhydride, pyromellitic acid anhydride, Benzophenone hydroxy acid three acid anhydride, maleic anhydride, 070 anhydride or 647
Anhydride.
Apply the most as claimed in claim 6, it is characterised in that: described defoamer is emulsified silicone oil, higher alcohols fatty acid ester
Complex, polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxy propanol amidogen ether, polypropylene glycerol aether, polyoxy third
Alkene polyoxyethylene glycerol ether or polydimethylsiloxane.
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| CN201610587418.6A CN106180749B (en) | 2016-07-23 | 2016-07-23 | It is a kind of doping big L/D ratio nano-silver thread graphene preparation method and its application in terms of preparing conducting resinl |
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| CN111171772A (en) * | 2020-02-24 | 2020-05-19 | 桂林电子科技大学 | Preparation method of epoxy conductive adhesive |
| CN112077328A (en) * | 2019-05-26 | 2020-12-15 | 重庆诺奖二维材料研究院有限公司 | Preparation method of silver nanowires |
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