CN107163624A - A kind of preparation method of silver-plated nano graphite microchip conductive filler - Google Patents
A kind of preparation method of silver-plated nano graphite microchip conductive filler Download PDFInfo
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- CN107163624A CN107163624A CN201710264888.3A CN201710264888A CN107163624A CN 107163624 A CN107163624 A CN 107163624A CN 201710264888 A CN201710264888 A CN 201710264888A CN 107163624 A CN107163624 A CN 107163624A
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/46—Graphite
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/066—Treatment or coating resulting in a free metal containing surface-region
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention belongs to the technical field of conductive material, and in particular to a kind of preparation method of silver-plated nano graphite microchip conductive filler.Crystalline flake graphite is first carried out oxidation processes by the present invention with potassium permanganate, washing carries out high-temperature calcination after drying, expanded graphite is made, expanded graphite is mixed with petroleum ether again, in under condition of high voltage, oil ether fume is set to enter in expanded graphite hole, again through moment pressure release, the petroleum liquid ether in hole is set to be converted into oil ether fume, form graphite nanosheets, again using acetaldehyde as reducing agent, reduction is deposited on graphite microchip surface and produces silver, final vacuum dried rear obtained silver-plated nano graphite microchip conductive filler.Super-large diameter and thickness ratio that the present invention possesses using graphite nanosheets, it is allowed to as filler, simultaneously in graphite nanosheets electroplate, improve product electric conductivity, reduce filler loading, efficiently solve conventional graphite conductive filler amount big, the problem of causing extrudate density height, mechanical properties decrease.
Description
Technical field
The invention belongs to the technical field of conductive material, and in particular to a kind of system of silver-plated nano graphite microchip conductive filler
Preparation Method.
Background technology
Conducting resinl refers to the special adhesive with certain electric conductivity, mainly by adding in organic polymer matrix
Enter the solidification such as curing agent, conductive filler and other additives and obtain, and with the electric conductivity close with metal.By conducting resinl
The species of middle conducting particles is different, can be divided into gold, silver, copper and carbon series conductive glue.
Graphite not only has natural electric conductivity, and has stable performance, good acid-fast alkali-proof and dispersiveness etc. concurrently
Advantage, is the excellent material for preparing conducting resinl.Graphite resource is abundant, with low cost, for metallic conductive fillers, graphite
With absolute price advantage, so, graphite conductive adhesive has a good application prospect.But, native graphite is generally with micron
Level scaly powder form is present, and directly using it as conductive filler, loading is larger, and the density of product is high, poor mechanical property, because
This, the application in terms of many conducting resinl products is restricted.
It is big that nano material is in meso-scale, specific surface area.It is the quantum confinement effect brought therefrom, skin effect, small
Dimensional effect, macro quanta tunnel effect make the physicochemical property that it possesses uniqueness.The characteristics of using nano material, leads to improve
The properties of electric glue, the conductive filler of modified tradition crystalline flake graphite into nanoscale is introduced in conducting resinl composite system
Central, related research has been increasingly becoming one of the new focus in conducting resinl field.
The content of the invention
The technical problems to be solved by the invention are：Directly added with natural flake graphite for conventional graphite conductive filler
Plus, loading is larger, and the problem of causing extrudate density height, mechanical properties decrease leads there is provided a kind of silver-plated nano graphite microchip
The preparation method of electric filler.
In order to solve the above technical problems, the present invention uses technical scheme as described below：
（1）Expanded graphite is made after being expanded after crystalline flake graphite is aoxidized, by moment pressure release after expanded graphite and petroleum ether pressurize, then
Graphite nanosheets are made through cooling, filtering and after drying；
（2）Silver ammino solution is mixed with graphite nanosheets, using acetaldehyde as reducing agent, it is reacted after be filtered, washed and dried, i.e.,
Obtain silver-plated nano graphite microchip conductive filler.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention make crystalline flake graphite expand after, under condition of high voltage, make oil ether fume enter expanded graphite hole in, and
Petroleum liquid ether is condensed into hole, then through moment pressure release, the petroleum liquid ether Transient transformation in hole is steamed for petroleum ether
Gas, and make expanded graphite fragmentation, graphite nanosheets are formed, then using acetaldehyde as reducing agent, in graphite microchip surface reduction deposition
Silver is produced, the electric conductivity of product is further enhanced；
（2）Products obtained therefrom of the present invention is applied in conducting resinl as conductive filler, because of the raising of electric conductivity, and loading is reduced,
The mechanical property of product is improved, and obtained conducting resinl specific insulation is 10-5~10-3Ω cm, shear strength is
180~200MPa, the more conventional conducting resinl of service life extends 2~4 years.
Embodiment
The required raw material of the present invention has：Crystalline flake graphite, 98% sulfuric acid, 65% nitric acid, potassium permanganate, nitrogen, expanded graphite, stone
Oily ether, 2% silver nitrate solution, 2~4% ammoniacal liquor.
Weigh 40~60kg crystalline flake graphites, pour into pallet, then pallet is transferred in vacuum drying chamber, in temperature be 80~
Under the conditions of 90 DEG C, 16~24h is dried, dry crystalline flake graphite is obtained, in polytetrafluoroethyllining lining reactor, sequentially add 20~
30L mass fractions are 98% sulfuric acid, and 10~12L mass fractions are 65% nitric acid, and 1~3kg potassium permanganate, 35~40kg gained is dried
Crystalline flake graphite, is 55~65 DEG C in temperature, rotating speed is under the conditions of 500~600r/min, constant temperature 12~18h of stirring reaction utilizes
Potassium permanganate in acid condition, aoxidizes crystalline flake graphite, question response terminates, by material mistake in polytetrafluoroethyllining lining reactor
Filter, obtains graphite oxide filter cake, and graphite oxide filter cake is washed with deionized until cleaning solution is in neutrality, then by the oxidation after washing
Graphite Cake is transferred in baking oven, Muffle furnace is transferred to after being dried under the conditions of temperature is 105~110 DEG C to constant weight, with 10~15mL/
Min speed is passed through nitrogen into stove, under nitrogen guard mode, persistently overheating to 1000~1100 with 10~15 DEG C/min speed
DEG C, 20~30s is incubated, graphite oxide is expanded through high-temperature calcination, cools to room temperature with the furnace, is discharged, is obtained expanded graphite, weigh 25
~30kg expanded graphites, are poured into the autoclave for filling 50~80L petroleum ethers, mixed with the stirring of 600~800r/min rotating speeds
Close after 20~40min, open reaction kettle heater, make reacting kettle inner pressure up to 1.6~1.8MPa, 30~45s of pressurize, then open
Reactor bottom discharge valve, makes material in reactor be injected into reception kettle, material naturally cools to room in kettle to be received
Temperature, will receive material filtering in kettle, obtains the filter residue containing graphite nanosheets, and the filter residue containing graphite nanosheets is placed in into vacuum
In drying box, dried under the conditions of temperature is 105~110 DEG C to constant weight, using under reactor condition of high voltage, steam petroleum ether
Gas enters in expanded graphite hole, and is condensed into hole petroleum liquid ether, then through moment pressure release, makes the liquid stone in hole
Oily ether Transient transformation is oil ether fume, and makes expanded graphite fragmentation, obtains graphite nanosheets, measures 300~500mL mass point
Number is 2% silver nitrate solution, is poured into three-necked flask, then three-necked flask immigration digital display is tested the speed in constant temperature blender with magnetic force, Yu Wen
Spend for 55~60 DEG C, rotating speed is under the conditions of 500~600r/min, mass fraction, which is added dropwise, into three-necked flask by dropping funel is
2~4% ammoniacal liquor, continue that ammoniacal liquor is added dropwise after precipitation is produced in three-necked flask, untill the precipitation produced is completely dissolved, are formed
Silver ammino solution, then the addition above-mentioned gained graphite nanosheets of 100~150g into three-necked flask, continuation constant temperature stirring mixing 45~
60min, treats that constant temperature stirring mixing terminates, 10~20mL acetaldehyde is added into three-necked flask by dropping funel, using acetaldehyde also
Former silver ammino solution, the silver-colored simple substance of generation is wrapped in graphite nanosheets surface, then by three-necked flask in sonic oscillation instrument, with 40
~45KHz frequency ultrasounds are handled after 10~15s, and three-necked flask is moved into water-bath, quiet under the conditions of temperature is 65~70 DEG C
15~20min is put, then by material filtering in three-necked flask, obtains silver-plated nano graphite microchip filter cake, and plating is washed with deionized
Silver nanoparticle graphite microchip filter cake 3~5 times, then silver-plated nano graphite microchip filter cake is transferred in vacuum drying chamber, it is to avoid silver is by oxygen
Change, dried under the conditions of temperature is 105~110 DEG C to constant weight, obtain silver-plated nano graphite microchip conductive filler.
Example 1
40kg crystalline flake graphites are weighed, are poured into pallet, then pallet is transferred in vacuum drying chamber, under the conditions of temperature is 80 DEG C,
16h is dried, dry crystalline flake graphite is obtained, in polytetrafluoroethyllining lining reactor, 20L mass fractions are sequentially added for 98% sulphur
Acid, 10L mass fractions are 65% nitric acid, and 1kg potassium permanganate, 35kg gained dries crystalline flake graphite, is 55 DEG C in temperature, rotating speed is
Under the conditions of 500r/min, constant temperature stirring reaction 12h, question response terminates, and material filtering in polytetrafluoroethyllining lining reactor is obtained
Graphite oxide filter cake, is washed with deionized graphite oxide filter cake until cleaning solution is in neutrality, then by the graphite oxide after washing
Filter cake is transferred in baking oven, Muffle furnace is transferred to after being dried under the conditions of temperature is 105 DEG C to constant weight, with 10mL/min speed into stove
Nitrogen is passed through, under nitrogen guard mode, with persistently overheating to 1000 DEG C of 10 DEG C/min speed, 20s is incubated, cools to room with the furnace
Temperature, discharging, obtains expanded graphite, weighs 25kg expanded graphites, pour into the autoclave for filling 50L petroleum ethers, with 600r/
After min rotating speeds stirring mixing 20min, reaction kettle heater is opened, reacting kettle inner pressure is reached 1.6MPa, pressurize 30s, then open
Reactor bottom discharge valve, makes material in reactor be injected into reception kettle, material naturally cools to room in kettle to be received
Temperature, will receive material filtering in kettle, obtains the filter residue containing graphite nanosheets, and the filter residue containing graphite nanosheets is placed in into vacuum
In drying box, dried under the conditions of temperature is 105 DEG C to constant weight, then through moment pressure release, make expanded graphite fragmentation, obtain nano-graphite
Microplate, measures 300mL mass fractions for 2% silver nitrate solution, pours into three-necked flask, then three-necked flask immigration digital display is tested the speed
In constant temperature blender with magnetic force, in temperature be 55 DEG C, rotating speed be 500r/min under the conditions of, dripped by dropping funel into three-necked flask
Plus mass fraction is 2% ammoniacal liquor, continue that ammoniacal liquor is added dropwise after precipitation is produced in three-necked flask, until the precipitation produced is completely dissolved
Untill, silver ammino solution is formed, then the above-mentioned gained graphite nanosheets of 100g are added into three-necked flask, continue constant temperature stirring mixing
45min, treats that constant temperature stirring mixing terminates, 10mL acetaldehyde is added into three-necked flask by dropping funel, acetaldehyde reduction silver is utilized
Ammonia solution, the silver-colored simple substance of generation is wrapped in graphite nanosheets surface, then by three-necked flask in sonic oscillation instrument, with 40KHz
After frequency ultrasound processing 10s, three-necked flask is moved into water-bath, 15min is stood under the conditions of temperature is 65 DEG C, then by three mouthfuls
Material filtering in flask, obtains silver-plated nano graphite microchip filter cake, and silver-plated nano graphite microchip filter cake 3 is washed with deionized
It is secondary, then silver-plated nano graphite microchip filter cake is transferred in vacuum drying chamber, dry to constant weight, obtain under the conditions of temperature is 105 DEG C
Silver-plated nano graphite microchip conductive filler.
Example 2
60kg crystalline flake graphites are weighed, are poured into pallet, then pallet is transferred in vacuum drying chamber, under the conditions of temperature is 90 DEG C,
24h is dried, dry crystalline flake graphite is obtained, in polytetrafluoroethyllining lining reactor, 30L mass fractions are sequentially added for 98% sulphur
Acid, 12L mass fractions are 65% nitric acid, and 3kg potassium permanganate, 40kg gained dries crystalline flake graphite, is 65 DEG C in temperature, rotating speed is
Under the conditions of 600r/min, constant temperature stirring reaction 18h, question response terminates, and material filtering in polytetrafluoroethyllining lining reactor is obtained
Graphite oxide filter cake, is washed with deionized graphite oxide filter cake until cleaning solution is in neutrality, then by the graphite oxide after washing
Filter cake is transferred in baking oven, Muffle furnace is transferred to after being dried under the conditions of temperature is 110 DEG C to constant weight, with 15mL/min speed into stove
Nitrogen is passed through, under nitrogen guard mode, with persistently overheating to 1100 DEG C of 15 DEG C/min speed, 30s is incubated, cools to room with the furnace
Temperature, discharging, obtains expanded graphite, weighs 30kg expanded graphites, pour into the autoclave for filling 80L petroleum ethers, with 800r/
After min rotating speeds stirring mixing 40min, reaction kettle heater is opened, reacting kettle inner pressure is reached 1.8MPa, pressurize 45s, then open
Reactor bottom discharge valve, makes material in reactor be injected into reception kettle, material naturally cools to room in kettle to be received
Temperature, will receive material filtering in kettle, obtains the filter residue containing graphite nanosheets, and the filter residue containing graphite nanosheets is placed in into vacuum
In drying box, dried under the conditions of temperature is 110 DEG C to constant weight, then through moment pressure release, make expanded graphite fragmentation, obtain nano-graphite
Microplate, measures 500mL mass fractions for 2% silver nitrate solution, pours into three-necked flask, then three-necked flask immigration digital display is tested the speed
In constant temperature blender with magnetic force, in temperature be 60 DEG C, rotating speed be 600r/min under the conditions of, dripped by dropping funel into three-necked flask
Plus mass fraction is 4% ammoniacal liquor, continue that ammoniacal liquor is added dropwise after precipitation is produced in three-necked flask, until the precipitation produced is completely dissolved
Untill, silver ammino solution is formed, then the above-mentioned gained graphite nanosheets of 150g are added into three-necked flask, continue constant temperature stirring mixing
60min, treats that constant temperature stirring mixing terminates, 20mL acetaldehyde is added into three-necked flask by dropping funel, acetaldehyde reduction silver is utilized
Ammonia solution, the silver-colored simple substance of generation is wrapped in graphite nanosheets surface, then by three-necked flask in sonic oscillation instrument, with 45KHz
After frequency ultrasound processing 15s, three-necked flask is moved into water-bath, 20min is stood under the conditions of temperature is 70 DEG C, then by three mouthfuls
Material filtering in flask, obtains silver-plated nano graphite microchip filter cake, and silver-plated nano graphite microchip filter cake 5 is washed with deionized
It is secondary, then silver-plated nano graphite microchip filter cake is transferred in vacuum drying chamber, dry to constant weight, obtain under the conditions of temperature is 110 DEG C
Silver-plated nano graphite microchip conductive filler.
Example 3
50kg crystalline flake graphites are weighed, are poured into pallet, then pallet is transferred in vacuum drying chamber, under the conditions of temperature is 85 DEG C,
20h is dried, dry crystalline flake graphite is obtained, in polytetrafluoroethyllining lining reactor, 25L mass fractions are sequentially added for 98% sulphur
Acid, 11L mass fractions are 65% nitric acid, and 2kg potassium permanganate, 38kg gained dries crystalline flake graphite, is 60 DEG C in temperature, rotating speed is
Under the conditions of 550r/min, constant temperature stirring reaction 15h, question response terminates, and material filtering in polytetrafluoroethyllining lining reactor is obtained
Graphite oxide filter cake, is washed with deionized graphite oxide filter cake until cleaning solution is in neutrality, then by the graphite oxide after washing
Filter cake is transferred in baking oven, Muffle furnace is transferred to after being dried under the conditions of temperature is 108 DEG C to constant weight, with 13mL/min speed into stove
Nitrogen is passed through, under nitrogen guard mode, with persistently overheating to 1050 DEG C of 13 DEG C/min speed, 25s is incubated, cools to room with the furnace
Temperature, discharging, obtains expanded graphite, weighs 28kg expanded graphites, pour into the autoclave for filling 65L petroleum ethers, with 700r/
After min rotating speeds stirring mixing 30min, reaction kettle heater is opened, reacting kettle inner pressure is reached 1.7MPa, pressurize 37s, then open
Reactor bottom discharge valve, makes material in reactor be injected into reception kettle, material naturally cools to room in kettle to be received
Temperature, will receive material filtering in kettle, obtains the filter residue containing graphite nanosheets, and the filter residue containing graphite nanosheets is placed in into vacuum
In drying box, dried under the conditions of temperature is 108 DEG C to constant weight, then through moment pressure release, make expanded graphite fragmentation, obtain nano-graphite
Microplate, measures 400mL mass fractions for 2% silver nitrate solution, pours into three-necked flask, then three-necked flask immigration digital display is tested the speed
In constant temperature blender with magnetic force, in temperature be 58 DEG C, rotating speed be 550r/min under the conditions of, dripped by dropping funel into three-necked flask
Plus mass fraction is 3% ammoniacal liquor, continue that ammoniacal liquor is added dropwise after precipitation is produced in three-necked flask, until the precipitation produced is completely dissolved
Untill, silver ammino solution is formed, then the above-mentioned gained graphite nanosheets of 125g are added into three-necked flask, continue constant temperature stirring mixing
52min, treats that constant temperature stirring mixing terminates, 15mL acetaldehyde is added into three-necked flask by dropping funel, acetaldehyde reduction silver is utilized
Ammonia solution, the silver-colored simple substance of generation is wrapped in graphite nanosheets surface, then by three-necked flask in sonic oscillation instrument, with 42KHz
After frequency ultrasound processing 13s, three-necked flask is moved into water-bath, 18min is stood under the conditions of temperature is 68 DEG C, then by three mouthfuls
Material filtering in flask, obtains silver-plated nano graphite microchip filter cake, and silver-plated nano graphite microchip filter cake 4 is washed with deionized
It is secondary, then silver-plated nano graphite microchip filter cake is transferred in vacuum drying chamber, dry to constant weight, obtain under the conditions of temperature is 108 DEG C
Silver-plated nano graphite microchip conductive filler.
Claims (5)
1. a kind of preparation method of silver-plated nano graphite microchip conductive filler, it is characterised in that specifically preparation process is：
（1）Expanded graphite is made after being expanded after crystalline flake graphite is aoxidized, by moment pressure release after expanded graphite and petroleum ether pressurize, then
Graphite nanosheets are made through cooling, filtering and after drying；
（2）Silver ammino solution is mixed with graphite nanosheets, using acetaldehyde as reducing agent, it is reacted after be filtered, washed and dried, i.e.,
Obtain silver-plated nano graphite microchip conductive filler.
2. a kind of preparation method of silver-plated nano graphite microchip conductive filler according to claim 1, it is characterised in that：Step
Suddenly（1）The specific oxidation step of described crystalline flake graphite is：40~60kg crystalline flake graphites are weighed, are poured into pallet, then pallet is turned
Enter in vacuum drying chamber, under the conditions of temperature is 80~90 DEG C, dry 16~24h, dry crystalline flake graphite is obtained, then at polytetrafluoroethyl-ne
In alkene liner reactor, 20~30L mass fractions are sequentially added for 98% sulfuric acid, and 10~12L mass fractions are 65% nitric acid, 1~
3kg potassium permanganate, dry crystalline flake graphite obtained by 35~40kg is 55~65 DEG C in temperature, rotating speed is 500~600r/min conditions
Under, it is filtered, washed and dried after 12~18h of constant temperature stirring reaction, produces graphite oxide.
3. a kind of preparation method of silver-plated nano graphite microchip conductive filler according to claim 1, it is characterised in that：Step
Suddenly（1）The specific preparation process of described expanded graphite is：Graphite oxide is transferred to Muffle furnace, with 10~15mL/min speed to stove
Nitrogen is inside passed through, under nitrogen guard mode, with persistently overheating to 1000~1100 DEG C of 10~15 DEG C/min speed, insulation 20~
30s, cools to room temperature with the furnace, discharging, obtains expanded graphite.
4. a kind of preparation method of silver-plated nano graphite microchip conductive filler according to claim 1, it is characterised in that：Step
Suddenly（1）The specific preparation process of described graphite nanosheets is：The above-mentioned gained expanded graphites of 25~30kg are weighed, pours into and fills 50
In the autoclave of~80L petroleum ethers, after 600~800r/min rotating speeds stirring mixing, 20~40min, in reactor internal pressure
Under the conditions of power is 1.6~1.8MPa, 30~45s of pressurize, then open reactor bottom discharge valve sprays material in reactor
Into receiving in kettle, material naturally cools to room temperature in kettle to be received, will receive material filtering in kettle, collects filter residue, and will filter
Slag is placed in vacuum drying chamber, is dried under the conditions of temperature is 105~110 DEG C to constant weight, is obtained graphite nanosheets；Described connects
Kettle is received by pipeline with autoclave bottom discharge valve to be connected.
5. a kind of preparation method of silver-plated nano graphite microchip conductive filler according to claim 1, it is characterised in that step
Suddenly（2）The described specific preparation process of silver-plated nano graphite microchip conductive filler is：
（1）300~500mL mass fractions are measured for 2% silver nitrate solution, are poured into three-necked flask, then three-necked flask is moved into number
In the aobvious constant temperature blender with magnetic force that tests the speed, it is 55~60 DEG C in temperature, under the conditions of rotating speed is 500~600r/min, is leaked by dropping liquid
It is 2~4% ammoniacal liquor to struggle against and mass fraction is added dropwise into three-necked flask, continues that ammoniacal liquor is added dropwise after precipitation is produced in three-necked flask, until
Untill the precipitation of generation is completely dissolved, silver ammino solution, then the addition above-mentioned gained nano-graphites of 100~150g into three-necked flask are obtained
Microplate, continues 45~60min of constant temperature stirring mixing；
（2）Treat that constant temperature stirring mixing terminates, 10~20mL acetaldehyde is added into three-necked flask, then by three-necked flask in sonic oscillation
In instrument, with 40~45KHz frequency ultrasounds handle 10~15s after, by three-necked flask move into water-bath in, in temperature be 65~70 DEG C
Under the conditions of stand 15~20min, then by material filtering in three-necked flask, washing and dry to constant weight, obtain silver-plated nano graphite micro-
Piece conductive filler.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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