CN105976893A - Lead-free graphene/nano-silver composite electronic silver paste and preparation method thereof - Google Patents
Lead-free graphene/nano-silver composite electronic silver paste and preparation method thereof Download PDFInfo
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Abstract
The invention discloses lead-free graphene/nano-silver composite electronic silver paste. The lead-free graphene/nano-silver composite electronic silver paste is prepared from the following components in percentage by mass: 55-85 percent of graphene/nano-silver composite powder, 5-40 percent of organic bonding agent and 0.5-20 percent of lead-free glass powder. The graphene/nano-silver composite powder is high-dispersion composite powder obtained through processes of modifying the surface of the nano-silver powder with amino, modifying the surface of the graphene with carboxyl and bonding the graphene with the nano-silver powder in an acid-amine condensation way. In the electronic silver paste, the graphene/nano-silver composite powder is adopted instead of conventional silver powder, so that the solid content of the silver powder is lowered, and the cost is reduced effectively. The lead-free glass powder is used in a preparation process of the silver paste, so that damage to the environment and human body is reduced greatly. The composite electronic silver paste is simple in preparation process and easy to operate, and facilitates industrial production.
Description
Technical field
The present invention relates to the technical field of electronic silver paste, be specifically related to a kind of unleaded graphene/nano silver composite electron silver
Slurry and preparation method thereof.
Background technology
Electric slurry is the key function material producing various electronic component products, and the most about 80% uses silver powder to make
For main functionality phase.From nineteen thirties, the U.S. developed in the first conductive silver slurry, by printing-sintering in ceramic electrical
Container both sides form electrode, since the silver/palladium slurry occurred to the fifties is as resistance application thick film integrated circuit, and so far 70
In the evolution in remaining year, the range of application of slurry constantly extends, and is widely used to Aeronautics and Astronautics, electronic computer, measurement
With fields such as control system, communication equipment, medical equipment, auto industrys, play irreplaceable effect in the electronics industry.
In particular with microelectric technique, Display Technique and surface mounting technique to miniaturization, integrated, intelligent and multifunction side
Face is developed, and electric slurry consumption quickly increases with unprecedented speed especially, there is the biggest development space.
Silver slurry is made up of argentum powder, glass dust, organic carrier three part, and wherein solids content is more than 70wt%.How to reduce
Argentum powder consumption, reduces cost and has become urgent problem.Graphene is a kind of monolayer two-dimensional layer being made up of carbon atom
Structure, has the electric conductivity of excellence, heat conductivity, the advantage of chemical stability.Graphene is combined with silver, makes Graphene/silver multiple
Close powder body and possess the premium properties of each constituent element, play the effect that homogenous material is difficult to play, utilize Graphene to provide for Argent grain
Three-dimensional conductive network and high-strength structure support, and can effectively reduce the consumption of silver, have economy and the functional advantage having both concurrently.
At present, the method that Graphene is compound with argentum powder also has a lot.But major part is all to use simple mechanical blending side
Formula, and then prepare electric slurry, such complex method makes Graphene uniform not with argentum powder doping, affects the property of slurry
Energy.Also having the mode using chemical modification to prepare Graphene/argentum composite powder body, the China such as Publication No. CN103811130A is special
Profit document discloses Graphene composite silver slurry and preparation method thereof, and preparation method is: first prepare silver/graphite alkene complex, then
Preparation silver cladding glass dust, then prepares organic carrier, finally by the silver/graphite alkene complex of above-mentioned acquisition, silver cladding glass
After powder and organic carrier are mixed by proportioning with inorganic additive, obtain Graphene composite silver slurry.Wherein, silver/graphite alkene complex
Preparation use silver reducing process, in silver nitrate solution add Graphene, add the first reducing agent, make graphenic surface deposit
Silver, the most scrubbed, be dried to obtain silver/graphite alkene complex.The and for example Chinese patent literature of Publication No. CN104700961A
In disclose the preparation method of a kind of graphene/silver composite material, be also with silver nitrate solution and graphene aqueous solution as raw material,
After reductant solution reduces, more freeze-dried with hydrogen atmosphere under reduction treatment, obtain Graphene/argentum composite powder.For another example
The Chinese patent literature of Publication No. CN103590089A discloses the preparation method of a kind of graphene/silver composite material, joins
Put graphene dispersing solution, then in graphene dispersing solution, add silver ion salt, use electrophoretic deposition to prepare Graphene/silver and be combined
Material.
Understand, prepared by chemic modified method at present in the method for Graphene/argentum composite powder body, be all former with silver ion salt
Material, then prepare nano silver powder through the mode such as reduction reaction or electrophoretic deposition, this mode complex steps, operation complexity,
It is applicable to research, is unfavorable for large-scale industrial production.
Lead oxide (PbO) can significantly reduce the softening temperature of glass dust, makes argentum powder and substrate obtain good adhesive force, institute
The glass dust containing PbO is used with traditional conductive silver paste majority.However as the development of society, the harm of lead has caused
The extensive concern of people, has the most all formulated a series of relevant law to limit using and discharging of lead.At present,
Electric slurry used on market still uses lead bearing glass powder, does not meets the megatrend of environmental protection, therefore opens
Send out lead-free silver slurry and become the Main way of research.
Summary of the invention
The invention provides a kind of unleaded graphene/nano silver composite electron silver slurry, on the one hand, with graphene/nano silver
Composite granule replaces traditional argentum powder, reduces the solid content of argentum powder, effectively reduces cost；On the other hand, at electronic silver
Slurry preparation process uses lead-free glass powder, greatly reduces the harm to environment and human body.
The invention discloses a kind of unleaded graphene/nano silver composite electron silver slurry, by mass percentage, consist of:
Graphene/nano silver composite granule 55～85%；
Organic bond 5～40%；
Lead-free glass powder 0.5～20%.
As preferably, described graphene/nano silver composite granule is by modifying amino on nanometer silver powder surface, at stone
Carboxyl is modified on ink alkene surface, then by the way of acid-amine condensation, makes Graphene be bonded together with nanometer silver powder, disperseed
Good composite granule.Specifically comprise the following steps that
(1) nanometer silver powder is mixed with deionized water-alcohol solvent, after being uniformly dispersed, add and contain the silane coupled of amino
Agent, after reacting by heating, more scrubbed is dried to obtain modified argentum powder；
The described silane coupler containing amino includes (3-aminopropyl) triethoxysilane, (3-aminopropyl) trimethoxy
Silane or aminopropyltriethoxy dimethoxysilane；
(2) mix dispersed for graphene powder with strong oxidizer again after adding alkaline matter in deionized water, super
After phonoresponse, scrubbed it is dried to obtain modified graphene；
Described graphene powder is 1:10～50 with the mass ratio of alkaline matter；
Described graphene powder is 1:5～20 with the mass ratio of strong oxidizer；
(3) modified argentum powder step (1) prepared and deionized water are mixed to get solution A, modified stone prepared by step (2)
Ink alkene is mixed to get solution B with deionized water, adds condensing agent with solution B, after reaction terminates, through washing after solution A being mixed
Wash, be dried to obtain described graphene/nano silver composite granule；
Described modified argentum powder is 1:0.01～0.2 with the mass ratio of modified graphene.
In step (1):
As preferably, described nanometer silver powder be particle diameter be the spherical powder of 0.4～1.5 μm；
As preferably, described nanometer silver powder is 5～20g/L with the mass volume ratio of deionized water-alcohol solvent；；Enter
One step is preferably 10～15g/L.
As preferably, in described deionized water-alcohol solvent, the volume ratio of deionization water-ethanol is 1:1～5；Enter one
Step is preferably 1:3.
As preferably, described nanometer silver powder is 50～200g/L with the mass volume ratio of the silane coupler containing amino；
More preferably 100～150g/L.
As preferably, the temperature of reacting by heating is 30～60 DEG C, and the time is 2～10h.Further preferably, described reaction
Being heated by water-bath, reaction is carried out under magnetic stirring.
As preferably, reacted product respectively with ethanol, deionized water wash for several times, removes the silicon containing amino of excess
Alkane coupling agent.
In step (2):
As preferably, described graphene powder is 0.5～5g/L with the mass volume ratio of deionized water；
As preferably, described alkaline matter is highly basic, including sodium hydroxide or potassium hydroxide；Further preferably, described
The mass ratio of graphene powder and alkaline matter be 1:20～40.
As preferably, described strong oxidizer is the strong oxidizer containing hypochlorite, including sodium hypochlorite or hypochlorous acid
Potassium；Further preferably, described graphene powder is 1:10～16 with the mass ratio of strong oxidizer.
As preferably, the time of described ultrasonic reaction is 2～10h.Reacted product is respectively through ethanol and deionized water
After washing, remove the strong oxidizer of excess, cation.
In step (3):
As preferably, the concentration of described solution A is 1～20g/L, and the concentration of solution B is 0.1～5g/L, solution A and solution
The volume ratio of B is 1:1～3；
As preferably, described condensing agent includes 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-
The coupling condenser agent of N-Hydroxysuccinimide composition, or be carbodiimide class condensing agent；Cumulative volume with solution A Yu solution B
On the basis of, the consumption of described condensing agent is 0.2～2g/L.
Further preferably, described condensing agent is 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-
The coupling condenser agent of N-Hydroxysuccinimide composition, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxyl
The mass ratio of base butanimide is 1:0.3～5.Further preferably, both mass ratioes are 1:0.5～2.
As preferably, described reaction is under agitation carried out, and the response time is 5～24h.
As preferably, in the graphene/nano silver composite granule prepared, the mass fraction of Graphene is 1～20%.
As preferably, described organic bond includes terpineol, adjacent dibutyl carboxylic acid, diethylene glycol monobutyl ether, second
Base cellulose, Oleum Ricini, Polyethylene Glycol and additive；
By mass percentage, consist of:
The preparation process of described organic bond is as follows:
The each component of precise by mass percentage, under stirring, mixes liquid charging stock, uniformly after, be heated to 70～120
DEG C, add solid material, after mix homogeneously, obtain described organic bond；
Described additive includes surfactant, defoamer, levelling agent, film former, thixotropic agent or coupling agent.
As preferably, need to dissolve 30～60min to mix homogeneously after adding solid material, obtain the organic viscous of homogeneous transparent
Mixture.
Further preferably, by mass percentage, the consisting of of organic bond:
As preferably, described lead-free glass powder includes B2O3、Bi2O3、SiO2、Al2O3, ZnO and V2O5；
By mass percentage, consist of:
The preparation process of described lead-free glass powder is as follows:
The each component of precise by mass percentage, after mix homogeneously at 1000～1400 DEG C melting 0.5～2h, through quenching
Cold, ball milling, sieving obtains described lead-free glass powder.
As preferably, each component is placed in crucible through ball milling mix homogeneously and carries out melting.
Further preferably, by mass percentage, the consisting of of lead-free glass powder:
Further preferably, by mass percentage, what described unleaded graphene/nano silver composite electron silver was starched consists of:
Graphene/nano silver composite granule 70～75%；
Organic bond 20～25%；
Lead-free glass powder 0.5～5%.
The invention also discloses the preparation method of this unleaded graphene/nano silver composite electron silver slurry, by graphene/nanometer
After argentum composite powder body, organic bond and lead-free glass powder mix homogeneously, grind and obtain, after rolling slurry, the electricity that fineness is below 20 μm
Son silver slurry.
As preferably, three-roll grinder is used to be ground.
Compared with prior art, present invention have the advantage that
1. the present invention uses graphene/nano silver composite granule to replace traditional argentum powder, reduces the solid content of argentum powder, has
Imitate reduces cost.
2. in electronic silver paste preparation process, use lead-free glass powder, greatly reduce the harm to environment and human body.
3. the preparation technology of the present invention is simple, it is easy to operation, beneficially industrialized production.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photo of the graphene/nano silver composite granule of embodiment 1 preparation.
Detailed description of the invention
Embodiment 1
1. the preparation of graphene/nano silver composite granule
Graphene/nano silver composite granule is compound uniformly, favorable dispersibility, nanometer silver powder be particle diameter be the Yin Na of 0.4 μm
Rice corpuscles, modified graphene mass fraction is 2%.Preparation process is as follows:
(1) Nano silver grain surface amino groups is modified:
Take Nano silver grain 5g, by its ultrasonic disperse (deionization in the mixed solution of 400mL ethanol and deionized water
The volume ratio of water-ethanol is 1:3), after being uniformly dispersed, add (3-aminopropyl) triethoxysilane reagent of 40mL, at water
At bathing 40 DEG C, magnetic agitation, react 6h.Clean for several times with ethanol, deionized water respectively, more vacuum dried i.e. available modification
Argentum powder.
(2) graphenic surface is carboxy-modified:
Take flake graphite alkene powder body 500mg, by its ultrasonic disperse in 500mL deionized water, after being uniformly dispersed, add
20g sodium hydroxide, after mix homogeneously, adds 8g sodium hypochlorite, continues to keep ultrasonic 4h, is finally respectively washed number with ethanol and water
Secondary, vacuum dried i.e. can get modified graphene.
(3) preparation of graphene/nano silver composite granule:
Take modified argentum powder ultrasonic disperse prepared by 3g step (1) in 1L deionized water, be uniformly dispersed and be designated as solution A.With
Time, taking carboxy-modified Graphene ultrasonic disperse prepared by 60mg step (2) in 2L deionized water, postscript to be uniformly dispersed is molten
Liquid B, after two kinds of solution mix homogeneously, changes magnetic agitation into, is slowly added to 1-ethyl-(3-dimethyl that 0.6g mass ratio is 1:1
Aminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, react 12h with vigorous stirring, reaction spends after terminating
Ionized water cleans for several times, and vacuum drying i.e. can get graphene/nano silver composite granule, modified graphite in the composite granule obtained
Alkene mass fraction is 2%.
2. the preparation of organic bond
By mass percentage, weigh 55% terpineol, the adjacent dibutyl carboxylic acid of 20%, the diethylene glycol list of 10%
Butyl ether, the Oleum Ricini of 3%, the Polyethylene Glycol of 2%, the additive (tributyl phosphate and Span 80, mass ratio is 1:2) of 3%, mixed
After closing uniformly, it is heated at 70 DEG C, is slowly added to the ethyl cellulose of 7%, after dissolving 50min, obtain the organic viscous of homogeneous transparent
Mixture.
3. the preparation of lead-free glass powder
Weigh the B of 30% by mass percentage2O3, the Bi of 45%2O3, the SiO of 10%2, the Al of 5%2O3, the ZnO of 5% and
The V of 5%2O5, it is placed in crucible through ball milling mix homogeneously, melting at 1000 DEG C, melting 2h.The vitreous humour obtained is being gone
Quenching in ionized water, obtains lead-free glass powder by the glass particle obtained through ball milling, 300 mesh sieves excessively.
4. the preparation of composite electron silver slurry
Weigh by mass percentage 75% graphene/nano silver composite granule, the organic bond of 20%, the nothing of 5%
Lead glass powder, after mix homogeneously, grinds with three-roll grinder and roll slurry to obtain fineness being that the silver-colored of below 20 μm is starched.
After testing, the technical specification of the unleaded graphene/nano silver composite electron silver slurry that prepared by the present embodiment is as follows:
(1) viscosity: 40-120PaS；
(2) adhesive force: ＞ 3N/mm2；
(3) sheet resistance: ＜ 10m Ω/c；
(4) appearance property is excellent, and printing adaptability is good.
Embodiment 2
1. the preparation of graphene/nano silver composite granule
Directly use the graphene/nano silver composite granule that Graphene content is 2% of embodiment 1 preparation.
2. the preparation of organic bond
By mass percentage, weigh 55% terpineol, the adjacent dibutyl carboxylic acid of 20%, the diethylene glycol list of 10%
Butyl ether, the Oleum Ricini of 3%, the Polyethylene Glycol of 2%, the additive (tributyl phosphate and Span 80, mass ratio is 1:2) of 3%, mixed
After closing uniformly, it is heated at 80 DEG C, is slowly added to the ethyl cellulose of 7%, dissolve 50min, it is thus achieved that the organic of homogeneous transparent glues
Mixture.
3. the preparation of lead-free glass powder
Weigh the B of 30% in mass ratio2O3, the Bi of 45%2O3, the SiO of 10%2, the Al of 5%2O3, the ZnO of 5%, 5%
V2O5, it is placed in crucible through ball milling mix homogeneously, melting at 1200 DEG C, melting 2h.By the vitreous humour that obtains at deionized water
Middle quenching, obtains required lead-free glass powder by the glass particle obtained through ball milling, 300 mesh sieves excessively.
4. the preparation of composite electron silver slurry
Weigh in mass ratio 73% graphene/nano silver composite granule, the organic bond of 22%, the unleaded glass of 5%
Glass powder, after mix homogeneously, grinds with three-roll grinder and roll slurry to obtain fineness being that the silver-colored of below 20 μm is starched.
Embodiment 3
1. the preparation of Graphene/silver silver powder
Directly use the graphene/nano silver composite granule that Graphene content is 2% of embodiment 1 preparation.
2. the preparation of organic bond
By mass percentage, weigh 55% terpineol, the adjacent dibutyl carboxylic acid of 20%, the diethylene glycol list of 10%
Butyl ether, the Oleum Ricini of 3%, the Polyethylene Glycol of 2%, the additive (tributyl phosphate and Span 80, mass ratio is 1:2) of 3%, mixed
After closing uniformly, it is heated at 100 DEG C, is slowly added to the ethyl cellulose of 7%, is dissolved as 50min, it is thus achieved that homogeneous transparent organic
Binding agent.
3. the preparation of lead-free glass powder
Weigh the B of 30% in mass ratio2O3, the Bi of 45%2O3, the SiO of 10%2, the Al of 5%2O3, the ZnO of 5%, 5%
V2O5, it is placed in crucible through ball milling mix homogeneously, melting at 1400 DEG C, melting 2h.By the vitreous humour that obtains at deionized water
Middle quenching, obtains required lead-free glass powder by the glass particle obtained through ball milling, 300 mesh sieves excessively.
4. the preparation of composite electron silver slurry
Weigh in mass ratio 70% graphene/nano silver composite granule, the organic bond of 25%, the unleaded glass of 5%
Glass powder, after mix homogeneously, grinds with three-roll grinder and roll slurry to obtain fineness being that the silver-colored of below 20 μm is starched.
Claims (10)
1. a unleaded graphene/nano silver composite electron silver slurry, it is characterised in that consist of by mass percentage:
Graphene/nano silver composite granule 55～85%；
Organic bond 5～40%；
Lead-free glass powder 0.5～20%.
Unleaded graphene/nano silver composite electron silver the most according to claim 1 is starched, it is characterised in that described graphite
Alkene/nanometer silver composite granule be by nanometer silver powder surface modify amino, graphenic surface modify carboxyl, then by acid-
The mode of amine condensation, makes Graphene be bonded together with nanometer silver powder, obtains finely disseminated composite granule.
Unleaded graphene/nano silver composite electron silver the most according to claim 2 is starched, it is characterised in that and described Graphene/
The concrete preparation process of nanometer silver composite granule is as follows:
(1) nanometer silver powder is mixed with deionized water-alcohol solvent, after being uniformly dispersed, add the silane coupler containing amino, add
After thermal response, more scrubbed it is dried to obtain modified argentum powder；
The described silane coupler containing amino includes (3-aminopropyl) triethoxysilane, (3-aminopropyl) trimethoxy silane
Or aminopropyltriethoxy dimethoxysilane；
(2) add after alkaline matter by dispersed for graphene powder and mix with strong oxidizer more in deionized water, ultrasonic instead
Ying Hou, scrubbed is dried to obtain modified graphene；
Described graphene powder is 1:10～50 with the mass ratio of alkaline matter；
Described graphene powder is 1:5～20 with the mass ratio of strong oxidizer；
(3) modified argentum powder step (1) prepared and deionized water are mixed to get solution A, modified graphene prepared by step (2)
It is mixed to get solution B with deionized water, after solution A being mixed with solution B, adds condensing agent, after reaction terminates, scrubbed, dry
Dry obtain described graphene/nano silver composite granule；
Described modified argentum powder is 1:0.01～0.2 with the mass ratio of modified graphene.
Unleaded graphene/nano silver composite electron silver the most according to claim 3 is starched, it is characterised in that described nanometer
Argentum powder be particle diameter be the spherical powder of 0.4～1.5 μm；
In described graphene/nano silver composite granule, the mass fraction of Graphene is 1～10%.
Unleaded graphene/nano silver composite electron silver the most according to claim 1 is starched, it is characterised in that described is organic
Binding agent includes terpineol, adjacent dibutyl carboxylic acid, diethylene glycol monobutyl ether, ethyl cellulose, Oleum Ricini, Polyethylene Glycol and adds
Add agent；
By mass percentage, consist of:
Unleaded graphene/nano silver composite electron silver the most according to claim 5 is starched, it is characterised in that described organic viscous
The preparation process of mixture is as follows:
The each component of precise by mass percentage, under stirring, mixes liquid charging stock, uniformly after, be heated to 70～120 DEG C,
Add solid material, after mix homogeneously, obtain described organic bond；
Described additive includes surfactant, defoamer, levelling agent, film former, thixotropic agent or coupling agent.
Unleaded graphene/nano silver composite electron silver the most according to claim 1 is starched, it is characterised in that described is unleaded
Glass dust includes B2O3、Bi2O3、SiO2、Al2O3, ZnO and V2O5；
By mass percentage, consist of:
Unleaded graphene/nano silver composite electron silver the most according to claim 7 is starched, it is characterised in that described unleaded glass
The preparation process of glass powder is as follows:
The each component of precise by mass percentage, after mix homogeneously at 1000～1400 DEG C melting 0.5～2h, through quenching,
Ball milling, sieving obtains described lead-free glass powder.
9. starch according to the unleaded graphene/nano silver composite electron silver described in claim 1～8 any claim, its feature
It is, consists of by mass percentage:
Graphene/nano silver composite granule 70～75%；
Organic bond 20～25%；
Lead-free glass powder 0.5～5%.
10. one kind according to described in claim 1～9 any claim unleaded graphene/nano silver composite electron silver starch
Preparation method, it is characterised in that after graphene/nano silver composite granule, organic bond and lead-free glass powder mix homogeneously,
Grind and obtain, after rolling slurry, the electronic silver paste that fineness is below 20 μm.
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