CN108711462A - A kind of conductive silver paste without glass powder and preparation method thereof and sintering method - Google Patents
A kind of conductive silver paste without glass powder and preparation method thereof and sintering method Download PDFInfo
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- CN108711462A CN108711462A CN201810516462.7A CN201810516462A CN108711462A CN 108711462 A CN108711462 A CN 108711462A CN 201810516462 A CN201810516462 A CN 201810516462A CN 108711462 A CN108711462 A CN 108711462A
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- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a kind of conductive silver paste without glass powder and preparation method thereof and sintering methods, the conductive silver paste, weight percentage, including mixing silver powder 80wt%~90wt% and organic carrier 10wt%~20wt%, the wherein described combined silver powder includes nano-silver powder, micro-silver powder and nano silver wire, and the organic carrier includes organic solvent, surfactant and thixotropic agent.The conductive silver paste of the present invention is a kind of high performance conductive silver paste, while with low melting point, high bonding strength, high conductivity and thermal conductivity, high solderability, silver-colored separation will not occur, therefore construct and be easy, reliability height, and will not occur to drip glue, hangover and the discontinuous phenomenon of coating.
Description
Technical field
The present invention relates to conductive material technical field more particularly to a kind of conductive silver pastes and its preparation side without glass powder
Method and sintering method.
Background technology
Semiconductor integrated circuit develops towards high density, miniaturization, high-power direction, and circuit level is increasing, work(
Rate is higher and higher, and the calorific value of electronic device steeply rises, caused electric signal, using the problems such as function, service life
As the bottleneck of integrated circuit development is restricted, for the heating problem of power electronic device, the key of solution is dissipating for device
Heat, the heat dissipation performance of especially each chip connecting material.
To meet the performance requirement of high power semiconductor device, generally connected using slug type conductive silver paste, this conduction
Slurry is usually to be made of silver powder, glass powder or oxide, organic carrier, using glass powder or oxide as bonding phase, with silver
Powder is conductive phase, can pass through the mode of (dispense print pattern) by way of spraying without pressure baking or printing
(stencil print pattern) pressure sintering technique is cured, and microstructural dense multicrystalline sintering is formed after solidification
The conductive silver paste of body, it has high-melting-point, high bonding strength, high conductivity and thermal conductivity, high solderability and high reliability etc.
Advantage, especially conductivity and thermal conductivity may even exceed soldering tin product.Particularly, active power thermal cycle is being used
(active power thermal cycle) and passive power thermal cycle (passive power thermal cycle) are tested
When reliability, reliability data value can reach as many as 10 times of scolding tin so that very high it is especially suitable for having to reliability
It is required that high power semiconductor chip device.
The content of the performances such as conductivity, thermal conductivity, adhesive force and the weldability of conductive silver paste and each component, purity, size,
Shape, order of addition, stir speed (S.S.) ratio, curing process suffer from close relationship, the small change of any material or process conditions
Change is likely to so that product is not achieved technology and requires, thus the formula of product and product using technique for the final of product
Performance all no less importants.Silver content in usual silver paste is very high, and galactic pole is susceptible to sedimentation when using, this problem one
Directly hamper its development.The universal problems faced of conductive silver paste currently on the market：Silver detaches (Ag Separation) seriously,
It needs to re-mix before use, even if easily occurring serious phase separation if spraying again during spraying after mixing
Phenomenon.Cause construction (workability) difficult not high with product reliability (reliability).
In addition, in sintering process, due to the problems such as containing air or too low glue viscosity in glue, it may occur that drip glue
Phenomenon；The problems such as too low due to the thixotropic index of glue, it may occur that the phenomenon that hangover；Due to being mixed with air or pin hole quilt in glue
The problems such as provisional blocking, it may occur that be coated with discontinuous phenomenon.Also it is exactly that current conductive silver paste generally all contains glass
Powder, and the heavy metal ion such as lead are usually contained in glass powder, it can cause environmental pollution.
Invention content
The present invention provide one kind can be applied to high-power chip and can with low sintering high-performance conductive silver paste and
Preparation method and sintering method.
According to the first aspect of the invention, the present invention provides a kind of conductive silver paste without glass powder, and percentage by weight contains
Gauge, including mixing silver powder 80wt%~90wt% and organic carrier 10wt%~20wt%, wherein above-mentioned mixing silver powder includes
Nano-silver powder, micro-silver powder and nano silver wire, above-mentioned organic carrier include organic solvent, surfactant and thixotropic agent.
As the preferred embodiment of the present invention, the shape of above-mentioned nano-silver powder is sheet, and grain size is 20~80nm；Above-mentioned micron
The shape of silver powder is sheet, and grain size is 1~4 μm；A diameter of 60nm~80nm of above-mentioned nano silver wire, length are 40~100 μm.
As the preferred embodiment of the present invention, the weight of nano-silver powder, micro-silver powder and nano silver wire in above-mentioned mixing silver powder
Percentage composition is respectively 70~90wt%, 5~15wt% and 5~15wt%.
Scheme as a further improvement on the present invention, above-mentioned organic carrier further include thickener, coupling agent, plasticizer, disappear
Infusion and sintering inhibitor.
As the preferred embodiment of the present invention, weight percentage, above-mentioned organic carrier includes solvent 15%~45%,
Surfactant 10%~60%, thickener 15%~25%, coupling agent 3%~5%, plasticizer 2%~5%, thixotropic agent 1%
~5%, antifoaming agent 0.5%~3%, sintering inhibitor 0.5%~3%.
As the preferred embodiment of the present invention, above-mentioned solvent is selected from terpinol.
As the preferred embodiment of the present invention, the one kind or more of above-mentioned surfactant in polybasic carboxylic acid, polyalcohol, ester
Kind, more preferable oleic acid, dioctyl phthalate, lecithin, dimethylbenzene, octanoic acid, triethanolamine, diethylene glycol ether acetate, diethylene glycol fourth
In ether acetate, polyvinylpyrrolidone, lauryl sodium sulfate, cetyl benzenesulfonic acid sodium, stearic acid and odium stearate
It is one or more.
As the preferred embodiment of the present invention, above-mentioned thickener is selected from Isobutyl methacrylate, ethyl cellulose, ethoxy
Cellulose, methyl hydroxyethylcellulose, ethylhydroxyethylcellulose, methylhydroxypropylcellulose, polyvinyl butyral, ethyl
It is one or more in cellulose.
As the preferred embodiment of the present invention, above-mentioned coupling agent is selected from silane coupling agent, more preferable gamma-aminopropyl-triethoxy
Silane, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-contracting
Water glycerine ether oxygen propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl methyldiethoxysilane, N- β-(aminoethyl)-
γ-aminopropyltriethoxy dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, γ-piperazinopropyl methyl dimethoxy oxygroup
Silane, vinyl three (2- methoxy ethoxies) silane, γ-methacryloxypropyl trimethoxy silane, β-(3,4- rings
Oxygen cyclohexyl) it is one or more in ethyl trimethoxy silane.
As the preferred embodiment of the present invention, above-mentioned plasticizer is selected from dibutyl phthalate.
As the preferred embodiment of the present invention, above-mentioned thixotropic agent is selected from polyamide wax.
As the preferred embodiment of the present invention, above-mentioned antifoaming agent is selected from polyethylene glycol.
As the preferred embodiment of the present invention, above-mentioned sintering inhibitor is selected from resin acid rhodium.
According to the second aspect of the invention, the present invention provides a kind of side preparing conductive silver paste as described in relation to the first aspect
Method, including：By formula ratio, organic solvent, surfactant and thixotropic agent are added in ethanol water bath, is optionally added into thickening
Agent, coupling agent, plasticizer, antifoaming agent and sintering inhibitor, stir evenly to form organic carrier；Then it includes nano silver to be added
The mixing silver powder of powder, micro-silver powder and nano silver wire, is uniformly mixing to obtain above-mentioned conductive silver paste.
As the preferred embodiment of the present invention, above-mentioned ethanol water bath is maintained at 50~80 DEG C, and stir evenly to be formed it is organic
It is kept the temperature at 50~80 DEG C after carrier；Then it cools down and is transferred to 0~5 DEG C and be kept at this temperature the above-mentioned mixing silver powder of addition.
According to the third aspect of the invention we, the present invention provides a kind of sintering using conductive silver paste as described in relation to the first aspect
Method, including：Above-mentioned conductive silver paste is sprayed or is screen printed onto on substrate, is sintered, obtains at 200~300 DEG C after drying
Final products.
As the preferred embodiment of the present invention, above-mentioned drying is 20~60min of progress at 100~150 DEG C.
As the preferred embodiment of the present invention, according to spraying, the time of above-mentioned sintering is 40~80min；According to silk screen
The time of printing, above-mentioned sintering is 60~120s.
The conductive silver paste of the present invention is a kind of high performance conductive silver paste, with high-melting-point, high bonding strength, highly conductive
While rate and thermal conductivity, high solderability, silver-colored separation will not occur, therefore construct and be easy, reliability height, and will not drip
Glue, hangover and the discontinuous phenomenon of coating.
Specific implementation mode
Below by specific implementation mode and further invention is further described in detail in conjunction with the embodiments.
The conductive silver paste of the present invention is known as the conductive silver paste without glass powder, it is a kind of low temperature sintering conductive silver
Slurry, low temperature sintering generally refer to sintering temperature at 200~300 DEG C, preferably 200~250 DEG C.
Influence of the formula of the conductive silver paste of the present invention to its performance is very crucial.One of the key point of the present invention is to mix
It closes silver powder 80wt%~90wt% and organic carrier 10wt%~20wt% mixtures forms conductive silver paste, and mix silver powder and include
Nano-silver powder, micro-silver powder and nano silver wire, above-mentioned organic carrier include organic solvent, surfactant and thixotropic agent.
The mixing silver powder of the present invention is a kind of silver powder of compounding.The different grain size of silver powder can have larger impact to electric conductivity,
Grain size, which crosses conference, causes the contact between particle relatively low, and larger gap is occupied by polymer between particle, influences electric conductivity.Silver
Powder diameter is smaller, and sintering temperature is lower, and resistivity is smaller, and electric conductivity is better, but its smaller specific surface energy of grain size is bigger, holds
Particle aggregation easily occurs, is not easy to disperse.Nano silver wire has big L/D ratio, and effect is greatly facilitated for anti-settling and conduction.
The compounding of silver powder makes the resistivity smaller of sintered conductive silver paste, conductive capability more preferable.
From the purpose for realizing more dominance energy, the preferably shape of nano-silver powder is sheet, and grain size is 20~80nm；Micron
The shape of silver powder is sheet, and grain size is 1~4 μm；A diameter of 60nm~80nm of nano silver wire, length are 40~100 μm.This
Outside, the grain size of micro-silver powder and nano-silver powder is than preferably 40~60.
Relative to other shapes of silver powder, flake silver powder has smaller resistivity, and conductive effect is more preferable after solidification.As for silver
The grain size of powder, grain size is too small to be easy to happen reunion, and grain size increases, and the temperature of sintering can increase, while grain size is excessive or too small
It will influence sintered resistivity.The grain size of micro-silver powder and nano-silver powder ratio there is also an optimum range, i.e., 40~60,
The conductivity of product after solidification may be influenced beyond the range.
It should be noted that in the case where the shape of nano-silver powder and micro-silver powder is sheet, " grain size " refers to it
The length of long radial direction.
Mix performance boost of the rational proportion of nano-silver powder, micro-silver powder and nano silver wire in silver powder for conductive silver paste
There is significant impact.From the purpose for realizing more dominance energy, nano-silver powder, micro-silver powder and silver nanoparticle in silver powder are preferably mixed
The weight percentage of line is respectively 70~90wt%, 5~15wt% and 5~15wt%.In above-mentioned weight percent ranges
Under ratio situation, product conducts electricity very well after solidification.In the most preferred embodiment of the present invention, silver powder is mixed
The weight percentage of middle nano-silver powder, micro-silver powder and nano silver wire is respectively 80wt%, 10wt% and 10wt%.
Although the present invention is not particularly limited the preparation process of nano-silver powder, micro-silver powder and nano silver wire, in order to
The explicit purpose of specification, the present invention provide the technique for preparing above-mentioned nano-silver powder, micro-silver powder and nano silver wire.It should
Understanding, the technique for preparing above-mentioned nano-silver powder, micro-silver powder and nano silver wire provided in the present invention is merely exemplary,
Do not constitute limiting the scope of the invention.
The preparation example of nano-silver powder：
By the PVP of 0.2mol/L, (Polyvinyl pyrrolidone, povidone, chemical name are polyvinylpyrrolidine
Ketone, dosage PVP/AgNO3=0.9 (mass ratio)) it dissolves in deionized water, HNO is added3PH to 2~3 is adjusted, is then added
The AgNO of a concentration of 0.1mol/L3With 2,3 dihydroxybutanedioic acid (the dosage 1mol of 1.8.mol/L：2mol), with 1200r/
Min speed stirs 40min, obtains the precipitation dispersion liquid of white, and precipitation dispersion liquid, which is placed in drying in vacuum environment, removes dispersion
Then liquid pours into dry sediment in the stainless steel pressure kettle with tetrafluoroethene liner, with tubular type heating mantle heats pressure
Kettle is to 120 DEG C, and reaction was completed after 15h, stops heating, takes out reaction kettle, makes its cooled to room temperature.Under vacuum,
60min is centrifuged with the rotating speed of 1500r/min, is washed out, filters, drying organics removal, 4~5 times repeatedly, being eventually adding steaming
Distilled water obtains the aqueous solution of flaky nanometer silver powder.20~80nm of silver powder grain size.Shape is sheet.
The preparation example of micro-silver powder：
By PVP (the dosage PVP/AgNO of 0.2mol/L3=0.2) in deionized water, HNO is added in dissolving3Adjust pH to
5~6, the AgNO of a concentration of 0.9mol/L is then added3With 2,3 dihydroxybutanedioic acid (the dosage 1mol of 1.8.mol/L：
2mol), 40min is stirred with 1200r/min speed, obtains the precipitation dispersion liquid of white, precipitation dispersion liquid is placed in vacuum environment
Dispersion liquid is removed in middle drying, then pours into the stainless steel pressure kettle with tetrafluoroethene liner dry sediment, uses tubular type
Heating mantle heats autoclave pressure is to 100 DEG C, and reaction was completed after 15h, stops heating, takes out reaction kettle, makes its cooled to room temperature.
Under vacuum, 60min is centrifuged with the rotating speed of 1500r/min, is washed out, filters, dries organics removal, repeatedly 4~5
It is secondary, it is eventually adding distilled water and obtains the aqueous solution of flake micron silver powder.1~4 μm of silver powder grain size.Micro-silver powder and nano-silver powder
Grain size ratio is 40~60, and shape is sheet.
The preparation example of nano silver wire：
Polyvinyl butyral 0.05g is added to PVP (the dosage PVP/AgNO of a concentration of 0.2mol/L of 20ml3=
0.9) in solution, 10min is stirred, by the AgNO of 0.1mol/L3Solution is instilled with the speed of 1mL per minute, after stirring 10min
Solution is poured into the stainless steel pressure kettle with tetrafluoroethene liner, with tubular type heating mantle heats autoclave pressure to 150 DEG C, 10h
Reaction was completed afterwards, stops heating, takes out reaction kettle, makes its cooled to room temperature.Under vacuum, products therefrom is spent
Ionized water and absolute ethyl alcohol washing, centrifuge 60min with the rotating speed of 1500r/min, are washed out, filter, dry organics removal,
4~5 times repeatedly, finally dry 4h under the conditions of 60 DEG C, obtains nano silver wire diameter 60nm~80nm, length is at 40~100 μm.
For mixing the preparation of silver powder, The present invention gives a kind of illustrative methods, including：By nano-silver powder, micron
Silver powder, nano silver wire are respectively placed in baking in baking oven (such as 220 DEG C of baking ovens) (such as baking 1h), by nanometer after being cooled to room temperature
Silver powder, micro-silver powder pour into terpinol/polyvinyl butyral solution, are heated up to such as 40 DEG C stirring 10min, are warming up to example
Such as 60 DEG C of stirring 20min, such as 90 DEG C stirring 30min are heated to, filtering rinses 20min with deionized water, then at such as 60 DEG C
1h is toasted, such as 100 DEG C baking 1h are heated up to, then by nano-silver powder, micro-silver powder, nano silver wire by weight proportion (80：
10：10) it mixes, obtains 2.5~5.5g/cm of tap density of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
In the present invention, organic carrier includes organic solvent, surfactant and thixotropic agent.Wherein, the work of surfactant
, can be evenly dispersed in organic carrier with being modified to conducting particles surface, it prevents silver powder from sintering sheet into, reduces silver
Powder fragmentation in spreading process prevents silver powder from making product due to the excessive generation recrystallization of surface energy after flake silver powder forming
Variation ensures stabilization of the silver powder under upper state.
In order to promote the otherwise performance of conductive silver paste, it can further comprise thickener, coupling in organic carrier
Agent, plasticizer, antifoaming agent and sintering inhibitor.
Thickener main function is the rheological equationm of state for changing rheology, and thixotropic fluid either pseudoplastic fluid is made in fluid
Body can adjust the viscosity under senior middle school's low shear rate；Object system viscosity is improved, under the effect of gravity pigment sedimentation speed and viscosity
It is inversely proportional, the big sedimentation of viscosity is slow, and thickener can make object system keep suspended state uniformly, stable or milkiness state.Coupling agent
Effect be, can metal surface formed one layer of organic protective film, play the role of isolating metal in metal surface, raising connects
The stability of electric shock resistance.The effect of plasticizer is, in the case where not changing the chemical property of organic carrier, reduces material forming
Melt viscosity when processing.The effect of antifoaming agent is that foam is inhibited to generate or eliminate the foam generated in whipping process.It burns
The effect for tying inhibitor is to prevent the contraction of the electrode in sintering process, inhibits the increase of contact resistance and the formation of micro-crack,
Improve conductive capability and sintering transforming factor.
From the purpose for realizing more dominance energy, it is preferable that weight percentage, above-mentioned organic carrier include solvent
15%~45%, surfactant 10%~60%, thickener 15%~25%, coupling agent 3%~5%, plasticizer 2%~
5%, thixotropic agent 1%~5%, antifoaming agent 0.5%~3%, sintering inhibitor 0.5%~3%.Said components are in above range
It is interior, enable to mixed conductive silver paste not settle, the electrical property of the product of sintering is best.
In the present invention, organic solvent, surfactant, thixotropic agent, thickener, coupling agent, plasticizer, antifoaming agent and sintering
Inhibitor can be selected from the common used material for be used to prepare conductive silver glue respectively.For example, solvent can be selected from terpinol；Surface
Activating agent can be selected from one or more in polybasic carboxylic acid, polyalcohol, ester, more preferable oleic acid, dioctyl phthalate, lecithin, diformazan
Benzene, octanoic acid, triethanolamine, diethylene glycol ether acetate, butyl acetate, polyvinylpyrrolidone, dodecyl
It is one or more in sodium sulphate, cetyl benzenesulfonic acid sodium, stearic acid and odium stearate；Thickener can be selected from metering system
Sour isobutyl ester, ethyl cellulose, hydroxyethyl cellulose, methyl hydroxyethylcellulose, ethylhydroxyethylcellulose, methylhydroxypropyl
It is one or more in cellulose, polyvinyl butyral, ethyl cellulose；Coupling agent can be selected from silane coupling agent, more excellent
Select gamma-aminopropyl-triethoxy-silane, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, γ-methacryloxy third
Base trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl methyl diethoxy
Base silane, N- β-(aminoethyl)-γ-aminopropyltriethoxies dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, γ-piperazine
Piperazine base hydroxypropyl methyl dimethoxysilane, vinyl three (2- methoxy ethoxies) silane, γ-methacryloxypropyl three
It is one or more in methoxy silane, β-(3,4- epoxycyclohexyls) ethyl trimethoxy silane；Plasticizer can be selected from neighbour
Dibatyl phithalate；Thixotropic agent can be selected from polyamide wax；Antifoaming agent can be selected from polyethylene glycol；Sintering inhibitor can select
From resin acid rhodium.
The present invention also provides the methods for preparing above-mentioned conductive silver paste, including：By formula ratio, it is added in ethanol water bath organic
Solvent, surfactant and thixotropic agent are optionally added into thickener, coupling agent, plasticizer, antifoaming agent and sintering inhibitor, stir
It mixes and is formed uniformly organic carrier；Then addition includes the mixing silver powder of nano-silver powder, micro-silver powder and nano silver wire, is stirred evenly
Obtain above-mentioned conductive silver paste.
As the preferred embodiment of the present invention, above-mentioned ethanol water bath is maintained at 50~80 DEG C, and stir evenly to be formed it is organic
It is kept the temperature at 50~80 DEG C after carrier；Then it cools down and is transferred to 0~5 DEG C and be kept at this temperature the above-mentioned mixing silver powder of addition.
The present invention an embodiment for most preferably preparing above-mentioned conductive silver paste include：First, by ethanol water bath plus
Heat is added organic solvent, surfactant, thixotropic agent, thickener, coupling agent, plasticizer, antifoaming agent and sintering and inhibits to 60 DEG C
Agent stirs evenly to form organic carrier.Then, 1h is kept the temperature at 60 DEG C, then cooled to room temperature, move to the super of 40KHz
In sound oscillator (needing to be put into temperature reducing substance, such as ice cube), 0~5 DEG C of temperature is kept.Finally, mixing silver powder is added, is carried out at the same time
Mechanical agitation is mixed 90~120min, finally takes out and put under vacuum conditions, obtain conductive silver paste.
The present invention also provides a kind of sintering methods using above-mentioned conductive silver paste, including：Above-mentioned conductive silver paste is sprayed or
It is screen printed onto on substrate, is sintered at 200~300 DEG C after drying, obtains final products.
As the preferred embodiment of the present invention, above-mentioned drying is 20~60min of progress at 100~150 DEG C.
As the preferred embodiment of the present invention, according to spraying, the time of above-mentioned sintering is 40~80min；According to silk screen
The time of printing, above-mentioned sintering is 60~120s.
The embodiment of a particularly preferred sintering method of the present invention includes：Using spraying process, by above-mentioned conduction
Silver paste is sprayed on substrate, and 40min is dried at 120 DEG C, and 1h is sintered at 200 DEG C~250 DEG C.More specifically, conductive silver paste is sprayed
It is coated onto on substrate, chip is fixed on above conductive silver paste, 120 DEG C of drying are heated to from room temperature with 10 DEG C/min heating rates
Then 40min is heated to 15 DEG C/min heating rates
200 DEG C~250 DEG C sintering 1h obtain final products.
The embodiment of another particularly preferred sintering method of the present invention includes：It, will be upper using silk-screen printing technique
It states conductive silver paste to be screen printed onto on substrate, 120 DEG C of drying 40min, in 30MPa, 250 DEG C of sintering 90s；Or 120 DEG C of drying
40min, in 10MPa, 250 DEG C of sintering 90s.More specifically, conductive silver paste is printed on by stainless steel cloth on substrate, remove
It is heated to 120 DEG C of drying 40min after silk screen, by die bonding above, under the conditions of 30MPa, is heated to 250 DEG C of sintering 90s and obtains
Product to the end；Or under the conditions of 10MPa, it is heated to 200 DEG C~250 DEG C sintering 90s and obtains final product.
Embodiment 1
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, be slowly added into successively terpinol 40g, octanoic acid 27g,
Polyvinyl butyral 15g, dibutyl phthalate 5g, polyamide wax 5g, polyethylene glycol 2g, gamma-aminopropyl-triethoxy
Silane 3g, resin acid rhodium 3g, mechanical agitation 60min~90min are for use.
Prepare mixing silver powder：Nano-silver powder, micro-silver powder, nano silver wire prepared by above-mentioned example are respectively placed in 220
DEG C baking oven in toast 1h, nano-silver powder, micro-silver powder are poured into terpinol/polyvinyl butyral solution after being cooled to room temperature
In, 40 DEG C of stirring 10min are heated up to, 60 DEG C of stirring 20min are warming up to, are heated to 90 DEG C of stirring 30min, deionization is used in filtering
Water rinses 20min, then 1h is toasted at 60 DEG C, 100 DEG C of baking 1h is heated up to, then by nano-silver powder, micro-silver powder, nano silver wire
By weight proportion (80：10：10) it mixes, obtains the tap density 5.5g/cm of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 20g, mechanical agitation is equal
It is even.60 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 80g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of conductive silver paste is as follows, wherein using Japan MUSASHI dispensing machinery arms SM500DS.
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 1.
Table 1
| Type | Specification |
| The specification of syringe needle | 21 |
| Needle point (spraying starts, terminates) at a distance from base material | 10cm |
| Syringe needle stops height (spraying process) | 5cm |
| The pressure size of air | 100psi |
| Needle/spray away from size | 2mm |
| The rise/fall rate of needle/nozzle | 10m/s |
| Spray rate | 10ms |
| The residence time of nozzle after spraying each time | 2s |
| The glue of nozzle is sucked back into the time in nozzle | 1s |
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 2.
Table 2
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 250 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
200 DEG C~250 DEG C sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in table 3.
Table 3
Embodiment 2
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, be slowly added into successively terpinol 20g, octanoic acid 45g,
Polyvinyl butyral 24g, dibutyl phthalate 2g, polyamide wax 2g, polyethylene glycol 1g, gamma-aminopropyl-triethoxy
Silane 5g, resin acid rhodium 1g, mechanical agitation 60min~90min are for use.
Prepare mixing silver powder：Nano-silver powder, micro-silver powder, nano silver wire prepared by above-mentioned example are respectively placed in 220
DEG C baking oven in toast 1h, nano-silver powder, micro-silver powder are poured into terpinol/polyvinyl butyral solution after being cooled to room temperature
In, 40 DEG C of stirring 10min are heated up to, 60 DEG C of stirring 20min are warming up to, are heated to 90 DEG C of stirring 30min, deionization is used in filtering
Water rinses 20min, then 1h is toasted at 60 DEG C, 100 DEG C of baking 1h is heated up to, then by nano-silver powder, micro-silver powder, nano silver wire
By weight proportion (75：15：10) it mixes, obtains the tap density 5.2g/cm of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 15g, mechanical agitation is equal
It is even.75 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 85g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of conductive silver paste：
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 4.
Table 4
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 5.
Table 5
| Type | Specification |
| The mesh number (mesh/inch) of silk screen | 355S |
| The hardness (Shore A) of rubber flap | 70 (60~80) |
| The width (mm) of rubber flap | 40 |
| The speed (m/s) of scraper plate | 5 |
| The pressure (MPa) of hot pressing | 30 |
| Scrape angle (°) | 20~30 |
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 250 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
200 DEG C~250 DEG C sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in table 6.
Table 6
Embodiment 3
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, is slowly added into terpinol 45g, dioctyl phthalate successively
12g, ethylhydroxyethylcellulose 25g, dibutyl phthalate 5g, polyamide wax 5g, polyethylene glycol 1.5g, 3- (2,3- rings
The third oxygen of oxygen) propyl trimethoxy silicane 5g, resin acid rhodium 1.5g, mechanical agitation 60min~90min be for use.
Prepare mixing silver powder：Nano-silver powder, micro-silver powder, nano silver wire prepared by above-mentioned example are respectively placed in 220
DEG C baking oven in toast 1h, nano-silver powder, micro-silver powder are poured into terpinol/polyvinyl butyral solution after being cooled to room temperature
In, 40 DEG C of stirring 10min are heated up to, 60 DEG C of stirring 20min are warming up to, are heated to 90 DEG C of stirring 30min, deionization is used in filtering
Water rinses 20min, then 1h is toasted at 60 DEG C, 100 DEG C of baking 1h is heated up to, then by nano-silver powder, micro-silver powder, nano silver wire
By weight proportion (85：10：5) it mixes, obtains the tap density 5.5g/cm of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 13g, mechanical agitation is equal
It is even.75 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 87g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of conductive silver paste：
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 7.
Table 7
| Type | Specification |
| The specification of syringe needle | 21 |
| Needle point (spraying starts, terminates) at a distance from base material | 10cm |
| Syringe needle stops height (spraying process) | 5cm |
| The pressure size of air | 100psi |
| Needle/spray away from size | 2mm |
| The rise/fall rate of needle/nozzle | 10m/s |
| Spray rate | 10ms |
| The residence time of nozzle after spraying each time | 2s |
| The glue of nozzle is sucked back into the time in nozzle | 1s |
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 8.
Table 8
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 250 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
200 DEG C~250 DEG C sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in table 9.
Table 9
Embodiment 4
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, is slowly added into terpinol 15g, lecithin successively
60g, Isobutyl methacrylate 15g, dibutyl phthalate 2g, polyamide wax 1g, polyethylene glycol 3g, γ-metering system
Acryloxypropylethoxysilane trimethoxy silane 3g, resin acid rhodium 1g, mechanical agitation 60min~90min are for use.
Prepare mixing silver powder：Nano-silver powder, micro-silver powder, nano silver wire prepared by above-mentioned example are respectively placed in 220
DEG C baking oven in toast 1h, nano-silver powder, micro-silver powder are poured into terpinol/polyvinyl butyral solution after being cooled to room temperature
In, 40 DEG C of stirring 10min are heated up to, 60 DEG C of stirring 20min are warming up to, are heated to 90 DEG C of stirring 30min, deionization is used in filtering
Water rinses 20min, then 1h is toasted at 60 DEG C, 100 DEG C of baking 1h is heated up to, then by nano-silver powder, micro-silver powder, nano silver wire
By weight proportion (80：10：10) it mixes, obtains the tap density 5.5g/cm of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 11g, mechanical agitation is equal
It is even.70 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 89g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of silver paste：
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 10.
Table 10
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 11.
Table 11
| Type | Specification |
| The mesh number (mesh/inch) of silk screen | 355S |
| The hardness (Shore A) of rubber flap | 70 (60~80) |
| The width (mm) of rubber flap | 40 |
| The speed (m/s) of scraper plate | 5 |
| The pressure (MPa) of hot pressing | 30 |
| Scrape angle (°) | 20~30 |
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 260 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
260 DEG C of sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in table 12.
Table 12
Embodiment 5
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, is slowly added into terpinol 15g, lecithin successively
60g, Isobutyl methacrylate 15g, dibutyl phthalate 2g, polyamide wax 1g, polyethylene glycol 3g, γ-metering system
Acryloxypropylethoxysilane trimethoxy silane 3g, resin acid rhodium 1g, mechanical agitation 60min~90min are for use.
Prepare mixing silver powder：Nano-silver powder, micro-silver powder, nano silver wire prepared by above-mentioned example are respectively placed in 220
DEG C baking oven in toast 1h, nano-silver powder, micro-silver powder are poured into terpinol/polyvinyl butyral solution after being cooled to room temperature
In, 40 DEG C of stirring 10min are heated up to, 60 DEG C of stirring 20min are warming up to, are heated to 90 DEG C of stirring 30min, deionization is used in filtering
Water rinses 20min, then 1h is toasted at 60 DEG C, 100 DEG C of baking 1h is heated up to, then by nano-silver powder, micro-silver powder, nano silver wire
By weight proportion (80：10：10) it mixes, obtains the tap density 5.5g/cm of mixing silver powder3, 0.4~2.1m of specific surface area2/g。
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 35g, mechanical agitation is equal
It is even.70 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 65g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of silver paste：
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 13.
Table 13
| Type | Specification |
| The specification of syringe needle | 21 |
| Needle point (spraying starts, terminates) at a distance from base material | 10cm |
| Syringe needle stops height (spraying process) | 5cm |
| The pressure size of air | 100psi |
| Needle/spray away from size | 2mm |
| The rise/fall rate of needle/nozzle | 10m/s |
| Spray rate | 10ms |
| The residence time of nozzle after spraying each time | 2s |
| The glue of nozzle is sucked back into the time in nozzle | 1s |
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 14.
Table 14
| Type | Specification |
| The mesh number (mesh/inch) of silk screen | 355S |
| The hardness (Shore A) of rubber flap | 70 (60~80) |
| The width (mm) of rubber flap | 40 |
| The speed (m/s) of scraper plate | 5 |
| The pressure (MPa) of hot pressing | 30 |
| Scrape angle (°) | 20~30 |
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 260 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
260 DEG C of sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in Table 15.
Table 15
Embodiment 6
Prepare 100g organic carriers：Ethanol water bath is heated to 60 DEG C, is slowly added into terpinol 15g, lecithin successively
60g, Isobutyl methacrylate 15g, dibutyl phthalate 2g, polyamide wax 1g, polyethylene glycol 3g, γ-metering system
Acryloxypropylethoxysilane trimethoxy silane 3g, resin acid rhodium 1g, mechanical agitation 60min~90min are for use.
Silver powder：ferro SF87
Prepare conductive silver paste：20ml ethanol water baths are heated to 75 DEG C, are slowly added into organic carrier 11g, mechanical agitation is equal
It is even.70 DEG C of constant temperature 1h, then cooled to room temperature, the ultrasonator for moving to 40KHz (need to be put into temperature reducing substance, such as ice
Block) in, keep 0~5 DEG C of temperature.It is slowly added into mixing silver powder 89g, is carried out at the same time mechanical agitation, 90~120min is mixed,
It finally takes out and puts under vacuum conditions, obtain conductive silver paste.
The spraying process of silver paste：
Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is packed into syringe device, spraying ginseng is set
Number, as shown in table 16.
Table 16
| Type | Specification |
| The specification of syringe needle | 21 |
| Needle point (spraying starts, terminates) at a distance from base material | 10cm |
| Syringe needle stops height (spraying process) | 5cm |
| The pressure size of air | 100psi |
| Needle/spray away from size | 2mm |
| The rise/fall rate of needle/nozzle | 10m/s |
| Spray rate | 10ms |
| The residence time of nozzle after spraying each time | 2s |
| The glue of nozzle is sucked back into the time in nozzle | 1s |
Conductive silver paste is sprayed on substrate according to the spray parameters set, chip is fixed on above conductive silver paste,
120 DEG C of drying 40min are heated to from room temperature with 10 DEG C/min heating rates, are then heated to 200 with 15 DEG C/min heating rates
DEG C~250 DEG C of sintering 1h, obtain final products.
The silk-screen printing technique of conductive silver paste：Conductive silver paste syringe is taken out into the 2~4h that rises again from -40 DEG C of refrigerator, is filled
Enter in syringe device, sets wire mark parameter, as shown in table 17.
Table 17
| Type | Specification |
| The mesh number (mesh/inch) of silk screen | 355S |
| The hardness (Shore A) of rubber flap | 70 (60~80) |
| The width (mm) of rubber flap | 40 |
| The speed (m/s) of scraper plate | 5 |
| The pressure (MPa) of hot pressing | 30 |
| Scrape angle (°) | 20~30 |
Conductive silver paste is printed on by stainless steel cloth on substrate, 120 DEG C of drying 40min are heated to after removing silk screen,
By die bonding above, under the conditions of 30MPa, 260 DEG C of sintering 90s is heated to, final product is obtained；Or under the conditions of 10MPa,
260 DEG C of sintering 90s are heated to, final product is obtained.
The properties of product that above-mentioned technique obtains are as shown in table 18.
Table 18
The above content is combining, specific embodiment is made for the present invention to be further described, and it cannot be said that this hair
Bright specific implementation is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the protection of the present invention
Range.
Claims (10)
1. a kind of conductive silver paste without glass powder, which is characterized in that weight percentage, including mixing silver powder 80wt%
~90wt% and organic carrier 10wt%~20wt%, wherein the combined silver powder includes nano-silver powder, micro-silver powder and Yin Na
Rice noodles, the organic carrier include organic solvent, surfactant and thixotropic agent.
2. conductive silver paste according to claim 1, which is characterized in that the shape of the nano-silver powder is sheet, and grain size is
20~80nm；The shape of the micro-silver powder is sheet, and grain size is 1~4 μm；A diameter of 60nm of the nano silver wire~
80nm, length are 40~100 μm.
3. conductive silver paste according to claim 1 or 2, which is characterized in that nano-silver powder, micron silver in the mixing silver powder
The weight percentage of powder and nano silver wire is respectively 70~90wt%, 5~15wt% and 5~15wt%.
4. conductive silver paste according to claim 1, which is characterized in that the organic carrier further include thickener, coupling agent,
Plasticizer, antifoaming agent and sintering inhibitor.
5. conductive silver paste according to claim 4, which is characterized in that weight percentage, the organic carrier packet
Include solvent 15%~45%, surfactant 10%~60%, thickener 15%~25%, coupling agent 3%~5%, plasticizer
2%~5%, thixotropic agent 1%~5%, antifoaming agent 0.5%~3%, sintering inhibitor 0.5%~3%.
6. conductive silver paste according to claim 5, which is characterized in that the solvent is selected from terpinol；
Preferably, the surfactant is one or more in polybasic carboxylic acid, polyalcohol, ester, more preferable oleic acid, diformazan
Acid, lecithin, dimethylbenzene, octanoic acid, triethanolamine, diethylene glycol ether acetate, butyl acetate, polyvinyl pyrrole
It is one or more in alkanone, lauryl sodium sulfate, cetyl benzenesulfonic acid sodium, stearic acid and odium stearate；
Preferably, the thickener is selected from Isobutyl methacrylate, ethyl cellulose, hydroxyethyl cellulose, dimethyl hydroxyethyl
One kind in cellulose, ethylhydroxyethylcellulose, methylhydroxypropylcellulose, polyvinyl butyral, ethyl cellulose or
It is a variety of；
Preferably, the coupling agent is selected from silane coupling agent, more preferable gamma-aminopropyl-triethoxy-silane, 3- (2,3- epoxies third
Oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-glycidyl ether oxygen propyl front three
Oxysilane, γ-glycidyl ether oxygen propyl methyldiethoxysilane, N- β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxies
Base silane, γ-aminopropyltriethoxy diethoxy silane, γ-piperazinopropyl methyl dimethoxysilane, (the 2- first of vinyl three
Oxygroup ethyoxyl) silane, γ-methacryloxypropyl trimethoxy silane, β-(3,4- epoxycyclohexyls) ethyl front three
It is one or more in oxysilane；
Preferably, the plasticizer is selected from dibutyl phthalate；
Preferably, the thixotropic agent is selected from polyamide wax；
Preferably, the antifoaming agent is selected from polyethylene glycol；
Preferably, the sintering inhibitor is selected from resin acid rhodium.
7. a kind of method preparing conductive silver paste as claimed in any one of claims 1 to 6, which is characterized in that including：By formula
Organic solvent, surfactant and thixotropic agent are added in ethanol water bath, is optionally added into thickener, coupling agent, plasticising for amount
Agent, antifoaming agent and sintering inhibitor, stir evenly to form organic carrier；Then it includes nano-silver powder, micro-silver powder and silver to be added
The mixing silver powder of nano wire, is uniformly mixing to obtain the conductive silver paste.
8. the method according to the description of claim 7 is characterized in that the ethanol water bath is maintained at 50~80 DEG C, and stirring
It is formed uniformly after organic carrier and is kept the temperature at 50~80 DEG C；Then it cools down and is transferred to 0~5 DEG C and be kept at this temperature described in addition
Mix silver powder.
9. a kind of sintering method using conductive silver paste as claimed in any one of claims 1 to 6, which is characterized in that led described
Electric silver paste spraying is screen printed onto on substrate, is sintered at 200~300 DEG C after drying, is obtained final products.
10. sintering method according to claim 9, which is characterized in that the drying is to carry out 20 at 100~150 DEG C
~60min；
Preferably, according to spraying, the time of the sintering is 40~80min；According to silk-screen printing, the time of the sintering
For 60~120s.
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| CN109686470A (en) * | 2018-12-21 | 2019-04-26 | 广东羚光新材料股份有限公司 | A kind of annular voltage-sensitive resistor electronic silver paste and preparation method thereof |
| CN110491543A (en) * | 2019-07-30 | 2019-11-22 | 北京氦舶科技有限责任公司 | A kind of conductive silver paste for touch screens and preparation method thereof |
| CN111755144A (en) * | 2020-07-31 | 2020-10-09 | 海泰纳鑫科技(成都)有限公司 | Low-temperature conductive silver paste and preparation method and application thereof |
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| CN116140942A (en) * | 2023-04-18 | 2023-05-23 | 南昌三盛半导体有限公司 | Method for welding nickel-platinum wire of thin film resistor chip |
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| CN109686470A (en) * | 2018-12-21 | 2019-04-26 | 广东羚光新材料股份有限公司 | A kind of annular voltage-sensitive resistor electronic silver paste and preparation method thereof |
| CN109686470B (en) * | 2018-12-21 | 2020-07-28 | 广东羚光新材料股份有限公司 | Electronic silver paste for annular piezoresistor and preparation method thereof |
| CN110491543A (en) * | 2019-07-30 | 2019-11-22 | 北京氦舶科技有限责任公司 | A kind of conductive silver paste for touch screens and preparation method thereof |
| CN111755144A (en) * | 2020-07-31 | 2020-10-09 | 海泰纳鑫科技(成都)有限公司 | Low-temperature conductive silver paste and preparation method and application thereof |
| CN114822992A (en) * | 2022-06-27 | 2022-07-29 | 江西理工大学南昌校区 | Preparation method of conductive silver paste for aerosol spraying process of electronic circuit |
| CN114822992B (en) * | 2022-06-27 | 2022-09-13 | 江西理工大学南昌校区 | Preparation method of conductive silver paste for aerosol spraying process of electronic circuit |
| CN116140942A (en) * | 2023-04-18 | 2023-05-23 | 南昌三盛半导体有限公司 | Method for welding nickel-platinum wire of thin film resistor chip |
| CN116871511A (en) * | 2023-07-13 | 2023-10-13 | 南京芯兴电子科技有限公司 | Preparation method and sintering method of crack-free low-hole nano silver paste |
| CN116665949A (en) * | 2023-07-18 | 2023-08-29 | 上海宝银电子材料有限公司 | Conductive silver paste for automobile coated glass and preparation method thereof |
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Application publication date: 20181026 |
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