CN108538444B - Conductive paste for semiconductor packaging and preparation method thereof - Google Patents
Conductive paste for semiconductor packaging and preparation method thereof Download PDFInfo
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- 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
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- H—ELECTRICITY
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- H01L23/482—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of lead-in layers inseparably applied to the semiconductor body
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Abstract
The invention belongs to the field of electronic fine chemicals, and particularly relates to conductive paste for semiconductor packaging and a preparation method thereof. The conductive slurry is prepared from conductive filler, a solvent, a dispersant and a viscosity regulator; the conductive filler is a conductive polymer coated nano metal. The conductive filler in the conductive slurry uses the conductive polymer as the coating material of the nano metal particles, can improve the agglomeration phenomenon easily caused by the high surface energy of the nano metal particles, effectively improve the oxidation resistance of the nano metal particles, not only can meet the requirement of preventing the agglomeration and oxidation of the nano metal particles, but also can ensure that the conductive polymer material which is not completely removed has conductivity when the nano metal particles are used, reduce the influence of the coating on the conductivity of the nano metal particles, and solve the problems that the conductivity of the nano metal particles is reduced and the performance of the conductive slurry is greatly influenced because the traditional polymer organically coats the nano metal.
Description
Technical Field
The invention belongs to the field of electronic fine chemicals, and particularly relates to conductive paste for semiconductor packaging and a preparation method thereof.
Background
The conductive paste is applied to the technical field of chip packaging, and is used for interconnection and die bonding of semiconductor chips, conductive ink, printed circuits and the like. When the conductive filler in the conductive slurry adopts nano metal particles, in order to prevent the nano metal particles from agglomerating due to high surface energy and prevent the nano metal particles from being oxidized, the nano metal particles are coated by adopting an organic material.
The traditional organic coating material is usually insulating, although the aggregation and oxidation of the nano metal particles can be prevented, if the coating material cannot be effectively removed before the nano metal particles are used, the conductivity of the nano metal particles and the like can be greatly influenced, and the performance of the conductive paste is greatly influenced.
Disclosure of Invention
The invention provides conductive paste for semiconductor packaging and a preparation method thereof, which are used for solving the problems that a coating material organically coated by nano metal particles is usually insulated, and if the coating material cannot be effectively removed before the nano metal particles are used, the conductivity and the like of the nano metal particles are greatly influenced, and the performance of the conductive paste is greatly influenced.
The specific technical scheme of the invention is as follows:
a conductive paste for semiconductor packaging is prepared from conductive filler, solvent, dispersant and viscosity regulator;
the conductive filler is a conductive polymer coated nano metal.
Preferably, the particle size of the nano metal particles is 50 nm-500 nm;
the nano metal particles are one or more of nano copper particles, nano palladium particles, nano nickel particles, nano silver particles and nano gold particles.
Preferably, the solvent is one or more of water, ethanol, acetone, ethylene glycol, glycerol, xylene isopropanol bisphenol A, epichlorohydrin, epoxy resin, primary amine, tertiary amine, acid anhydride, phenol, furfural and resorcinol;
the dispersing agent is one or more of Arabic gum, polyvinyl alcohol, polyethylene glycol, gelatin, polyvinylpyrrolidone imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, phenylimidazole and 2-ethylimidazole;
the viscosity regulator is one or more of methyl cellulose, ethyl cellulose, hydroxyl cellulose, primary amine, tertiary amine and acid anhydride.
Preferably, the weight percentage of the conductive filler, the solvent, the dispersant and the viscosity regulator is 8-90%: 8% -90%: 1% -10%: 1 to 10 percent.
The invention also provides a preparation method of the conductive paste for semiconductor packaging, which comprises the following steps:
a) stirring and adding nano metal particles into a mixed solution of protonic acid and a doping agent, and then adding a conductive polymer monomer to obtain a conductive polymer in-situ polymerization reaction solution containing the nano metal particles;
b) conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles under stirring to obtain a dispersion solution containing conducting polymer coated nano metal;
c) drying the dispersion solution containing the conductive polymer coated nano metal to obtain the conductive polymer coated nano metal;
d) and mixing the solvent, the dispersant and the viscosity regulator, stirring, adding the conductive polymer coated nano metal, and dispersing to obtain the conductive slurry.
Preferably, the molar ratio of the dopant to the nano-metal particles in step a) is 1: 1 to 5.
Preferably, the temperature of the in-situ polymerization reaction of the conductive polymer in the step b) is 20-40 ℃;
the time of the in-situ polymerization reaction of the conductive polymer in the step b) is 10-300 min.
Preferably, the protonic acid in step a) is one or more of sulfuric acid, acetic acid, hydrochloric acid, perchloric acid and nitric acid;
in the step a), the dopant is one or more of sodium persulfate, potassium dichromate, potassium iodate, hydrogen peroxide, ammonium persulfate and ferric chloride;
in the step a), the conductive polymer monomer is one or more of aniline, pyrrole, thiophene, phenylalkyne, naphthalene and furan.
Preferably, the concentration of the protonic acid in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-1M;
the concentration of the dopant in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-0.5M.
Preferably, the concentration of the conductive polymer monomer in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-0.5M.
In summary, the present invention provides a conductive paste for semiconductor packaging, which is made of conductive filler, solvent, dispersant and viscosity modifier; the conductive filler is a conductive polymer coated nano metal. The conductive filler in the conductive slurry uses the conductive polymer as the coating material of the nano metal particles, can improve the agglomeration phenomenon easily caused by the high surface energy of the nano metal particles, effectively improve the oxidation resistance of the nano metal particles, not only can meet the requirement of preventing the agglomeration and oxidation of the nano metal particles, but also can ensure that the conductive polymer material which is not completely removed has conductivity when the nano metal particles are used, reduce the influence of the coating on the conductivity of the nano metal particles, and solve the problems that the conductivity of the nano metal particles is reduced and the performance of the conductive slurry is greatly influenced because the traditional polymer organically coats the nano metal.
Detailed Description
The invention provides conductive paste for semiconductor packaging and a preparation method thereof, which are used for solving the problems that a coating material organically coated by nano metal particles is usually insulated, and if the coating material cannot be effectively removed before the nano metal particles are used, the conductivity and the like of the nano metal particles are greatly influenced, and the performance of the conductive paste is greatly influenced.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A conductive paste for semiconductor packaging is prepared from conductive filler, solvent, dispersant and viscosity regulator;
the conductive filler is a conductive polymer coated nano metal.
In the invention, the conductive filler of the conductive slurry uses the conductive polymer as the coating material of the nano metal particles, can improve the easy agglomeration phenomenon caused by the high surface energy of the nano metal particles, effectively improve the oxidation resistance of the nano metal particles, not only can meet the requirement of preventing the agglomeration and oxidation of the nano metal particles, but also when the nano metal particles are used, the conductive polymer material which is not completely removed has conductivity, reduces the influence of the coating on the conductivity of the nano metal particles, and solves the problems that the conductivity of the nano metal particles is reduced and the performance of the conductive slurry is greatly influenced because the traditional polymer is used for carrying out organic coating on the nano metal.
In the invention, the particle size of the nano metal particles is 50 nm-500 nm;
the nano metal particles are one or more of nano copper particles, nano palladium particles, nano nickel particles, nano silver particles and nano gold particles.
In the invention, the solvent is one or more of water, ethanol, acetone, ethylene glycol, glycerol, xylene isopropanol bisphenol A, epichlorohydrin, epoxy resin, primary amine, tertiary amine, acid anhydride, phenol, furfural and resorcinol;
the dispersant is one or more of acacia, polyvinyl alcohol, polyethylene glycol, gelatin, polyvinylpyrrolidone imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, phenylimidazole and 2-ethylimidazole;
the viscosity regulator is one or more of methyl cellulose, ethyl cellulose, hydroxy cellulose, primary amine, tertiary amine and acid anhydride.
In the invention, the weight percentage of the conductive filler, the solvent, the dispersant and the viscosity regulator is 8-90%: 8% -90%: 1% -10%: 1 to 10 percent.
The invention also provides a preparation method of the conductive paste for semiconductor packaging, which comprises the following steps:
a) stirring and adding nano metal particles into a mixed solution of protonic acid and a doping agent, and then adding a conductive polymer monomer to obtain a conductive polymer in-situ polymerization reaction solution containing the nano metal particles;
b) conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles under stirring to obtain a dispersion solution containing the conducting polymer coated nano metal;
c) drying the dispersion solution containing the conductive polymer coated nano metal to obtain the conductive polymer coated nano metal;
d) and mixing the solvent, the dispersant and the viscosity regulator, stirring, adding the conductive polymer coated nano metal, and dispersing to obtain the conductive slurry.
In the invention, before the step a), the method further comprises the following steps: and (3) pretreating the nano metal particles to remove oxides on the surfaces of the nano metal particles.
The nano metal particles are more specifically nano copper particles, and the pretreatment of the nano metal particles is more specifically:
adding the nano-copper particles into dilute sulfuric acid, and stirring and reacting at 10-40 ℃ to obtain a dilute sulfuric acid solution containing the nano-copper particles;
washing the dilute sulfuric acid solution containing the nano-copper particles by using deionized water at 10-40 ℃, wherein the washing times are 2-4 times, and obtaining the nano-copper particles washed by the deionized water;
the stirring speed of the stirring reaction is 300-3000 rpm; stirring and reacting for 1-10 min; the stirring reaction is more specifically a magnetic stirring reaction.
The ratio of the mass of the nano copper particles to the volume of the dilute sulfuric acid is 0.001-0.01 g: 1 mL; the mass fraction of the dilute sulfuric acid is 1-10%.
In the present invention, the molar ratio of the dopant to the nano-metal particles in step a) is 1: 1 to 5.
In the invention, the temperature of the conductive polymer in-situ polymerization reaction in the step b) is 20-40 ℃;
the time of the in-situ polymerization reaction of the conductive polymer in the step b) is 10-300 min.
In the invention, the stirring speed of the stirring in the step a) is 300-3000 rpm;
stirring speed of stirring in the step b) is 300-3000 rpm;
the stirring speed of the stirring in the step d) is 300-3000 rpm.
In the invention, the drying in the step c) is vacuum drying;
the temperature of vacuum drying is 20-50 ℃;
the vacuum drying time is 1-12 h.
In the present invention, after the step b) obtains the dispersion solution containing conductive polymer-coated nano-metal, and before the step c) dries the dispersion solution containing conductive polymer-coated nano-metal, the method further includes:
carrying out centrifugal separation on the dispersion solution containing the conductive polymer coated nano metal to obtain wet conductive polymer coated nano metal;
and (3) washing the wet nano metal coated with the conductive polymer for 3-5 times by using deionized water, and then washing for 2-5 times by using absolute ethyl alcohol.
In the invention, the protonic acid in the step a) is one or more of sulfuric acid, acetic acid, hydrochloric acid, perchloric acid and nitric acid;
in the step a), the doping agent is one or more of sodium persulfate, potassium dichromate, potassium iodate, hydrogen peroxide, ammonium persulfate and ferric chloride;
in the step a), the conductive polymer monomer is one or more of aniline, pyrrole, thiophene, phenylalkyne, naphthalene and furan.
In the invention, the concentration of protonic acid in the conductive polymer in-situ polymerization reaction liquid containing nano metal particles is 0.001-1M;
the concentration of the dopant in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-0.5M.
The concentration of the conductive polymer monomer in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-0.5M.
In the invention, in the step d), the solvent, the dispersant and the viscosity regulator are mixed and stirred, and then the conductive polymer coated nano metal is added for dispersion, so that the conductive slurry is obtained by the following steps:
mixing a solvent, a dispersant and a viscosity regulator for 1-10 min under the stirring of 300-3000 rpm to obtain a conductive slurry solution;
and stirring and adding the conductive polymer coated nano metal into the conductive slurry solution, mixing for 1-10 min, and then performing ultrasonic dispersion for 1-60 min to obtain the conductive slurry.
In the invention, the stirring is specifically magnetic stirring.
According to the invention, the conductive slurry is prepared by using the conductive polymer coated nano metal, so that the agglomeration of nano metal particles in the preparation and storage processes of the conductive slurry can be effectively reduced, the oxidation of the nano metal particles in the preparation and storage processes of the conductive slurry is reduced, and the influence of an organic coating material on the conductive performance of the electronic slurry is reduced.
For a further understanding of the invention, reference will now be made in detail to the following examples.
Example 1
Adding 20g of copper powder with the average diameter of 100nm into 100ml of dilute sulfuric acid with the mass fraction of 5%, and reacting for 5min at 25 ℃ under the magnetic stirring of 1000rpm to obtain a dilute sulfuric acid solution containing nano-copper particles;
washing the dilute sulfuric acid solution containing the nano-copper particles for 3 times by using deionized water at 25 ℃ to obtain the nano-copper particles washed by the deionized water;
adding 0.06mol of sodium persulfate into the reaction vessel, and adding dilute sulfuric acid and water into the reaction vessel to ensure that the concentration of the dilute sulfuric acid in the reaction vessel is 0.05M and the concentration of the sodium persulfate is 0.05M;
under the magnetic stirring of 1200rpm, adding deionized water washed nano copper particles into a reaction vessel, and then adding aniline into the reaction vessel to obtain a conductive polymer in-situ polymerization reaction solution containing nano metal particles;
conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles for 60min under the stirring of the temperature of 30 ℃ and the rotation speed of 1200rpm to obtain a dispersing solution containing the nano metal coated by the conducting polymer;
centrifugally separating the dispersion solution containing the conductive polymer coated nano metal to obtain wet conductive polymer coated nano metal;
and (3) washing the wet nano metal coated with the conductive polymer for 3-5 times by using deionized water, washing for 2-5 times by using absolute ethyl alcohol, and drying in vacuum at 40 ℃ to obtain the nano metal coated with the conductive polymer.
Stirring 70g of ethanol, 2g of polyethylene glycol and 5g of methyl cellulose for 2min in 1200rpm magnetic stirring, adding conductive polymer coated nano metal, stirring for 2min in 1200rpm magnetic stirring, and finally dispersing for 5min by using ultrasonic to obtain the conductive slurry for semiconductor packaging.
Example 2
Adding 20g of copper powder with the average diameter of 100nm into 100ml of dilute sulfuric acid with the mass fraction of 5%, and reacting for 5min at 25 ℃ under the magnetic stirring of 1000rpm to obtain a dilute sulfuric acid solution containing nano-copper particles;
washing the dilute sulfuric acid solution containing the nano-copper particles for 3 times by using deionized water at 25 ℃ to obtain the nano-copper particles washed by the deionized water;
adding 0.06mol of sodium persulfate into the reaction vessel, and adding dilute sulfuric acid and water into the reaction vessel to ensure that the concentration of the dilute sulfuric acid in the reaction vessel is 0.05M and the concentration of the sodium persulfate is 0.05M;
under the magnetic stirring of 1200rpm, adding deionized water washed nano copper particles into a reaction vessel, and then adding aniline into the reaction vessel to obtain a conductive polymer in-situ polymerization reaction solution containing nano metal particles;
conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles for 60min under the stirring of the temperature of 30 ℃ and the rotation speed of 1200rpm to obtain a dispersing solution containing the nano metal coated by the conducting polymer;
centrifugally separating the dispersion solution containing the conductive polymer coated nano metal to obtain wet conductive polymer coated nano metal;
and (3) washing the wet nano metal coated with the conductive polymer for 3-5 times by using deionized water, washing for 2-5 times by using absolute ethyl alcohol, and drying in vacuum at 40 ℃ to obtain the nano metal coated with the conductive polymer.
Stirring 70g of ethanol, 2g of polyethylene glycol and 5g of ethyl cellulose for 2min in magnetic stirring at 1200rpm, adding the conductive polymer coated nano metal, stirring for 2min in magnetic stirring at 1200rpm, and finally dispersing for 5min by using ultrasonic to obtain the conductive slurry for semiconductor packaging.
Example 3
Adding 20g of copper powder with the average diameter of 100nm into 100ml of dilute sulfuric acid with the mass fraction of 5%, and reacting for 5min at 25 ℃ under the magnetic stirring of 1000rpm to obtain a dilute sulfuric acid solution containing nano-copper particles;
washing the dilute sulfuric acid solution containing the nano-copper particles for 3 times by using deionized water at 25 ℃ to obtain the nano-copper particles washed by the deionized water;
adding 0.06mol of sodium persulfate into the reaction vessel, and adding dilute sulfuric acid and water into the reaction vessel to ensure that the concentration of the dilute sulfuric acid in the reaction vessel is 0.05M and the concentration of the sodium persulfate is 0.05M;
under the magnetic stirring of 1200rpm, adding deionized water washed nano copper particles into a reaction vessel, and then adding aniline into the reaction vessel to obtain a conductive polymer in-situ polymerization reaction solution containing nano metal particles;
conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles for 60min under the stirring of the temperature of 30 ℃ and the rotation speed of 1200rpm to obtain a dispersing solution containing the nano metal coated by the conducting polymer;
centrifugally separating the dispersion solution containing the conductive polymer coated nano metal to obtain wet conductive polymer coated nano metal;
and (3) washing the wet nano metal coated with the conductive polymer for 3-5 times by using deionized water, washing for 2-5 times by using absolute ethyl alcohol, and drying in vacuum at 40 ℃ to obtain the nano metal coated with the conductive polymer.
Stirring 70g of ethanol, 2g of polyethylene glycol and 5g of ethyl cellulose for 2min in magnetic stirring at 1200rpm, adding the conductive polymer coated nano metal, stirring for 2min in magnetic stirring at 1200rpm, and finally dispersing for 10min by using ultrasonic to obtain the conductive slurry for semiconductor packaging.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of conductive paste for semiconductor packaging is characterized by comprising the following steps:
a) stirring and adding nano metal particles into a mixed solution of protonic acid and a doping agent, and then adding a conductive polymer monomer to obtain a conductive polymer in-situ polymerization reaction solution containing the nano metal particles;
b) conducting polymer in-situ polymerization reaction on the conducting polymer in-situ polymerization reaction liquid containing the nano metal particles under stirring to obtain a dispersion solution containing conducting polymer coated nano metal;
c) drying the dispersion solution containing the conductive polymer coated nano metal to obtain the conductive polymer coated nano metal;
d) mixing a solvent, a dispersant and a viscosity regulator, stirring, adding the conductive polymer coated nano metal, and dispersing to obtain conductive slurry;
the conductive slurry is prepared from a conductive filler, a solvent, a dispersant and a viscosity regulator, wherein the conductive filler is conductive polymer coated nano metal.
2. The method according to claim 1, wherein the nano-metal particles have a particle size of 50 to 500 nm;
the nano metal particles are one or more of nano copper particles, nano palladium particles, nano nickel particles, nano silver particles and nano gold particles.
3. The production method according to claim 1, wherein the solvent is one or more of water, ethanol, acetone, ethylene glycol, glycerol, xylene isopropanol bisphenol a, epichlorohydrin, epoxy resin, primary amine, tertiary amine, acid anhydride, phenol, furfural, and resorcinol;
the dispersing agent is one or more of Arabic gum, polyvinyl alcohol, polyethylene glycol, gelatin, polyvinylpyrrolidone imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, phenylimidazole and 2-ethylimidazole;
the viscosity regulator is one or more of methyl cellulose, ethyl cellulose, hydroxyl cellulose, primary amine, tertiary amine and acid anhydride.
4. The method according to claim 3, wherein the weight percentage of the conductive filler, the solvent, the dispersant and the viscosity modifier is 8% to 90%: 8% -90%: 1% -10%: 1 to 10 percent.
5. The method according to claim 1, wherein the molar ratio of the dopant to the nano-metal particles in step a) is 1: 1 to 5.
6. The preparation method of claim 1, wherein the temperature of the in-situ polymerization reaction of the conductive polymer in the step b) is 20-40 ℃;
the time of the in-situ polymerization reaction of the conductive polymer in the step b) is 10-300 min.
7. The method according to claim 1, wherein the protonic acid in step a) is one or more of sulfuric acid, acetic acid, hydrochloric acid, perchloric acid and nitric acid;
in the step a), the dopant is one or more of sodium persulfate, potassium dichromate, potassium iodate, hydrogen peroxide, ammonium persulfate and ferric chloride;
in the step a), the conductive polymer monomer is one or more of aniline, pyrrole, thiophene, phenylalkyne, naphthalene and furan.
8. The preparation method according to claim 7, wherein the concentration of the protonic acid in the conductive polymer in-situ polymerization reaction solution containing the nano-metal particles is 0.001-1M;
the concentration of the dopant in the conductive polymer in-situ polymerization reaction liquid containing the nano metal particles is 0.001-0.5M.
9. The method according to claim 7, wherein the concentration of the conductive polymer monomer in the conductive polymer in-situ polymerization reaction solution containing the metal nanoparticles is 0.001-0.5M.
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