CN105788703A - Anti-oxidation silver copper paste for electromagnetic shielding, and preparation method thereof - Google Patents
Anti-oxidation silver copper paste for electromagnetic shielding, and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to an anti-oxidation silver copper paste for electromagnetic shielding. The silver copper paste includes following components by weight percent: 50-60% of silver-coated copper powder, 5-8% of flake silver powder, 7-10% of high molecular resin, 2-4% of organic additive, and 20-30% of organic solvent. The high molecular resin and the organic solvent are added to a dissolution kettle according to the foregoing weight percent, and then are stirred so as to fully dissolve the high molecular resin, after standing for a while, the mixed solution is filtered to remove impurities to obtain a carrier; and the prepared carrier and other components are added to a high-speed disperser to be grinded, the fineness degree of the silver copper paste is controlled to be less than 10 mum, the viscosity of the silver copper paste is adjusted to be 10-20Pa.S, and impurities are filtered so as to prepare a silver copper paste product. Compared with the prior art, the preparation method combines the silver-coated copper powder and the flake silver powder, thereby exerting the synergetic effect of the silver-coated copper powder and the flake silver powder, and saving cost; the prepared silver copper paste has excellent electromagnetic shielding performance, and the shielding energy efficiency can reach between -60db and -90db; and the process is simple, energy consumption is reduced, and the preparation method is applicable to large-scale line production.
Description
Technical field
The invention belongs to technical field of electronic materials, relate to a kind of antioxidation silver-bearing copper slurry, particularly relate to a kind of antioxidation silver-bearing copper slurry for electromagnetic shielding and preparation method thereof.
Background technology
Along with developing rapidly of electronics industry, electromagnetic interference, information security, personal security problem increasingly come into one's own.Therefore, exploitation good combination property, the suitability is strong and cost is low electromagnetic shielding material have now become study hotspot.Electromagnetic shielding conductive slurry because of its have that cost is low, simple process (can spray, blade coating, brushing), practical, easily realize the advantages such as coated technique automatization, strong adaptability, have broad application prospects.Wherein, the exploitation of high-performance conductive electromagnetic shielding slurry is still the development trend of this industry.
At present, commercially available electromagnetic shielding conductive slurry is generally silver system slurry, nickel system slurry or charcoal system slurry.Silver system slurry has that conductivity height, conductive stability be good and the feature such as substrate bond strength is big, its electromagnetic shielding capability will be good than nickel system, charcoal system, but, silver system slurry is expensive, and the silver powder major part in existing silver system slurry is micron powder, the thicknesses of layers of the slurry being made from, printing performance etc. have significant limitation for present high-end precision instrument, which limits the range of application of silver system slurry；Meanwhile, the finished product viscosity of silver system slurry is higher, and the printing performance of slurry is poor, the as easy as rolling off a log service life caused rete uneven, and then affect conductor paste.But, nickel system slurry, charcoal system slurry shield effectiveness relatively poor, all there is bigger limitation in many applications.
Now, for processing type unit increasingly with keen competition, the production cost reducing electrocondution slurry as much as possible seems all the more important.For the silver system expensive cost disadvantage of slurry, copper powder price is relatively low, is only about the 1/20 of silver, and its electric conductivity is only second to silver in all metals, is the desirable substitution material of silver.But copper powder character is active, very easily oxidation generates the oxide of insulation, significantly impacts its electric conductivity, limits its application in electrocondution slurry.In recent years, for improving the non-oxidizability of copper powder, having carried out substantial amounts of trial and exploration both at home and abroad, and silver-coated copper powder effect is best, its principle is mainly by plating one layer of silver at Copper Powder Surface, it is to avoid copper and air contact, improves the non-oxidizability of copper powder.Silver-coated copper powder combines the advantage of copper powder and argentum powder, overcomes shortcoming during single use, has great application prospect in the field such as electric slurry, electromagnetic shielding.
Application number be 201010297324.8 Chinese invention patent disclose a kind of conductor pulp for printed circuit board and preparation method thereof, this conductor paste in mass fraction, silver-coated copper powder including 55～80%, the organic binder bond of 10～25%, 1～8% leadless glass powder and 5～12% additive；In the middle of described silver-coated copper powder, the weight/mass percentage composition of silver is 50～60%.The silver-coated copper powder adopted in this patent is main conductive material, and leadless glass powder, additive and organic binder bond in addition, compared to traditional fine silver conductor paste, production cost can be reduced, improve printing performance and connect fixing, and compared to traditional pure cu conductor slurry, it is possible to it is effectively improved the electric conductivity of slurry.But, the technical scheme in above-mentioned patent still suffers from the place required further improvement, for instance, it is possible to silver-coated copper powder is combined use, in order to improve the electric conductivity of slurry further with flake silver powder；That reduces leadless glass powder further makes consumption, in order to save cost etc..
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and a kind of antioxidation silver-bearing copper slurry for electromagnetic shielding and preparation method thereof is provided.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 50～60%, flake silver powder 5～8%, macromolecule resin 7～10%, organic additive 2～4% and organic solvent 20～30%.
Described silver-coated copper powder is micron order dendroid silver-coated copper powder, and the particle diameter of this silver-coated copper powder is 4～8 μm, and tap density is 3.5～4.5g/ml, and in described silver-coated copper powder, the weight percent content of silver is 8～12%.
The particle diameter of described flake silver powder is 4～7 μm, and tap density is 2.3～3.0g/ml.
Described silver-coated copper powder has bigger tap density, and argentum powder that can be relatively low with tap density becomes good overlap joint phase, it is possible to resistance is greatly lowered, and occurs the probability of pin hole, trachoma after reducing printing.
Described macromolecule resin is acrylic resin, and this acrylic resin ingredient is BMA/MMA copolymer, and itself does not contain halogen, relatively other resins, and acrylic resin self-resistance rate is less, and has stronger adhesive force between the base material such as PET, PC.At present, vinyl chloride-vinyl acetate resin generally selected by commercially available silver-bearing copper slurry, although it has relatively small resistance, but because containing halogen in this resin, has not met European Union environmental protection standard.
Described organic additive includes firming agent, thickening agent, Hardening agent, silane coupler and levelling agent.
Described firming agent is closure firming agent, and this firming agent is hexamethylene diisocyanate, and isocyanate group content is 15%～17%, and this firming agent can be effectively improved the wearability of silver slurry, solvent resistance and chemical resistance.
Described thickening agent is aerosil, and the bulk density of this aerosil is 50g/L, and mean diameter is 12 nanometers, and silica purity is more than 99.8%.Described silicon dioxide can be effectively prevented silver slurry sagging, sedimentation.
Described Hardening agent is electrically conductive graphite, and the specific surface area of this electrically conductive graphite is 125m2/ g, mean diameter 20～30 nanometers, oil absorption is 150, and this electrically conductive graphite can be effectively improved silver-bearing copper and starch the anti-wear performance toasted.
Described silane coupler includes one or more in Silane coupling agent KH550, KH560, KH570.
Described levelling agent is organic siliconresin, and this organic siliconresin is methyl silicon resin, and it can significantly improve the flow leveling of silver slurry.
Described organic solvent is one or both in isophorone, dibasic ester.Wherein, described dibasic ester is mixed for 3:4:3 in mass ratio by dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate, and after described dibasic ester and isophorone dissolve each other, the dissolubility in resin can be better.
The preparation method that a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, the method comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 20～30 DEG C, mixing speed is 1000～3000r/min, stirs 5～6h, until macromolecule resin is completely dissolved in organic solvent, granular sensation without resin, after standing 2h, then it is filtered remove impurity with 300～400 order polyester webs, namely prepares carrier；
(3) silver-bearing copper starches half-finished preparation: add in high speed dispersor with other each component by the carrier that step (2) prepares together with the percentage by weight in step (1), rate of dispersion is 1000～3000r/min, dispersion 20～30min, until being uniformly dispersed without powdered granule sense, namely prepare silver-bearing copper slurry semi-finished product；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 60～80r/min, it is 3 ± 0.25MPa that force value controls, roll 4～5 times, reach the effect being fully ground, until the fineness of silver-bearing copper slurry is less than 10 μm, the fine setting of silver-bearing copper slurry viscosity is carried out by adding appropriate organic solvent, making silver-bearing copper slurry viscosity is 10～20Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
The action principle of electromagnetic shielding is to utilize shield to electromagnetic reflection, absorption and guiding function, and these act on shielding construction (resin argentum powder inclusion enclave) surface and residual charge in shield, electric current and polarization phenomena close association.Argentum powder, copper powder have good electric conductivity and radar absorption characteristic, therefore in combination with reaching the shield effectiveness of excellence.
Compared with starching with similar silver-bearing copper, due to the collocation of argentum powder, the present invention prepares the antioxidation silver-bearing copper slurry of gained, finer and close in microcosmic situation, smooth.In oxidizing process, the partial points oxidation of other silver-bearing coppers slurry relatively, the silver-bearing copper slurry of the present invention is integrated oxidation, therefore the time of antioxidation variable color is longer.
Compared with prior art, the invention have the characteristics that:
1) preparation for processing is easy, mild condition；
2) the antioxidation silver-bearing copper preparing gained is starched without ROSH banned substance, belongs to environment-friendly type slurry；
3) processing cost is low, antioxidation silver-bearing copper slurry processing cost is conventional silver system shielding slurry processing cost 1/3rd of the present invention；
4) the antioxidation silver-bearing copper slurry preparing gained has the capability of electromagnetic shielding of excellence, and shielding efficiency is up to-60db to-90db；
5) the antioxidation silver-bearing copper slurry preparing gained belongs to low-temperature bake type slurry, saves power consumption, is suitable for high-volume line production.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 52%, flake silver powder 8%, macromolecule resin 10%, organic additive 2% and organic solvent 28%.
Wherein, the mean diameter of silver-coated copper powder is 5.2 μm, and tap density is that in 3.5g/ml silver-coated copper powder, the weight percent content of silver is 9%；Flake silver powder mean diameter is 5.7 μm, and tap density is 2.8g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, silane coupler KH560 and organic siliconresin is 2:2:2:1:3.Wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 15%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 20mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2；In dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 25 DEG C, mixing speed 2000r/min, stirring 5h, until macromolecule resin is completely dissolved in organic solvent, stands 2h, it is filtered remove impurity with 300 order polyester webs again, namely prepares carrier；
(3) preparation of silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 2000r/min, dispersion 30min, until being uniformly dispersed without powdered granule sense, after fully dispersed, namely prepare uniform silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 70r/min, force value controls at 3MPa, roll reaches the effect being fully ground for 5 times, until the fineness of silver-bearing copper slurry is less than 10 μm, carry out the fine setting of silver-bearing copper slurry viscosity by adding appropriate organic solvent so that silver-bearing copper slurry viscosity is 15Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Embodiment 2:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 56%, flake silver powder 6%, macromolecule resin 8%, organic additive 3% and organic solvent 27%.
Wherein, the mean diameter of silver-coated copper powder is 5.7 μm, and tap density is 3.8g/ml, and in silver-coated copper powder, the weight percent content of silver is 10%；Flake silver powder mean diameter is 5.1 μm, and tap density is 2.9g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, Silane coupling agent KH550 and organic siliconresin is 2:2:2:1:3.Wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 17%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 30mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2, and in dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 30 DEG C, mixing speed is 2000r/min, stir 6 hours, until macromolecule resin is completely dissolved in organic solvent, stand 2h, it is filtered remove impurity with 400 order polyester webs again, namely prepares carrier；
(3) preparation of silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 2000r/min, dispersion 20min, until being uniformly dispersed without powdered granule sense, after fully dispersed, namely prepare uniform silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 70r/min, force value controls at 3MPa, roll reaches the effect being fully ground for 4 times, until the fineness of silver-bearing copper slurry is less than 10 μm, carry out the fine setting of silver-bearing copper slurry viscosity by adding appropriate organic solvent so that silver-bearing copper slurry viscosity is 16Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Embodiment 3:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 50%, flake silver powder 7%, macromolecule resin 10%, organic additive 4% and organic solvent 29%.
Wherein, the mean diameter of silver-coated copper powder is 5.3 μm, and tap density is 4.5g/ml, and in silver-coated copper powder, the weight percent content of silver is 9%；Flake silver powder mean diameter is 5.5 μm, and tap density is 2.9g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, silane coupler KH570 and organic siliconresin is 2:2:2:1:3.Wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 16%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 28mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2, and in dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 28 DEG C, mixing speed 1000r/min, stirring 5h, until macromolecule resin is completely dissolved in organic solvent, stands 2h, it is filtered remove impurity with 300 order polyester webs again, namely prepares carrier；
(3) preparation of silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 1000r/min, dispersion 25min, until being uniformly dispersed without powdered granule sense, namely prepare uniform silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 60r/min, force value controls at 3.25MPa, roll reaches the effect being fully ground for 5 times, until the fineness of silver-bearing copper slurry is less than 10 μm, carry out the fine setting of silver-bearing copper slurry viscosity by adding appropriate organic solvent so that silver-bearing copper slurry viscosity is 20Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Embodiment 4:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 60%, flake silver powder 5%, macromolecule resin 7%, organic additive 3% and organic solvent 25%.
Wherein, the mean diameter of silver-coated copper powder is 4 μm, and tap density is 4g/ml, and in silver-coated copper powder, the weight percent content of silver is 10%；Flake silver powder mean diameter is 4 μm, and tap density is 2.3g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, silane coupler KH560 and organic siliconresin is 2:2:2:1:3.Wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 16%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 25mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2, and in dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 27 DEG C, mixing speed 3000r/min, stirring 5.5h, until macromolecule resin is completely dissolved in organic solvent, stands 2h, it is filtered remove impurity with 300 order polyester webs again, namely prepares carrier；
(3) preparation of semi-finished product silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 3000r/min, dispersion 30min, until being uniformly dispersed without powdered granule sense, namely prepare uniform semi-finished product silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: semi-finished product silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 80r/min, force value controls at 2.75MPa, roll reaches the effect being fully ground for 5 times, until the fineness of silver-bearing copper slurry is less than 10 μm, the fine setting of silver-bearing copper slurry viscosity is carried out by adding appropriate organic solvent, making silver-bearing copper slurry viscosity is 10Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Embodiment 5:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 60%, flake silver powder 6%, macromolecule resin 10%, organic additive 4% and organic solvent 20%.
Wherein, the mean diameter of silver-coated copper powder is 8 μm, and tap density is 4.2g/ml, and in silver-coated copper powder, the weight percent content of silver is 8%；Flake silver powder mean diameter is 7 μm, and tap density is 2.8g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, silane coupler KH560, silane coupler KH570 and organic siliconresin is 2:2:2:1:1:3, wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 16%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 28mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2, and in dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 25 DEG C, mixing speed 2500r/min, stirring 6h, until macromolecule resin is completely dissolved in organic solvent, stands 2h, it is filtered remove impurity with 400 order polyester webs again, namely prepares carrier；
(3) preparation of silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 2500r/min, dispersion 28min, until being uniformly dispersed without powdered granule sense, after fully dispersed, namely prepare uniform silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 80r/min, force value controls at 3MPa, roll reaches the effect being fully ground for 5 times, until the fineness of silver-bearing copper slurry is less than 8 μm, carry out the fine setting of silver-bearing copper slurry viscosity by adding appropriate organic solvent so that silver-bearing copper slurry viscosity is 12Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Embodiment 6:
In the present embodiment, a kind of antioxidation silver-bearing copper for electromagnetic shielding is starched, and this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 55%, flake silver powder 6%, macromolecule resin 7%, organic additive 2% and organic solvent 30%.
Wherein, the mean diameter of silver-coated copper powder is 8 μm, and tap density is 3.6g/ml, and in silver-coated copper powder, the weight percent content of silver is 12%；Flake silver powder mean diameter is 6 μm, and tap density is 2.7g/ml.
Macromolecule resin is acrylic resin.
In organic additive, the mass ratio of closure firming agent, aerosil, electrically conductive graphite, Silane coupling agent KH550, silane coupler KH570 and organic siliconresin is 2:2:2:1:1:3, wherein, closure firming agent is isocyanate group content is the hexamethylene diisocyanate of 16%；The bulk density of aerosil is 50g/L, and mean diameter is 12nm, and silica purity is more than 99.8%；The specific surface area of electrically conductive graphite is 125m2/ g, mean diameter 26mm, oil absorption is 150；Organic siliconresin is methyl silicon resin.
Organic solvent is the mixed solvent of dibasic ester and isophorone, and wherein, the mass ratio of dibasic ester and isophorone is 5:2, and in dibasic ester, the mass ratio of dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate is 3:4:3.
In the present embodiment, the preparation method of antioxidation silver-bearing copper slurry comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, dissolution kettle temperature is 30 DEG C, mixing speed 2200r/min, stirring 6h, until macromolecule resin is completely dissolved in organic solvent, stands 2h, it is filtered remove impurity with 300 order polyester webs again, namely prepares carrier；
(3) preparation of silver-bearing copper slurry: the carrier that step (2) prepares is added in high speed dispersor with other each component together with the percentage by weight in step (1), rate of dispersion is 2200r/min, dispersion 30min, until being uniformly dispersed without powdered granule sense,, namely prepare uniform silver-bearing copper slurry；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry step (3) prepared joins in three-high mill, the roller rotating speed of three-high mill is adjusted to 75r/min, force value controls at 2.8MPa, roll reaches the effect being fully ground for 5 times, until the fineness of silver-bearing copper slurry is less than 9 μm, carry out the fine setting of silver-bearing copper slurry viscosity by adding appropriate organic solvent so that silver-bearing copper slurry viscosity is 15Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
Claims (10)
1. the antioxidation silver-bearing copper for electromagnetic shielding is starched, it is characterized in that, this silver-bearing copper slurry includes following components and weight percent content: silver-coated copper powder 50～60%, flake silver powder 5～8%, macromolecule resin 7～10%, organic additive 2～4% and organic solvent 20～30%.
2. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 1 is starched, it is characterized in that, described silver-coated copper powder is micron order dendroid silver-coated copper powder, the particle diameter of this silver-coated copper powder is 4～8 μm, tap density is 3.5～4.5g/ml, and in described silver-coated copper powder, the weight percent content of silver is 8～12%.
3. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 1 is starched, it is characterised in that the particle diameter of described flake silver powder is 4～7 μm, and tap density is 2.3～3.0g/ml.
4. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 1 is starched, it is characterised in that macromolecule resin is acrylic resin.
5. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 1 is starched, it is characterised in that described organic additive includes firming agent, thickening agent, Hardening agent, silane coupler and levelling agent；Described firming agent is closure firming agent, described thickening agent is aerosil, described Hardening agent is electrically conductive graphite, and described silane coupler includes one or more in Silane coupling agent KH550, KH560, KH570, and described levelling agent is organic siliconresin.
6. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 5 is starched, it is characterized in that, the preferred isocyanate group content of described closure firming agent is the hexamethylene diisocyanate of 15～17%, the preferred bulk density of described aerosil is 50g/L, mean diameter is 12nm, the silica purity aerosil more than 99.8%, the preferred specific surface area of described electrically conductive graphite is 125m2/g, mean diameter 20～30mm, oil absorption is the electrically conductive graphite of 150, the preferred methyl silicon resin of described organic siliconresin.
7. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 1 is starched, it is characterised in that described organic solvent is one or both in isophorone, dibasic ester.
8. a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 7 is starched, it is characterised in that described dibasic ester is that dimethyl succinate, Glutaric Acid Dimethyl ester and dimethyl adipate are in mass ratio for the 3:4:3 dibasic ester mixed.
9. the preparation method starched for the antioxidation silver-bearing copper of electromagnetic shielding as claimed in claim 1, it is characterised in that the method comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of carrier: according to the percentage by weight of each component in step (1), first macromolecule resin is added in dissolution kettle together with organic solvent, it is sufficiently stirred for, until macromolecule resin is completely dissolved in organic solvent, granular sensation without resin, after standing 2h, then it is filtered remove impurity with 300～400 order polyester webs, namely prepares carrier；
(3) silver-bearing copper starches half-finished preparation: add in high speed dispersor with other each component by the carrier that step (2) prepares together with the percentage by weight in step (1), fully dispersed, until without powdered granule sense, namely preparing silver-bearing copper slurry semi-finished product；
(4) production of silver-bearing copper slurry: silver-bearing copper slurry semi-finished product step (3) prepared join in three-high mill, it is fully ground, until the fineness of silver-bearing copper slurry is less than 10 μm, the fine setting of silver-bearing copper slurry viscosity is carried out by adding appropriate organic solvent, making silver-bearing copper slurry viscosity is 10～20Pa S, it is filtered with 300 order stainless (steel) wires again, namely prepares the antioxidation silver-bearing copper for electromagnetic shielding and starch.
10. the preparation method that a kind of antioxidation silver-bearing copper for electromagnetic shielding according to claim 9 is starched, it is characterised in that the temperature of the dissolution kettle described in step (2) is 25～30 DEG C, and control mixing speed is 1000～3000r/min, stirs 5～6h；The rate of dispersion of the high speed dispersor described in step (3)；Step is 1000～3000r/min, disperses 20～30min；The roller rotating speed of the three-high mill described in step (4) is 60～80r/min, and it is 3 ± 0.25MPa that force value controls, roll 4～5 times.
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| CN109102917A (en) * | 2018-07-03 | 2018-12-28 | 北京中科纳通电子技术有限公司 | Electromagnetic shielding conductive slurry and preparation method thereof |
| CN111205719A (en) * | 2020-03-03 | 2020-05-29 | 深圳市利红金科技有限公司 | Silver-copper conductive paint and preparation method thereof |
| CN114334221A (en) * | 2022-01-10 | 2022-04-12 | 珠海方正科技多层电路板有限公司 | Hole plugging copper paste, preparation method thereof and printed circuit board |
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| CN114334221A (en) * | 2022-01-10 | 2022-04-12 | 珠海方正科技多层电路板有限公司 | Hole plugging copper paste, preparation method thereof and printed circuit board |
| CN114334221B (en) * | 2022-01-10 | 2024-02-09 | 珠海方正科技多层电路板有限公司 | Plug hole copper paste, preparation method thereof and printed circuit board |
| CN114464343A (en) * | 2022-01-20 | 2022-05-10 | 无锡晶睿光电新材料有限公司 | High-wear-resistance high-conductivity low-temperature curing silver paste and preparation method thereof |
| CN114464343B (en) * | 2022-01-20 | 2024-06-11 | 无锡晶睿光电新材料有限公司 | High-wear-resistance high-conductivity low-temperature cured silver paste and preparation method thereof |
| CN114639500A (en) * | 2022-03-29 | 2022-06-17 | 深圳市绚图新材科技有限公司 | Silver-doped silver-coated copper double-component sintered conductive paste and preparation method thereof |
| CN114603133A (en) * | 2022-04-02 | 2022-06-10 | 苏州博濬新材料科技有限公司 | Conductive silver paste containing multilevel-structure nano filler and preparation method thereof |
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