CN101214547A - Micrometer silver-copper granule containing nano level surface structure and preparation and application thereof - Google Patents
Micrometer silver-copper granule containing nano level surface structure and preparation and application thereof Download PDFInfo
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- CN101214547A CN101214547A CNA2008100256614A CN200810025661A CN101214547A CN 101214547 A CN101214547 A CN 101214547A CN A2008100256614 A CNA2008100256614 A CN A2008100256614A CN 200810025661 A CN200810025661 A CN 200810025661A CN 101214547 A CN101214547 A CN 101214547A
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Abstract
The invention discloses a micron silver-copper particle with a nanometer-grade surface structure and a preparing method and usage for the particle. The invention takes silver powder, sliver copper clad powder or silver-copper mixed power with micron dimensions as a carrying stroma; firstly disperses the silver powder, the sliver copper clad powder or the silver-copper mixed power body into a solvent, then uses a reducing compound to reduce silver salt into nanometer silver power and precipitate on the surface of the carrying stroma; and finally filters and dries to acquire the micron silver-copper particle with a nanometer-grade surface structure which can be used as fillings for preparing an electromagnetic shielding paint or an conductive adhesive. The invention utilizes a principle of chemical reducing to change the surface topography layout of the sliver-copper particle with nanometer-grade to lead the silver-copper particle to contain a nanometer-grade surface structure, thus reducing the surface sintering or melting temperature and improving the overall conductive performance.
Description
Technical field
The present invention relates to the macromolecule conducting material field, particularly a kind of micrometer silver-copper granule that contains nano level surface structure and preparation method thereof.
Background technology
Conductive polymer glue replaces lead/tin class welding material in a plurality of fields, is widely used in industries such as electronics, information.But, to compare with lead/tin class welding material, the major defect of conductive polymer glue is relatively low electric conductivity and expensive noble metal filler price.
The monolithic conductive of conductive polymer glue depends on three factors: the resistance of metal packing itself, the contact resistance between filler, and the contact resistance between this electrically-conducting paint and the electronic original part.Wherein, the effective method of overall electrical resistance that reduces conductive polymer glue is the uniformity that reduces the contact resistance between filler and improve fillers dispersed.Therefore, the size of conducting metal filler and pattern, and its filling rate and dispersion effect in the middle of resin has very important influence for material monolithic electric conductivity.The isotropism macromolecule conducting material must be through the operation of hot setting when using.In the solidification process, because the effect of resin material polymerization shrinkage, the chance that is in contact with one another between the metal packing increases, thereby has formed numerous local tie point between metal packing, and the last integral body of material embodies electric conductivity.
But, because the existing reproducibility of metal itself, and molecular resin is to the influence of metal surface, even very high metal filled amount (for example quality accounts for 80% fine silver powder filling rate) also may not necessarily make the isotropism macromolecule conducting material obtain excellent conducting performance.Its reason mainly is that burning at high temperature produces the relatively poor sull of electric conductivity or forms metal complex with resin additive (as catalyst).In addition, because the fusing point of conductive filler silver powder commonly used surpasses 900 ℃, conventional curing means can't make the abundant sintering of filler particle.Above-mentioned these make the extensive use of isotropism macromolecule conducting material face very big challenge.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art, provide a kind of and conduct electricity very well, good stability, the micrometer silver-copper granule that contains nano level surface structure that cost is low.
Another object of the present invention is to provide a kind of above-mentioned preparation method who contains the micrometer silver-copper granule of nano level surface structure.
A further object of the present invention is to provide a kind of above-mentioned purposes that contains the micrometer silver-copper granule of nano level surface structure.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method who contains the micrometer silver-copper granule of nano level surface structure, comprise the steps: that silver powder, silver-coated copper powder or silver-copper mixed powder with micron-scale is for supporting matrix, at first silver powder, silver-coated copper powder or silver-copper mixed powder is dispersed in the solvent, make silver salt be reduced to nano-silver powder with the reproducibility compound then, and be deposited on the described stromal surface that supports, refilter, drying, obtain containing the micrometer silver-copper granule of nano level surface structure.
The average-size of the silver powder of described micron-scale, silver-coated copper powder or silver-copper mixed powder is 1～100 micron, and the pattern of powder comprises sheet, spherical, graininess, bar-shaped, wire, helical form or 3-d modelling, or the mixed powder of above-mentioned various patterns.
Described reproducibility compound is one or more mixtures in vitamin C (ascorbic acid), citric acid, citrate, lithium aluminium hydride, sodium borohydride, polyphenol compound, the aldehyde compound.Described polyphenol compound can be catechol, pyrogallol, connection-catechol, 3,4-dihydroxy benzenes propionic acid, 3,4-dihydroxy benzenes propylamine or anthocyan compound.Described aldehyde compound can be formic acid, formaldehyde, acetaldehyde, benzaldehyde, fatty aldehyde compounds or benzaldehyde derivative.
Described silver salt is that silver nitrate, silver acetate, silver iodide, silver bromide, silver chlorate, silver tetrafluoroborate, acetopyruvic acid silver or silver-colored ammino close reagent; Described silver-colored ammino closes reagent and can be that ethylenediamine closes silver, silver-colored ammonia or other contains the silver complex that contains of primary amine, secondary amine structure.
It is that 1: 0.5～10 ratio adds silver powder, silver-coated copper powder or silver-copper mixed powder in the solvent that described dispersion is meant in mass ratio, and the mechanical agitation rotating speed is 20～3000 rev/mins, disperses 1～60 minute, until no obvious solids precipitation.Described solvent is one or more mixtures in methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, new butanols, acetone, MEK, ethylene glycol, acetonitrile, chloroform, carrene, oxolane, pure water or the dilution salt solution.
The mol ratio of described silver salt and reproducibility compound is 10: 1～0.1: 1.Described silver salt is 1: 10000～1: 5 with the mass ratio that supports matrix.After can be earlier reproducibility compound and silver salt dissolved respectively or disperseing, join simultaneously in silver powder, silver-coated copper powder or silver-copper mixed powder slurries, the joining day was controlled at 0.5～120 minute again; Reaction temperature is 0～70 ℃.
The temperature of described drying is 0～100 ℃; Or adopting pump to drain solvent, pressure range is carried out drying between 1～0.0001 atmospheric pressure.
Adopt the micrometer silver-copper granule that contains nano level surface structure of method for preparing, the quality that wherein is deposited on the nano-silver powder particle on micrometer silver-copper granule surface accounts for 0.1～90% of gross mass; Size range is 0.1～500 nanometer; Active force each other is simple absorption or lattice combination; This nano particle is fine silver crystal (can contain the residual of small amounts silver or raw material silver salt).
The described micrometer silver-copper granule that contains nano level surface structure can be used as filler and is used to prepare electromagnetic shielding lacquer or conducting resinl.Technology such as prepared electromagnetic shielding lacquer or conductive silver glue coating can be used for the chip encapsulation, and pin-hole encapsulates, and the interface bonds, and dot matrix is printd, and the printing of circuit and antenna and chip are integrated.The product of using this technology can comprise computer, image display, mobile phone, Digital A equipment, palm PC, electronic toy, electronic game machine, signal emission and recognition device etc.
The present invention compared with prior art has following advantage and effect:
(1) the present invention utilizes the principle of electronation, changes the surface topography layout of micron order silver-copper granule, makes it contain nano level surface structure, has reduced surperficial sintering or melt temperature, has improved the monolithic conductive performance.
(2) raw materials technology involved in the present invention is with cheap silver powder particles, and silver-coated copper powder particle and silver-copper hybrid particles is that primary raw material is aided with a small amount of silver salt and reducing agent is processed; Owing to have toxic byproduct is not arranged, solvent produces any pollution hardly after reclaiming; The technological process easy operating, properties of product are reliable and stable.
Description of drawings
The electron scanning micrograph of the micron flake silver powder that contains the Nanosurface structure that Fig. 1 prepares for embodiment 1.
The specific embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiments of the present invention are not limited thereto.
Embodiment 1
Under the room temperature, be 30 microns (99.5%) 1 kilogram in sheet fine silver powder with particle mean size, 3,4-dihydroxy benzenes propionic acid 2 grams (0.5%).Speed with 100 rev/mins in 10 liters of ethanolic solutions stirred 30 minutes, and then added silver nitrate 17 grams, sodium borohydride 4 grams; Continuation was stirred 60 minutes with 100 rev/mins speed.Filter out silver powder, powder liquid is sloughed unnecessary solvent through 500 rev/mins the centrifuge solvent of leaving away with vavuum pump, obtains containing the micron flake silver powder of Nanosurface structure.
As shown in Figure 1, this shown molecule nano-silver powder in micro-silver powder surface for producing through this PROCESS FOR TREATMENT.
Embodiment 2
Under the room temperature, be 24 microns 20 kilograms of sheet silver-coated copper powders (silver: the mass ratio of copper is 5: 5), in 200 liters of ethanolic solutions, stirred 30 minutes with particle mean size.And then adding chlorination silver powder 560 grams, citric acid 780 restrains; Continuation was stirred 120 minutes with 100 rev/mins speed.Powder liquid filters and drains through filter paper, obtains containing the micron sheet silver-coated copper powder of Nanosurface structure.
Embodiment 3
Under the room temperature, with particle mean size is that 30 microns sheet fine silver powder (99.5%) 5 kg.p.m. is dispersed in 50 liters of ethanolic solutions, stirred 30 minutes, drip 500 milliliters of ethanolic solutions containing 22 gram acetaldehyde simultaneously and contain 500 milliliters of ethanolic solutions of 85 gram silver nitrates, the speed that continues with 100 rev/mins stirred 120 minutes.Powder liquid filters and drains through filter paper, obtains containing the micron flake silver powder of Nanosurface structure.
Embodiment 4
Under the room temperature, with particle mean size is that 50 microns sheet fine silver powder (99.5%) 1 kg.p.m. is dispersed in 10 liters of ethanolic solutions, stirred 30 minutes, drip 100 milliliters of ethanolic solutions containing 1.1 gram catechols simultaneously and contain 100 milliliters of ethanolic solutions of 17 gram silver nitrates, the speed that continues with 100 rev/mins stirred 100 minutes.Powder liquid filters and drains through filter paper, obtains containing the micron flake silver powder of Nanosurface structure.
Table 1
| Embodiment 1 sample (mass percent) | Specific insulation | Control sample (mass percent) | Specific insulation |
| ?80％ | 1.1×10 -5ohm-cm | ?80％ | 9.5×10 -5ohm-cm |
| ?77.5％ | 1.9×10 -5ohm-cm | ?77.5％ | 1.3×10 -4ohm-cm |
| ?75％ | 2.9×10 -5ohm-cm | ?75％ | 2.9×10 -4ohm-cm |
| ?72.5％ | 3.8×10 -5ohm-cm | ?72.5％ | 7.6×10 -4ohm-cm |
| ?70％ | 5.4×10 -5ohm-cm | ?70％ | 9.1×10 -3ohm-cm |
Specific insulation after the sample that table 1 prepares for process embodiment 1 fully mixes, solidifies with resin with different mass percents respectively.The measurement way is 4 point probe probe methods.The control sample of being taked is not surface treated fine silver powder particles, and buying is from Greatwall Gold ﹠ Silver Refinery.Resin is DER383 (DOW) epoxy resin, and curing agent is a methyl tetrahydrochysene base phthalic anhydride, and catalyst is the 2-ethyl, 4-methyl amidine Cuo.Condition of cure is 160 ℃, 5 minutes.
Table 2
| Embodiment 2 samples (mass percent) | Specific insulation | Control sample (mass percent) | Specific insulation |
| ?80％ | 8.9×10 -4ohm-cm | ?80％ | 5.5×10 -3ohm-cm |
| ?77.5％ | 1.8×10 -3ohm-cm | ?77.5％ | 8.5×10 -3ohm-cm |
| ?75％ | 2.4×10 -3ohm-cm | ?75％ | 3.9×10 -2ohm-cm |
| ?72.5％ | 7.6×10 -3ohm-cm | ?72.5％ | 8.6×10 -2ohm-cm |
| ?70％ | 1.4×10 -2ohm-cm | ?70％ | 7.4×10 -1ohm-cm |
Specific insulation after the sample that table 2 prepares for embodiment 2 fully mixes, solidifies with resin with different mass percents respectively.The measurement way is 4 point probe probe methods.The control sample of being taked uses not surface treated silver-coated copper powder particle, and buying is from Wuxi City Ou Manke metal powder factory.Resin is DER383 (DOW) epoxy resin, and curing agent is a methyl tetrahydrochysene base phthalic anhydride, and catalyst is the 2-ethyl, 4-methyl amidine Cuo.Condition of cure is 160 ℃, 5 minutes.
By table 1 and table 2 as seen, the micrometer silver-copper granule with nano level surface structure through and mixed with resin processing after, show comparatively superior electric conductivity.
Claims (10)
1. preparation method who contains the micrometer silver-copper granule of nano level surface structure, it is characterized in that comprising the steps: that silver powder, silver-coated copper powder or silver-copper mixed powder with micron-scale is for supporting matrix, at first silver powder, silver-coated copper powder or silver-copper mixed powder is dispersed in the solvent, make silver salt be reduced to nano-silver powder with the reproducibility compound then, and be deposited on the described stromal surface that supports, refilter, drying, obtain containing the micrometer silver-copper granule of nano level surface structure.
2. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1 is characterized in that: described reproducibility compound is one or more mixtures in vitamin C, citric acid, citrate, lithium aluminium hydride, sodium borohydride, polyphenol compound, the aldehyde compound.
3. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1 is characterized in that: described silver salt is that silver nitrate, silver acetate, silver iodide, silver bromide, silver chlorate, silver tetrafluoroborate, acetopyruvic acid silver or silver-colored ammino close reagent.
4. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1, it is characterized in that: it is that 1: 0.5～10 ratio adds silver powder, silver-coated copper powder or silver-copper mixed powder in the solvent that described dispersion is meant in mass ratio, the mechanical agitation rotating speed is 20～3000 rev/mins, disperseed 1～60 minute, until no obvious solids precipitation.
5. according to claim 1 or the 4 described preparation methods that contain the micrometer silver-copper granule of nano level surface structure, it is characterized in that: described solvent is one or more mixtures in methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, new butanols, acetone, MEK, ethylene glycol, acetonitrile, chloroform, carrene, oxolane, pure water or the dilution salt solution.
6. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1 is characterized in that: the mol ratio of described silver salt and reproducibility compound is 10: 1～0.1: 1.
7. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1 is characterized in that: described silver salt is 1: 10000～1: 5 with the mass ratio that supports matrix.
8. the preparation method who contains the micrometer silver-copper granule of nano level surface structure according to claim 1, it is characterized in that: after earlier reproducibility compound and silver salt being dissolved respectively or disperseing, join simultaneously in silver powder, silver-coated copper powder or silver-copper mixed powder slurries, the joining day was controlled at 0.5～120 minute again; Reaction temperature is 0～70 ℃.
9. micrometer silver-copper granule that contains nano level surface structure, it is characterized in that: each described method prepares in the employing claim 1～8, and the quality that wherein is deposited on the nano-silver powder particle on micrometer silver-copper granule surface accounts for 0.1～90% of gross mass; Size range is 0.1～500 nanometer; Active force each other is simple absorption or lattice combination.
10. a purposes that contains the micrometer silver-copper granule of nano level surface structure is characterized in that: be used to prepare electromagnetic shielding lacquer or conducting resinl as filler.
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