CN105436515B - A kind of preparation method of ultrafine electricity conductive circuit Nano silver solution - Google Patents

A kind of preparation method of ultrafine electricity conductive circuit Nano silver solution Download PDF

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CN105436515B
CN105436515B CN201510873988.7A CN201510873988A CN105436515B CN 105436515 B CN105436515 B CN 105436515B CN 201510873988 A CN201510873988 A CN 201510873988A CN 105436515 B CN105436515 B CN 105436515B
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solution
water
silver
preparation
dispersion
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CN105436515A (en
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邹敏昌
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Qingyuan Bajing New Material Co., Ltd.
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Foshan Solar Material & Equipment Co Ltd
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Abstract

The present invention relates to a kind of ultrafine electricity conductive circuit Nano silver solution, it is comprising following each component and its mass percentage content:Silver nitrate solution, tallow amine solution, triethanolamine solution, formalin and water soluble acrylic resin's dispersion;Its preparation method comprises the following steps:Silver nitrate solution first to constant temperature at 5 DEG C is stirred, while adding tallow amine;Triethanolamine is added as dilution, the pH value of whole solution is reached 7.2 7.9, formalin is added, the redox reaction to silver is carried out so that solution is translucent shape;Finally, water-based acrylic resin dispersion is added, until the transparent liquid of solution, now solution is finished product.

Description

A kind of preparation method of ultrafine electricity conductive circuit Nano silver solution
Technical field
The present invention is a kind of Nano silver solution for being used to print ultrafine electricity conductive circuit, is widely used in electronic product, for example It is alternative original to use silver powder system on computor-keyboard, thin film switch, touch-screen, solar cell, the electronic component such as capacitor and inductor Into the conducting wire of silver paste silk-screen manufacture craft, the consumption that can save silver reaches suitable electrical property, while reducing cost Quality standard does not drop.
Background technology
Very widely used today electric slurry is all made of using silver powder and organic solvent and resin bonding material.Silver powder conduct Conducting medium, has larger consumption just to reach good electric conductivity, because conductivity principle is closely connected by silver powder Electric action is produced together, silver content is small, cannot reach required conductive effectiveness, therefore cost will be higher, thus make With electric conductivity more preferably, more inexpensive products substitution silver powder just turns into the R&D direction of industry.
The content of the invention
The purpose of the present invention is can be directly reduced to elemental silver at a lower temperature using Nano silver solution, forms circuit and leads Superior electrical property, usage amount is low, meets electronics industry demand for development.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of ultrafine electricity conductive circuit Nano silver solution, it is characterized in that, contain comprising following each component and its mass percent Amount is:
Silver nitrate solution 20-70%;
Tallow amine solution 1-10%;
Triethanolamine solution 1-10%;
Formalin 10-30%;
Water soluble acrylic resin's dispersion 5-25%.
Another object of the present invention is to provide a kind of method for preparing ultrafine electricity conductive circuit Nano silver solution, it is characterized in that, Comprise the following steps:Silver nitrate solution first to constant temperature at 5 DEG C is stirred, while adding tallow amine;Add three Monoethanolamine makes the pH value of whole solution reach 7.2-7.9 as dilution, adds formalin, carries out the oxidation to silver also Original reaction so that solution is translucent shape;Finally, water-based acrylic resin dispersion is added, until the transparent liquid of solution, this When solution be finished product.
The preparation method of the silver nitrate solution is:Silver nitrate is used with 10% ratio and the quality for removing water ion water 90% After part ratio mixing, it is placed on the container of 5 DEG C of constant temperature or refrigeration is kept under 5 DEG C of solution temperature, use dasher stirring turn Speed is 30 turns/min, and silver nitrate solution is made.
The preparation method of the tallow amine solution is:Using single product of the active ingredient of tallow amine 100%, by matter The tallow amine of amount percentage 5% is mixed with 95% deionization hot water, is likewise cooled to 5 DEG C, and tallow amine solution is made.
The preparation method of the triethanolamine solution is:Single product of the active ingredient of triethanolamine 99%, take 40% mass parts Triethanolamine mixed with 60% deionized water, be placed under 5 DEG C of low temperature environment keep 2 hours after, be made triethanolamine solution.
The preparation method of the formalin is:After 10% formaldehyde is mixed with 90% deionized water by mass percentage, put In under 5 DEG C of low temperature, formalin is made.
The preparation method of water soluble acrylic resin's dispersion is:Using the water-soluble acrylic of solids content 35% Resin list product, then mixed by the single product of 1 part of water soluble acrylic resin with the mass parts of 4 parts of deionized waters, obtain acrylic resin Dispersion, acrylic dispersion and the mixing of 80% deionized water according still further to mass percent 20% are dispersed into solid and contained The liquid for 1.4% is measured, surfactant is added, protected as matrix, acrylic dispersion is dispersed in the aqueous solution In, water soluble acrylic resin's dispersion is made.
The beneficial effects of the invention are as follows:
A kind of ultrafine electricity conductive circuit Nano silver solution and preparation method thereof of the present invention, be using Nano silver solution compared with Elemental silver can be directly reduced under low temperature, formation circuit electric conductivity is superior, and usage amount is low, meeting electronics industry development will Ask.
Embodiment
With reference to embodiment, the present invention is further described.
A kind of ultrafine electricity conductive circuit Nano silver solution, it is characterized in that, contain comprising following each component and its mass percent Amount is:
Silver nitrate solution 55%;
Tallow amine solution 5.5%;
Triethanolamine solution 9.5%;
Formalin 25%;
Water soluble acrylic resin's dispersion 5%.
Another object of the present invention is to provide a kind of method for preparing ultrafine electricity conductive circuit Nano silver solution, it is characterized in that, Comprise the following steps:Silver nitrate solution first to constant temperature at 5 DEG C is stirred, while being slowly added to tallow amine, makes two After kind liquid is well mixed;Triethanolamine is added as dilution, the pH value of whole solution is reached 7.5(Can just negative bias Poor 0.2), formalin is slow added into, the redox reaction to silver is carried out so that part silver is with nanometer-level silver particle shape Into suspension so that solution is translucent shape Nano silver solution;Finally, water-based acrylic resin dispersion is slowly added to, until The transparent liquid of solution, calculates the addition of now water-based acrylic resin dispersion, and now solution is finished product, you can for applying Cloth is printed on electronic product and produces conducting wire, Nano Silver now by 130 DEG C, 30min baking temperature and when Between after, it is already possible to sintering be in close silver wire, meticulously spread over and conducting wire formed on electronic product, water soluble acrylic acid tree Then as binding agent, silver wire and ground are combined together for fat dispersion, and the electric conductivity of silver is not influenceed.
In the present invention, with tallow amine as dispersant in silver nitrate solution, and triethanolamine is used as reducing agent.
The preparation method of the silver nitrate solution is:Silver nitrate is used with 10% ratio and the quality for removing water ion water 90% After part ratio mixing, it is placed on the container of 5 DEG C of constant temperature or refrigeration is kept under 5 DEG C of solution temperature, use dasher stirring turn Speed is 30 turns/min, and silver nitrate solution is made.
The preparation method of the tallow amine solution is:Using single product of the active ingredient of tallow amine 100%(Dan Pin For the existing goods of Akzo Nobel's surfactant company), by mass percentage 5% tallow amine and 95% go from Sub- hot water(80℃)Mixing, is likewise cooled to 5 DEG C, and tallow amine solution is made.
The preparation method of the triethanolamine solution is:Single product of the active ingredient of triethanolamine 99%, analyze pure product, take Mixed, be placed in after being kept for 2 hours under 5 DEG C of low temperature environment with 60% deionized water with the triethanolamine of 40% mass parts, be made three Ethanolamine solutions.
The preparation method of the formalin is:Using commercial goods, by mass percentage 10% formaldehyde and 90% go from After sub- water mixing, it is placed under 5 DEG C of low temperature, formalin is made.
The preparation method of water soluble acrylic resin's dispersion is:Using the water-soluble acrylic of solids content 35% Resin list product, are dispersed into solid and contain according to the acrylic dispersion of mass percent 20% and the mixing of 80% deionized water Amount(That is acrylic resin content)For 1.4% liquid, 0.01% Du Pont's Zonyl fluorocarbon surfactants are added, base is used as Body is protected, and is dispersed in the aqueous solution with enabling acrylic dispersion more fine uniform, and water soluble acrylic resin is made Dispersion.
Nano silver grain can be wrapped in this low surface when silver-colored solution is added to after water soluble acrylic resin's dispersion , can be with resin after exactly these resin microspheres for containing Nano silver grain are heated in the acrylic resin dispersion microsphere of tension force With reference to sticking on electronic product, again can by Nano silver grain closely network together into conductive line.
The main points and effect principle of the present invention:
This invention core is that the particle diameter of the selection of water-based acrylic resin dispersion, wherein pH value and dispersion is big Small is the key of selection, and the pH value of present invention selection water-based acrylic resin dispersion is 7.8 commercial goods, dispersible granule seed Footpath is 0.2 micron.The operating method for adding technique is also crucial, end product is turned into transparency liquid, could illustrate now Silver be liquid nano, can just form low-temperature sintering when being toasted for last heating, Nano silver grain is sintered into integral chain The silver wire connect, electric conductivity is superior.
The present invention is to utilize sufficient dispersant(Tallow amine)And surfactant(Fluorocarbon surfactant)To nitre Silver in sour silver solution forms the silver particles of nanometer particle size when being reduced into silver powder, select such a dispersant and surfactant to be Necessary key technology.

Claims (6)

1. a kind of method for preparing ultrafine electricity conductive circuit Nano silver solution, it is characterized in that, include following each component and its quality Degree is:
Silver nitrate solution 20-70%;
Tallow amine solution 1-10%;
Triethanolamine solution 1-10%;
Formalin 10-30%;
Water soluble acrylic resin's dispersion 5-25%;
Its preparation method comprises the following steps:Silver nitrate solution first to constant temperature at 5 DEG C is stirred, while adding tallow Fat amine;Triethanolamine is added as dilution, the pH value of whole solution is reached 7.2-7.9, adds formalin, is carried out To the redox reaction of silver so that solution is translucent shape;Finally, water-based acrylic resin dispersion is added, until solution Transparent liquid, now solution is finished product.
2. the method for ultrafine electricity conductive circuit Nano silver solution is prepared according to claim 1, it is characterized in that, the silver nitrate The preparation method of solution is:Silver nitrate is used after the mass parts ratio of water ion water 90% mixes, to be placed on 10% ratio with going The container or refrigeration that 5 DEG C of constant temperature are kept under 5 DEG C of solution temperature, the use of dasher speed of agitator are 30 turns/min, are made Silver nitrate solution.
3. the method for ultrafine electricity conductive circuit Nano silver solution is prepared according to claim 1, it is characterized in that, the tallow The preparation method of fat amine aqueous solution is:Using the tallow of the single product, by mass percentage 5% of the active ingredient of tallow amine 100% Fat amine is mixed with 95% deionization hot water, is likewise cooled to 5 DEG C, and tallow amine solution is made.
4. the method for ultrafine electricity conductive circuit Nano silver solution is prepared according to claim 1, it is characterized in that, three ethanol The preparation method of amine aqueous solution is:Single product of the active ingredient of triethanolamine 99%, the triethanolamine and 60% for taking 40% mass parts go from Sub- water mixing, is placed in after being kept for 2 hours under 5 DEG C of low temperature environment, triethanolamine solution is made.
5. the method for ultrafine electricity conductive circuit Nano silver solution is prepared according to claim 1, it is characterized in that, the formaldehyde is molten The preparation method of liquid is:After 10% formaldehyde is mixed with 90% deionized water by mass percentage, it is placed under 5 DEG C of low temperature, first is made Aldehyde solution.
6. the method for ultrafine electricity conductive circuit Nano silver solution is prepared according to claim 1, it is characterized in that, the water solubility The preparation method of acrylic dispersion is:Using the single product of the water soluble acrylic resin of solids content 35%, then by 1 part of water Soluble acrylic resin list product are mixed with the mass parts of 4 parts of deionized waters, obtain acrylic dispersion, according still further to quality hundred Divide acrylic dispersion and 80% deionized water than 20% to mix the liquid for being dispersed into that solids content is 1.4%, then add Enter surfactant, protected as matrix, acrylic dispersion is dispersed in the aqueous solution, water-soluble acrylic tree is made Fat dispersion.
CN201510873988.7A 2015-12-03 2015-12-03 A kind of preparation method of ultrafine electricity conductive circuit Nano silver solution Active CN105436515B (en)

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Effective date of registration: 20180614

Address after: 513499 Qingyuan City, Guangdong province Lianzhou city Qingyuan South National Industrial Park (land number):06380100017)

Patentee after: Qingyuan Bajing New Material Co., Ltd.

Address before: 528308 Shunde District, Foshan City, Guangdong Province, Xintang world long industrial zone Shilong Avenue (Shilin gloves Co., Ltd., the first floor of the workshop)

Patentee before: FOSHAN SOLAR MATERIAL & EQUIPMENT CO., LTD.