CN107135602A - A kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit - Google Patents
A kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit Download PDFInfo
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- CN107135602A CN107135602A CN201710345090.1A CN201710345090A CN107135602A CN 107135602 A CN107135602 A CN 107135602A CN 201710345090 A CN201710345090 A CN 201710345090A CN 107135602 A CN107135602 A CN 107135602A
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- silver
- grain
- nano
- low
- temperature sintering
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1241—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing
- H05K3/125—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing by ink-jet printing
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1283—After-treatment of the printed patterns, e.g. sintering or curing methods
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/11—Treatments characterised by their effect, e.g. heating, cooling, roughening
- H05K2203/1131—Sintering, i.e. fusing of metal particles to achieve or improve electrical conductivity
Abstract
The high method for leading Nano silver grain flexible conductive circuit is prepared the invention discloses a kind of low-temperature sintering.This method is using silver acetate solutions and silver nano-grain dispersion liquid formation composite conducting ink, obtained composite conducting ink is injected in neutral signature pen or ink-jet printer cartridge, circuit pattern needed for directly writing or print on fexible film substrate, the fexible film substrate for being printed with circuit pattern is placed on low-temperature sintering in thermal station, the height is obtained on fexible film substrate and leads Nano silver grain flexible conductive circuit.The inventive method solves the problem of high sintering temperature influences on flexible substrate, and i.e. sinterable at low temperature to prepare, reduction sintering temperature and reduction have saved cost to the demand of silver nano-grain solid content.
Description
Technical field
The present invention relates to flexible printing electronic technology field, and in particular to a kind of low-temperature sintering prepares height and leads Nano silver grain
The method of flexible conductive circuit.
Background technology
As printed electronics develop to flexibility, portable, wearable and inexpensive etc. direction, with plastics, paper
, the flexible material such as cloth is also being continuously increased as the demand of the circuit of substrate.In addition to conventional printed circuit methods, make
Directly write with neutral signature pen or ink-jet printer printing, even more a kind of convenient flexible circuit preparation means.
Macromolecule dispersant is often added in the preparation process of metal nanoparticle ink, metal nano is coated on
Grain surface, so as to improve the stability of metallic conduction ink.But the protective agent on metal nanoparticle is coated on, is often hindered
Hinder transmission of the electronics between metal nanoparticle, it is impossible to play a part of conductive path.So circuit after the printing is needed
Want the process of a post processing to promote particle to sinter, improve circuit conductive.
Lesyuk etc.（Lesyuk et al., Microelectron Eng, 2011, 88: 318–321）In ceramic base
Silver particles are printed on bottom and with the YAG of 1064 nm wavelength:Nd pulse lasers sinter silver wire into；Yang etc.（Yang et
al., Adv Mater, 2011, 23: 3052–3056）Formed on paper after nano grain of silver sub-pattern, then the side through hot pressing
Method obtains the silver wire circuit of conduction；Magdassi etc.（Magdassi et al., ACS Nano, 2010, 4: 1943–
1948）It was found that, when the electronegative silver particles that Sodium Polyacrylate is coated and the diallyl dimethyl chlorine for carrying opposite charges
When changing ammonium (PDAC) contact, it can spontaneously assemble and obtain preferable electric conductivity.Above physics and chemical processing means equipment
It is required that high, step is complicated, cost is high.
Nano effect just refers to that nano material has unusual or unusual physics, chemistry not available for traditional material special
Property.Solid matter is when its form is large scale, and its fusing point is fixed, has been found that its fusing point will significantly drop after Ultrafine
It is low.Silver point is about 960 DEG C, and particle diameter for 50 nm Argent grain fusing point at 200 DEG C or so.Therefore, super fine silver powder is made
Electrocondution slurry can carry out low-temperature sintering.
The content of the invention
Nano silver grain compliant conductive is led in view of the deficiencies of the prior art, the present invention provides a kind of low-temperature sintering prepares height
The method of circuit.This method is according to the small-size effect in nano effect, using without seed activity ink（Silver acetate solutions）With
Conventional particles ink（Silver nano-grain dispersion liquid）Composite conducting ink prepared by the mode being combined, without using high temperature, but
Using simple low-temperature sintering silver nanoparticles sinter together, be by the silver ion reduction being filled between silver nano-grain
Silver-colored simple substance, is sintered at low temperature, so as to form conductive path.
The present invention is achieved through the following technical solutions.
A kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit, comprises the following steps：
（1）Silver acetate solutions are well mixed with silver nano-grain dispersion liquid, composite conducting ink is obtained；
（2）Obtained composite conducting ink is injected in neutral signature pen or ink-jet printer cartridge, on fexible film substrate
Circuit pattern needed for directly writing or print；
（3）The fexible film substrate for being printed with circuit pattern is placed on low-temperature sintering in thermal station, on fexible film substrate
Nano silver grain conducting channel is led to the height.
Further, step（1）In, the concentration of the silver acetate solutions is 2 ~ 4wt%.
Further, step（1）In, the solvent of the silver acetate solutions is ethanol and the mixed solvent of ethylene glycol.
Further, the volume ratio of the in the mixed solvent of the ethanol and ethylene glycol, ethanol and ethylene glycol is 10 ~ 15:
1。
Further, step（1）In, the concentration of the silver nano-grain dispersion liquid is 20-35wt%.
Further, step（1）In, the solvent of silver nano-grain dispersion liquid is triethylene glycol monomethyl ether.
Further, step（1）In, in the silver nano-grain dispersion liquid, the particle diameter of silver nano-grain is 20 ~ 50 nm.
Further, step（1）In, the mixed volume ratio of the silver acetate solutions and silver nano-grain dispersion liquid for 2 ~
1.5:1。
Further, step（2）In, the fexible film substrate includes polyethylene terephthalate's substrate, polyamides
Imines substrate, dimethyl silicone polymer substrate, polymethyl methacrylate substrate or polycarbonate substrate.
Further, step（3）In, the low-temperature sintering is 3 ~ 5min of heating at 80 ~ 100 DEG C.
Compared with prior art, the invention has the advantages that and beneficial effect：
（1）Active composite conducting ink is made in the mode that the inventive method is combined using silver acetate solutions and silver nano-grain dispersion liquid
Water, the introducing of silver ion can strengthen the connection between silver nano-grain, so as to obtain the circuit of high conductivity at low temperature, solution
The problem of high sintering temperature of having determined influences on flexible substrate；
（2）The inventive method uses neutrality label using silver acetate solutions and silver nano-grain dispersion liquid formation composite conducting ink
Conductive pattern needed for word pen or ink-jet printer printing, silver acetate is filled between silver nano-grain, utilizes reduction of ethylene glycol
The silver ion reduction being introduced into is silver-colored simple substance, so as to form conductive path between silver nano-grain, reduces sintering temperature and subtracts
The small demand to silver nano-grain solid content, has saved cost.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention；
Fig. 2 is principle schematic of the invention；
Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d be embodiment 1 in sinter after ink transmission electron microscope picture；
Fig. 4 a and Fig. 4 b scheme for the resistivity contrasts of circuit after being sintered in embodiment 1.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment, but protection domain of the presently claimed invention is simultaneously
It is not limited to following examples.
The preparation method of the present invention according to the small-size effect of metal nanoparticle, and using without seed activity ink with passing
Composite conducting ink is made in the mode that system particle ink is combined, and realizes that height leads the low-temperature sintering system of Nano silver grain conducting channel
Standby, concrete technology flow process is as shown in figure 1, including step：（1）The preparation of silver acetate solutions and silver nano-grain dispersion liquid, by second
Sour silver solution and silver nano-grain dispersion liquid are mixed with composite conducting ink；（2）Composite conducting ink neutrality label will be prepared
Word pen or ink-jet printer print required conductive pattern on flexible substrates；（3）Low-temperature sintering, is obtained on fexible film substrate
The height leads Nano silver grain conducting channel.
The principle schematic of preparation method of the present invention is as shown in Fig. 2 silver acetate is dispersed in around silver nano-grain, profit
The silver ion reduction that spent glycol reproducibility is introduced into is silver-colored simple substance, so as to form conductive path between silver nano-grain.
Embodiment 1
Low-temperature sintering prepares height and leads Nano silver grain flexible conductive circuit, comprises the following steps：
（1）Take 3.75 ml ethanol and 0.25 ml ethylene glycol to be mixed into beaker, mixed solvent is made；
（2）Weigh 66.76 mg acetic acid silver powders and be dissolved in step（1）In the mixed solvent, beaker is positioned on magnetic stirring apparatus
Stirring 1 hour, carries out suction filtration with 0.45 μm of filter membrane afterwards, obtains silver acetate solutions, standby；
（3）20 ~ 50 nm silver nano-grain is dispersed in triethylene glycol monomethyl ether, the silver nano-grain for forming 20wt% disperses
Liquid；
（4）By step（2）Obtained silver acetate solutions and step（3）Obtained silver nano-grain dispersion liquid is with 2:1 volume ratio
Mixing, is made composite conducting ink；
（5）Empty pen core is cleaned with ethanol, the Kapton of cutting 2cm × 2cm sizes is simultaneously clean with ethanol；
（6）With needle tubing by step（4）Obtained composite conducting ink is injected into the Neutral ball-point for ball-point pen of cleaning；
（7）With the pen core containing active composite conducting ink, required circuit pattern is directly write out on Kapton；
（8）The Kapton that writing has circuit is placed in thermal station, temperature is slowly increased to 100 DEG C, heated 5 minutes, system
Obtain flexible conductive circuit pattern.
Fig. 3 a ~ Fig. 3 d are the transmission electron microscope picture of the ink after sintering；Fig. 3 a are shown after oversintering, the silver in silver acetate
Ion is silver-colored simple substance by reduction of ethylene glycol, and the particle diameter of silver-colored simple substance is mainly distributed on 10 ~ 15nm；Fig. 3 b show the ink after sintering
In silver nano-grain, its particle diameter is mainly distributed on 35 ~ 45 nm；Fig. 3 c show the compound particles of ink of activity, and its particle diameter is main
It is distributed in 30 ~ 70nm；As can be seen that the silver ion in compound ink is reduced to silver-colored list around former silver nano-grain well
Matter, increases its particle diameter；Fig. 3 d show that silver nano-grain is with the help of silver ion in the compound ink of activity, and good is viscous
Knot together, i.e., there occurs following reaction in sintering process：
OH-CH2-CH2-OH → CH3CHO+H2
CH3CHO+Ag+ → Ag0+H++CH3CO-CO-CH3 。
Fig. 4 a and Fig. 4 b illustrate the compound ink of activity and silver nano-grain（AgNPs）Dispersion liquid is at 80 DEG C and 100 DEG C
The contrast of electric conductivity after sintering 3 minutes, 5 minutes respectively, the AgNPs dispersion liquids of wherein control group are added and composite ink aqueous phase
Ethanol, the ethylene glycol of same volume；As can be seen from Figure, after oversintering, the introducing of silver ion makes the resistivity of conducting channel
There is obvious decline, 100 DEG C of sintering 5min of the present embodiment 1 resistivity, the introducing of silver ion makes the resistance of conducting channel
Rate is changed into 60.89 μ Ω cm from 80.08 μ Ω cm.
Embodiment 2
Low-temperature sintering prepares height and leads Nano silver grain flexible conductive circuit, comprises the following steps：
（1）Take 3.75 ml ethanol and 0.3 ml ethylene glycol to be mixed into beaker, mixed solvent is made；
（2）Weigh 91.24 mg acetic acid silver powders and be dissolved in step（1）In the mixed solvent, beaker is positioned on magnetic stirring apparatus
Stirring 1 hour, carries out suction filtration with 0.45 μm of filter membrane afterwards, obtains silver acetate solutions, standby；
（3）20 ~ 50 nm silver nano-grain is dispersed in triethylene glycol monomethyl ether, the silver nano-grain for forming 30wt% disperses
Liquid；
（4）By step（2）Obtained silver acetate solutions and step（3）Obtained silver nano-grain dispersion liquid is with 1.8:1 volume
Than mixing, composite conducting ink is made；
（5）Empty pen core is cleaned with ethanol, the polycarbonate membrane of cutting 2cm × 2cm sizes is simultaneously clean with ethanol；
（6）With needle tubing by step（4）Obtained composite conducting ink is injected into the Neutral ball-point for ball-point pen of cleaning；
（7）With the pen core containing active composite conducting ink, required circuit pattern is directly write out on polycarbonate membrane；
（8）The polycarbonate membrane that writing has circuit is placed in thermal station, temperature is slowly increased to 95 DEG C, heated 3 minutes, is made
Flexible conductive circuit pattern.
After oversintering, silver ion in silver acetate is silver-colored simple substance by reduction of ethylene glycol, and the particle diameter of silver-colored simple substance is mainly distributed
In 12 ~ 15nm；The silver nano-grain in ink after sintering, its particle diameter is mainly distributed on 35 ~ 40 nm；The compound ink of activity
The particle diameter of grain is mainly distributed on 40 ~ 60nm；Silver ion in compound ink is reduced to around former silver nano-grain well
Silver-colored simple substance, increases its particle diameter, and silver nano-grain is with the help of silver ion in the compound ink of activity, and good is bonded in
Together.
95 DEG C of the present embodiment 2 sintering 3min resistivity, the introducing of silver ion makes the resistivity of conducting channel from 83.12
μ Ω cm are changed into 69.77 μ Ω cm.
Embodiment 3
Low-temperature sintering prepares height and leads Nano silver grain flexible conductive circuit, comprises the following steps：
（1）Take 3.75 ml ethanol and 0.37 ml ethylene glycol to be mixed into beaker, mixed solvent is made；
（2）Weigh 136.45 mg acetic acid silver powders and be dissolved in step（1）In the mixed solvent, beaker is positioned over magnetic stirring apparatus
Upper stirring 1 hour, carries out suction filtration with 0.45 μm of filter membrane afterwards, obtains silver acetate solutions, standby；
（3）20 ~ 50 nm silver nano-grain is dispersed in triethylene glycol monomethyl ether, the silver nano-grain for forming 35wt% disperses
Liquid；
（4）By step（2）Obtained silver acetate solutions and step（3）Obtained silver nano-grain dispersion liquid is with 1.5:1 volume
Than mixing, composite conducting ink is made；
（5）Empty pen core is cleaned with ethanol, the polydimethylsiloxanefilm film of cutting 2cm × 2cm sizes is simultaneously clean with ethanol；
（6）With needle tubing by step（4）Obtained composite conducting ink is injected into the Neutral ball-point for ball-point pen of cleaning；
（7）With the pen core containing active composite conducting ink, required circuit is directly write out in polydimethylsiloxanefilm film
Pattern；
（8）The polydimethylsiloxanefilm film that writing has circuit is placed in thermal station, temperature is slowly increased to 80 DEG C, heats 4 points
Clock, is made flexible conductive circuit pattern.
After oversintering, silver ion in silver acetate is silver-colored simple substance by reduction of ethylene glycol, and the particle diameter of silver-colored simple substance is mainly distributed
In 11 ~ 15nm；The silver nano-grain in ink after sintering, its particle diameter is mainly distributed on 37 ~ 43 nm；The compound ink of activity
The particle diameter of grain is mainly distributed on 35 ~ 70nm；Silver ion in compound ink is reduced to around former silver nano-grain well
Silver-colored simple substance, increases its particle diameter, and silver nano-grain is with the help of silver ion in the compound ink of activity, and good is bonded in
Together.
80 DEG C of the present embodiment 3 sintering 4min resistivity, the introducing of silver ion makes the resistivity of conducting channel from 82.36
μ Ω cm are changed into 71.24 μ Ω cm.
Claims (9)
1. a kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit, it is characterised in that including following step
Suddenly：
（1）Silver acetate solutions are well mixed with silver nano-grain dispersion liquid, composite conducting ink is obtained；
（2）Obtained composite conducting ink is injected in neutral signature pen or ink-jet printer cartridge, on fexible film substrate
Circuit pattern needed for directly writing or print；
（3）The fexible film substrate for being printed with circuit pattern is placed on low-temperature sintering in thermal station, on fexible film substrate
Nano silver grain flexible conductive circuit is led to the height.
2. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, the concentration of the silver acetate solutions is 2 ~ 4wt%.
3. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, the solvent of the silver acetate solutions is ethanol and the mixed solvent of ethylene glycol；The ethanol and second
The volume ratio of the in the mixed solvent of glycol, ethanol and ethylene glycol is 10 ~ 15:1.
4. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, the concentration of the silver nano-grain dispersion liquid is 20 ~ 35wt%.
5. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, the solvent of silver nano-grain dispersion liquid is triethylene glycol monomethyl ether.
6. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, in the silver nano-grain dispersion liquid, the particle diameter of silver nano-grain is 20 ~ 50 nm.
7. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（1）In, the mixed volume ratio of silver acetate solutions and the silver nano-grain dispersion liquid is 2 ~ 1.5:1.
8. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（2）In, the fexible film substrate include polyethylene terephthalate's substrate, polyimide substrate,
Dimethyl silicone polymer substrate, polymethyl methacrylate substrate or polycarbonate substrate.
9. a kind of low-temperature sintering according to claim 1 prepares the high method for leading Nano silver grain flexible conductive circuit, its
It is characterised by, step（3）In, the low-temperature sintering is 3 ~ 5min of heating at 80 ~ 100 DEG C.
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| CN201710345090.1A CN107135602A (en) | 2017-05-16 | 2017-05-16 | A kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit |
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| CN201710345090.1A CN107135602A (en) | 2017-05-16 | 2017-05-16 | A kind of low-temperature sintering prepares the high method for leading Nano silver grain flexible conductive circuit |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007145947A (en) * | 2005-11-25 | 2007-06-14 | Mitsuboshi Belting Ltd | Electroconductive ink composition and its manufacturing method |
| CN102391716A (en) * | 2011-09-06 | 2012-03-28 | 天津大学 | Flexo-printing nano silver conductive ink and preparation method thereof |
| CN104140717A (en) * | 2013-05-06 | 2014-11-12 | 北京中科纳通电子技术有限公司 | High-solid content jet-printing conductive ink |
| CN105377449A (en) * | 2013-07-10 | 2016-03-02 | 柯尼卡美能达株式会社 | Coating film formation method, base material with transparent conducting film, device and electronic apparatus |
-
2017
- 2017-05-16 CN CN201710345090.1A patent/CN107135602A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007145947A (en) * | 2005-11-25 | 2007-06-14 | Mitsuboshi Belting Ltd | Electroconductive ink composition and its manufacturing method |
| CN102391716A (en) * | 2011-09-06 | 2012-03-28 | 天津大学 | Flexo-printing nano silver conductive ink and preparation method thereof |
| CN104140717A (en) * | 2013-05-06 | 2014-11-12 | 北京中科纳通电子技术有限公司 | High-solid content jet-printing conductive ink |
| CN105377449A (en) * | 2013-07-10 | 2016-03-02 | 柯尼卡美能达株式会社 | Coating film formation method, base material with transparent conducting film, device and electronic apparatus |
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