CN106128543A - Conductive silver paste that a kind of anti-settling is effective and preparation method thereof - Google Patents
Conductive silver paste that a kind of anti-settling is effective and preparation method thereof Download PDFInfo
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- CN106128543A CN106128543A CN201610565136.6A CN201610565136A CN106128543A CN 106128543 A CN106128543 A CN 106128543A CN 201610565136 A CN201610565136 A CN 201610565136A CN 106128543 A CN106128543 A CN 106128543A
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- settling
- effective
- silver paste
- conductive silver
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses effective conductive silver paste of a kind of anti-settling and preparation method thereof, including by weight: flake silver powder 75 85 parts, epoxy resin 6 10 parts, phthalic anhydride 13 parts, tetraethyl titanate 01 parts, sodium lauryl sulphate 0.2 0.8 parts, dodecylbenzene sodium sulfonate 0.05 0.5 parts, its preparation method comprises the steps: to prepare flake silver powder, prepare electrocondution slurry, anti-settling process.The present invention as dispersant, effectively inhibits argentum powder precipitation in organic resin by addition sodium lauryl sulphate and dodecylbenzene sodium sulfonate in the silver slurry prepared, and slurry is played Stabilization by steric hindrance or electrostatic mechanism by dispersant.
Description
Technical field
The present invention relates to a kind of conductive silver paste and preparation method thereof, conductive silver paste that a kind of anti-settling is effective and
Its preparation method.
Background technology
Silver slurry is low-temperature conductive slurry in one, is by the composite of homogeneous to elemental silver powder and resin liquid mixing.Cause
Its solidification temperature is low, stability, good conductivity and adhesive force good, be mainly used on non-conductive substrate formation electric conductivity, electricity
Resistive, dielectric film etc..The CSP-3163CSP-3310 series silver slurry properties of product of Chang Xing company of Korea S are stable, printing, attachment
Power, elasticity are splendid, and resistance coefficient is low, and linear resolution is clear.The conductive silver paste tool that Shenzhen Ming Bo Electron Material Co., Ltd produces
There is functional excellent, cost performance high.Be widely used in thin film switch, flexible circuit, the soft circuit of FPC, toy circuit,
The industry-by-industry such as remote controller, printed circuit board (PCB).
Now current, silver slurry mainly forms with conductive filler, organic resin, additive.Argentum powder is as in impregnated silver pulp
Main component, due to its powder body have that specific surface area is big, surface atom number is many, surface can high, there is substantial amounts of surface defect
And dangling bonds, easily reunite between granule, form larger-size aggregate, thus affect the exploitation application of its product.
Summary of the invention
It is an object of the invention to, it is provided that conductive silver paste that a kind of anti-settling is effective and preparation method thereof.The present invention's
Slurry has more preferable dispersibility, anti-settling effect, stability and electric conductivity.
Technical scheme: the conductive silver paste that a kind of anti-settling is effective, by weight, includes: lamellar silver
Powder 75-85 part, epoxy resin 6-10 part, phthalic anhydride 1-3 part, tetraethyl titanate 0-1 part, sodium lauryl sulphate 0.2-
0.8 part, dodecylbenzene sodium sulfonate 0.05-0.5 part.
The conductive silver paste that aforesaid anti-settling is effective, by weight, includes: flake silver powder 80 parts, epoxy resin 8
Part, phthalic anhydride 2 parts, tetraethyl titanate 0.5 part, sodium lauryl sulphate 0.3 part, dodecylbenzene sodium sulfonate 0.1
Part.
The conductive silver paste that aforesaid anti-settling is effective, described epoxy resin is bisphenol A type epoxy resin E55 or E51.
The preparation method of the conductive silver paste that a kind of aforesaid anti-settling is effective, described method comprises the steps:
(1) flake silver powder is prepared: first by AgNO3The aqueous solution being configured to, to AgNO3Aqueous solution adds surface activity
Agent, is then heated to reductant solution 50 DEG C and regulates pH=13, then by the AgNO added with surfactant3Aqueous solution and also
Former agent solution hybrid reaction, filters, is more first washed with deionized, then with washes of absolute alcohol, then dry, i.e. can get sheet
Shape argentum powder；
(2) electrocondution slurry is prepared: add hot epoxy resin to 80-90 DEG C, the flake silver powder that then will prepare in step (1)
It is directly added in the epoxy resin heated, stirs, be subsequently adding phthalic anhydride and tetraethyl titanate stirs,
I.e. form electrocondution slurry；
(3) anti-settling processes: add sodium lauryl sulphate and detergent alkylate in the silver slurry prepared through step (2)
Sodium sulfonate, after stirring is pre-dissolved, i.e. obtains the conductive silver paste that anti-settling is effective.
The preparation method of the conductive silver paste that aforesaid anti-settling is effective, in described step (1), described surfactant is
Cetyl trimethylammonium bromide, surfactant addition is the 0.1% of total amount.
The preparation method of the conductive silver paste that aforesaid anti-settling is effective, in described step (1), reductant solution is anti-bad
Hematic acid aqueous solution.
The preparation method of the conductive silver paste that aforesaid anti-settling is effective, in described step (2), the temperature of epoxy resin heating
Degree is for for 85 DEG C.
In the preparation method of the conductive silver paste that aforesaid anti-settling is effective, described step (2) and step (3), stirring is mixed
Ultrasonic disperse is all used to process during conjunction.
The preparation method of the conductive silver paste that aforesaid anti-settling is effective, the lamellar prepared in described step (1) silver
The average diameter of powder is 2-5 micron.
Beneficial effects of the present invention: the present invention is by adding sodium lauryl sulphate and dodecane in the silver slurry prepared
Base benzene sulfonic acid sodium salt, as dispersant, effectively inhibits argentum powder precipitation in organic resin, improves stablizing of conductive silver paste
Property and dispersion, thus improve the conductive effect of silver slurry, slurry is played stable work by steric hindrance or electrostatic are machine-processed by dispersant
With.
In order to further illustrate beneficial effects of the present invention, inventor has done following experiment:
Experimental example 1: the interpolation of the dispersant impact on silver slurry stability
Take two groups of conductive silver pastes processed without anti-settling prepared through the present invention, wherein one group adds this
Bright described sodium lauryl sulphate (SDS) and dodecylbenzene sodium sulfonate (SDBS), utilize method of the present invention to carry out
Anti-settling processes, and is designated as SDS+SDBS group；Another group is left intact, and is designated as original group.By measuring two groups of conductions respectively
Silver slurry RSH in 300h characterizes the stability of conductive silver paste.Result is as shown in Figure 1.
Remarks: RSH is in infall process, and the supernatant height h and slurry overall height H are with their ratio (Ratio
sediment height,RSH).From formula (1), the overall height H of same volume slurry is constant, and sedimentation clear liquid is the most, and h value is more
Greatly, RSH value is the biggest, and silver slurry is the most unstable.
As shown in Figure 1, can be seen that within any sedimentation time, the RSH value of two groups of conductive silver pastes is original group > SDS+
SDBS group, therefore, the stability of SDS+SDBS group > stability of original group.
Experimental example 2: the different dispersant concentrations impact on silver slurry stability
Take four groups of conductive silver pastes processed without anti-settling prepared through the present invention, in four groups of conductive silver pastes respectively
Add sodium lauryl sulphate (SDS) and the dodecylbenzene sodium sulfonate of Different Weight component according to the method described in the present invention
(SDBS) sodium lauryl sulphate (SDS), added in four groups of conductive silver pastes and the weight of dodecylbenzene sodium sulfonate (SDBS)
Component is respectively: SDS+SDBS (0.3 part+0.1 part), SDS+SDBS (0.8 part+0.1 part), SDS+SDBS (0.8 part+0.5 part),
SDS+SDBS (0.3 part+0.5 part), measures the RSH value of conductive silver paste respectively after being disposed, test result as shown in Figure 2,
From figure 2 it can be seen that the concentration of SDS+SDBS is when (0.3 part+0.1 part), RSH value is minimum, illustrates to add this components by weight percent
SDS+SDBS after, the stability of conductive silver paste is best.
Experimental example 3:SEM measures
Choose one group through the present invention prepare without anti-settling process conductive silver paste and one group through system of the present invention
The standby conductive silver paste processed through anti-settling obtained, carries out SEM mensuration to it respectively, and the SEM figure obtained is respectively such as accompanying drawing 3 and attached
Shown in Fig. 4.
Contrast accompanying drawing 3 and accompanying drawing 4 understand, and the silver powder particles of the conductive silver paste (Fig. 4) carrying out anti-settling process disperses more
Uniformly.
Experimental example 4: conducting performance test
Taking two groups of conductive silver pastes processed without anti-settling prepared through the present invention, one of which is according to institute of the present invention
The method stated carries out anti-settling process, is designated as SDS+SDBS group, and another group is left intact, and is designated as original group, leads both sides
Electricity silver slurry carries out conductive silver powder fineness measurement respectively, silver slurry grain graininess is measured, silver slurry viscosity measures and body resistivity is surveyed
Examination, result is as shown in table 1, and the conductive silver powder fineness of two groups of conductive silver pastes, silver slurry viscosity are consistent with body resistivity, but, SDS
The granularity (4 μm) of the granularity (3.5 μm) of the silver slurry granule of+SDBS group silver slurry granule less than original group.
Table 1
Accompanying drawing explanation
Accompanying drawing 1 is the RSH value of the conductive silver paste before and after anti-settling process；
The RSH value of conductive silver paste when accompanying drawing 2 is the SDS+SDBS adding variable concentrations；
Accompanying drawing 3 is the SEM figure of the conductive silver paste processed without anti-settling；
Accompanying drawing 4 be processed by the invention after conductive silver paste SEM figure.
Detailed description of the invention
Embodiments of the invention:
Embodiment 1: the conductive silver paste that a kind of anti-settling is effective, includes by weight: flake silver powder 80 parts, A type
Epoxy resin E55 8 parts, phthalic anhydride 2 parts, tetraethyl titanate 0.5 part, sodium lauryl sulphate 0.3 part, dodecyl
Benzene sulfonic acid sodium salt 0.1 part.
The preparation method of the conductive silver paste that above-mentioned anti-settling is effective, comprises the steps:
(1) flake silver powder is prepared: first by AgNO3The aqueous solution being configured to, to AgNO3Aqueous solution adds AgNO3Water-soluble
The cetyl trimethylammonium bromide of the 0.1% of liquid total amount, is then heated to aqueous ascorbic acid 50 DEG C and regulates pH=
13, then by the AgNO added with cetyl trimethylammonium bromide3Aqueous solution and aqueous ascorbic acid hybrid reaction, filter, then
First it is washed with deionized, then with washes of absolute alcohol, then dries, i.e. can get the lamellar silver that average diameter is 2-5 micron
Powder；
(2) electrocondution slurry is prepared: epoxy resin E55 to 85 DEG C of A type of heating, the lamellar that then will prepare in step (1)
Argentum powder is directly added in the A type epoxy resin E55 heated, and stirs, is subsequently adding phthalic anhydride and metatitanic acid tetrem
Ester stirs, and i.e. forms electrocondution slurry；
(3) anti-settling processes: add sodium lauryl sulphate and detergent alkylate in the silver slurry prepared through step (2)
Sodium sulfonate, after stirring is pre-dissolved, i.e. obtains the conductive silver paste that anti-settling is effective.
Embodiment 2: the conductive silver paste that a kind of anti-settling is effective, includes by weight: flake silver powder 85 parts, epoxy
Resin 10 parts, phthalic anhydride 3 parts, tetraethyl titanate 1 part, sodium lauryl sulphate 0.8 part, dodecylbenzene sodium sulfonate
0.5 part.
The preparation method of the conductive silver paste that above-mentioned anti-settling is effective, described method comprises the steps:
(1) flake silver powder is prepared: first by AgNO3The aqueous solution being configured to, to AgNO3Aqueous solution adds AgNO3Water-soluble
The cetyl trimethylammonium bromide of the 0.1% of liquid total amount, is then heated to aqueous ascorbic acid 50 DEG C and regulates pH=
13, then by the AgNO added with cetyl trimethylammonium bromide3Aqueous solution and aqueous ascorbic acid hybrid reaction, filter, then
First it is washed with deionized, then with washes of absolute alcohol, then dries, i.e. can get the lamellar silver that average diameter is 2-5 micron
Powder；
(2) electrocondution slurry is prepared: epoxy resin E55 to 90 DEG C of A type of heating, the lamellar that then will prepare in step (1)
Argentum powder is directly added in the A type epoxy resin E55 heated, and stirs and sonic oscillation, is subsequently adding phthalic anhydride
Stir with tetraethyl titanate, carry out sonic oscillation during stirring equally, i.e. form electrocondution slurry；
(3) anti-settling processes: add sodium lauryl sulphate and detergent alkylate in the silver slurry prepared through step (2)
Sodium sulfonate, after stirring is pre-dissolved, i.e. obtains the conductive silver paste that anti-settling is effective.
Embodiment 3: the conductive silver paste that a kind of anti-settling is effective, includes by weight: flake silver powder 75 parts, A type
Epoxy resin E51 6 parts, phthalic anhydride 1 part, sodium lauryl sulphate 0.2 part, dodecylbenzene sodium sulfonate 0.05 part.
The preparation method of the conductive silver paste that above-mentioned anti-settling is effective, described method comprises the steps:
(1) flake silver powder is prepared: first by AgNO3The aqueous solution being configured to, to AgNO3Aqueous solution adds AgNO3Water-soluble
The cetyl trimethylammonium bromide of the 0.1% of liquid total amount, is then heated to aqueous ascorbic acid 50 DEG C and regulates pH=
13, then by the AgNO added with cetyl trimethylammonium bromide3Aqueous solution and aqueous ascorbic acid hybrid reaction, filter, then
First it is washed with deionized, then with washes of absolute alcohol, then dries, i.e. can get the lamellar silver that average diameter is 2-5 micron
Powder；
(2) electrocondution slurry is prepared: epoxy resin E51 to 80 DEG C of A type of heating, the lamellar that then will prepare in step (1)
Argentum powder is directly added in the A type epoxy resin E51 heated, and stirs, is subsequently adding phthalic anhydride and metatitanic acid tetrem
Ester stirs, and i.e. forms electrocondution slurry；
(3) anti-settling processes: add sodium lauryl sulphate and detergent alkylate in the silver slurry prepared through step (2)
Sodium sulfonate, after stirring is pre-dissolved, i.e. obtains the conductive silver paste that anti-settling is effective.
Claims (9)
1. the conductive silver paste that an anti-settling is effective, it is characterised in that by weight, includes: flake silver powder 75-85
Part, epoxy resin 6-10 part, phthalic anhydride 1-3 part, tetraethyl titanate 0-1 part, sodium lauryl sulphate 0.2-0.8 part,
Dodecylbenzene sodium sulfonate 0.05-0.5 part.
2. the conductive silver paste that anti-settling as claimed in claim 1 is effective, it is characterised in that by weight, include: sheet
80 parts of shape argentum powder, epoxy resin 8 parts, phthalic anhydride 2 parts, tetraethyl titanate 0.5 part, sodium lauryl sulphate 0.3 part, ten
0.1 part of dialkyl benzene sulfonic acids sodium.
3. the conductive silver paste that anti-settling as claimed in claim 1 or 2 is effective, it is characterised in that: described epoxy resin is double
Phenol A type epoxy resin E55 or E51.
4. a preparation method for the conductive silver paste that anti-settling as according to any one of claim 1-3 is effective, its feature
Being, described method comprises the steps:
(1) flake silver powder is prepared: first by AgNO3The aqueous solution being configured to, to AgNO3Aqueous solution adds surfactant, so
After reductant solution is heated to 50 DEG C and regulates pH=13, then by the AgNO added with surfactant3Aqueous solution and reducing agent
Solution hybrid reaction, filters, is more first washed with deionized, then with washes of absolute alcohol, then dry, and i.e. can get lamellar silver
Powder；
(2) electrocondution slurry is prepared: add hot epoxy resin to 80-90 DEG C, then by direct for the flake silver powder for preparing in step (1)
In the epoxy resin heated, stir, be subsequently adding phthalic anhydride and tetraethyl titanate stirs, i.e. shape
Become electrocondution slurry；
(3) anti-settling processes: add sodium lauryl sulphate and DBSA in the silver slurry prepared through step (2)
Sodium, after stirring is pre-dissolved, i.e. obtains the conductive silver paste that anti-settling is effective.
5. the preparation method of the conductive silver paste that anti-settling as claimed in claim 4 is effective, it is characterised in that: described step
(1) in, described surfactant is cetyl trimethylammonium bromide, and surfactant addition is the 0.1% of total amount.
6. the preparation method of the conductive silver paste that anti-settling as claimed in claim 4 is effective, it is characterised in that: described step
(1), in, reductant solution is aqueous ascorbic acid.
7. the preparation method of the conductive silver paste that anti-settling as claimed in claim 4 is effective, it is characterised in that: described step
(2), in, the temperature of epoxy resin heating is for for 85 DEG C.
8. the preparation method of the conductive silver paste that anti-settling as claimed in claim 4 is effective, it is characterised in that: described step
(2) and in step (3), during stirring mixing, ultrasonic disperse is all used to process.
9. the preparation method of the conductive silver paste that anti-settling as claimed in claim 4 is effective, it is characterised in that: described step
(1) average diameter of the flake silver powder prepared in is 2-5 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610565136.6A CN106128543B (en) | 2016-07-18 | 2016-07-18 | Conductive silver paste with good anti-settling effect and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610565136.6A CN106128543B (en) | 2016-07-18 | 2016-07-18 | Conductive silver paste with good anti-settling effect and preparation method thereof |
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| CN106128543A true CN106128543A (en) | 2016-11-16 |
| CN106128543B CN106128543B (en) | 2021-02-02 |
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Cited By (2)
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| CN106601334A (en) * | 2016-12-29 | 2017-04-26 | 广州凯耀资产管理有限公司 | Electronic paste for touch screens and preparation method thereof |
| CN107393626A (en) * | 2017-06-27 | 2017-11-24 | 西安工程大学 | A kind of hot method powdery electric slurry and preparation method thereof |
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| CN106128543B (en) | 2021-02-02 |
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