CN109637693A - A kind of conductive silver paste and preparation method thereof based on from the silver-colored frame of sintering - Google Patents
A kind of conductive silver paste and preparation method thereof based on from the silver-colored frame of sintering Download PDFInfo
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- CN109637693A CN109637693A CN201811539879.1A CN201811539879A CN109637693A CN 109637693 A CN109637693 A CN 109637693A CN 201811539879 A CN201811539879 A CN 201811539879A CN 109637693 A CN109637693 A CN 109637693A
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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
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising 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
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Abstract
The present invention relates to a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, belongs to conductive silver paste preparation technical field.The present invention provides a kind of preparation method of conductive silver paste that can be used for flexible occasion, to pass through the frame silver powder from sintering processes as conductive filling material, suitable organic additive and high polymer binder are dissolved in respectively in suitable organic solvent, and in the warp that certain content is wherein added from the frame silver powder of sintering processes, it will be by being uniformly distributed therein from the frame silver powder of sintering processes by homogenizer, it is finally ground into the silver paste with certain fineness, certain viscosity, finally obtains the conductive silver paste that can be used for flexible occasion.Have the characteristics that fabulous bending resistance, low silver powder content, electric conductivity are preferable using conductive silver paste prepared by such method.
Description
Technical field
The present invention relates to conductive silver paste preparation technical fields, and in particular to a kind of conductive silver paste based on from the silver-colored frame of sintering
And preparation method thereof.
Background technique
With the rapid expansion of electronics industry, the dosage of electrocondution slurry also increases year by year.In existing electrocondution slurry, use
Electrocondution slurry in electronics industry is still based on conductive silver paste.Currently, such conductive silver paste has been widely used
In printed wiring board, integrated antenna package, display, thin film switch, sensor, radio frequency label, electromagnetic induction and shielding
Equal fields.Conductive silver paste is mainly by silver powder, macromolecule resin, organic solvent and additive with various functions according to one
Fixed ratio is successively prepared by techniques such as mechanical stirring mixing, the grindings of three rollers.
In recent years, electronic component develops to directions such as miniaturization, multifunction, flexibilities.In order to meet thin film switch,
The requirement in the flexible applications such as flexible circuit, flexible sensing field, conductive silver paste need to have following feature request: highly conductive
Property, high adhesion, high bending resistance and high stability etc..But silver powder price used in conductive silver paste is relatively high, and
Conductive silver paste is printed as after the striped needed, and bending resistance is poor.In view of the foregoing, seek a kind of low silver powder content, lead
Excellent electrical property, and the conductive silver paste with fabulous bending resistance has become one of urgent problem in the industry.
Summary of the invention
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of low silver powder that can be used for flexible occasion to contain
The conductive silver paste of amount, the conductive silver paste are to be fitted by a kind of based on being prepared from the conductive silver paste for being sintered silver-colored frame with meeting
Close the demand of the conductive silver paste of flexible applications.The silver paste that the present invention obtains have the advantage that can be used for flexible occasion,
It is excellent with low silver powder content, electric conductivity, and there is fabulous bending resistance etc..
In order to achieve the above object, the present invention specifically provides following technical solution:
A kind of preparation method for the conductive silver paste can be used for flexible occasion, this method is first by flake silver powder by being chemically treated
It obtains from the frame silver powder being sintered, then, as conductive filling material, to have suitable by the frame silver powder from sintering processes
Machine additive and high polymer binder are dissolved in respectively in suitable organic solvent, and be wherein added certain content process from
The frame silver powder of sintering processes will be passed through from the frame silver powder of sintering processes by homogenizer and be uniformly dispersed therein, finally
It is ground into the electrocondution slurry with certain fineness, certain viscosity.The conductive silver paste that can be used for flexible occasion is finally obtained, it is specific to walk
It is rapid as follows:
(1), flake silver powder preliminary treatment.Flake silver powder is distributed in deionized water, is then added in the solution certain dense
The sodium nitrate of degree or the aqueous solution of potassium nitrate, ultrasound 5 minutes, the silver powder deionized water and ethyl alcohol for finally obtaining centrifugation are clear
It washes；
(2) silver powder is further processed.The silver powder by preliminary treatment that step (1) obtains is added to certain density succinic acid
Or in the aqueous solution of glutaric acid, then ultrasound 30 minutes cleans the silver powder that centrifugation obtains with deionized water and ethyl alcohol；Finally will
Obtained silver powder is dried in 50 DEG C of vacuum drying oven, is obtained by the frame silver powder from sintering processes；
(3), organic carrier is prepared.A certain amount of high polymer binder is taken, mechanical stirring in organic solvent is added to and mixes to complete
Fully dissolved；Then a certain amount of organic additive is taken, mechanical stirring in above-mentioned organic solvent is added to and mixes to being completely dissolved；
(4), slurry is prepared.By obtained in step (2) by being added to from the frame silver powder of sintering processes by above-mentioned steps (3)
It in obtained organic carrier solution, is uniformly dispersed using homogenizer, is finally ground into certain fineness, the conductive paste of certain viscosity
Material.
It is described a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, sheet used in step (1)
Silver powder is that chemical synthesis or mechanical attrition method or chemical synthesis and mechanical attrition method are combined and obtained, the diameter of flake silver powder
Range is 800 nanometers -10 microns.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, handles the nitric acid of flake silver powder
The concentration range of the aqueous solution of sodium or potassium nitrate is 0.02 mol/L-2 mol/L.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, handles the fourth two of flake silver powder
The concentration of aqueous solution range of acid or glutaric acid is 0.5 mol/L-2 mol/L.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, and processing flake silver powder needs certain
The aqueous solution of the sodium nitrate of concentration or the aqueous solution of potassium nitrate and certain density succinic acid or glutaric acid combines.First with certain dense
The aqueous solution processing of the sodium nitrate or potassium nitrate of degree, then handled with the aqueous solution of certain density succinic acid or glutaric acid.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, and high polymer binder selects polyester
Resin and thermoplastic polyurethane resin, its ratio be 1:0.3-1:1.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, and organic additive is polyamide
Any one in cured, organobentonite, rilanit special and polyureas.
Described is a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, and solvent is dibasic ester, diethyl
Any one in glycol butyl ether acetic acid esters.
Compared with prior art, the advantages of technical solution of the present invention and beneficial effect is:
(1), the method for the present invention is easy to operate, halogen-free introducing in chemical treatment, and technical process is environmental-friendly and easy realization industry
Change；
(2), the conductive silver paste of flexible applications prepared by the method for the present invention has low silver powder content, and its electric conductivity
It can also be able to maintain that in higher level；
(3), the conductive silver paste that can be used for flexible occasion prepared by the method for the present invention has fabulous bending resistance.
Detailed description of the invention
Illustrate the embodiment of the present invention in order to clearer, embodiment will be described below used in attached drawing make it is simple
Explanation.
Fig. 1 is the embodiment of the present invention 1 by oneself of sodium nitrate (0.5 mol/L) and succinic acid (1.0 mol/L) processing
It is sintered the sem test result of frame silver powder.
Fig. 2 is to handle according to embodiment 2 is resulting by sodium nitrate (1.5 mol/L) and succinic acid (1.0 mol/L)
From the sem test result of sintering frame silver powder.
Fig. 3 is oneself handled according to resulting process sodium nitrate (1 mol/L) of embodiment 3 and succinic acid (1.5 mol/L)
It is sintered the sem test result of frame silver powder.
Fig. 4 is oneself handled according to resulting process sodium nitrate (1 mol/L) of embodiment 4 and succinic acid (1.0 mol/L)
It is sintered the sem test result of frame silver powder.
Fig. 5 be according to comparative example it is resulting merely through succinic acid (1.0 mol/L) processing without the silver from sintering processes
The sem test result of powder.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples, it should be appreciated that following embodiments are only used for
The bright present invention, is not intended to limit the present invention.Based on the embodiments of the present invention, scientific research technical staff in this field is not making creation
Property labour under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1.
The conductive silver paste based on sintering frame certainly of the present embodiment, the raw material including following weight percent:
From silver-colored 48 wt.% of frame silver powder of sintering, 9.5 wt.% of high polymer binder, 42 wt.% of solvent, organic additive 0.5
wt.%。
Macromolecule in the present embodiment is bonded as polyester resin and thermoplastic polyurethane resin, and weight ratio between the two is
1:0.6。
Solvent in the present embodiment is dibasic ester.
Being made as follows from sintering frame silver powder in the present embodiment:
(1), flake silver powder is distributed in the deionized water of 20 ml, then ultrasound 10 minutes is added 0.5 in the solution
Then 60 ml of sodium nitrate solution of mol/L, ultrasound 5 minutes clean the silver powder that centrifugation obtains with deionized water and ethyl alcohol；
(2), the silver powder that step (1) obtains is added in the succinic acid aqueous solution of 1.0 mol/L, ultrasound 30 minutes, then will
Obtained silver powder is centrifuged to be cleaned with deionized water and ethyl alcohol；Obtained silver powder is dried 12 hours in 50 DEG C of vacuum drying oven, is obtained
It obtains by the frame silver powder from sintering processes.
The scanning electron microscope from sintering frame silver powder in the present embodiment is as shown in Figure 1.It can from the scanning electron microscope result in Fig. 1
To find out that the silver powder of original sheet becomes the silver powder frame network of the similar strip structure in part.
Embodiment 2.
The conductive silver paste based on sintering frame certainly of the present embodiment, the raw material including following weight percent:
From silver-colored 48 wt.% of frame silver powder of sintering, 9.5 wt.% of high polymer binder, 42 wt.% of solvent, organic additive 0.5
wt.%。
Macromolecule in the present embodiment is bonded as polyester resin and thermoplastic polyurethane resin, and weight ratio between the two is
1:0.6。
Solvent in the present embodiment is dibasic ester.
Being made as follows from sintering frame silver powder in the present embodiment:
(1), flake silver powder is distributed in the deionized water of 20 ml, then ultrasound 10 minutes is added 1.5 in the solution
Then 60 ml of sodium nitrate solution of mol/L, ultrasound 5 minutes clean the silver powder that centrifugation obtains with deionized water and ethyl alcohol；
(2), the silver powder that step (1) obtains is added in the succinic acid aqueous solution of 1.0 mol/L, ultrasound 30 minutes, then will
Obtained silver powder is centrifuged to be cleaned with deionized water and ethyl alcohol；Obtained silver powder is dried 12 hours in 50 DEG C of vacuum drying oven, is obtained
It obtains by the frame silver powder from sintering processes.
The scanning electron microscope from sintering frame silver powder in the present embodiment is as shown in Figure 2.It can from the scanning electron microscope result in Fig. 2
To find out that the silver powder of original sheet becomes the silver powder frame network of similar strip structure, compared to the silver powder strip in embodiment 1
Structure is more, and diameter is thicker, more preferable from sintering effect.
Embodiment 3.
The conductive silver paste based on sintering frame certainly of the present embodiment, the raw material including following weight percent:
From silver-colored 48 wt.% of frame silver powder of sintering, 9.5 wt.% of high polymer binder, 42 wt.% of solvent, organic additive 0.5
wt.%。
Macromolecule in the present embodiment is bonded as polyester resin and thermoplastic polyurethane resin, and weight ratio between the two is
1:0.6。
Solvent in the present embodiment is dibasic ester.
Being made as follows from sintering frame silver powder in the present embodiment:
(1), flake silver powder is distributed in the deionized water of 20 ml, then 1 mol/ is added in ultrasound 10 minutes in the solution
Then 60 ml of sodium nitrate solution of L, ultrasound 5 minutes clean the silver powder that centrifugation obtains with deionized water and ethyl alcohol；
(2), the silver powder that step (1) obtains is added in the succinic acid aqueous solution of 1.5 mol/L, ultrasound 30 minutes, then will
Obtained silver powder is centrifuged to be cleaned with deionized water and ethyl alcohol；Obtained silver powder is dried 12 hours in 50 DEG C of vacuum drying oven, is obtained
It obtains by the frame silver powder from sintering processes.
The scanning electron microscope from sintering frame silver powder in the present embodiment is as shown in Figure 3.It can from the scanning electron microscope result in Fig. 3
To find out that the silver powder of original sheet becomes the silver powder frame network of similar strip structure.
Embodiment 4.
The conductive silver paste based on sintering frame certainly of the present embodiment, the raw material including following weight percent:
From silver-colored 48 wt.% of frame silver powder of sintering, 9.5 wt.% of high polymer binder, 42 wt.% of solvent, organic additive 0.5
wt.%。
Macromolecule in the present embodiment is bonded as polyester resin and thermoplastic polyurethane resin, and weight ratio between the two is
1:0.6。
Solvent in the present embodiment is dibasic ester.
Being made as follows from sintering frame silver powder in the present embodiment:
(1), flake silver powder is distributed in the deionized water of 20 ml, then 1 mol/ is added in ultrasound 10 minutes in the solution
Then 60 ml of sodium nitrate solution of L, ultrasound 5 minutes clean the silver powder that centrifugation obtains with deionized water and ethyl alcohol；
(2), the silver powder that step (1) obtains is added in the succinic acid aqueous solution of 1.0 mol/L, ultrasound 30 minutes, then will
Obtained silver powder is centrifuged to be cleaned with deionized water and ethyl alcohol；Obtained silver powder is dried 12 hours in 50 DEG C of vacuum drying oven, is obtained
It obtains by the frame silver powder from sintering processes.
The scanning electron microscope from sintering frame silver powder in the present embodiment is as shown in Figure 4.It can from the scanning electron microscope result in Fig. 4
To find out that the silver powder of original sheet becomes the silver powder frame network of similar strip structure, compared to the silver powder strip in embodiment 3
Diameter of movement is thicker, and particle is bigger.
Comparative example.
This comparative example based on without the conductive silver paste from sintering processes, the raw material including following weight percent:
From silver-colored 48 wt.% of frame silver powder of sintering, 9.5 wt.% of high polymer binder, 42 wt.% of solvent, organic additive 0.5
wt.%。
Macromolecule in this comparative example is bonded as polyester resin and thermoplastic polyurethane resin, and weight ratio between the two is
1:0.6。
Solvent in this comparative example is dibasic ester.
In this comparative example based on being made as follows without the silver powder from sintering processes:
Flake silver powder is added in the succinic acid aqueous solution of 1.0 mol/L, ultrasound 30 minutes, the silver powder for then obtaining centrifugation
It is cleaned with deionized water and ethyl alcohol；Obtained silver powder is dried 12 hours in 50 DEG C of vacuum drying oven, is obtained without from sintering
The flake silver powder of reason.
The scanning electron microscope from sintering frame silver powder in this comparative example is as shown in Figure 5.It can from the scanning electron microscope result in Fig. 5
To find out that the silver powder of original sheet its microscopic appearance after succinic acid processing is still sheet, do not find silver strip from burning
Tie the microscopic appearance of feature.
The resistivity measurement result for the conductive silver paste that the above various embodiments and comparative example obtain is as follows:
Table 1
| Example | Resistivity (Ω m) |
| Embodiment 1 | 8.47×10-6 |
| Embodiment 2 | 5.88×10-6 |
| Embodiment 3 | 8.36×10-6 |
| Embodiment 4 | 1.08×10-6 |
| Comparative example | 5.23×10-6 |
As can be seen from Table 1, compared with comparative example, the conductive silver paste of the invention based on from the silver-colored frame of sintering, if conductive silver paste
Used in flake silver powder respectively by certain density sodium nitrate (1.0 mol/L) and succinic acid (1.0 mol/L) cleaning after,
That is embodiment 4 has lower resistivity, and resistivity is by 5.23 × 10-6 Ω m is reduced to 1.08 × 10-6 Ω m is reduced
5 times.
In addition, the silver paste of the embodiment 4 also has extraordinary bending resistance and adhesion property.Bending front and back resistance variations
Only 7.28%, adhesive force grade is 5B.
Claims (9)
1. a kind of conductive silver paste and preparation method thereof based on from the silver-colored frame of sintering, it is characterised in that include the following steps: step
(1), silver powder is from sintering processes；Silver powder is added in organic carrier by step (2), and organic carrier includes high polymer binder, has
Machine additive and organic solvent, are uniformly dispersed using homogenizer, and are ground into certain fineness, the conduction of certain viscosity
Silver paste.
2. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: silver powder used in the step (1) is flake silver powder.Flake silver powder is that chemical synthesis or mechanical attrition method or chemistry close
It is obtained at method and mechanical attrition method combination, the diameter range of flake silver powder is 800 nanometers -10 microns.
3. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: the flake silver powder in the step (1) is made of from sintering processes following two step.(1), flake silver powder is distributed to
In ionized water, the aqueous solution of certain density nitrate compound is then added in the solution, ultrasound 5 minutes then will centrifugation
Obtained silver powder is cleaned with deionized water and ethyl alcohol；(2) silver powder that step (1) obtains is added to certain density organic acid
In aqueous solution, then ultrasound 30 minutes cleans the silver powder that centrifugation obtains with deionized water and ethyl alcohol.Certainly by obtained warp finally
The silver powder that sintering processes are crossed is dried in 50 DEG C of vacuum drying oven, is obtained through the frame silver powder from sintering processes.
4. according to claim 3 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: the flake silver powder nitrate compound used in sintering processes step (1) be sodium nitrate, any one in potassium nitrate.Piece
Shape silver powder organic acid used in sintering processes step (2) is short chain organic acid, is succinic acid, any one in glutaric acid
Kind.
5. according to claim 3 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In the concentration of aqueous solution range of: the flake silver powder nitrate compound used in the sintering processes be 0.02 mol/L-2 mol/L,
The concentration range of the aqueous solution of organic acid is 0.5 mol/L-2 mol/L.
6. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: silver powder used in step (2) is treated sintering frame silver powder certainly in step (1).
7. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: high polymer binder used in step (2) is polyester resin and polyurethane resin, and its ratio be 1:0.3-1:1.
8. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: organic additive used in step (2) is any one in cured polyamide, organobentonite, rilanit special and polyureas
Kind.
9. according to claim 1 a kind of based on from the conductive silver paste and preparation method thereof for being sintered silver-colored frame, feature exists
In: organic solvent used in step (2) be dibasic ester, any one in butyl acetic acid esters.
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| Application Number | Priority Date | Filing Date | Title |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811539879.1A CN109637693A (en) | 2018-12-17 | 2018-12-17 | A kind of conductive silver paste and preparation method thereof based on from the silver-colored frame of sintering |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111276296A (en) * | 2020-03-05 | 2020-06-12 | 南京理工大学 | Conductive silver paste composite sintering method and device |
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Application publication date: 20190416 |