CN104021840A - Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film - Google Patents
Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film Download PDFInfo
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Abstract
The invention discloses a low-temperature curing high-conductive silver paste and a preparation method of the low-temperature curing high-conductive silver paste, a conductive film made of the low-temperature curing high-conductive silver paste and a preparation method of the conductive film. The low-temperature curing high-conductive silver paste is formed by blending silver nano-wires and organic binder, wherein the silver nano-wires are adopted as conductive elements. The length of the silver nano-wires ranges from 1 micron-20 microns, and the section diameter of the silver nano-wires ranges from 10 nm-300 nm. The organic binder is one of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, hydroxymethyl cellulose and methylcellulose or polymer blends composed of two or more of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, hydroxymethyl cellulose and methylcellulose. The amount of the silver nano-wires is 50 wt%. The square resistance of the prepared film is lower than 0.1 ohm/sq. Bulk resistivity reaches 2*10-5 ohm*cm. Pencil hardness reaches 9H, and good resistance to bending fatigue is achieved. Compared with the prior art, the low-temperature curing high-conductive silver paste has the advantages that curing can be performed at low temperature, electric conductivity is high, and the silver paste can be widely applied to various consumer electronic devices.
Description
Technical field
The present invention relates to electronic material preparing technical field, be specifically related to high conductive silver paste of a kind of low-temperature setting and preparation method thereof and application.
Background technology
Along with the develop rapidly of electronics industry, the demand of thin film switch, flexible printed circuit board, electromagnetic shielding, potentiometer, radio frequency identification system, solar cell etc. is increasing sharply, and conductive silver paste as preparation these type of electronic devices and components key function material, its development and application also get more and more people's extensive concerning.Conductivity is the key factor that affects conduction data application, and argent has excellent conductivity and be widely used in the conduction primitive of electrocondution slurry because of it.
At present, on market, widely used silver slurry is generally to adopt epoxy-resin systems or oxide system, epoxy-resin systems is to add silver powder in epoxy resin and curing agent, oxide system is in several low melting point oxides, to add nano level silver powder, (Keunju Park as shown in Figures 1 and 2, Dongseok Seo, Jongkook Lee. Colloids and Surfaces A:Physicochem.Eng.Aspects 313-314 (2008) 351-354.).The former is solidified into product by being not less than 100 DEG C, and the latter needs high temperature sintering to form.After the silver slurry of epoxy-resin systems solidifies, silver powder is connected together by epoxy resin, and its advantage is that operating temperature is low, and shortcoming is that thermal conductivity and conductance are very low, can not be used for powerful occasion.The silver slurry of oxide system adopts the prepared conductive silver paste contact effect of conventional silver nano particle bad as can be seen from Figure 1, can find out that from Fig. 2 (X-ray diffractogram) this material is argent structure, therefore its shortcoming is to need 400～500 DEG C of high annealings just can make silver nano-grain melting just can reach good conductance, condition harshness, applicable surface is wide not, can not be applied in flexible substrate.
Summary of the invention
The technical problem to be solved in the present invention is to provide high conductive silver paste of a kind of low-temperature setting and preparation method thereof and application.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of high conductive silver paste of low-temperature setting, it adopts nano silver wire to form as conduction primitive and organic adhesive blend, described nano silver wire length range is 1 ~ 20 μ m, diameter of section scope is 10 ~ 300nm, described organic adhesive is one or more in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, CMC, methylcellulose, and nano silver wire amount is 50wt%.
A preparation method for the high conductive silver paste of low-temperature setting, comprises the steps:
Step 1, get appropriate organic adhesive and add in deionized water, 70 DEG C of stirring in water bath 10-30min, obtain colourless transparent solution, it is 1-5%wt that the amount of control organic adhesive makes the concentration of organic adhesive in solution, and described organic adhesive is a kind of, two or more the blend in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, CMC, methylcellulose.
Step 2, to get length range be 1 ~ 20 μ m, the nano silver wire that diameter of section scope is 10 ~ 300nm, and the organic bonding agent solution that adds step 1 to obtain, nano silver wire amount is 50wt%, stirs, and obtains mixed liquor.
Wherein, the nano silver wire in described step 2 is made by following steps:
Step 3.1, get polyvinylpyrrolidone, reducing agent, metal halide and mix, obtain mixed liquor; Reducing agent is selected from the one in ethylene glycol, polyethylene glycol, EGME, ethanol; In described mixed liquor, the mass body volume concentrations of polyvinylpyrrolidone is 1-100g/L; The molal volume concentration of metal halide is 0.0001-0.01mol/L;
Step 3.2, the solution of step 3.1 compounding is heated to after 100-170 DEG C, the disposable silver salt that adds reacts wherein, and reaction finishes rear product to be carried out to eccentric cleaning, obtains nano silver wire; The amount control that the addition of silver salt is 0.001 ~ 0.20mol/L by the concentration of silver element in reaction system.
Wherein, described organic adhesive is polyvinyl alcohol.
A kind of conductive film, its high conductive silver paste low-temperature setting by the high conductive silver paste of above-mentioned low-temperature setting or the low-temperature setting that made by above-mentioned preparation method forms.
Wherein, its square resistance is lower than 0.1ohm/sq, and volume resistivity is less than 2x10
-5Ω cm, pencil hardness is 9H.
A preparation method for conductive film, comprises the steps 4: stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
Wherein, repeating step 4 once or twice.
Compared with prior art, the invention has the advantages that: can low-temperature setting, widely applicable, and conductance is higher, can be used for powerful occasion.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that conventional silver is starched nano-sized silver particles used;
Fig. 2 is the X-ray diffractogram that conventional silver is starched nano-sized silver particles used;
Fig. 3 is the staple diagram of embodiment 1 nano silver wire used;
Fig. 4 is the diameter of section distribution map of embodiment 1 all nano silver wires;
Fig. 5 is the staple diagram of embodiment 2 to 6 nano silver wires used;
Fig. 6 is the diameter of section distribution map of embodiment 2 to 6 nano silver wires used;
Fig. 7 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 1;
Fig. 8 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 1;
Fig. 9 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 2;
Figure 10 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 2;
Figure 11 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 3;
Figure 12 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 3;
Figure 13 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 4;
Figure 14 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 4;
Figure 15 is the scanning electron microscope (SEM) photograph (amplifying 10000 times) of the prepared conductive silver paste film thickness of embodiment 4
Figure 16 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 5;
Figure 17 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 5;
Figure 18 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste film thickness of embodiment 5
Figure 19 is the scanning electron microscope (SEM) photograph (amplifying 2000 times) of the prepared conductive silver paste of embodiment 6;
Figure 20 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste of embodiment 6;
Figure 21 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste film thickness of embodiment 4;
Figure 22 is 5.4 μ m for adopting average length, prepared corresponding different sheet resistances and the conductance of the different film thicknesses of conductive silver paste film of nano silver wire that diameter of section is 127nm;
Figure 23 is 7.1 μ m for adopting average length, prepared corresponding different sheet resistances and the conductance of the different film thicknesses of conductive silver paste film of nano silver wire that diameter of section is 287nm;
Figure 24 is the X-ray diffractogram that adopts the conductive silver paste prepared of nano silver wire;
Figure 25 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of preparing conductive silver paste nano silver wire used;
Figure 26 adopts knife coating to prepare the pictorial diagram of conductive silver paste.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
In the present embodiment, nano silver wire length, diameter test mode are:
The length of nano silver wire and diameter adopt particle diameter distribution tests software (version 1.1.33, Fudan University) to measure.In measuring process, first measure the screen pixels length scale of picture acceptance of the bid chi, then according to scale size preset proportion coefficient; Then measure the corresponding screen pixels length scale of length, diameter of nano wire, and calculate length and the diameter of nano wire according to proportionality coefficient.
Resistivity measurement adopts four point probe tester (Guangzhou semiconductor company), film thickness test adopts contourgraph (VeecoDektak 150), and hardness test is to use successively the Chinese pencil that hardness is 1H ~ 9H, and 45 degree tilt, power with 20N is streaked, and then sees whether film is scratched.
embodiment 1
1) measure 95mL deionized water, 5mg polyvinylpyrrolidone (PVP) is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains polyvinylpyrrolidonesolution solution;
2) get appropriate nano silver wire (average length 5.4 μ m, diameter 127nm, as Fig. 3 and Fig. 4), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
Above-mentioned nano silver wire makes (preparation method of the nano silver wire in each embodiment is also like this) below by following steps:
Step 1, get polyvinylpyrrolidone, reducing agent, metal halide and mix, obtain mixed liquor; Reducing agent is selected from the one in ethylene glycol, polyethylene glycol, EGME, ethanol; In mixed liquor, the mass body volume concentrations of polyvinylpyrrolidone is 1-100g/L; The molal volume concentration of metal halide is 0.0001-0.01mol/L;
Step 2, the solution of step 1 institute compounding is heated to after 100-170 DEG C, the disposable silver salt that adds reacts wherein, and reaction finishes rear product to be carried out to eccentric cleaning, obtains nano silver wire; The amount control that the addition of silver salt is 0.001 ~ 0.20mol/L by the concentration of silver element in reaction system.
Interpretation: Fig. 7 and Fig. 8 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, can see that silver slurry is uniformly dispersed.Measure film thickness and be about 1.6 μ m, sheet resistance is about 1.18ohm/sq, and resistivity is about 1.9*10
-4Ω cm, hardness is 7H.It is 5.4 μ m that accompanying drawing 22 has also been described as adopting average length, prepared corresponding different sheet resistances and the conductance of the different film thicknesses of conductive silver paste film of nano silver wire that diameter of section is 127nm.
embodiment 2
1) measure 99mL deionized water, 1mg polyvinyl alcohol (PVA) is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains poly-vinyl alcohol solution;
2) get appropriate nano silver wire (average length 7.1 μ m, diameter 287nm, as shown in Fig. 5, Fig. 6 and Figure 25), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
Interpretation: Fig. 9 and Figure 10 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, can see that silver slurry toughness is bad, and PVA content is less, and nano silver wire content is more.The X-ray diffractogram that accompanying drawing 24 is the conductive silver paste that adopts nano silver wire and prepare, can find out that this nano wire is argent structure.Measure film thickness and be about 1.9 μ m, sheet resistance is about 0.33ohm/sq, and resistivity is about 6.3*10
-5Ω cm, hardness is 2H.It is 7.1 μ m that accompanying drawing 23 has also been described as adopting average length, prepared corresponding different sheet resistances and the conductance of the different film thicknesses of conductive silver paste film of nano silver wire that diameter of section is 287nm.
embodiment 3
1) measure 98mL deionized water, 2mg polyethylene glycol (PEG) is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains polyglycol solution;
2) get appropriate nano silver wire (average length 7.1 μ m, diameter 287nm, as Fig. 5 and Fig. 6), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
Interpretation: Figure 11 and Figure 12 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, can see that silver slurry toughness is general, and PVA content is not high, and nano silver wire content is relatively many.Measure film thickness and be about 1.7 μ m, sheet resistance is about 0.43ohm/sq, and resistivity is about 7.3*10
-5Ω cm, hardness is 5H.
embodiment 4
1) measure 95mL deionized water, 5mg CMC is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains CMC solution;
2) get appropriate nano silver wire (average length 7.1 μ m, diameter 287nm, as Fig. 5 and Fig. 6), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
Interpretation: Figure 13 and Figure 14 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, can see that silver slurry is uniformly dispersed.Accompanying drawing 15 is the scanning electron microscope (SEM) photograph (amplifying 10000 times) of the prepared conductive silver paste film thickness of the present embodiment, measures film thickness and is about 1.5 μ m, and sheet resistance is about 0.72ohm/sq, and resistivity is about 1.1*10
-4Ω cm, hardness is 7H.
embodiment 5
1) measure 95mL deionized water, 5mg methylcellulose is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains methocel solution;
2) get appropriate nano silver wire (average length 7.1 μ m, diameter 287nm, as Fig. 5 and Fig. 6), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C;
5) repeat 4) once.
Interpretation: Figure 16 and Figure 17 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, can see that silver slurry is uniformly dispersed.Accompanying drawing 18 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste film thickness of the present embodiment, measures film thickness and is about 3.2 μ m, and sheet resistance is about 0.18ohm/sq, and resistivity is about 5.8*10
-5Ω cm, hardness is 9H.
embodiment 6
1) measure 95mL deionized water, 5mg polyvinyl alcohol (PVA) is configured to mixed liquor, is heated to 70 ° of C and stirs 20 minutes, treats that solution clarification is stable, obtains poly-vinyl alcohol solution;
2) get appropriate nano silver wire (average length 7.1 μ m, diameter 287nm, as Fig. 5 and Fig. 6), add 1) in the solution that obtains (nano silver wire amount is 50wt%), stir 0.5 hour, obtain the conductive silver paste of thickness;
3) get a slide, cut into needed size, use successively acetone, ethanol, deionized water ultrasonic cleaning 10 minutes, then dry up with nitrogen;
4) stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C;
5) repeat 4) twice.
Interpretation: Figure 19 and Figure 20 are the scanning electron microscope (SEM) photograph (amplify respectively 2000 times with 5000 times) of the prepared conductive silver paste of the present embodiment, and pictorial diagram as shown in figure 26, can see that silver slurry is uniformly dispersed.Accompanying drawing 21 is the scanning electron microscope (SEM) photograph (amplifying 5000 times) of the prepared conductive silver paste film thickness of the present embodiment, measures film thickness and is about 4.6 μ m, and sheet resistance is about 0.04ohm/sq, and resistivity is about 1.8*10
-5Ω cm, hardness is 9H.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is also not only confined to above-described embodiment.For those skilled in the art, also should be considered as protection scope of the present invention not departing from the improvement and the conversion that obtain under the technology of the present invention design prerequisite.
Claims (8)
1. the high conductive silver paste of a low-temperature setting, it is characterized in that, it adopts nano silver wire to form as conduction primitive and organic adhesive blend, described nano silver wire length range is 1 ~ 20 μ m, diameter of section scope is 10 ~ 300nm, described organic adhesive is one or more in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, CMC, methylcellulose, and nano silver wire amount is 50wt%.
2. a preparation method for the high conductive silver paste of low-temperature setting, is characterized in that comprising the steps:
Step 1, get appropriate organic adhesive and add in deionized water, 70 DEG C of stirring in water bath 10-30min, obtain colourless transparent solution, it is 1-5%wt that the amount of control organic adhesive makes the concentration of organic adhesive in solution, and described organic adhesive is a kind of, two or more the blend in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, CMC, methylcellulose;
Step 2, to get length range be 1 ~ 20 μ m, the nano silver wire that diameter of section scope is 10 ~ 300nm, and the organic bonding agent solution that adds step 1 to obtain, nano silver wire amount is 50wt%, stirs, and obtains mixed liquor.
3. the preparation method of the high conductive silver paste of low-temperature setting as claimed in claim 2, is characterized in that, the nano silver wire in described step 2 is made by following steps:
Step 3.1, get polyvinylpyrrolidone, reducing agent, metal halide and mix, obtain mixed liquor; Reducing agent is selected from the one in ethylene glycol, polyethylene glycol, EGME, ethanol; In described mixed liquor, the mass body volume concentrations of polyvinylpyrrolidone is 1-100g/L; The molal volume concentration of metal halide is 0.0001-0.01mol/L;
Step 3.2, the solution of step 3.1 compounding is heated to after 100-170 DEG C, the disposable silver salt that adds reacts wherein, and reaction finishes rear product to be carried out to eccentric cleaning, obtains nano silver wire; The amount control that the addition of silver salt is 0.001 ~ 0.20mol/L by the concentration of silver element in reaction system.
4. the preparation method of the high conductive silver paste of low-temperature setting as claimed in claim 2, is characterized in that, described organic adhesive is polyvinyl alcohol.
5. a conductive film, is characterized in that, the high conductive silver paste low-temperature setting of its low-temperature setting making by the high conductive silver paste of low-temperature setting claimed in claim 1 or by the arbitrary described preparation method of claim 2 to 4 forms.
6. conductive film as claimed in claim 5, is characterized in that, its square resistance is lower than 0.1ohm/sq, and volume resistivity is less than 2*10
-5Ω cm, pencil hardness is 9H.
7. the preparation method of the conductive film as described in claim 5 or 6, is characterized in that, comprises the steps 4: stick adhesive tape on sheet glass both sides, get appropriate silver slurry and drop in glass blank space, along a direction blade coating, guarantee that silver slurry is dispersed, anneal 10 minutes for 100 DEG C.
8. the preparation method of conductive film as claimed in claim 7, is characterized in that, repeating step 4 once or twice.
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