CN109887638A - The multi-dimension nano silver paste and preparation method thereof that nano-Ag particles are mixed with silver-plated silicon-carbide particle - Google Patents
The multi-dimension nano silver paste and preparation method thereof that nano-Ag particles are mixed with silver-plated silicon-carbide particle Download PDFInfo
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Abstract
The invention discloses the multi-dimension nano silver pastes and preparation method thereof that a kind of nano-Ag particles are mixed with silver-plated silicon-carbide particle; it is related to a kind of novel interfacial interconnection material; in particular to a kind of multi-dimension nano silver paste for being added to silver-plated silicon-carbide particle, including its formula and preparation flow.The present invention is prepared by triethylene glycol, polyvinyl butyral, terpinol, nano-Ag particles and the silver-plated silicon-carbide particle of sub-micron and is formed, each component mass percent are as follows: triethylene glycol 0.5-1.2%, polyvinyl butyral 5.6-12.2%, terpinol 3.89-8.56%, nano-Ag particles 76-90%, silver-plated silicon-carbide particle 0.5-2%.The present invention replaces part nano-Ag particles to be added in silver paste using silicon-carbide particle, reduces the porosity of silver paste after sintering, improves the performance of silver paste, reduces nanometer silver paste cost, and improve the sintered performance of silver paste.
Description
Technical field
The present invention relates to a kind of nano silver materials and preparation method thereof, more particularly to a kind of nanometer silver paste and its preparation side
Method is applied to interface interconnection material and technology field.
Background technique
With the development of semiconductor technology, chip output power increases, frequency improves, electronic product moves towards miniaturization, especially
It is the appearance for the silicon carbide new type integrated circuit chip that can be worked in 250 DEG C or more of hot environment, so that chip operation
Environment temperature increase substantially, and high temperature will lead to solder reflow influences its reliability, and the relatively low-heat of traditional interface material
Conductance has been unable to meet requirement of the high power density package system to heat dissipation, and nanometer silver paste relies on its low-temperature sintering high-temperature service
This excellent properties and become current most promising interface interconnection material.
Main stuffing of the nano-Ag particles as nanometer silver paste, the height of cost constrain the development of nanometer silver paste and answer
With.Silicon carbide has the heating conduction that can be matched in excellence or beauty with silver, but the price of silicon carbide is several times lower than than silver, is that one kind is expected to replace silver
The inexpensive Heat Conduction Material of particle, in addition, silicon carbide also has many excellent characteristics, as hardness is high, intensity is big, creep-resistant property
It is good, resistant to chemical etching, antioxygenic property is good, thermal expansion coefficient is small, high heat conductance etc., but the temperature of silicon carbide sintering is high, burns
Porosity after knot is high, and the sintered material fragility of silicon carbide is big, not ideal enough with the interconnection of semiconductor substrate, influences to radiate
Effect.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The multi-dimension nano silver paste and preparation method thereof that nano-Ag particles are mixed with silver-plated silicon-carbide particle, is replaced using silicon-carbide particle
Part nano-Ag particles are added in silver paste, and after the particle mixing of two kinds of sizes, small sized particles be can be filled in large-size particle
Between gap in, reduce silver paste porosity after sintering, improve the performance of silver paste, silicon carbide also has lower thermal expansion
Coefficient, can be improved the reliability of silver paste, improve nanometer silver paste Mechanical Reliability energy well, and reduce silver paste cost.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle, by triethylene glycol, polyethylene
Butyral, terpinol, nano-Ag particles and the silver-plated silicon-carbide particle of sub-micron are prepared and are formed, and each component mass percent is such as
Under:
Above-mentioned whole each component mass percent summation is 100%.
As currently preferred technical solution, the multi-dimension nano that nano-Ag particles are mixed with silver-plated silicon-carbide particle is silver-colored
Slurry, each component mass percent are as follows:
Above-mentioned whole each component mass percent summation is 100%.
As currently preferred technical solution, above-mentioned silver-plated silicon-carbide particle is silicon B-carbide, and average grain diameter is
0.1-5 microns, the structure of silver-plated silicon-carbide particle are as follows: coat the silver with a thickness of 10-100 nanometers on the surface of silicon-carbide particle
Layer, form the silver-colored shell of package has metal-inorganic non-metallic composite construction compound carbonizing silicon particle.
It is preferred that the surface silver layer of above-mentioned silver-plated silicon-carbide particle is by chemical plating, deposition or sputtering method in silicon-carbide particle
Surface Creation.
It is preferred that the average grain diameter of above-mentioned nano-Ag particles is 5-30 nanometers.
It is preferred that above-mentioned triethylene glycol is used as dispersing agent, start to decompose at not less than 100 DEG C.
It is preferred that above-mentioned polyvinyl butyral is used as organic carrier, start to decompose not less than 300 DEG C.
It is preferred that terpinol is used as diluent, start to decompose not less than 60 DEG C.
A kind of preparation method for the multi-dimension nano silver paste that nano-Ag particles of the present invention are mixed with silver-plated silicon-carbide particle, is pressed
The component formula in multi-dimension nano silver paste mixed according to the nano-Ag particles of target preparation with silver-plated silicon-carbide particle is taken respectively
Component raw material includes the following steps:
A. dehydrated alcohol is added into beaker as basic solvent, after heating, polyethylene is added into beaker while stirring
Butyral makes polyvinyl butyral and ethyl alcohol be thoroughly mixed to form carrier solvent, spare；It is preferred that heating temperature is not less than 60
DEG C, and it is lower than the boiling temperature of ethyl alcohol；
B. the mixed carrier solvent prepared in step a is cooled down, after being cooled to room temperature, is added to mixed carrier solvent
Triethylene glycol and terpinol are dispersed and are diluted to mixed carrier solvent, obtain support dispersion；
C. at room temperature, the support dispersion prepared in stepb is stirred, and while stirring to carrier point
Nano-Ag particles and silver-plated silicon-carbide particle are added in dispersion liquid, controls mixing time at least 15min, obtains nano-Ag particles and plating
The mixed serum of silver-colored silicon-carbide particle；
D. the mixed serum prepared in step c is post-processed, is handled using ultrasonic homogenation, mixed serum is carried out
When ultrasonic, by cooling down to mixed serum addition ice cube or ice water, and control mixed serum and be not higher than 28 DEG C, ultrasonic time
No less than 30min, after ultrasonic homogenation treatment process, obtain nano-Ag particles mixed with silver-plated silicon-carbide particle it is more
Scale nanometer silver paste.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the present invention fills out the nano-Ag particles of small size by mixing nano particle and the silver-plated silicon-carbide particle of sub-micron
It fills in the gap between the silver-plated silicon-carbide particle of larger size, the porosity of silver paste after sintering can be reduced, improve silver paste
Performance, silicon carbide also has lower thermal expansion coefficient, the reliability of silver paste can be improved, and improves the sintered property of silver paste
Energy；
2. the present invention substitutes a small amount of nano-Ag particles using silicon-carbide particle and also reduces the cost of silver paste；
3. the preparation method of composite Nano silver paste of the present invention is simple, easily controllable, nano-Ag particles and carbon are taken full advantage of
The material property advantage of silicon carbide particle makes silicon-carbide particle and nano silver by the surface modification and optimization to silicon-carbide particle
Sufficiently fusion forms nano-Ag particles-silicon-carbide particle composite silver slurry system, is preferably used as interface interconnection material forerunner's somaplasm
Liquid material.
Detailed description of the invention
Fig. 1 is that the silver-plated silicon-carbide particle SEM of the preferred embodiment of the present invention schemes.
Fig. 2 is the multi-dimension nano silver paste that the nano-Ag particles of the preferred embodiment of the present invention are mixed with silver-plated silicon-carbide particle
The multiple dimensioned particle mixing schematic diagram of the agglomerated material obtained after being sintered.
Fig. 3 is the silver paste preparation technology flow chart of the preferred embodiment of the present invention.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under:
Embodiment one:
In the present embodiment, referring to figures 1-3, what a kind of nano-Ag particles were mixed with silver-plated silicon-carbide particle multiple dimensioned receives
The preparation method of rice silver paste, includes the following steps:
A. the dehydrated alcohol of 30ml is added into beaker as basic solvent, is put on warm table and is heated to 60 DEG C, use
Balance weighs 0.8g polyvinyl butyral, and polyvinyl butyral is added into beaker while stirring, makes polyvinyl alcohol contracting fourth
Aldehyde and ethyl alcohol are thoroughly mixed to form carrier solvent, spare；Heating temperature is lower than the boiling temperature of ethyl alcohol, reduces the volatilization of ethyl alcohol
Amount, saves solvent, reduces solvent consumption, while being conducive to polyvinyl butyral polymer in a heated condition in ethyl alcohol
Uniform mixing in base solvent；
B. the mixed carrier solvent prepared in step a is cooled down, after being cooled to room temperature, beaker is put on balance,
0.08g triethylene glycol and 0.56g terpinol is added to mixed carrier solvent, mixed carrier solvent is dispersed and diluted, is obtained
To support dispersion；
C. at room temperature, place the beaker under mechanical agitator, the support dispersion prepared in stepb is carried out
Stirring, and into support dispersion, addition 6.52g nano-Ag particles and the silver-plated silicon-carbide particle of 0.04g, control are stirred while stirring
Mixing the time is 15min, obtains the mixed serum of nano-Ag particles and silver-plated silicon-carbide particle；The average grain diameter of nano-Ag particles is
5-30 nanometers；
D. the mixed serum prepared in step c is post-processed, is handled using ultrasonic homogenation, mixed serum is carried out
When ultrasonic, by cooling down to mixed serum addition ice cube or ice water, and mixed serum is controlled lower than 28 DEG C, ultrasonic time is
30min, after ultrasonic homogenation treatment process, obtain that nano-Ag particles mix with silver-plated silicon-carbide particle multiple dimensioned is received
Rice silver paste.
In the present embodiment, microcosmic SEM observation is carried out to the silver-plated silicon-carbide particle that the present embodiment uses, Fig. 1 is silver-plated
Silicon-carbide particle SEM figure, silver-plated silicon-carbide particle are silicon B-carbide, and average grain diameter is 0.1-5 microns, silver-plated silicon-carbide particle
Structure are as follows: on the surface of silicon-carbide particle, cladding is with a thickness of 10-100 nanometer of silver layer, forms that wrap up having for silver-colored shell golden
Category-inorganic non-metallic composite construction compound carbonizing silicon particle.It is modified by surface of the chemical vapor deposition to silicon-carbide particle
And silver-plated silicon-carbide particle is made in silicon-carbide particle Surface Creation surface silver layer in optimization.The nano-Ag particles of the present embodiment with
Thermal conductivity of the agglomerated material that the multi-dimension nano silver paste of silver-plated silicon-carbide particle mixing obtains after being sintered as interconnection material
Rate is 124W/m-K, and thermal expansion coefficient is 2.82 × 10-5/K.Fig. 2 is the nano-Ag particles and silver-plated silicon carbide of the present embodiment
The multiple dimensioned particle mixing schematic diagram for the agglomerated material that the multi-dimension nano silver paste of grain mixing obtains after being sintered, passes through mixing
Nano particle and the silver-plated silicon-carbide particle of sub-micron, make the nano-Ag particles of small size be filled in the silver-plated silicon carbide of larger size
In gap between particle, the porosity of silver paste after sintering is reduced, improves the performance of silver paste, silicon carbide also has lower
The reliability of silver paste can be improved in thermal expansion coefficient.
Embodiment two:
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, referring to figures 1-3, what a kind of nano-Ag particles were mixed with silver-plated silicon-carbide particle multiple dimensioned receives
The preparation method of rice silver paste, includes the following steps:
A. the dehydrated alcohol of 30ml is added into beaker as basic solvent, is put on warm table and is heated to 60 DEG C, use
Balance weighs 0.444g polyvinyl butyral, and polyvinyl butyral is added into beaker while stirring, polyvinyl alcohol is made to contract
Butyraldehyde and ethyl alcohol are thoroughly mixed to form carrier solvent, spare；Heating temperature is lower than the boiling temperature of ethyl alcohol, reduces the volatilization of ethyl alcohol
Amount, saves solvent, reduces solvent consumption, while being conducive to polyvinyl butyral polymer in a heated condition in ethyl alcohol
Uniform mixing in base solvent；
B. the mixed carrier solvent prepared in step a is cooled down, after being cooled to room temperature, beaker is put on balance,
0.044g triethylene glycol and 0.311g terpinol is added to mixed carrier solvent, mixed carrier solvent is dispersed and diluted,
Obtain support dispersion；
C. at room temperature, place the beaker under mechanical agitator, the support dispersion prepared in stepb is carried out
Stirring, and into support dispersion, addition 7.16g nano-Ag particles and the silver-plated silicon-carbide particle of 0.04g, control are stirred while stirring
Mixing the time is 15min, obtains the mixed serum of nano-Ag particles and silver-plated silicon-carbide particle；
D. the mixed serum prepared in step c is post-processed, is handled using ultrasonic homogenation, mixed serum is carried out
When ultrasonic, by cooling down to mixed serum addition ice cube or ice water, and mixed serum is controlled lower than 28 DEG C, ultrasonic time is
30min, after ultrasonic homogenation treatment process, obtain that nano-Ag particles mix with silver-plated silicon-carbide particle multiple dimensioned is received
Rice silver paste.
In the present embodiment, as shown in Figure 1-Figure 3.Microcosmic SEM is carried out to the silver-plated silicon-carbide particle that the present embodiment uses
Observation, Fig. 1 are silver-plated silicon-carbide particle SEM figure, and silver-plated silicon-carbide particle is silicon B-carbide, and average grain diameter is 0.1-5 microns,
The structure of silver-plated silicon-carbide particle are as follows: cladding forms package with a thickness of 10-100 nanometers of silver layer on the surface of silicon-carbide particle
Silver-colored shell has metal-inorganic non-metallic composite construction compound carbonizing silicon particle.By chemical plating to silicon-carbide particle
Surface is modified and optimizes, and in silicon-carbide particle Surface Creation surface silver layer, silver-plated silicon-carbide particle is made.The nanometer of the present embodiment
The agglomerated material that the multi-dimension nano silver paste that Argent grain is mixed with silver-plated silicon-carbide particle obtains after being sintered is as interconnection material
The thermal conductivity of material is 124W/m-K, and thermal expansion coefficient is 2.82 × 10-5/K.Fig. 2 be the present embodiment nano-Ag particles with it is silver-plated
The multiple dimensioned particle mixing schematic diagram for the agglomerated material that the multi-dimension nano silver paste of silicon-carbide particle mixing obtains after being sintered,
By mixing nano particle and the silver-plated silicon-carbide particle of sub-micron, the nano-Ag particles of small size is made to be filled in the plating of larger size
In gap between silver-colored silicon-carbide particle, the porosity of silver paste after sintering is reduced, the performance of silver paste is improved, silicon carbide also has
There is lower thermal expansion coefficient, the reliability of silver paste can be improved.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, referring to figures 1-3, what a kind of nano-Ag particles were mixed with silver-plated silicon-carbide particle multiple dimensioned receives
The preparation method of rice silver paste, includes the following steps:
A. the dehydrated alcohol of 30ml is added into beaker as basic solvent, is put on warm table and is heated to 60 DEG C, use
Balance weighs 0.8g polyvinyl butyral, and polyvinyl butyral is added into beaker while stirring, makes polyvinyl alcohol contracting fourth
Aldehyde and ethyl alcohol are thoroughly mixed to form carrier solvent, spare；Heating temperature is lower than the boiling temperature of ethyl alcohol, reduces the volatilization of ethyl alcohol
Amount, saves solvent, reduces solvent consumption, while being conducive to polyvinyl butyral polymer in a heated condition in ethyl alcohol
Uniform mixing in base solvent；
B. the mixed carrier solvent prepared in step a is cooled down, after being cooled to room temperature, beaker is put on balance,
0.08g triethylene glycol and 0.56g terpinol is added to mixed carrier solvent, mixed carrier solvent is dispersed and diluted, is obtained
To support dispersion；
C. at room temperature, place the beaker under mechanical agitator, the support dispersion prepared in stepb is carried out
Stirring, and 6.4g nano-Ag particles and the silver-plated silicon-carbide particle of 0.16g is added into support dispersion while stirring, control stirring
Time is 15min, obtains the mixed serum of nano-Ag particles and silver-plated silicon-carbide particle；
D. the mixed serum prepared in step c is post-processed, is handled using ultrasonic homogenation, mixed serum is carried out
When ultrasonic, by cooling down to mixed serum addition ice cube or ice water, and mixed serum is controlled lower than 28 DEG C, ultrasonic time is
30min, after ultrasonic homogenation treatment process, obtain that nano-Ag particles mix with silver-plated silicon-carbide particle multiple dimensioned is received
Rice silver paste.
In the present embodiment, as shown in Figure 1-Figure 3.Microcosmic SEM is carried out to the silver-plated silicon-carbide particle that the present embodiment uses
Observation, Fig. 1 are silver-plated silicon-carbide particle SEM figure, and silver-plated silicon-carbide particle is silicon B-carbide, and average grain diameter is 0.1-5 microns,
The structure of silver-plated silicon-carbide particle are as follows: cladding forms package with a thickness of 10-100 nanometers of silver layer on the surface of silicon-carbide particle
Silver-colored shell has metal-inorganic non-metallic composite construction compound carbonizing silicon particle.By sputtering method to silicon-carbide particle
Surface is modified and optimization, in silicon-carbide particle Surface Creation surface silver layer, silver-plated silicon-carbide particle is made.The present embodiment is received
The agglomerated material that the multi-dimension nano silver paste that rice Argent grain is mixed with silver-plated silicon-carbide particle obtains after being sintered is as interconnection
The thermal conductivity of material is 124W/m-K, and thermal expansion coefficient is 2.82 × 10-5/K.Fig. 2 is the nano-Ag particles and plating of the present embodiment
The multiple dimensioned particle mixing signal for the agglomerated material that the multi-dimension nano silver paste of silver-colored silicon-carbide particle mixing obtains after being sintered
Figure makes the nano-Ag particles of small size be filled in larger size by mixing nano particle and the silver-plated silicon-carbide particle of sub-micron
Silver-plated silicon-carbide particle between gap in, reduce the porosity of silver paste after sintering, improve the performance of silver paste, silicon carbide
Also there is lower thermal expansion coefficient, the reliability of silver paste can be improved.
In summary, the multi-dimension nano silver paste that above-described embodiment nano-Ag particles are mixed with silver-plated silicon-carbide particle uses
Silicon-carbide particle replaces part nano-Ag particles to be added into silver paste, and silicon carbide has the heating conduction that can be matched in excellence or beauty with silver, but
The price of silicon carbide is but several times lower than than silver, substitutes part nano-Ag particles using the silicon-carbide particle of sub-micron, can reduce silver paste
Cost, meanwhile, after the particle mixing of two kinds of sizes, small sized particles be can be filled in the gap between large-size particle, drop
The porosity of low silver paste after sintering, improves the performance of silver paste.It can not be mutual with Argent grain in order to solve silicon carbide in sintering process
Even the problem of, above-described embodiment plate nano-silver layer in silicon carbide by chemical plating, evaporation and the method for sputtering.This is multiple dimensioned
Silver paste is prepared and group by triethylene glycol, polyvinyl butyral, terpinol, nano-Ag particles and the silver-plated silicon-carbide particle of sub-micron
At.Above-described embodiment is prepared for novel interfacial interconnection material, is added to the multi-dimension nano silver paste of silver-plated silicon-carbide particle, uses
Above-mentioned formula and preparation flow replace part nano-Ag particles to be added into silver paste using silicon-carbide particle, not only can be with
Reduce cost, moreover it is possible to improve nanometer silver paste Mechanical Reliability energy well, have in microelectronic field, especially aerospace electron field
There is good application value.The multi-dimension nano silver that nano-Ag particles prepared in the above embodiments are mixed with silver-plated silicon-carbide particle
Slurry is used as agglomerated material persursor material, and in sintering temperature-rise period and in sintering process, ethyl alcohol constantly volatilizees；Terpinol is used as
Diluent starts to decompose at 60 DEG C；Triethylene glycol is used as dispersing agent and starts to decompose at 100 DEG C；Polyvinyl butyral, which is used as, to be had
Airborne body starts to decompose at 300 DEG C.Composite Nano silver paste prepared in the above embodiments by its low-temperature sintering high-temperature service this
Excellent properties and become current most promising interface interconnection material, the cost of nanometer silver paste can be reduced, and improve silver paste sintering
Performance afterwards.Above-described embodiment is prepared for multi-dimension nano silver paste, passes through mixing nano particle and the silver-plated silicon carbide of sub-micron
Grain, is filled in the nano-Ag particles of small size in the gap between the silver-plated silicon-carbide particle of larger size, can reduce silver paste
Porosity after sintering improves the performance of silver paste, and silicon carbide also has lower thermal expansion coefficient, and can be improved silver paste can
By property.In addition, the cost of silver paste can be reduced by substituting a small amount of nano-Ag particles also using silicon-carbide particle.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, substitution, combination or the simplification made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
The multi-dimension nano silver paste mixed without departing from nano-Ag particles of the present invention with silver-plated silicon-carbide particle and preparation method thereof
Technical principle and inventive concept, belong to protection scope of the present invention.
Claims (10)
1. the multi-dimension nano silver paste that a kind of nano-Ag particles are mixed with silver-plated silicon-carbide particle, which is characterized in that You Sanyi bis-
Alcohol, polyvinyl butyral, terpinol, nano-Ag particles and the silver-plated silicon-carbide particle of sub-micron are prepared and are formed, each group sub-prime
It is as follows to measure percentage:
Above-mentioned whole each component mass percent summation is 100%.
2. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
It is, each component mass percent is as follows:
Above-mentioned whole each component mass percent summation is 100%.
3. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
Be: the silver-plated silicon-carbide particle is silicon B-carbide, and average grain diameter is 0.1-5 microns, the structure of silver-plated silicon-carbide particle
Are as follows: on the surface of silicon-carbide particle, cladding forms with a thickness of 10-100 nanometers of silver layer and wraps up the inorganic with metal-of silver-colored shell
The compound carbonizing silicon particle of Nonmetallic Composite Structure.
4. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 3, feature
Be: the surface silver layer of the silver-plated silicon-carbide particle is by chemical plating, deposition or sputtering method on silicon-carbide particle surface
It generates.
5. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
Be: the average grain diameter of the nano-Ag particles is 5-30 nanometers.
6. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
Be: the triethylene glycol is used as dispersing agent, starts to decompose at not less than 100 DEG C.
7. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
Be: the polyvinyl butyral is used as organic carrier, starts to decompose not less than 300 DEG C.
8. the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 1, feature
Be: the terpinol is used as diluent, starts to decompose not less than 60 DEG C.
9. the preparation side for the multi-dimension nano silver paste that nano-Ag particles described in a kind of claim 1 are mixed with silver-plated silicon-carbide particle
Method, which is characterized in that in the multi-dimension nano silver paste mixed according to nano-Ag particles prepared by target with silver-plated silicon-carbide particle
Component formula take each component raw material, include the following steps:
A. dehydrated alcohol is added into beaker as basic solvent, after heating, polyvinyl alcohol contracting is added into beaker while stirring
Butyraldehyde makes polyvinyl butyral and ethyl alcohol be thoroughly mixed to form carrier solvent, spare；
B. the mixed carrier solvent prepared in the step a is cooled down, after being cooled to room temperature, is added to mixed carrier solvent
Triethylene glycol and terpinol are dispersed and are diluted to mixed carrier solvent, obtain support dispersion；
C. at room temperature, the support dispersion prepared in the step b is stirred, and while stirring to carrier point
Nano-Ag particles and silver-plated silicon-carbide particle are added in dispersion liquid, controls mixing time at least 15min, obtains nano-Ag particles and plating
The mixed serum of silver-colored silicon-carbide particle；
D. the mixed serum prepared in the step c is post-processed, is handled using ultrasonic homogenation, mixed serum is carried out
When ultrasonic, by cooling down to mixed serum addition ice cube or ice water, and control mixed serum and be not higher than 28 DEG C, ultrasonic time
No less than 30min, after ultrasonic homogenation treatment process, obtain nano-Ag particles mixed with silver-plated silicon-carbide particle it is more
Scale nanometer silver paste.
10. the preparation for the multi-dimension nano silver paste that nano-Ag particles are mixed with silver-plated silicon-carbide particle according to claim 9
Method, it is characterised in that: in the step a, heating temperature is not less than 60 DEG C, and is lower than the boiling temperature of ethyl alcohol.
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| CN110773908A (en) * | 2019-10-28 | 2020-02-11 | 深圳第三代半导体研究院 | Preparation method and sintering method of low-temperature sintered indium-doped nano-silver sintering paste |
| CN111360280A (en) * | 2020-04-09 | 2020-07-03 | 大连海事大学 | Raman enhancement material and rapid preparation method thereof |
| WO2022037317A1 (en) * | 2020-08-17 | 2022-02-24 | 深圳市绎立锐光科技开发有限公司 | Wavelength conversion apparatus and manufacturing method therefor |
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