CN109979681A - A kind of preparation method of composite carbon nanometer tube nanometer silver paste - Google Patents
A kind of preparation method of composite carbon nanometer tube nanometer silver paste Download PDFInfo
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- CN109979681A CN109979681A CN201910230173.5A CN201910230173A CN109979681A CN 109979681 A CN109979681 A CN 109979681A CN 201910230173 A CN201910230173 A CN 201910230173A CN 109979681 A CN109979681 A CN 109979681A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 90
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 34
- 239000004332 silver Substances 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 37
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 21
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 21
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 6
- 239000011630 iodine Substances 0.000 claims abstract description 6
- 239000001509 sodium citrate Substances 0.000 claims description 30
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 239000011790 ferrous sulphate Substances 0.000 claims description 18
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 18
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 18
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 12
- 229960004756 ethanol Drugs 0.000 claims description 12
- 239000002048 multi walled nanotube Substances 0.000 claims description 12
- 238000006722 reduction reaction Methods 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 238000005189 flocculation Methods 0.000 claims description 6
- 230000016615 flocculation Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 238000009766 low-temperature sintering Methods 0.000 abstract description 2
- 239000010944 silver (metal) Substances 0.000 abstract 3
- 239000010946 fine silver Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 description 7
- 238000012958 reprocessing Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002083 iodinating effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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 a kind of preparation method of composite carbon nanometer tube nanometer silver paste, the composite carbon nanometer tube nanometer silver paste preparation method includes preparing super fine silver powder, being attached in carbon nanotube using iodine modified superfine silver powder, by super fine silver powder.The preparation method enables the nano-Ag particles of growth effectively to combine on the surface of carbon nanotubes, and enhance the bond strength between nano-Ag particles and carbon nanotube, guarantee that nano-Ag particles can uniformly disperse and combine on the surface of carbon nanotubes simultaneously, and activity is high, the contact resistance between carbon nanotube is effectively reduced, and there is low-temperature sintering characteristic.
Description
Technical field
The present invention relates to the preparations of a kind of chip-scale or the composite carbon nanometer tube nanometer silver paste of other micro devices attachments
Method.
Background technique
Carbon nanotube also known as Baji-tube are that a kind of have special construction (radial dimension is nanometer scale, and axial dimension is
Micron dimension, pipe both ends are substantially all sealing) One-dimensional Quantum material.Carbon nanotube is mainly former by the carbon of hexagonal arrangement
Son constitutes several layers to tens of layers of coaxial round tube.The distance being kept fixed between layers, about 0.34nm, diameter are generally 2-
20nm；And zigzag, armchair and three kinds of screw type can be divided into along axial different orientation according to carbon hexagon.
Wherein the carbon nanotube of screw type has chirality, and zigzag and armchair carbon nanotubes are without chirality.Due to carbon nanotube
Architectural characteristic, with many abnormal mechanics, electricity and chemical property；In recent years as carbon nanotube and nano material are ground
Its wide application prospect of going deep into studied carefully also constantly is shown.
Nanometer silver paste is as a kind of New-core chip level interconnection material, and compared to traditional solder solder tool, there are three excellent
Gesture: without interconnection welding spot remelting phenomenon, high heat-conductivity conducting performance, high reliability.
But the silver paste only containing smaller size nano-Ag particles there is a problem of sintering interconnection joint dimension it is unstable.It should
The nanometer silver paste of seed type be sintered to be formed interconnection connector after, during high-temperature service, microstructure does not reach final
Stable state, dimensional contraction can be occurred with the raising of service temperature by macroscopically showing as interconnection connector, influence interlinking reliability；
Also, only the sintered average grain size of the nanometer silver paste containing small size is small, and crystal boundary proportion is big, is situated between to as heat transfer
The scattering effect of the electronics of matter increases, and the thermal conductivity of sample reduces after causing nanometer silver paste to be sintered.
On the other hand, when only nano-Ag particles containing larger size in silver paste, the sintering of nano-material dimensional effect of silver paste
It can be reduced with the increase of nano-Ag particles partial size, temperature needed for leading to sintering interconnection improves, the time extends, for temperature-sensitive
For inductor component and substrate, it has been more than it by thermal energy power, has not had practical application.
Summary of the invention
It is an object of that present invention to provide a kind of preparation method of composite carbon nanometer tube nanometer silver paste, this method is prepared compound
Silver paste can improve thermal conductivity.
Steps are as follows for the method for the present invention:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；It will restore under agitation molten
Drop is added in silver nitrate solution, carries out reduction reaction；The nano-Ag particles that reduction is precipitated are by way of centrifuge separation
It is separated from solution, removes upper solution；Nano-Ag particles are placed in ultrapure water, ultrasonic disperse is uniform, is formed dense
Degree is 0.4-0.6mol/L nano silver colloidal sol；The sodium citrate solution that mass concentration is 0.3-0.5% is added into nano silver colloidal sol
It flocculates, is centrifugated；Water dispersion, sodium citrate solution flocculation, centrifugation, so at repetition is added in nano-Ag particles again
Reason 2 times or more, obtains partial size in the nano-Ag particles of 8-20nm, wherein in nano silver colloidal sol with the volume ratio of sodium citrate solution
For 2:1-3:1；
The molar ratio of the sodium citrate and ferrous sulfate is 1:30-1:40；The molar ratio of ferrous sulfate and silver nitrate is 3:1-
5:1；
The mixing speed is 100-200r/min；Centrifugation is that 3-5min is carried out at 3000-4000rpm；
(2) dispersed nano-silver particles made from step (1) are stirred at room temperature in iodine-alcohol dissolution solution, become limpid to liquid
Afterwards, it filters, vacuum drying obtains modified silver powder；
The iodine-alcohol dissolution solution is that every 100mL dehydrated alcohol addition 1-5g iodine is made；
(3) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, modified silver powder is then added to multi wall
In carbon nanotube emulsion, ethanol washing is used after mixing at room temperature, composite carbon nanometer tube nanometer silver paste is made in vacuum drying；
The mass ratio of modified silver powder and multi-walled carbon nanotube is 15:1-25:1 in step (3).
The thermally conductive overlap joint dependent between silver powder of thermally conductive silver paste, contraction when this is silver paste solidification, silver powder are drawn by epoxy molecule
Recently it realizes；Silver paste viscosity is generally up to 8000mPaS and curing reaction is completed within the shorter time；So silver powder
There is no the enough time to complete overlap joint, is formd among silver powder much seriously affect thermally conductive hole in this way；This hole
It is also impossible to disappear after silver paste solidification.
The inventors of the present application found that the heat transfer efficiency of silver paste can be improved in carbon nanotube, because carbon nanotube is a kind of
Nanometer materials, draw ratio are up to 108, so high draw ratio determines that it is deposited among silver powder with a kind of sinuous state
A nanotube can touch several silver powder particles simultaneously and fill up the gap between silver powder.
The advantages of the method for the present invention and technical effect:
The method of the present invention enables the nano-Ag particles of growth effectively to combine on the surface of carbon nanotubes, and enhances nanometer
Bond strength between Argent grain and carbon nanotube, while guaranteeing that nano-Ag particles can uniformly disperse and be incorporated in carbon nanometer
On the surface of pipe, and activity is high, and the contact resistance effectively reduced between carbon nanotube is (thermally conductive relative to conventional composite silver paste
600%) rate improves, and have low-temperature sintering characteristic.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1: steps are as follows for the preparation method of this composite carbon nanometer tube nanometer silver paste:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；In 100 r/min stirring conditions
It is lower that reducing solution is added dropwise in silver nitrate solution, carry out reduction reaction；The nano-Ag particles that reduction is precipitated are passed through into centrifugation
Isolated mode is separated from solution and (carries out 5min at 3,000 rpm), and upper solution is removed；Nano-Ag particles are placed
In ultrapure water, ultrasonic disperse is uniform, and forming concentration is 0.4mol/L nano silver colloidal sol；It is dense that quality is added into nano silver colloidal sol
Degree flocculates for 0.3% sodium citrate solution, is centrifugated (3min is carried out at 4000rpm)；Again in nano-Ag particles
Water dispersion, sodium citrate solution flocculation is added, centrifugation, so reprocessing 2 times obtain partial size in the nano silver of 8-20nm
Grain, wherein the molar ratio of sodium citrate and ferrous sulfate is 1:30；The molar ratio of ferrous sulfate and silver nitrate is 3:1, nano silver
In colloidal sol with the volume ratio of sodium citrate solution be 2:1；
(2) by dispersed nano-silver particles made from step (1), in iodine-alcohol dissolution solution, (every 100mL dehydrated alcohol adds 2g iodine system
) in, it is stirred at room temperature, after liquid becomes limpid, filters, vacuum drying obtains modified silver powder；
(3) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, modified silver powder is then added to multi wall
In carbon nanotube emulsion, ethanol washing is used after mixing at room temperature, is dried in vacuo 12h, composite carbon nanometer tube nano silver is made
Slurry, wherein the mass ratio of modified silver powder and multi-walled carbon nanotube is 15:1.
Embodiment 2: steps are as follows for the preparation method of this composite carbon nanometer tube nanometer silver paste:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；Under 150r/min stirring condition
Reducing solution is added dropwise in silver nitrate solution, reduction reaction is carried out；The nano-Ag particles that reduction is precipitated pass through centrifugation point
From mode from being separated in solution and (carry out 4min at 3500rpm), remove upper solution；Nano-Ag particles are placed in
In ultrapure water, ultrasonic disperse is uniform, and forming concentration is 0.5mol/L nano silver colloidal sol；Mass concentration is added into nano silver colloidal sol
It flocculates, is centrifugated (carrying out 5min at 3,000 rpm) for 0.5% sodium citrate solution；Add in nano-Ag particles again
Entering water dispersion, sodium citrate solution flocculation, centrifugation, so reprocessing 2 times obtain partial size in the nano-Ag particles of 8-20nm,
Wherein the molar ratio of sodium citrate and ferrous sulfate is 1:40；The molar ratio of ferrous sulfate and silver nitrate is 4:1, nano silver colloidal sol
In with the volume ratio of sodium citrate solution be 3:1；
(2) by dispersed nano-silver particles made from step (1), in iodine-alcohol dissolution solution, (every 100mL dehydrated alcohol adds 3g iodine system
) in, it is stirred at room temperature, after liquid becomes limpid, filters, vacuum drying obtains modified silver powder；
(3) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, modified silver powder is then added to multi wall
In carbon nanotube emulsion, ethanol washing is used after mixing at room temperature, is dried in vacuo 12h, composite carbon nanometer tube nano silver is made
Slurry, wherein the mass ratio of modified silver powder and multi-walled carbon nanotube is 20:1.
Embodiment 3: steps are as follows for the preparation method of this composite carbon nanometer tube nanometer silver paste:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；Under 200r/min stirring condition
Reducing solution is added dropwise in silver nitrate solution, reduction reaction is carried out；The nano-Ag particles that reduction is precipitated pass through centrifugation point
From mode from being separated in solution and (carry out 3min at 4000rpm), remove upper solution；Nano-Ag particles are placed in
In ultrapure water, ultrasonic disperse is uniform, and forming concentration is 0.6mol/L nano silver colloidal sol；Mass concentration is added into nano silver colloidal sol
It flocculates, is centrifugated (carrying out 4min at 3500rpm) for 0.4% sodium citrate solution；Add in nano-Ag particles again
Entering water dispersion, sodium citrate solution flocculation, centrifugation, so reprocessing 3 times obtain partial size in the nano-Ag particles of 8-20nm,
Wherein the molar ratio of sodium citrate and ferrous sulfate is 1:35；The molar ratio of ferrous sulfate and silver nitrate is 5:1, nano silver colloidal sol
In with the volume ratio of sodium citrate solution be 2.5:1；
(2) by dispersed nano-silver particles made from step (1), in iodine-alcohol dissolution solution, (every 100mL dehydrated alcohol adds 5g iodine system
) in, it is stirred at room temperature, after liquid becomes limpid, filters, vacuum drying obtains modified silver powder；
(3) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, modified silver powder is then added to multi wall
In carbon nanotube emulsion, ethanol washing is used after mixing at room temperature, is dried in vacuo 12h, composite carbon nanometer tube nano silver is made
Slurry, wherein the mass ratio of modified silver powder and multi-walled carbon nanotube is 25:1.
The composite carbon nanometer tube nanometer silver paste without iodinating has been done simultaneously as control；
Comparative example: steps are as follows for the preparation method of this composite carbon nanometer tube nanometer silver paste:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；In 100 r/min stirring conditions
It is lower that reducing solution is added dropwise in silver nitrate solution, carry out reduction reaction；The nano-Ag particles that reduction is precipitated are passed through into centrifugation
Isolated mode is separated from solution and (carries out 5min at 3,000 rpm), and upper solution is removed；Nano-Ag particles are placed
In ultrapure water, ultrasonic disperse is uniform, and forming concentration is 0.4mol/L nano silver colloidal sol；It is dense that quality is added into nano silver colloidal sol
Degree flocculates for 0.3% sodium citrate solution, is centrifugated (3min is carried out at 4000rpm)；Again in nano-Ag particles
Water dispersion, sodium citrate solution flocculation is added, centrifugation, so reprocessing 2 times obtain partial size in the nano silver of 8-20nm
Grain, wherein the molar ratio of sodium citrate and ferrous sulfate is 1:30；The molar ratio of ferrous sulfate and silver nitrate is 3:1, nano silver
In colloidal sol with the volume ratio of sodium citrate solution be 2:1；
(2) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, nano-Ag particles is then added to multi wall carbon
In nanotube emulsion, ethanol washing is used after mixing at room temperature, is dried in vacuo 12h, composite carbon nanometer tube nanometer silver paste is made,
Wherein the mass ratio of modified silver powder and multi-walled carbon nanotube is 15:1.
Composite carbon nanometer tube nanometer silver paste prepared by above-described embodiment and comparative example is subjected to heating conduction test, it is specific to survey
Method for testing is as follows.
Electrically and thermally conductive adhesive after solidification is milled into the disc-shaped of upper and lower surface smooth parallel, diameter in 11.8 mm or so,
Then thickness about 1mm sprays carbon shading in sample surfaces, measures electrically and thermally conductive adhesive using 447 thermal conductivity instrument of model Netch LFA
Heat transfer property.
Test result is as follows
。
Claims (6)
1. a kind of preparation method of composite carbon nanometer tube nanometer silver paste, which is characterized in that steps are as follows:
(1) sodium citrate solution is uniformly mixed with ferrous sulfate solution, reducing solution is made；It will restore under agitation molten
Drop is added in silver nitrate solution, carries out reduction reaction；The nano-Ag particles that reduction is precipitated are by way of centrifuge separation
It is separated from solution, removes upper solution；Nano-Ag particles are placed in ultrapure water, ultrasonic disperse is uniform, is formed dense
Degree is 0.4-0.6mol/L nano silver colloidal sol；The sodium citrate solution that mass concentration is 0.3-0.5% is added into nano silver colloidal sol
It flocculates, is centrifugated；Water dispersion, sodium citrate solution flocculation, centrifugation, so at repetition is added in nano-Ag particles again
Reason 2 times or more, obtains partial size in the nano-Ag particles of 8-20nm, wherein in nano silver colloidal sol with the volume ratio of sodium citrate solution
For 2:1-3:1；
(2) dispersed nano-silver particles made from step (1) are stirred at room temperature in iodine-alcohol dissolution solution, become limpid to liquid
Afterwards, it filters, vacuum drying obtains modified silver powder；
(3) multi-walled carbon nanotube is added in ethanol, carries out ultrasonic emulsification processing, modified silver powder is then added to multi wall
In carbon nanotube emulsion, ethanol washing is used after mixing at room temperature, composite carbon nanometer tube nanometer silver paste is made in vacuum drying.
2. the preparation method of composite carbon nanometer tube nanometer silver paste according to claim 1, it is characterised in that: sodium citrate with
The molar ratio of ferrous sulfate is 1:30-1:40；The molar ratio of ferrous sulfate and silver nitrate is 3:1-5:1.
3. the preparation method of composite carbon nanometer tube nanometer silver paste according to claim 1, it is characterised in that: in step (1)
Mixing speed is 100-200r/min.
4. the preparation method of composite carbon nanometer tube nanometer silver paste according to claim 1, it is characterised in that: in step (1)
Centrifugation is that 3-5min is carried out at 3000-4000rpm.
5. the preparation method of composite carbon nanometer tube nanometer silver paste according to claim 1, it is characterised in that: iodine-alcohol dissolution is molten
Liquid is that every 100mL dehydrated alcohol addition 1-5g iodine is made.
6. the preparation method of composite carbon nanometer tube nanometer silver paste according to claim 1, it is characterised in that: in step (3)
The mass ratio of modified silver powder and multi-walled carbon nanotube is 15:1-25:1.
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| CN111077129A (en) * | 2019-12-19 | 2020-04-28 | 江汉大学 | Surface-enhanced Raman spectrum substrate and preparation method thereof |
| CN111403081A (en) * | 2020-03-19 | 2020-07-10 | 深圳市金百纳纳米科技有限公司 | Carbon nanotube conductive slurry and preparation method thereof |
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