CN109570814A - A kind of composite solder paste adding micro-nano granules - Google Patents
A kind of composite solder paste adding micro-nano granules Download PDFInfo
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- CN109570814A CN109570814A CN201910031132.3A CN201910031132A CN109570814A CN 109570814 A CN109570814 A CN 109570814A CN 201910031132 A CN201910031132 A CN 201910031132A CN 109570814 A CN109570814 A CN 109570814A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
A kind of composite solder paste adding micro-nano granules, the invention belongs to leadless composite solder technical fields, and in particular to a kind of tin antimony system composite solder paste and preparation method thereof of addition micro-nano coated granular enhancing.Present invention mainly solves Sn-Sb brazing filler metal wetability, thermal conductivity and mechanical property in current high-temp solder are poor, the problem of limiting its application.It is good relative to SnSb system soldering paste wetability that the NEW TYPE OF COMPOSITE soldering paste is mainly characterized by, excellent in mechanical performance.Solder of the present invention is made of 1% ~ 5% Cu@Ag nucleocapsid particles and 95% ~ 99% SnSb, is to be realized using Sn-Sb soldering paste as matrix by adding reinforced phase Cu@Ag particle.The method of the present invention: one, Cu@Ag nucleocapsid particles are prepared；Two, scaling powder is prepared；Three, Cu@Ag nucleocapsid particles and Sn-Sb system soldering paste are prepared into composite solder paste by way of mechanical mixture.Composite solder paste of the invention has refined the microstructure of solder joint, greatly improves the wetability and shear strength of solder.The present invention is used to prepare Sn-Sb system composite soldering, is a kind of composite soldering for meeting present electronics industry development trend.
Description
Technical field
The present invention relates to a kind of composite solder pastes and preparation method thereof.
Background technique
IC industry is constantly to high density, high-power, multifunctional direction development, and packaging density is higher and higher, solder joint
Smaller and smaller, mechanics, the electricity and heat load carried is then increasingly heavier, thus proposes today for the reliability of solder joint
It is higher to ask.
Using SiC as the third generation semiconductor and its power device of representative, fieldtron, Schottky diode etc. by
It is widely applied, operating temperature is higher, but is not resistant to but for the solder that electrode draws material and chip package so high
Temperature, therefore the microelectronics Packaging lead-free brazing that exploitation can be on active service under the environment such as high temperature and pressure is needed, but high temperature pricker at present
The use of material is still in the majority with high lead solder, due to forbidding in current world wide, limiting solder containing lead element in electronic product
Use, it requires that searching develops novel connecting material to substitute the high lead high temperature solder materials of tradition.
Current existing mainstream lead-free brazing is Sn-Ag-Cu brazing filler metal, using SAC305 as representative, has good wetting
Property, higher Joint Reliability and thermal fatigue resistance etc., but its fusing point is about at 217 DEG C or so.With great-power electronic
The continuous popularization in fields such as automotive electronics, nuclear energy exploitation, municipal power supply systems of device, encapsulation solder reliably take at high temperature
Labour faces test, so needing the high-temp solder that exploitation can be on active service under high temperature environment.
And high-temp solder used at present, such as AuSn, nano mattisolda etc., although can be on active service under high temperature environment,
It is that its large-scale application largely, is limited due to its high cost.SnSb alloy melting point is at 249 DEG C or so, just
There is higher melt, there is certain advantage on high-temperature service.Compared with existing Sn-Ag-Cu brazing filler metal, SnSb series leadless solder
It is with the obvious advantage especially in terms of high temperature creep-resisting with better high-temperature service performance.Nevertheless, Sn-Sb system soldering paste shapes
The poor, thermal conductivity of property and electric conductivity is poor and mechanical property is poor, which also limits its applications, therefore propose to SnSb
Reinforced phase particle is added in system, improves performance, and is researched and developed and be suitable for high temperature power device encapsulation novel lead-free soldering paste.
Summary of the invention
The purpose of the present invention is to solve existing soldering paste formabilities poor, poor thermal conductivity, poorly conductive and poor mechanical property
Etc. technical problems, provide it is a kind of add micro-nano granules composite solder paste and preparation method thereof.
It is a kind of add micro-nano granules composite solder paste be made of metal powder and scaling powder: it is described it is a kind of addition it is micro-nano
The mass fraction of metal powder in the composite solder paste of particle is 80%-90%, and the mass fraction of scaling powder is 10%-20%.
Metal powder mass content be respectively Cu@Ag be 0.10% ~ 5.00%, Ag be 0.30%~1.20%, Cu be 0.50% ~
0.90%, Ni is 0.03%~0.05%, remaining is Sn10Sb powder.
Scaling powder is according to mass content by 15% activating agent, 37.5% film forming agent, 1% thixotropic agent, 1.5% regulator, 1.5% table
Face activating agent, 0.5% corrosion inhibiter and solvent composition.
A kind of preparation method of composite solder paste that adding micro-nano granules carries out according to the following steps.
One, Cu@Ag particle is prepared using liquid phase reduction.
Step 1: weighing appropriate copper powder.The sulfuric acid cleaned that configuration volumetric concentration is 20% is added, is centrifuged, washs.Together
When prepare forerunner's reaction solution, in the post-processing copper powder of pickling.
Step 2: preparing silver ammino solution, silver nitrate solution is mixed with sodium hydroxide solution, ammonium hydroxide is added.
Step 3: dehydrated alcohol and deionized water are mixed according to volume ratio 1:4, it is added in three-necked flask, is added
Dispersing agent PVP is added silver ammino solution and reducing agent simultaneously later, is stirred with blender, when weighed copper powder size 30 ~
When 70nm, the reaction time is 0.8 ~ 1.2h；When copper powder size is at 3 ~ 7 μm, the reaction time is 1.2 ~ 1.8h；When copper powder size exists
At 15 ~ 25 μm, the reaction time is 1.8 ~ 2.5h.
Step 4: acetone etc. is washed, is centrifuged, is placed in drying box by reaction product by dehydrated alcohol, do
Dry 12 ~ for 24 hours.
Step 5: preparing scaling powder: adjusting 15% activating agent, 37.5% film forming agent, 1% thixotropic agent, 1.5% according to mass content
The ratio stirring for saving agent, 1.5% surfactant, 0.5% corrosion inhibiter and remaining solvent, obtains scaling powder.
Step 6: Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag particle are mixed with scaling powder, it is then mechanical
0.5h ~ 1h is stirred to get the composite solder paste of addition micro-nano granules.
The present invention in SnSb system soldering paste by adding Cu@Ag particle, and Ag particle, Cu particle, Ni particle etc. solves mesh
For preceding SnSb system soldering paste there are electric conductivity poor thermal conductivity, formability is poor, and copper particle is easy in previous addition nano copper particle soldering paste
Be oxidized, the nano-Ag particles that welding joint structure can have more stomata and addition is excessive cause cost increase and
Ag Ion transfer occurs in tissue and leads to failure, so that it is simple to obtain preparation process, has excellent performance, it is lower-cost
It can be used for the interconnection material of Electronic Packaging component.
Mechanism of the invention: the cost is relatively high by Ag, and there is a problem of deelectric transferred ability difference, and Cu is easily by oxygen
Change, but its cost is relatively low, and with Ag have similar electrical and thermal conductivity performance, by preparing this novel Cu@Ag particle knot
Structure both can solve that the deelectric transferred ability of Ag is poor, the problem of Cu inoxidizability difference, but also can keep similar conductive and heat-conductive
Performance, significant save the cost.
The wetability that solder can be obviously improved by adding Cu@Ag particle into matrix solder, improves thermal conductivity, and
Its mechanical property, and multiple dimensioned micro-nano compound Cu@Ag particle can be added, relative to more single addition nanometer Cu@
Ag particle can significant save the cost, and the micron order Cu@Ag added can increase electrical and thermal conductivity performance, add Cu powder, can
To form compound with the part Sn in solder, it is possible to reduce the tendency that the Cu in Cu@Ag particle is reacted with Sn in solder, addition
The content of Ag powder, adjustable body solder inside Ag maintains original nucleocapsid knot so that the consumption of Ag element weakens in Cu@Ag shell
Structure is not destroyed, and adds Ni powder, can further refine the microstructure of solder joint body solder, improves toughness.
Advantage of the present invention is as follows.
1, Cu@Ag prepared by the present invention controls different reaction items by coating Ag layers on the Cu powder surface of different-grain diameter
Ag layers of cladding thickness of part and then control, solve the disadvantage that current Cu powder inoxidizability difference is difficult to save in this way.
2, for the present invention with copper powder, silver nitrate etc. is raw material, by simple controllable technique, is provided simultaneously with the invention excellent
Controllability, compatibility and adaptability, and can be according to the Cu@Ag particle for actually preparing different-grain diameter difference coating thickness.
3, composite soldering simple process prepared by the present invention, Cu@Ag particle, Cu particle, the Ag particle of addition, which can increase, to be mentioned
The thermal conductivity and electric conductivity of high tin antimony base solder.
4, the Cu@Ag particle that the soldering paste that the present invention is formed is added in postwelding weld seam interior tissue, the refinement of Ni particle, and
It is even to be distributed in seam organization, realize refined crystalline strengthening, thus its intensity obviously gets a promotion.
5, the present invention can all form effective connection, and simple process, cost by Reflow Soldering, the methods of heating platform welding
It is lower, excellent weldability.
Detailed description of the invention
Fig. 1 be embodiment 1 prepare composite solder paste in add micro-nano granules TEM figure.
Fig. 2 be embodiment 3 prepare composite solder paste thermal conductivity compared with matrix solder Sn10Sb figure.
Fig. 3 is that the wetability of composite solder paste prepared by embodiment 3 to embodiment 6 compares figure.
Fig. 4 is the shear strength comparison diagram of composite solder paste prepared by embodiment 3 to embodiment 6.
Fig. 5 is the organization chart of the composite solder paste of addition micro-nano granules prepared by embodiment 3.
Fig. 6 is the organization chart of the composite solder paste of addition micro-nano granules prepared by embodiment 4.
Fig. 7 is the organization chart of the composite solder paste of addition micro-nano granules prepared by embodiment 5.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: a kind of composite solder paste for adding micro-nano granules of present embodiment is by metal powder and to help
Solder flux composition: it is described it is a kind of add micro-nano granules composite solder paste in metal powder mass fraction be 80%-90%, help weldering
The mass fraction of agent is 10%-20%.
Specific embodiment 2: the present embodiment is different from the first embodiment in that；A kind of addition is micro-nano
Metal powder in the composite solder paste of particle is by Cu@Ag particle, Cu@Ag particle, Ag particle, Cu particle, Ni particle and Sn10Sb
Particle composition, metal powder according to mass content Cu@Ag be 0.10% ~ 5.00%, Ag be 0.30%~1.20%, Cu be 0.50% ~
0.90%, Ni is 0.03%~0.05%, remaining is Sn10Sb powder composition, a kind of composite solder paste adding micro-nano granules
Scaling powder according to mass content by 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% regulator, 1.5% surface-active
Agent, 1% corrosion inhibiter and remaining be solvent composition, it is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two, described one kind
Add micro-nano granules composite solder paste, it is characterised in that the partial size of the metal powder Cu@Ag of addition be 30 ~ 70nm, 3 ~ 7 μm or
15~25μm；The partial size of Ag is 1 ~ 2 μm；The partial size of Cu is 4 ~ 6 μm；The partial size of Ni is 40 ~ 50nm；The partial size of Sn10Sb is 30 ~ 70
μm, it is other identical as one of specific embodiment one or two.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three, described one kind
The mass fraction for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 0.01%, other and specific embodiment
One of one to three is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four, described one kind
The mass fraction for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 1%, other and specific embodiment one
It is identical to one of four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five, described one kind
The mass fraction for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 3%, other and specific embodiment one
It is identical to one of five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six, described one kind
The mass fraction for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 5%, other and specific embodiment one
It is identical to one of six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven, described one kind
The partial size for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 30 ~ 70nm other with specific embodiment one
It is identical to one of seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight, described one kind
Add Cu@Ag in the metal powder of the composite solder paste of micro-nano granules partial size be 3 ~ 7 μm it is other with specific embodiments one to
One of eight is identical.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine, described one kind
The partial size for adding Cu@Ag in the metal powder of the composite solder paste of micro-nano granules is 15 ~ 25 μm of other and specific embodiments one
It is identical to one of nine.
Specific embodiment 11: unlike one of present embodiment and specific embodiment one to ten, described one
The partial size of Cu@Ag is 30 ~ 70nm and 3 ~ 7 μm in the metal powder of the composite solder paste of kind addition micro-nano granules, and mass ratio is
1:1 is other identical as one of specific embodiment one to ten.
Specific embodiment 12: present embodiment is described unlike specific embodiment one to one of 11
It is a kind of add micro-nano granules composite solder paste metal powder in Cu@Ag partial size be 30 ~ 70nm and 15 ~ 25 μm of its mass ratio
It is other identical as specific embodiment one to one of 11 for 1:1.
Specific embodiment 13: present embodiment is described unlike specific embodiment one to one of 12
It is a kind of add micro-nano granules composite solder paste metal powder in Cu@Ag partial size be 30 ~ 70nm, 3 ~ 7 μm with 15 ~ 25 μm its
Mass ratio is 5:3:2, other identical as specific embodiment one to one of 12.
Specific embodiment 14: present embodiment is described unlike specific embodiment one to one of 13
A kind of preparation method of composite solder paste that adding micro-nano granules carries out according to the following steps.
One, metal powder Cu@Ag, Ag, Cu, Ni, Sn10Sb are weighed out according to respective mass content.
Two, by activating agent, film forming agent, thixotropic agent, regulator, surfactant, corrosion inhibiter, solvent in scaling powder according to each
From mass content weigh out.
Three, metal powder and scaling powder are subjected to 30 ~ 60min of mechanical mixture.
It is other identical as specific embodiment one to one of 13.
Specific embodiment 15: present embodiment is described to add unlike specific embodiment one to one of 14
The preparation method of the Cu@Ag particle added carries out according to the following steps.
One, copper powder is added in the sulfuric acid solution that volumetric concentration is 20% and is cleaned, be centrifuged, washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears, when copper powder size is 50nm
When, the silver nitrate concentration of addition is 0.08g/L；When copper powder size is 5 μm, the silver nitrate solution concentration of addition is 0.2625g/
L, when copper powder size is 20 μm, the silver nitrate solution concentration of addition is 0.6575g/L.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, dispersing agent PVP 0.5g is added, while being added above-mentioned prepared
Silver ammino solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react.
When copper powder size is 30 ~ 70nm, the reaction time is 0.8 ~ 1.2h；When copper powder size is 3 ~ 7 μm, the reaction time is
1.2~1.8h；When copper powder size is 15 ~ 25 μm, the reaction time is 1.8 ~ 2.5h, obtains Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
It is other identical as specific embodiment one to one of 14.
Specific embodiment 16: present embodiment is described unlike specific embodiment one to one of 15
A kind of scaling powder of composite solder paste adding micro-nano granules is made of following component.
The film forming agent is made of mixed rosin and polyethylene glycol 2000 according to 4 ﹕, 1 mass ratio, and wherein mixed rosin is by pine
The mass ratio of fragrant and hydrogenated rosin composition, rosin and hydrogenated rosin is 1 ﹕ 1.
The thixotropic agent is castor oil.
The regulator is triethanolamine.
The surfactant is octyl phenol polyoxydivinyl ether.
The corrosion inhibiter is benzotriazole.
The solvent is that isopropanol and butyl glycol ether form, and the mass ratio of isopropanol and butyl glycol ether is 3:1, other
It is identical as specific embodiment one to one of 15.
Effect of the present invention is verified using following embodiments.
Embodiment one.
One, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining stirred for the ratio of solvent, obtain scaling powder, two, by Cu particle, Ag
Grain, Ni particle, SnSb particle, Cu@Ag particle are mixed with scaling powder, and then mechanical stirring 0.5h ~ 1h is to get composite solder paste.
Embodiment two.
The preparation method for adding the composite solder paste of micro-nano granules is as follows.
One, the copper powder for being 50nm by partial size is added to the sulfuric acid cleaned that volumetric concentration is 20%, is centrifuged, is washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, and 0.5g is added in dispersing agent PVP, while above-mentioned prepared silver is added
Ammonia solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react, and the reaction time is 0.8 ~ 1.2h,
Obtain Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
Five, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining for solvent ratio stir, obtain scaling powder.
Six, Cu particle, Ag particle, Ni particle, SnSb particle, Cu Ag copper silver nucleocapsid particles are mixed with scaling powder, then
Mechanical stirring 0.5h ~ 1h is to get the composite solder paste for adding micro-nano granules.
It adds and is made of according to mass content 80% metal powder and 20% scaling powder in the composite solder paste of micro-nano granules, institute
Metal powder is stated according to mass content by 0.10% ~ 5.00%Cu@Ag, 0.5%Ag, 0.7%Cu, 0.04%Ni, remaining is SnSb powder
Composition, activating agent matter described in step 5 are formed by measuring stearic acid than 2 ﹕ 3 and adipic acid, and the film forming agent is by mixed rosin
It is formed with polyethylene glycol 2000 according to 4 ﹕, 1 mass ratio, wherein mixed rosin is made of rosin and hydrogenated rosin, rosin and hydrogenation pine
Fragrant mass ratio is 1 ﹕ 1, and the thixotropic agent is castor oil, and the regulator is triethanolamine, and the surfactant is octyl
Phenol polyoxydivinyl ether, the corrosion inhibiter are benzotriazole, and the solvent is that isopropanol and butyl glycol ether form, isopropanol with
Butyl glycol ether and mass ratio be 3:1.
Embodiment three.
The preparation method for adding the composite solder paste of micro-nano granules is as follows.
One, the copper powder for being 50nm by partial size is added to the sulfuric acid cleaned that volumetric concentration is 20%, is centrifuged, is washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, and 0.5g is added in dispersing agent PVP, while above-mentioned prepared silver is added
Ammonia solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react, and the reaction time is 0.8 ~ 1.2h,
Obtain Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
Five, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining for solvent ratio stir, obtain scaling powder.
Six, Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag particle are mixed with scaling powder, then mechanical stirring
0.5h ~ 1h is to get the composite solder paste (Sn9.576Sb-3Cu@Ag-0.5Ag-0.7Cu-0.04Ni) for adding micro-nano granules.
It adds and is made of according to mass content 80% metal powder and 20% scaling powder in the composite solder paste of micro-nano granules, institute
Metal powder is stated according to mass content by 3%Cu@Ag, 0.5%Ag, 0.7%Cu, 0.04%Ni, remaining is SnSb powder, in step 5
The activating agent is the stearic acid that mass ratio is 2 ﹕ 3 and adipic acid composition, and the film forming agent is by mixed rosin and polyethylene glycol
2000 form according to 4 ﹕, 1 mass ratio, and wherein mixed rosin is made of rosin and hydrogenated rosin, the mass ratio of rosin and hydrogenated rosin
For 1 ﹕ 1, the thixotropic agent is castor oil, and the regulator is triethanolamine, and the surfactant is that octyl phenol polyoxy second is dilute
Ether, the corrosion inhibiter are benzotriazole, and the solvent is that isopropanol and butyl glycol ether form, isopropanol and butyl glycol ether
With mass ratio be 3:1.
Example IV.
The preparation method for adding the composite solder paste of micro-nano granules is as follows.
One, the copper powder for being 50nm by partial size is added to the sulfuric acid cleaned that volumetric concentration is 20%, is centrifuged, is washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, and 0.5g is added in dispersing agent PVP, while above-mentioned prepared silver is added
Ammonia solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react, and the reaction time is 0.8 ~ 1.2h,
Obtain Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
Five, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining for solvent ratio stir, obtain scaling powder.
Six, Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag are mixed with scaling powder, then mechanical stirring 0.5h
~ 1h is to get the composite solder paste (Sn9.866Sb-0.1Cu@Ag-0.5Ag-0.7Cu-0.04Ni) for adding micro-nano granules.
It adds and is made of according to mass content 80% metal powder and 20% scaling powder in the composite solder paste of micro-nano granules, the gold
Belong to powder according to mass content by 0.1%Cu@Ag, 0.5%Ag, 0.7%Cu, 0.04%Ni, remaining is SnSb powder, institute in step 5
Stating activating agent is the stearic acid and adipic acid composition that mass ratio is 2 ﹕ 3, and the film forming agent is by mixed rosin and polyethylene glycol 2000
It is formed according to 4 ﹕, 1 mass ratio, wherein mixed rosin is made of rosin and hydrogenated rosin, and the mass ratio of rosin and hydrogenated rosin is 1 ﹕
1, the thixotropic agent is castor oil, and the regulator is triethanolamine, and the surfactant is octyl phenol polyoxydivinyl ether, institute
Stating corrosion inhibiter is benzotriazole, and the solvent is that isopropanol and butyl glycol ether form, isopropanol and butyl glycol ether and
Mass ratio is 3:1.
Embodiment five.
The preparation method for adding the composite solder paste of micro-nano granules is as follows.
One, the copper powder for being 50nm by partial size is added to the sulfuric acid cleaned that volumetric concentration is 20%, is centrifuged, is washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, and 0.5g is added in dispersing agent PVP, while above-mentioned prepared silver is added
Ammonia solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react, and the reaction time is 0.8 ~ 1.2h,
Obtain Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
Five, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining for solvent ratio stir, obtain scaling powder.
Six, Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag particle are mixed with scaling powder, then mechanical stirring
0.5h ~ 1h is to get the composite solder paste (Sn9.766Sb-1Cu@Ag-0.5Ag-0.7Cu-0.04Ni) for adding micro-nano granules.
It adds and is made of according to mass content 80% metal powder and 20% scaling powder in the composite solder paste of micro-nano granules, institute
Metal powder is stated according to mass content by 1%Cu@Ag, 0.5%Ag, 0.7%Cu, 0.04%Ni, remaining is SnSb powder, in step 5
The activating agent is the stearic acid that mass ratio is 2 ﹕ 3 and adipic acid composition, and the film forming agent is by mixed rosin and polyethylene glycol
2000 form according to 4 ﹕, 1 mass ratio, and wherein mixed rosin is made of rosin and hydrogenated rosin, the mass ratio of rosin and hydrogenated rosin
For 1 ﹕ 1, the thixotropic agent is castor oil, and the regulator is triethanolamine, and the surfactant is that octyl phenol polyoxy second is dilute
Ether, the corrosion inhibiter are benzotriazole, and the solvent is that isopropanol and butyl glycol ether form, isopropanol and butyl glycol ether
With mass ratio be 3:1.
Embodiment six.
The preparation method for adding the composite solder paste of micro-nano granules is as follows.
One, the copper powder for being 50nm by partial size is added to the sulfuric acid cleaned that volumetric concentration is 20%, is centrifuged, is washed.
Two, it prepares silver ammino solution: concentration being mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, so
The ammonium hydroxide that mass fraction is 20% is added dropwise afterwards and is configured to silver ammino solution until precipitating disappears.
Three, dehydrated alcohol and deionized water are mixed according to the ratio that volume ratio is 1 ﹕ 4, ethyl alcohol 40ml is added, goes
The copper powder by step 1 processing is added in ionized water 160ml, and 0.5g is added in dispersing agent PVP, while above-mentioned prepared silver is added
Ammonia solution and 0.75g reducing agent hydrazine hydrate, the pH value for adjusting reaction solution is 9 ~ 13, is stirred to react, and the reaction time is 0.8 ~ 1.2h,
Obtain Cu@Ag wicker copper nucleocapsid particles.
Four, the product of step 3 is centrifuged by dehydrated alcohol, acetone washing, dry 12 ~ for 24 hours.
Five, it prepares scaling powder: adjusting 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% according to mass content
Agent, 1.5% surfactant, 1% corrosion inhibiter and remaining for solvent ratio stir, obtain scaling powder.
Six, Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag particle are mixed with scaling powder, then mechanical stirring
0.5h ~ 1h is to get the composite solder paste (Sn9.376Sb-5Cu@Ag-0.5Ag-0.7Cu-0.04Ni) for adding micro-nano granules.
It adds and is made of according to mass content 80% metal powder and 20% scaling powder in the composite solder paste of micro-nano granules, institute
Metal powder is stated according to mass content by 5%Cu@Ag, 0.5%Ag, 0.7%Cu, 0.04%Ni, remaining is SnSb powder, in step 5
The activating agent is the stearic acid that mass ratio is 2 ﹕ 3 and adipic acid composition, and the film forming agent is by mixed rosin and polyethylene glycol
2000 form according to 4 ﹕, 1 mass ratio, and wherein mixed rosin is made of rosin and hydrogenated rosin, the mass ratio of rosin and hydrogenated rosin
For 1 ﹕ 1, the thixotropic agent is castor oil, and the regulator is triethanolamine, and the surfactant is that octyl phenol polyoxy second is dilute
Ether, the corrosion inhibiter are benzotriazole, and the solvent is that isopropanol and butyl glycol ether form, isopropanol and butyl glycol ether
With mass ratio be 3:1.
It is measured using thermal coefficient of the laser heat conducting instrument to material, which is heated to molten condition then
It is cooling, it is prepared into required test sample, is known according to national standard, measurement solder heating conduction chooses 12.6~12.7 millimeters
Solder diameter emits light pulse by laser source at a temperature of 25 DEG C of furnace body control with a thickness of the disk sample of 2.0 ± 0.1mm
Uniform irradiation is evenly heated sample in sample lower surface, and the change of sample surfaces relevant temperature is continuously measured by infrared detector
Change, obtain the relation curve of temperature detector signal raising and time, prepared by embodiment three adds the compound of micro-nano granules
Soldering paste (Sn9.576Sb-3Cu@Ag-0.5Ag-0.7Cu-0.04Ni) is as shown in Fig. 2 with the thermal conductivity of Sn10Sb.
The angle of wetting of solder is measured by using laboratory solder wetting dynamic and visual system, the system is by Sony
The superior D20 type heating platform produced with Science and Technology Ltd. of CCD camera and Shenzhen and angle of wetting Survey Software composition,
Wetting is FR4 type copper-clad base plate with substrate, having a size of 15*15*1mm.The composite solder paste for weighing 0.2g ± 0.01g preparation is placed on
Sample centre completes welding on heating platform, and welding temperature is 290 DEG C, and weld interval is 40 s, by postwelding sample table
Its angle of wetting is measured using device for measuring wetting angle after the cleaning treatment of face, is commented using their angle of wettings on the copper-clad base plate
Its wetability of valence, angle of wetting are as shown in Fig. 3.
The shear strength of the microbonding point prepared using the Japanese PTR-1100 type shear strength tester composite solder paste is carried out
Test, setting shear velocity are 0.05 mm/s, and 0.5 mm of cutting stroke, 20 μm of shear height, the value of shearing force passes through software
Real-time display, shear strength are as shown in Fig. 4.
It can be seen that the thermal conductivity for being added to the composite solder paste of micro-nano granules is obviously increased from attached drawing 2, show that its is thermally conductive
Property be obviously improved, this is because the Cu@Ag particle of addition, Cu particle, Ag particle all has good thermal conductivity, thus
Improve the thermal conductivity of the composite solder paste.
Can clearly it find out from attached drawing 3, the wetability of the composite solder paste of the micro-nano granules of addition will be substantially better than
The wetability of matrix soldering paste, and it can be found that its angle of wetting is minimum when the content of the Cu@Ag particle of addition is 3%
Value, wetability is best.
Can clearly it find out from attached drawing 4, the shear strength of the composite solder paste of the micro-nano granules of addition is obvious excellent
In the shear strength of matrix soldering paste, and it can be found that when addition Cu@Ag particle content be 3% when its shear strength
Maximum, mechanical property are best.
Claims (7)
1. a kind of composite solder paste for adding micro-nano granules, it is characterised in that add in the composite solder paste of micro-nano granules according to matter
Amount content is made of 70% ~ 90% metal powder and 10% ~ 30% scaling powder, the metal powder according to mass content by 0.01% ~
10.00% Cu@Ag, 0.10%~2.00%Ag, 0.10% ~ 1.50%Cu, 0.02%~1.00%Ni, remaining is that (x is that Sb exists to Sn-xSb
Mass content in SnSb alloy powder, 1% ~ 20%) powder composition.
2. a kind of composite solder paste for adding micro-nano granules according to claim 1, it is characterised in that micro-nano of addition
It is made of according to mass content 80% ~ 90% metal powder and 10% ~ 20% scaling powder in the composite solder paste of grain, the metal powder is pressed
According to mass content by 0.10% ~ 5.00% Cu@Ag, 0.30%~1.20%Ag, 0.50% ~ 0.90%Cu, 0.03%~0.05%Ni,
It is remaining to be constituted for Sn10Sb powder.
3. a kind of composite solder paste for adding micro-nano granules according to claim 1, it is characterised in that the metal powder of addition
The partial size of last Cu@Ag is (1) 30 ~ 70nm or 3 ~ 7 μm or 15 ~ 25 μm；(2) 30 ~ 70nm and 3 ~ 7 μm, 30 ~ 70nm and 15 ~ 25 μ
m；(3) 30 ~ 70nm, 3 ~ 7 μm and 15 ~ 25 μm of Ag partial size be 1 ~ 2 μm；The partial size of Cu is 4 ~ 6 μm；The partial size of Ni is 40 ~ 50nm；
The partial size of Sn10Sb is 30 ~ 70 μm.
4. adding the composite solder paste of micro-nano granules according to claim 1, it is characterised in that the scaling powder is according to quality
Content by 20% activating agent, 32.5% film forming agent, 1.5% thixotropic agent, 1% regulator, 1.5% surfactant, 1% corrosion inhibiter and remaining
For solvent composition；The activating agent is the stearic acid that mass ratio is 2 ﹕ 3 and adipic acid composition；The film forming agent by mixed rosin and
Polyethylene glycol 2000 is formed according to 5 ﹕, 1 mass ratio, and wherein mixed rosin is made of rosin and hydrogenated rosin, rosin and hydrogenated rosin
Mass ratio is 1 ﹕ 1；The thixotropic agent is castor oil；The regulator is triethanolamine；The surfactant is octylphenol polyethylene
The dilute ether of oxygen second；The corrosion inhibiter is benzotriazole；The solvent is that isopropanol and butyl glycol ether form, isopropanol and second two
Alcohol butyl ether mass ratio is 3:1.
5. adding the preparation method of the composite solder paste of micro-nano granules described in claim 1, it is characterised in that the addition is micro-nano
The composite solder paste of particle the preparation method is as follows: one, by copper powder, be added in the sulfuric acid solution that volumetric concentration is 20% and clean, into
Row centrifugation, washing；Two, concentration is mixed for 0.08g/L silver nitrate solution with 3.2% sodium hydroxide solution, is then added dropwise
The ammonium hydroxide that mass fraction is 20% is configured to silver ammino solution until precipitating disappears, when copper powder size is 50nm, the nitre of addition
Sour silver concentration is 0.08g/L；When copper powder size is 5 μm, the silver nitrate solution concentration of addition is 0.2625g/L；When copper powder grain
When diameter is 20 μm, the silver nitrate solution concentration of addition is 0.6575g/L；Three, by dehydrated alcohol and deionized water according to volume ratio
Ratio for 1 ﹕ 4 is mixed, and ethyl alcohol 40ml, deionized water 160ml is added, and the copper powder by step 1 processing is added, and is added
0.5g dispersing agent PVP, while above-mentioned prepared silver ammino solution and 0.75g reducing agent hydrazine hydrate is added, adjust the pH of reaction solution
Value is 9 ~ 13, is stirred to react, and when copper powder size is 30 ~ 70nm, the reaction time is 0.8 ~ 1.2h；When copper powder size be 3 ~ 7 μm, instead
It is 1.2 ~ 1.8h between seasonable；When copper powder size is 15 ~ 25 μm, the reaction time is 1.8 ~ 2.5h, obtains Cu@Ag wicker copper nucleocapsid
Grain；Four, by the product of step 3 by dehydrated alcohol, acetone washing, centrifugation, finally dry 12 ~ for 24 hours；Five, according to mass content
By 15% activating agent, 37.5% film forming agent, 1% thixotropic agent, 1.5% regulator, 1.5% surfactant, 0.5% corrosion inhibiter and remaining is molten
The ratio of agent stirs, and obtains scaling powder；Six, by Cu particle, Ag particle, Ni particle, SnSb particle, Cu@Ag particle and scaling powder
Mixing, then mechanical stirring 0.5h ~ 1h is to get the composite solder paste for adding micro-nano granules；Add the Combined Welding of micro-nano granules
It is made of according to mass content 80% ~ 90% metal powder and 10% ~ 20% scaling powder in cream, the metal powder is according to mass content
By 0.10% ~ 5.00% Cu@Ag, 0.30%~1.20%Ag, 0.50% ~ 0.70%Cu, 0.03%~0.05%Ni, remaining is SnSb powder
End is constituted；Activating agent described in step 5 is made of the stearic acid that mass ratio is 2 ﹕ 3 and adipic acid；The film forming agent is by mixing
Rosin and polyethylene glycol 2000 are formed according to 4 ﹕, 1 mass ratio, and wherein mixed rosin is made of rosin and hydrogenated rosin, rosin and hydrogen
The mass ratio for changing rosin is 1 ﹕ 1；The thixotropic agent is castor oil；The regulator is triethanolamine；The surfactant is
Octyl phenol polyoxydivinyl ether；The corrosion inhibiter is benzotriazole；The solvent is made of isopropanol and butyl glycol ether, wherein
The mass ratio of isopropanol and butyl glycol ether is 3:1.
6. adding the preparation method of the composite solder paste of micro-nano granules according to claim 3, it is characterised in that in step 1
The centrifugation, centrifuge speed are 6000r/min ~ 8000r/min.
7. adding the preparation method of the composite solder paste of micro-nano granules according to claim 3, it is characterised in that in step 6
The mechanical stirring carries out heating stirring 20min first in 55 DEG C of water-baths, then takes out from water-bath and be placed on constant temperature constant speed
It carries out at the uniform velocity stirring 15min on magnetic stirring apparatus, is finally placed on and cools down 15min at room temperature.
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