CN109128569A - A kind of middle low-temperature lead-free solder and preparation method thereof - Google Patents
A kind of middle low-temperature lead-free solder and preparation method thereof Download PDFInfo
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- CN109128569A CN109128569A CN201811165653.XA CN201811165653A CN109128569A CN 109128569 A CN109128569 A CN 109128569A CN 201811165653 A CN201811165653 A CN 201811165653A CN 109128569 A CN109128569 A CN 109128569A
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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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
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Abstract
The present invention relates to a kind of middle low-temperature lead-free solders, it is characterized in that it is by In:1.5~3.0%, Bi:3~7%, Sb:0.1~0.6%, Cu:0.3~0.8%, Ni:0.02~0.06%, La:0.008~0.05% and surplus are Sn raw material composition, preparation method is by In, Bi, Sb, Cu, Ni and La prepare intermediate alloy, it is smelted into lead-free solder product again, the product has fusing point low, with use scaling powder good compatibility, with it is small by the interfacial tension between weldering base material, increase the toughness and wetting and spreading performance of solder, reduce the surface tension of solder, promote the adhesive force of solder and base material to be welded, the advantages of improving the shear strength and toughness of solder and effect.
Description
Technical field
The present invention relates to lead-free solder, in particular to a kind of middle low-temperature lead-free solder belongs to electronic product solder technology
Field.
The invention further relates to the preparation methods of the lead-free solder.
Background technique
In electronic product process for assembling and welding, the tin-lead solder of last 100 years has been used, has been referred to from ROHS on July 1st, 2006
It has enabled since China implements, electronic product welding material is unleaded to enter electronic product assembly welding field.Because lead is one
The toxic metallic element of kind, modern industry developed country increasingly payes attention to environmental protection problem, exports to the electronics of EU market
Power product cannot be again containing six kinds of poisonous and harmful substances such as lead.Over more than ten years, SnAgCu that electronics industry generallys use,
There is kupper solder in the series leadless solder part SnAg, SnCu instead of traditional Sn63Pb37, the lead-free solder compared with having kupper solder
Although being all but to be very different in physical property on alloy composition using tin metal element as matrix, this
A little lead-free solders do not have the essential characteristic that Sn63Pb37 has kupper solder.Especially fusing point, the fusing point of lead-free solder is at 217 DEG C
Between~227 DEG C, it is higher by 34 DEG C~44 DEG C of 183 DEG C of kupper solder fusing point.Traditional manual welding, wave soldering and Reflow Soldering
It connects technological parameter and is all not suitable with the requirement of pb-free solder technique.By taking wave soldering processes as an example, lead jointing temperature peak is at 240 DEG C
~245 DEG C, pb-free solder temperature is 260 DEG C~265 DEG C.Although pb-free solder temperature improves 20 DEG C, but with lead jointing phase
Have that kupper solder is small than, the wetting and spreading ratio of lead-free solder, wetting time is also longer than there is kupper solder.Since lead-free solder itself soaks
Performance is bad, and oxidation-resistance property is poor, soldering test show pb-free solder temperature at 270 DEG C, and need it is more strongly active
Scaling powder can be only achieved the effect of lead jointing processing quality, but part electronic component and printed circuit board heat resistance are
It cannot withstand.The especially high speed development of microelectric technique, it is desirable that electronic product is short and small, frivolous, multi-functional, and component is highly dense
Spend it is highly integrated since, when small frivolous chip, heat sensitive component, multilayer sub-assembly and flexible circuit board weld and intolerant to height
Temperature, this is subject to certain restrictions the application of high temperature lead-free solder also.
Related statistical data shows the electricity using high-temp leadless welding process equipment than lead jointing increase about 30% or so
It can consumption.CO in welding procedure2Discharge amount, including printed circuit board hot wind is whole or electroplate lead-free solder layer, component down-lead
The increases such as the pre-treatment of pole about 40% or so, lead-free solder scruff forming amount increases 25% or more in welding.Lead-free solder
Using high cost, high energy consumption is caused, the high added value of product is not obviously brought.When overcoming the harm of lead, and shape
The atmosphere pollution of Cheng Xin, China also will enter comprehensively emission and charge the epoch thus, and enterprise will also be included in carbon emission management unit,
The historic responsibility of energy-saving and emission-reduction low-temperature environment-friendly is shouldered jointly.
Electronic product constantly updates development, the division of labor of electronic component also constantly refinement and diversification and energy-saving and emission-reduction
Requirement also reduce the application market of high temperature lead-free solder increasingly in some specific electronic products.Currently used fusing point
Higher unleaded series solder substitute completely leaded solder be also it is unrealistic, in view of problem above, in electronic product group
Researched and developed in dress technique it is a kind of it is practicable with conventional tin-lead solders with the melting range being close, with printed circuit board pad
And component substrate wetting and spreading is good, the middle low-temperature lead-free solder of good mechanical performance, which seems, to be even more important.
Summary of the invention
The purpose of the present invention is to overcome high energy consumption in the existing production and use process of the prior art, Gao Cheng
This, the discharge of high pollution object, the high disadvantage of slag yield and deficiency and to provide a kind of welding temperature low in 160~190 DEG C one kind
Warm lead-free solder, so as to which there is the melting range being close with conventional tin-lead solders, with printed circuit board pad and component
Substrate wetting and spreading is good, the middle low-temperature lead-free solder of good mechanical performance, while also can save energy emission reduction, environmental protection.
The present invention also provides the preparation methods of the lead-free solder.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of middle low-temperature lead-free solder, it is made of the raw material of following weight percents:
In:1.5~3.0%, Bi:3~7%, Sb:0.1~0.6%, Cu:0.3~0.8%, Ni:0.02~0.06%,
La:0.008~0.05% and surplus are Sn.
The weight percent preferred scope of described In, Bi, Sb, Cu, the Ni is In:2~3%, Bi:4~6%, Sb:0.2
~0.5%, Cu:0.4~0.7%, Ni:0.03~0.05%；The preferred scope of the La is 0.01~0.03%.
The preparation method of the middle low-temperature lead-free solder, it is carried out in the steps below:
A), Sn48In52 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
48% tin material is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to 400 DEG C ± 5 DEG C, then be by purity
It in 99.95% 52% indium material point, 4 addition crucibles and stirs, after indium material all melting, crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions on asbestos board and stir 10min, pull the dross on surface out with stainless steel spoon, stand 2~3min, is cast, is cold
But 5~6min obtains Sn48In52 intermediate alloy；
B) Sn43Bi57 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
43% tin material is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to 450 DEG C ± 5 DEG C, then be by purity
It in 99.95% 57% bismuth material point, 4 addition crucibles and stirs, after bismuth material all melting, crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions on asbestos board and stir 10min, pull the dross on surface out with stainless steel spoon, stand 1~2min, is cast, is cold
But 5~6min obtains Sn43Bi57 intermediate alloy；
C), Sn90Sb10 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 2/3 of 90% tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 450 DEG C ± 5 DEG C,
It in 10% antimony material point, the 4 addition crucibles for being again 99.95% by purity and stirs, after antimony material all melting, crucible is removed
Smelting furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 1/3 tin material, is again stirring for 10min, with not
Rust steel spoon pulls the dross on surface out, stands 1~2min, is cast, cools down 5~6min, obtain Sn90Sb10 intermediate alloy；
D), Sn80Cu20 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 2/3 of 80% tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 500 DEG C ± 5 DEG C,
The 20% bronze medal material that purity is 99.95% is divided 5 times again and is added and stirs, after copper material all melting, crucible is removed smelting furnace,
It is placed on asbestos board and continues both forward and reverse directions stirring, be subsequently placed into remaining 1/3 tin material, be again stirring for 10min, fished out with stainless steel spoon
The dross on surface out stands 2~3min, is cast, cools down 5~6min, obtain Sn80Cu20 intermediate alloy；
E), Sn95Ni5 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 3/4 of 95% tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 800 DEG C ± 5 DEG C,
The 5% nickel material that purity is 99.95% is divided 2 times again and is added and stirs, after expecting all to melt, crucible is removed smelting furnace, is put
Continue both forward and reverse directions stirring on asbestos board, is subsequently placed into remaining 1/4 tin material, is again stirring for 60min, pulled out with stainless steel spoon
The dross on surface stands 2~3min, is cast, cools down 5~6min, obtain Sn95Ni5 intermediate alloy；
F), Sn99La1 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
Graphite is put after tin material all melting and is covered in molten tin material, adds crucible cover, continues to heat up in crucible in the 3/4 of 99% tin material
It when molten tin material is to 900 DEG C ± 5 DEG C, uncaps and takes out graphite cover, the 1% lanthanum material that purity is 99.95% is put into molten tin material,
Quickly it then is covered in molten tin material surface with potassium chloride, capping is warming up in lanthanum material indentation molten tin material with graphite cover
1000 DEG C~1020 DEG C, after keeping the temperature 10~15min, it is multiple to move up and down graphite cover, stirs simultaneously, turns molten tin material in crucible
It is dynamic, it is covered in fused materials surface with potassium chloride at any time, takes out graphite cover, crucible is taken out when being cooled to 800 DEG C~780 DEG C and is placed on
On asbestos board, remaining tin material 1/4 is added in crucible, fused materials is stirred with graphite rod or so, is cooled to 500 DEG C ± 5 DEG C,
It pulls the dross on surface out with stainless steel spoon, stands 2~3min, cast, cool down 5~6min and obtain Sn99La1 intermediate alloy；
G), low-temperature lead-free solder in preparation
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, by the 2.88~5.77% of the preparation of a) item
Sn48ln52 intermediate alloy, b) item preparation 5.26~12.28% Sn43Bi57 intermediate alloy, c) item preparation 1.0~
The 0.4 of 6.0% Sn90Sb10 intermediate alloy, d) 1.5~4.0% Sn80Cu20 intermediate alloy of item preparation, e) item preparation
0.8~5.0% Sn99La1 intermediate alloy and surplus tin of~1.2% Sn95Ni5 intermediate alloy, f) item preparation subtract
Melting in crucible is added in 69.09~79.48% insufficient tin amounts after stating the tin in intermediate alloy, and anti-oxidation in surface covering
Agent, capping are continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, and uncap 5~10min of stirring, then crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions stirring on asbestos board, when temperature is down to 350 DEG C ± 5 DEG C, pull the dross on surface out with stainless steel spoon, stands
2~3min is cast, cools down 5~6min, and middle low-temperature lead-free solder product is obtained.
The antioxidant is terpene resin and organic dibasic acid compound, and proportion is 10: 0.3；Described organic two
First acid is succinic acid, glutaric acid or adipic acid.
The present invention is that ln element and Bi element are added on tinbase, it can greatly reduce the melting temperature of solder,
Increase the toughness and wetting and spreading performance of solder；The addition of Cu element reduces the surface tension of solder, promotes solder
With the adhesive force of base material to be welded, while it can effectively inhibit the phase transformation of Sn, experiment shows pure Sn meeting when being cooled to 13 DEG C~16 DEG C
The phase transformation by β phase transition for α phase occurs, this will lead to the increase of about 25% volume, and destroy the complete of Sn structure, this can butt welding point
Intensity and service life be very unfavorable；The addition of Sb element and Ni element greatly enhances the shearing of solder
Intensity and toughness, while keeping the fusing to form solder and solidification temperature range close, improve solder
Mechanical strength and antioxygenic property；Rare-earth elements La inserts, and has refined the crystalline structure of solder, further increases conjunction
The mechanical strength of gold solder especially soaks mobility significant effect to the processing performance of solder.It fully and rationally used simultaneously
Surplus lanthanum resource, reduces production cost.
The element of addition is first prepared intermediate alloy by preparation method of the invention, and the smelting furnace of use can slowly heat up, gently
Put raw material and by several times and under different temperatures be added raw material and both forward and reverse directions stirring molten tin material, accelerate fusing addition element material with
The fusion of tin material, guarantees product quality.
Due to taking above-mentioned technical proposal to have the following advantages that the technology of the present invention compared with existing skill and effect:
1), the fusing point of low-temperature lead-free solder is low in the present invention, and the addition of In element and Bi element keeps the fusing point of solder
Between 160 DEG C~190 DEG C, hence it is evident that lower than 217 DEG C~227 DEG C of the fusing point of currently used lead-free solder, with now extensively
It is and small by the interfacial tension between weldering base material using scaling powder good compatibility, facilitate shape between component down-lead pole and pad
At firm pad, the toughness and wetting and spreading performance of solder are increased.Adding a certain amount of Cu element reduces solder
Surface tension, promotes the adhesive force of solder and base material to be welded, while can effectively inhibit the phase transformation of Sn, and experiment shows that pure Sn exists
The phase transformation by β phase transition for α phase can occur when being cooled to 13 DEG C~16 DEG C, this will lead to the increase of about 25% volume, and destroy Sn
Structure it is complete, this can butt welding point intensity and service life be very unfavorable；The addition of Sb element and Ni element is largely
On improve the shear strength and toughness of solder, while making the fusing to form solder and solidification temperature range
It is close, improve the mechanical strength and antioxygenic property of solder.The addition of rare-earth elements La has refined the knot of solder
Crystalline substance tissue, further increases the mechanical strength of solder, and it is aobvious especially to soak mobility effect to the processing performance of solder
It writes.Superfluous lanthanum resource is fully and rationally used simultaneously, reduces production cost.
2), solve in the unleaded processing procedure of electronics industry low-temperature lead-free solder in use complete it is temperature sensitive or intolerant to
The welding of high temperature high-end product, related statistical data show to reduce by 30% or so power consumption, reduce in welding procedure
CO2Discharge amount and scruff forming amount.
Specific embodiment
Embodiment 1
A), Sn48In52 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
48kg tin material is added in crucible, all melts to tin material, continues to be warming up to 400 DEG C ± 5 DEG C, then by purity is 99.95%
It in 4 addition crucibles of 52kg indium material point and stirs, after indium material all melting, crucible is removed smelting furnace, is placed on asbestos board
Continue both forward and reverse directions and stir 10min, pull the dross on surface out with stainless steel spoon, stands 3min, cast, cool down 5min, obtained
Sn48In52 intermediate alloy；
B), graphite crucible is put into smelting furnace by preparation Sn43Bi57 intermediate alloy, is slowly warming up to 300 DEG C ± 5 DEG C, first
Lightly the 43kg tin material that purity is 99.95% is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to
It uncaps at 450 DEG C ± 5 DEG C, then the 57kg bismuth material that purity is 99.95% is divided 4 times and is added and stirs, after bismuth material all melting,
Crucible is removed smelting furnace, is placed on asbestos board and continues both forward and reverse directions stirring 10min, pull the dross on surface out with stainless steel spoon,
1min is stood, cast, cool down 6min, obtain Sn43Bi57 intermediate alloy；
C), Sn90Sb10 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 60kg of 90kg tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 450 DEG C ± 5 DEG C,
The 10kg antimony material that purity is 99.95% is divided 4 times again and is added and stirs, after antimony material all melting, crucible is removed smelting furnace,
It is placed on asbestos board and continues both forward and reverse directions stirring, be subsequently placed into remaining 30kg tin material, be again stirring for 10min, with stainless steel spoon
It pulls the dross on surface out, stands 2min, cast, cool down 6min, obtain Sn90Sb10 intermediate alloy；
D), Sn80Cu20 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 53.3kg of 80kg tin material is added in crucible, adds crucible cover after tin material all melting, continues to open when being warming up to 500 DEG C ± 5 DEG C
Lid, then the 20kg copper material that purity is 99.95% is divided 5 times and is added and stirs, after copper material all melting, crucible is removed melting
Furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 26.7kg tin material, is again stirring for 10min, use is stainless
Steel spoon pulls the dross on surface out, stands 3min, is cast, and cooling 5min obtains Sn80Cu20 intermediate alloy；
E), Sn95Ni5 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 71.25kg of 95% tin material is added in crucible, adds crucible cover after tin material all melting, continues to open when being warming up to 800 DEG C ± 5 DEG C
Lid, then the 5kg nickel material that purity is 99.95% is divided 2 times and is added and stirs, after copper material all melting, crucible is removed melting
Furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 23.75kg tin material, is again stirring for 60min, with not
Rust steel spoon pulls the dross on surface out, stands 3min, is cast, cools down 5min, obtain Sn95Ni5 intermediate alloy；
F), Sn99La1 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 74.25kg of 99kg tin material is put graphite after tin material all melting and is covered in molten tin material, add earthenware in melting tin material in crucible
Crucible lid uncaps when the molten tin material that continues to heat up is to 900 DEG C ± 5 DEG C and takes out graphite cover, the 1kg lanthanum material that purity is 99.95% is put
Enter in tin liquor, is quickly then covered in molten tin material surface in lanthanum material indentation molten tin material with graphite cover with potassium chloride, covered
It is warming up to 1020 DEG C, after keeping the temperature 10min, it is multiple to move up and down graphite cover, and it stirs simultaneously, rotates molten tin material in crucible, with
When with potassium chloride be covered in surface, take out graphite cover, lanthanum material all takes out crucible after melting, when being cooled to 780 DEG C and is placed on asbestos
On plate, remaining tin material 24.75kg is added in crucible, liquid is stirred with graphite rod or so, 500 DEG C ± 5 DEG C is cooled to, with not
Rust steel spoon pulls the dross on surface out, stands 2min, is cast, and cooling 6min obtains Sn99La1 intermediate alloy；
G), low-temperature lead-free solder in preparation
Raw material dosage: In:1.5%, Bi:7%, Sb:0.6%, Cu:0.3%, Ni:0.04%, La:0.008% and surplus
Sn 90.55%,
Graphite crucible is put into smelting furnace, 300 DEG C ± 5 DEG C is slowly warming up to, takes the Sn48ln52 of the 2.88kg of preparation
Intermediate alloy, the Sn43Bi57 intermediate alloy of 12.28kg, the Sn90Sb10 intermediate alloy of 6kg, 1.5kg Sn80Cu20 among
Alloy, the Sn95Ni5 intermediate alloy of 0.8kg, the Sn99La1 intermediate alloy of 0.8kg and surplus tin subtract in above-mentioned intermediate alloy
Tin after 75.74kg tin addition crucible in shortage in a melting, and cover on surface and answered by terpene resin and fourth binary acid
With object, proportion is 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 5min, then
Crucible is removed smelting furnace, is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C, use stainless steel
Spoon pulls the dross on surface out, stands 2min, is cast, cools down 6min, obtain SnIn1.5 Bi7 Sb0.6 Cu0.3Ni0.04
Low-temperature lead-free solder product in La0.008.
Embodiment 2
A), Sn48In52 intermediate alloy；
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
48kg tin material is added in crucible, all melts to tin material, continues to be warming up to 400 DEG C ± 5 DEG C, then by purity is 99.95%
It in 4 addition crucibles of 52kg indium material point and stirs, after indium material all melting, crucible is removed smelting furnace, is placed on asbestos board
Continue both forward and reverse directions and stir 10min, pull the dross on surface out with stainless steel spoon, stands 2min, cast, cool down 6min, obtained
Sn48In52 intermediate alloy；
B), graphite crucible is put into smelting furnace by preparation Sn43Bi57 intermediate alloy, is slowly warming up to 300 DEG C ± 5 DEG C, first
Lightly the 43kg tin material that purity is 99.95% is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to
It uncaps at 450 DEG C ± 5 DEG C, then the 57kg bismuth material that purity is 99.95% is divided 4 times and is added and stirs, after bismuth material all melting,
Crucible is removed smelting furnace, is placed on asbestos board and continues both forward and reverse directions stirring 10min, pull the dross on surface out with stainless steel spoon,
2min is stood, cast, cool down 5min, obtain Sn43Bi57 intermediate alloy；
C), Sn90Sb10 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 60kg of 90kg tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 450 DEG C ± 5 DEG C,
The 10kg antimony material that purity is 99.95% is divided 4 times again and is added and stirs, after antimony material all melting, crucible is removed smelting furnace,
It is placed on asbestos board and continues both forward and reverse directions stirring, be subsequently placed into remaining 30kg tin material, be again stirring for 10min, with stainless steel spoon
It pulls the dross on surface out, stands 1min, cast, cool down 5min, obtain Sn90Sb10 intermediate alloy；
D), Sn80Cu20 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 53.3kg of 80kg tin material is added in crucible, adds crucible cover after tin material all melting, continues to open when being warming up to 500 DEG C ± 5 DEG C
Lid, then the 20kg copper material that purity is 99.95% is divided 5 times and is added and stirs, after copper material all melting, crucible is removed melting
Furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 26.7kg tin material, is again stirring for 10min, use is stainless
Steel spoon pulls the dross on surface out, stands 2min, is cast, and cooling 6min obtains Sn80Cu20 intermediate alloy；
E), Sn95Ni5 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 71.25kg of 95% tin material is added in crucible, adds crucible cover after tin material all melting, continues to open when being warming up to 800 DEG C ± 5 DEG C
Lid, then the 5kg nickel material that purity is 99.95% is divided 2 times and is added and stirs, after copper material all melting, crucible is removed melting
Furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 23.75kg tin material, is again stirring for 60min, with not
Rust steel spoon pulls the dross on surface out, stands 2min, is cast, cools down 6min, obtain Sn95Ni5 intermediate alloy；
F), Sn99La1 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first is lightly 99.95% by purity
The 74.25kg of 99% tin material, which is added in crucible, melts tin material, puts graphite after tin material all melting and covers in molten tin material, adds
Crucible cover uncaps when the molten tin material that continues to heat up is to 900 DEG C ± 5 DEG C and takes out graphite cover, 1% lanthanum for being 99.95% purity
Material 1kg is put into tin liquor, is quickly then covered in liquid surface with potassium chloride in lanthanum material indentation molten tin material with graphite cover,
Capping is warming up to 1000 DEG C, and after keeping the temperature 15min, it is multiple to move up and down graphite cover, stirs simultaneously, rotates liquid in crucible, with
When with potassium chloride be covered in liquid surface, take out graphite cover, lanthanum material all takes out crucible after fusing, when being cooled to 800 DEG C and is placed on
On asbestos board, remaining tin material 24.75kg is added in crucible, liquid is stirred with graphite rod or so, is cooled to 500 DEG C ± 5 DEG C,
It pulls the dross of liquid surface out with stainless steel spoon, stands 3min, cast, cooling 6min obtains Sn99La1 intermediate alloy；
G), low-temperature lead-free solder % in preparation
Raw material dosage: In:3%, Bi:3%, Sb:0.1%, Cu:0.8%, Ni:0.06%, La:0.05% and surplus
Sn92.99%,
Graphite crucible is put into smelting furnace, 300 DEG C ± 5 DEG C is slowly warming up to, takes the Sn48ln52 of the 5.77kg of preparation
The centre the Sn80Cu20 conjunction of intermediate alloy, the Sn43Bi57 intermediate alloy of 5.26kg, the Sn90Sb10 intermediate alloy of 1kg, 4kg
Gold, the Sn95Ni5 intermediate alloy of 1.2kg, the Sn99La1 intermediate alloy of 5kg and surplus tin subtract the tin in above-mentioned intermediate alloy
Melting in the addition crucible in shortage of 77.77kg tin afterwards, and cover on surface by terpene resin and penta binary acid compound,
Proportion is 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 10min, then crucible
Smelting furnace is removed, both forward and reverse directions on asbestos board is placed on and continues to stir, when temperature is down to 350 DEG C ± 5 DEG C, pulled out with stainless steel spoon
The dross on surface stands 3min, is cast, cools down 5min, obtained in SnIn3 Bi3 Sb0.1 Cu0.8 Ni0.06La0.05
Low-temperature lead-free solder product.
Embodiment 3
Raw material dosage In:2%, Bi:5%, Sb:0.4%, Cu:0.5%, Ni:0.02%, La:0.01% and surplus
Sn92.07%,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 3.85kg's prepared by Example 1
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 8.77kg, the Sn90Sb10 intermediate alloy of 4kg, 2.5kg
Sn80Cu20 intermediate alloy, the Sn95Ni5 intermediate alloy of 0.4kg, the Sn99La1 intermediate alloy of 1kg and surplus tin subtract above-mentioned
Melting in the addition crucible in shortage of 79.48kg tin after tin in intermediate alloy, and cover on surface by terpene resin and penta
Binary acid compound, proportion are 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, stirring of uncapping
10min, then crucible is removed smelting furnace, it is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C,
It pulls the dross on surface out with stainless steel spoon, stands 3min, cast, cool down 5min, obtain SnIn2 Bi5 Sb0.4Cu0.5
Low-temperature lead-free solder product in Ni0.02 La0.01.
Embodiment 4
Raw material dosage: In:1.8%, Bi:6%, Sb:0.3%, Cu:0.4%, Ni:0.03%, La:0.02% and surplus
Sn91.45%,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 3.46kg's prepared by Example 2
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 10.53kg, the Sn90Sb10 intermediate alloy of 3kg, 2kg
The Sn95Ni5 intermediate alloy of Sn80Cu20 intermediate alloy, 0.6Kg, the Sn99La1 intermediate alloy and surplus tin of 2kg subtract above-mentioned
Fusing in the addition crucible in shortage of 78.41kg tin after tin in intermediate alloy, and surface covering by terpene resin with
Binary acid compound, proportion are 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, stirring of uncapping
10min, then crucible is removed smelting furnace, it is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C,
It pulls the dross on surface out with stainless steel spoon, stands 3min, cast, cool down 5min, obtain SnIn1.8 Bi6 Sb0.3 Cu0.4
Low-temperature lead-free solder product in Ni0.03La0.02.
Embodiment 5
Raw material dosage: In:2.5%, Bi:4%, Sb:0.2%, Cu:0.7%, Ni:0.05%, La:0.03% and surplus
Sn92.52%,
Graphite crucible is put into smelting furnace, 0 DEG C ± 5 DEG C of 30 are slowly warming up to, 4.81g's prepared by Example 1
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 7.02kg, the Sn90Sb10 intermediate alloy of 2kg, 3.5kg
Sn80Cu20 intermediate alloy, the Sn95Ni5 intermediate alloy of 1kg, the Sn99La1 intermediate alloy of 3kg and surplus tin subtract among the above
Between 78.67kg tin amount after tin in alloy fusing in crucible is added, and cover on surface and answered by terpene resin and fourth binary acid
With object, proportion is 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 10min, then
Crucible is removed smelting furnace, is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C, use stainless steel
Spoon pulls the dross on surface out, stands 3min, is cast, cools down 5min, obtain SnIn2.5 Bi4 Sb0.2 Cu0.7
Low-temperature lead-free solder product in Ni0.05La0.03.
Embodiment 6
Raw material dosage: In:2.7%, Bi:5.5%, Sb:0.5%, Cu:0.5%, Ni:0.04%, La:0.04% and remaining
Sn90.72% is measured,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 5.19kg's prepared by Example 2
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 9.65kg, the Sn90Sb10 intermediate alloy of 5kg, 2.5kg
Sn80Cu20 intermediate alloy, the Sn95Ni5 intermediate alloy of 0.8kg, the Sn99La1 intermediate alloy of 4kg and surplus tin subtract above-mentioned
Melting in the addition crucible in shortage of 72.86kg tin after tin in intermediate alloy, and cover on surface by terpene resin and penta
Binary acid compound, proportion are 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, stirring of uncapping
10min, then crucible is removed smelting furnace, it is placed on asbestos board and is just continuing opposite direction stirring, when temperature is down to 350 DEG C ± 5 DEG C,
It pulls the dross on surface out with stainless steel spoon, stands 3min, cast, cool down 5min, obtain SnIn2.7 Bi5.5
Low-temperature lead-free solder product in Sb0.5Cu0.5 Ni0.04 La0.04.
Embodiment 7
Raw material dosage: In:3%, Bi:4.5%, Sb:0.4%, Cu:0.6%, Ni:0.05%, La:0.01% and surplus
Sn91.44%,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 5.77kg's prepared by Example 1
Sn48ln52 intermediate alloy, the intermediate alloy of 7.89kgSn43Bi57, the Sn90Sb10 intermediate alloy of 4kg, 3kg Sn80Cu20
Intermediate alloy, the Sn95Ni5 intermediate alloy of 1.0kg, the Sn99La1 intermediate alloy of 1.0kg and surplus tin subtract above-mentioned intermediate conjunction
Fusing in the addition crucible in shortage of 76.86kg tin after tin in gold, and cover on surface by terpene resin and penta binary acid
Compound, proportion are 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 10min,
Crucible is removed smelting furnace again, is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C, use is stainless
Steel spoon pulls the dross on surface out, stands 3min, is cast, cools down 5min, obtain SnIn3Bi4.5Sb0.4Cu0.6Ni0.05L
Low-temperature lead-free solder product in a0.01.
Embodiment 8
Raw material dosage: In2.4%, Bi:6.5%, Sb:0.6%, Cu:0.7%, Ni:0.02%, La:0.05% and surplus
Sn89.73%,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 4.61kg's prepared by Example 2
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 11.40kg, the Sn90Sb10 intermediate alloy of 6kg, 3.5kg
Sn80Cu20 intermediate alloy, the Sn95Ni5 intermediate alloy of 0.4kg, the Sn99La1 intermediate alloy of 5kg and surplus tin subtract above-mentioned
Fusing in crucible is added in 69.09kg tin amount after tin in intermediate alloy, and covers on surface by terpene resin and fourth binary acid
Compound, proportion are 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 10min,
Crucible is removed smelting furnace again, is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C, use is stainless
Steel spoon pulls the dross on surface out, stands 3min, is cast, cools down 5min, obtain SnIn2.4 Bi6.5 Sb0.6 Cu0.7
Low-temperature lead-free solder product in Ni0.02La0.05.
Embodiment 9
Raw material dosage: In:2.6%, Bi:5%, Sb:0.6%, Cu:0.8%, Ni:0.06%, La:0.04% and surplus
Sn90.9%,
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, 5.0kg's prepared by Example 1
Sn48ln52 intermediate alloy, the Sn43Bi57 intermediate alloy of 8.77kg, the Sn90Sb10 intermediate alloy of 6kg, 4kg Sn80Cu20
Intermediate alloy, the Sn95Ni5 intermediate alloy of 1.2kg, the Sn99La1 intermediate alloy of 4kg and surplus tin subtract above-mentioned intermediate alloy
In tin after 71.03kg tin addition crucible in shortage in fusing, and cover on surface and answered by terpene resin and binary acid
With object, proportion is 10: 0.3 antioxidants, and capping is continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, uncaps and stir 10min, then
Crucible is removed smelting furnace, is placed on asbestos board and continues both forward and reverse directions stirring, when temperature is down to 350 DEG C ± 5 DEG C, use stainless steel
Spoon pulls the dross on surface out, stands 3min, is cast, cools down 5min, obtain SnIn2.6 Bi5 Sb0.6 Cu0.8
Low-temperature lead-free solder product in Ni0.06La0.04.
Under the same test conditions, to embodiment 1 to embodiment 9 and comparative example solder carry out fusing point, temperature, the rate of spread,
Shear strength, test for tensile strength and assessment, test result is as shown in table 1,
1 embodiment 1 of table is to embodiment 9 and comparative example solder main performance test result
Fusing point by low-temperature lead-free solder in the present invention it can be seen from the test result of table 1 between 160 DEG C~190 DEG C,
183 DEG C of the fusing point with Sn63Pb37 eutectic tin-lead solder is very close to shear strength is more than or equal to 50Mpa, and tensile strength is preferable, weldering
It connects the rate of spread and reaches and meet welding process requirement, can achieve the requirement of middle low temperature column lead-free solder Technological adaptability, this hair
It is bright especially suitable for low-temperature lead-free welding procedure in the electronic products such as high-end instrument and meter, computer.
Claims (6)
1. a kind of middle low-temperature lead-free solder, it is characterised in that it is made of the raw material of following weight percents:
In:1.5~3.0%, Bi:3~7%, Sb:0.1~0.6%, Cu:0.3~0.8%, Ni:0.02~0.06%, La:
0.008~0.05% and surplus be Sn.
2. low-temperature lead-free solder according to claim 1, it is characterised in that the weight hundred of described In, Bi, Sb, Cu, the Ni
Point than preferred scope be In:2~3%, Bi:4~6%, Sb:0.2~0.5%, Cu:0.4~0.7%, Ni:0.03~
0.05%.
3. according to claim 1 in low-temperature lead-free solder, it is characterised in that the preferred scope of the La be 0.01~
0.03%.
4. the preparation method of low-temperature lead-free solder in as described in claim 1, it is characterised in that it is carried out in the steps below:
A), Sn48In52 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first lightly by purity is 99.95% 48%
Tin material is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to 400 DEG C ± 5 DEG C, then be by purity
It in 99.95% 52% indium material point, 4 addition crucibles and stirs, after indium material all melting, crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions on asbestos board and stir 10min, pull the dross on surface out with stainless steel spoon, stand 2~3min, is cast, is cold
But 5~6min obtains Sn48In52 intermediate alloy；
B) Sn43Bi57 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first lightly by purity is 99.95% 43%
Tin material is added in crucible, adds crucible cover after tin material all melting, continues to be warming up to 450 DEG C ± 5 DEG C, then be by purity
It in 99.95% 57% bismuth material point, 4 addition crucibles and stirs, after bismuth material all melting, crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions on asbestos board and stir 10min, pull the dross on surface out with stainless steel spoon, stand 1~2min, is cast, is cold
But 5~6min obtains Sn43Bi57 intermediate alloy；
C), Sn90Sb10 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first lightly by purity is 99.95% 90%
The 2/3 of tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 450 DEG C ± 5 DEG C, then will
It in 10% antimony material point, 4 addition crucibles that purity is 99.95% and stirs, after antimony material all melting, crucible is removed melting
Furnace is placed on asbestos board and continues both forward and reverse directions stirring, is subsequently placed into remaining 1/3 tin material, is again stirring for 10min, uses stainless steel
Spoon pulls the dross on surface out, stands 1~2min, is cast, cools down 5~6min, obtain Sn90Sb10 intermediate alloy；
D), Sn80Cu20 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, first lightly by purity is 99.95% 80%
The 2/3 of tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 500 DEG C ± 5 DEG C, then will
The 20% bronze medal material point that purity is 99.95%, 5 additions are simultaneously stirred, and after copper material all melting, crucible are removed smelting furnace, is placed on
Continue both forward and reverse directions stirring on asbestos board, is subsequently placed into remaining 1/3 tin material, is again stirring for 10min, pull table out with stainless steel spoon
The dross in face stands 2~3min, is cast, cools down 5~6min, obtain Sn80Cu20 intermediate alloy；
E), Sn95Ni5 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first lightly by purity is 99.95% 95%
The 3/4 of tin material is added in crucible, adds crucible cover after tin material all melting, continues to uncap when being warming up to 800 DEG C ± 5 DEG C, then will
The 5% nickel material point that purity is 99.95%, 2 additions are simultaneously stirred, and after copper material all melting, crucible are removed smelting furnace, is placed on
Continue both forward and reverse directions stirring on asbestos board, is subsequently placed into remaining 1/4 tin material, is again stirring for 60min, pull table out with stainless steel spoon
The dross in face stands 2~3min, is cast, cools down 5~6min, obtain Sn95Ni5 intermediate alloy；
F), Sn99La1 intermediate alloy is prepared
Graphite crucible is put into smelting furnace, is slowly warming up to 400 DEG C ± 5 DEG C, first lightly by purity is 99.95% 99%
The 3/4 of tin material is put graphite after tin material all melting and is covered in molten tin material, add crucible cover in crucible, continues heating melting
It when tin material is to 900 DEG C ± 5 DEG C, uncaps and takes out graphite cover, the 1% lanthanum material that purity is 99.95% is put into molten tin material, quickly
With graphite cover in lanthanum material indentation molten tin material, it then is covered in molten tin material surface with potassium chloride, capping is warming up to 1000 DEG C
~1020 DEG C, after keeping the temperature 10~15min, it is multiple to move up and down graphite cover, stirs simultaneously, rotates molten tin material in crucible, with
When with potassium chloride be covered in fused materials surface, take out graphite cover, crucible taken out when being cooled to 800 DEG C~780 DEG C and is placed on asbestos
On plate, remaining tin material 1/4 is added in crucible, fused materials is stirred with graphite rod or so, 500 DEG C ± 5 DEG C is cooled to, with not
Rust steel spoon pulls the dross on surface out, stands 2~3min, is cast, cools down 5~6min and obtain Sn99La1 intermediate alloy；
G), low-temperature lead-free solder in preparation
Graphite crucible is put into smelting furnace, is slowly warming up to 300 DEG C ± 5 DEG C, by the 2.88~5.77% of the preparation of a) item
The 1.0 of Sn48ln52 intermediate alloy, b) 5.26~12.28% Sn43Bi57 intermediate alloy of item preparation, c) item preparation~
The 0.4 of 6.0% Sn90Sb10 intermediate alloy, d) 1.5~4.0% Sn80Cu20 intermediate alloy of item preparation, e) item preparation
0.8~5.0% Sn99La1 intermediate alloy and surplus tin of~1.2% Sn95Ni5 intermediate alloy, f) item preparation subtract
Melting in crucible is added in 69.09~79.48% insufficient tin amounts after stating the tin in intermediate alloy, and anti-oxidation in surface covering
Agent, capping are continuously heating to 450 DEG C of ± 5 DEG C of stoppings heating, and uncap 5~10min of stirring, then crucible is removed smelting furnace, is placed on
Continue both forward and reverse directions stirring on asbestos board, when temperature is down to 350 DEG C ± 5 DEG C, pull the dross on surface out with stainless steel spoon, stands
2~3min is cast, cools down 5~6min, and middle low-temperature lead-free solder product is obtained.
5. the preparation method of low-temperature lead-free solder according to claim 4, it is characterised in that the antioxidant is terpenes
Resin and organic dibasic acid compound, proportion are 10: 0.3.
6. the preparation method of low-temperature lead-free solder according to claim 5, it is characterised in that the organic dibasic acid is
Succinic acid, glutaric acid or adipic acid.
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