WO2015166945A1 - 鉛フリーはんだ合金 - Google Patents
鉛フリーはんだ合金 Download PDFInfo
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- WO2015166945A1 WO2015166945A1 PCT/JP2015/062818 JP2015062818W WO2015166945A1 WO 2015166945 A1 WO2015166945 A1 WO 2015166945A1 JP 2015062818 W JP2015062818 W JP 2015062818W WO 2015166945 A1 WO2015166945 A1 WO 2015166945A1
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 107
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 55
- 239000000956 alloy Substances 0.000 title claims abstract description 55
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 229910052797 bismuth Inorganic materials 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052732 germanium Inorganic materials 0.000 claims description 8
- 229910052738 indium Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 57
- 229910020882 Sn-Cu-Ni Inorganic materials 0.000 abstract description 8
- 238000005476 soldering Methods 0.000 abstract description 8
- 230000032683 aging Effects 0.000 description 66
- 238000005259 measurement Methods 0.000 description 47
- 230000000694 effects Effects 0.000 description 22
- 238000000034 method Methods 0.000 description 22
- 239000000654 additive Substances 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
- 229910000765 intermetallic Inorganic materials 0.000 description 6
- 229910052787 antimony Inorganic materials 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 229910017944 Ag—Cu Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 206010035148 Plague Diseases 0.000 description 1
- 229910020830 Sn-Bi Inorganic materials 0.000 description 1
- 229910020994 Sn-Zn Inorganic materials 0.000 description 1
- 229910018728 Sn—Bi Inorganic materials 0.000 description 1
- 229910019343 Sn—Cu—Sb Inorganic materials 0.000 description 1
- 229910009069 Sn—Zn Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- -1 preform Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
- B23K1/0016—Brazing of electronic components
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
- C22C13/02—Alloys based on tin with antimony or bismuth as the next major constituent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
- H01R4/02—Soldered or welded connections
-
- 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
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- 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
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3613—Polymers, e.g. resins
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
Definitions
- the present invention relates to a lead-free solder alloy with little deterioration over time and excellent long-term reliability, and a solder joint using the solder alloy.
- Lead-free solder is widely used as a bonding material for electronic components in order to reduce the global environmental load, and Sn—Ag—Cu solder alloys and Sn—Cu—Ni solder alloys are typical compositions.
- Sn—Ag—Cu solder alloys and Sn—Cu—Ni solder alloys are typical compositions.
- lead-free solder alloys have been proposed.
- Patent Document 1 discloses a lead-free solder alloy in which 0.01 to 3% by weight of Bi is added to a Sn—Cu—Ni basic composition to facilitate control of the melting point of the solder.
- Patent Document 2 discloses a lead-free solder alloy in which Bi is added to the basic composition of Sn—Cu—Sb at a ratio of 1 wt% or less to improve mechanical strength.
- Patent Document 3 discloses a lead-free solder alloy having an effect of improving adhesion strength and lowering the solidus temperature by adding Cu, Ni, and Bi to Sn in an amount of 0.001 to 5% by weight. Furthermore, in the patent document 4, the applicant has added a certain amount of Ni and Cu to the Sn—Bi eutectic composition, so that the intermetallic compound has a hexagonal close-packed structure at the solder joint and the solder joint interface. A lead-free solder alloy having strong joint strength during solder joining is disclosed.
- the solder alloy composition disclosed in Patent Document 1 has a Cu content of 2 to 5% by weight.
- the solder alloy composition disclosed in Patent Document 2 contains 10% by weight or more of Sb in the basic composition, the solidus temperature is 230 ° C. or more as shown in the Examples.
- a soldering process at a high temperature is required as compared with the conventional typical lead-free solder composition.
- the technique currently disclosed by patent document 3 is a solder alloy composition limited to extra fine wire solder, and does not respond
- the technique disclosed in Patent Document 5 is a solder alloy composition made of Sn—Cu—Ni—Bi, which prevents tin plague from being generated at an extremely low temperature and has good wettability and impact resistance.
- the Cu compounding amount is limited to 0.5 to 0.8 mass%
- the Ni compounding amount is 0.02 to 0.04 mass%
- the Bi compounding amount is limited to 0.1 mass% or more and less than 1 mass%. It has become a numerical value.
- the solder joint portion of the electronic device is usually in a state where the solder joint portion is energized, and the solder joint portion may be exposed to a high temperature. Therefore, not only the bonding strength at the time of solder bonding but also the bonding strength when exposed to high temperatures is important for the reliability of solder bonding.
- the techniques disclosed in Patent Documents 1 to 5 have no suggestion regarding the bonding strength when exposed to a high temperature for a long time. There is a need for a lead-free solder alloy that can be soldered with high reliability enough to withstand long-term use of electronic equipment and that is versatile in soldering.
- the present invention provides a versatile lead-free solder alloy and solder joint that maintains high joint strength and maintains high joint strength even in a high temperature state after solder joint, and has high reliability. Objective.
- the present inventors have made extensive studies focusing on the lead-free solder alloy composition and intermetallic compounds.
- the lead-free solder alloy having a basic composition of Sn-Cu-Ni has a certain amount.
- Bi By adding Bi, it was found that even when the solder joint was exposed to a high temperature, a decrease in joint strength was suppressed, and the present invention was completed.
- the present invention has Sn—Cu—Ni as a basic composition, Sn is 76.0 to 99.5% by mass, Cu is 0.1 to 2.0% by mass, and Ni is 0.01 to 0.5% by mass.
- lead-free solder alloy composition containing 0.1 to 5.0% by mass of Bi the joint strength of the solder joint is reduced not only during joining but also during exposure to high temperatures for a long time. Therefore, it is possible to perform solder bonding with high reliability for maintaining the bonding strength.
- the present invention is a general-purpose lead-free solder alloy that is not limited to the method and form of use of the solder product, and the bonding strength does not decrease even when the solder joint is exposed to a high temperature state for a long time.
- the present invention can be widely applied not only to the joining of electronic equipment but also to equipment having a solder joint where a large current flows or equipment exposed to a high temperature state.
- FIG. It is a graph which shows a test result. It is the graph which put together the measurement result of the tensile strength of each sample which has a composition of Table 2.
- FIG. It is the graph which put together the measurement result of the tensile strength of each sample which has a composition of Table 4.
- FIG. It is the graph which put together the measurement result of the tensile strength of the sample from which the addition amount of Cu differs. It is the graph which put together the measurement result of the tensile strength of the sample from which the addition amount of Ni differs. It is the graph which put together the measurement result of the tensile strength of the sample from which the addition amount of Ge differs. It is the graph which put together the measurement result of the tensile strength of the sample from which the addition amount of In differs. It is the graph which put together the measurement result of the elongation rate of In change sample. It is the graph which put together the measurement result of the tensile strength of the sample to which the additive element was added.
- solder joints of electronic devices or the like Conventionally, as an important item for solder joints of electronic devices or the like, the joint strength at the time of solder joint is mentioned, and development and provision of solder alloys with improved joint strength at the time of solder joint has been made.
- solder joints used in electronic devices and the like are often in a state where a current flows or is exposed to a high temperature particularly in the use of electronic devices, and the temperature of the solder joints depends on the external environment. In some cases, the increase is accelerated, and it is necessary to suppress the deterioration of the solder joints with time at high temperatures in order to increase the reliability of the solder joints.
- the present invention relates to a solder that suppresses a decrease in bonding strength of a solder joint due to continuous exposure of the solder joint to a high temperature state, which is an example of a situation according to the actual use situation of an electronic device.
- the invention relates to the alloy composition.
- Sn is 76.0 to 99.5% by mass
- Cu is 0.1 to 2.0% by mass
- Ni is 0.01 to 0.5% by mass
- Bi is 0.1 to 5.0% by mass. %
- a lead-free solder alloy characterized in that it is a solder joint using the lead-free solder alloy.
- Sn is 76.0 to 99.5% by mass
- Cu is 0.1 to 2.0% by mass
- Ni is 0.01 to 0.5% by mass
- Bi is 0.1 to 5.0% by mass.
- the basic composition contained is 0.1 to 5.0% by mass of Sb, 0.1 to 10.0% by mass of In, 0.001 to 1.0% by mass of Ge, and 0.001 to 1 of Ga. It is also possible to add one or more selected from 0.0% by mass.
- the lead-free solder alloy having the basic composition of Sn-Cu-Ni-Bi according to the present invention can be arbitrarily added with elements such as P, Co, Al, Ti, and Ag within the range having the effects of the present invention. It is also possible to add.
- the mechanical strength of the solder joint can be synergistically expected while having the effects of the present invention.
- In when In is added, even when the content of Cu or Sb exceeds 1 mass% and is blended in the solder alloy, it has the effect of lowering the solidus temperature while having the effect of the present invention.
- it can be expected to reduce the load of electronic parts to be joined to electronic devices and soldering work.
- Ge or Ga is added, the oxidation of the solder joint can be suppressed and the wettability can be improved while having the effects of the present invention, and the long-term reliability and solder joint characteristics of the solder joint can be synergistically improved. Can be expected to improve.
- the lead-free solder alloy of the present invention was evaluated by performing an aging test described below.
- [Aging test] (Method) 1) A solder alloy having the composition shown in Table 1 is prepared and dissolved, and then cast into a dog-bone mold having a cross section of 10 mm ⁇ 10 mm to prepare a measurement sample. 2) The measurement sample is left at 150 ° C. for 500 hours and subjected to an aging treatment. 3) Using a tester AG-IS manufactured by Shimadzu Corporation, pull the sample that was not subjected to the aging treatment and the sample that was performed at room temperature (20 ° C. to 25 ° C.) at 10 mm / min until each sample was cut, Measure the tensile strength of the sample. (result) The results are shown in FIG.
- the left side shows the measurement result of the unaged sample
- the right side shows the measurement result of the sample subjected to the aging treatment.
- the samples of the present invention are Nos. 2 to 5, and it can be seen that there is little decrease in tensile strength when the aging treatment is performed or when compared with the untreated product.
- Sample No. 1 and Sample No. which are comparative products, are used.
- Nos. 6 to 9 the decrease in tensile strength of the aging-treated product is significant compared to the unaged product.
- the lead-free solder alloy of the present invention based on Sn—Cu—Ni—Bi has a lower tensile strength than other lead-free solder alloy compositions while being exposed to a high temperature of 150 ° C. for 500 hours. It can be clearly seen that is suppressed.
- samples containing Bi are sample ii “sample name: +0.1 Bi *”, sample iii “sample name: +0.5 Bi *”, sample iv “sample name: +1.0 Bi *”, sample v “sample name”. : +1.5 Bi * ”, sample vi“ sample name: +2.0 Bi * ”, sample vii“ sample name: +3.0 Bi * ”, sample viii“ sample name: +4.0 Bi * ”, sample ix“ sample name: +5 ” .0Bi * "and sample x" sample name: + 6.0Bi * ".
- Bi is 0.1% by mass, 0.5% by mass, 1.0% by mass, 1.5% by mass, 2.0% by mass, 3.0% by mass, 4.0% by mass, 5.0 mass% and 6.0 mass% are contained.
- Samples i to x having the composition shown in Table 2 were produced by the method described above in 0016. Thereafter, after aging treatment at 150 ° C. for 0 hour and 500 hours, the tensile strength was measured.
- Table 3 is a table showing measurement results for samples i to x.
- “A” in Table 3 is a measurement result of tensile strength after aging for 0 hours
- “C” in Table 3 is a measurement result of tensile strength after aging for 500 hours
- the rate of change in strength is the tensile strength after aging for 500 hours. It is the result which showed the change of intensity
- FIG. 2 is a graph summarizing the measurement results of tensile strength of samples i to x.
- Table 4 is a composition table showing the composition of the sample used for the measurement of the tensile strength. As shown in FIG. 3, sample 1 “SAC305” and sample 2 “SN1” do not contain Bi, and sample 3 “+0.1 Bi”, sample 4 “+0.5 Bi”, and sample 5 “ +1.0 Bi ”, Sample 6“ +1.5 Bi ”, Sample 7“ +2.0 Bi ”, Sample 8“ +3.0 Bi ”, Sample 9“ +4.0 Bi ”, Sample 10“ +5.0 Bi ”and Sample 11“ +6. "0Bi” includes 0.1 mass%, 0.5 mass%, 1 mass%, 1.5 mass%, 2 mass%, 3 mass%, 4 mass%, 5 mass% and 6 mass%, respectively. ing.
- Sample 1 “SAC305” contains 3% by mass and 0.5% by mass of Ag and Cu, respectively, and the balance is Sn.
- sample 1 “SAC305”, sample 2 “SN1”, sample 3 “+10.1 Bi”, sample 4 “+0.5 Bi”, sample 5 “+1.0 Bi”, sample 6 “+1.5 Bi”, Sample 7 “+2.0 Bi”, Sample 8 “+3.0 Bi”, Sample 9 “+4.0 Bi Bi mass%”, Sample 10 “+5.0 Bi”, Sample 11 “+6.0 Bi” are designated as “Sample 1”, “ “Sample 2”, “Sample 3”, “Sample 4”, “Sample 5”, “Sample 6”, “Sample 7”, “Sample 8”, “Sample 9”, “Sample 10”, “Sample 11”. .
- Samples 1 to 11 having compositions as shown in Table 4 were produced by the method described above.
- the produced samples 1 to 11 were subjected to aging treatment at 150 ° C. for 0 hour and 500 hours, and then the tensile strength was measured by the method described above.
- Table 5 is a table showing the measurement results for samples 1 to 11.
- “A” in Table 5 is a measurement result of tensile strength after aging for 0 hours
- “C” in Table 5 is a measurement result of tensile strength after aging for 500 hours
- the rate of change in strength is the tensile strength after aging for 500 hours. It is the result which showed the change of intensity in%.
- FIG. 3 is a graph summarizing the measurement results of the tensile strengths of Samples 1-11.
- the amount of Bi added is 0.5 mass% or more in a harsh usage environment that is exposed to a high temperature of 150 ° C. for a long time.
- the content is preferably 4.0% by mass
- the addition amount of Bi is preferably 1.0% by mass to 3.0% by mass.
- a high tensile strength can be obtained even for an aging treatment time of 500 hours. Further, there is no difference in tensile strength between the case where there is no aging treatment and the case where the aging treatment is performed, and a stable tensile strength can be obtained.
- the tensile strength after the aging treatment is lower than that in the case where the aging treatment is not performed.
- the amount of Bi added is 0.1 mass% to 5.0 mass%. It may be.
- Ni, Bi, and Ge are included in 0.05 mass%, 1.5 mass%, and 0.006 mass%, respectively, and Cu is 0.05 mass% to 2.2 mass%, respectively. It is added and the balance is Sn.
- a sample to which 0.05% by mass of Cu is added is “0.05Cu”
- a sample to which 0.1% by mass is added is “0.1Cu”
- a sample to which 0.7% by mass is added Is referred to as “0.7 Cu”
- a sample added with 2 mass% is referred to as “2 Cu”
- a sample added with 2.2 mass% is referred to as “2.2 Cu”.
- Such a sample was prepared by the above-described method, and the prepared sample was subjected to aging treatment at 150 ° C. for 0 hour and 500 hours, and then the tensile strength was measured by the above-described method.
- Table 6 is a table showing the measurement results of the tensile strength for the samples having different Cu addition amounts.
- “A” in Table 6 is a measurement result of tensile strength after aging for 0 hour
- “C” in Table 4 is a measurement result of tensile strength after aging for 500 hours.
- FIG. 4 is a graph summarizing the measurement results of tensile strength of samples with different amounts of Cu.
- the amount of Cu added may be 0.1 mass% to 2.0 mass%. desirable.
- Ni is from 0.005% by mass to 0.55% by mass. It is added and the balance is Sn.
- a sample added with 0.005% by mass of Ni is “0.005Ni”
- a sample added with 0.01% by mass is “0.01Ni”
- a sample added with 0.05% by mass is referred to as “0.05Ni”
- a sample added with 0.5 mass% is referred to as “0.5Ni”
- a sample added with 0.55 mass% is referred to as “0.55Ni”.
- Such a sample was prepared by the above-described method, and the prepared sample was subjected to aging treatment at 150 ° C. for 0 hour and 500 hours, and then the tensile strength was measured by the above-described method.
- Table 7 is a table showing the measurement results of the tensile strength for the samples having different Ni addition amounts. “A” in Table 7 is a measurement result of tensile strength after aging for 0 hour, and “C” in Table 7 is a measurement result of tensile strength after aging for 500 hours. FIG. 5 is a graph summarizing the measurement results of tensile strength of samples with different amounts of Ni added.
- the amount of Ni added may be 0.01 mass% to 0.5 mass%. desirable.
- Cu, Ni, and Bi are contained in an amount of 0.7 mass%, 0.05 mass%, and 1.5 mass%, respectively, and Ge is added from 0.0001 mass% to 1 mass%. And the balance is Sn.
- a sample to which 0.0001 mass% of Ge is added is “0.0001Ge”
- a sample to which 0.001 mass% is added is “0.001Ge”
- a sample to which 0.006 mass% is added is added. Is referred to as “0.006Ge”
- a sample added with 0.1 mass% is referred to as “0.1Ge”
- a sample added with 1 mass% is referred to as “1Ge”.
- Such a sample was prepared by the above-described method, and the prepared sample was subjected to aging treatment at 150 ° C. for 0 hour and 500 hours, and then the tensile strength was measured by the above-described method.
- Table 8 is a table showing the measurement results of tensile strength for samples having different Ge addition amounts. “A” in Table 8 is a measurement result of tensile strength after aging for 0 hour, and “C” in Table 8 is a measurement result of tensile strength after aging for 500 hours. FIG. 6 is a graph summarizing the measurement results of tensile strength of samples having different Ge addition amounts.
- the addition amount of Ge is 0.001% by mass to 0.1% by mass. desirable.
- the Ge addition amount can also be 0.001% by mass to 1.0% by mass.
- Cu, Ni, Bi, and Ge are contained in 0.7 mass%, 0.05 mass%, 1.5 mass%, and 0.006 mass%, respectively, and In is 0 mass%. It is added up to 10% by weight, and the balance is Sn.
- a sample to which 0 mass% In is added is “0In”
- a sample to which 0.1 mass% is added is “0.1In”
- a sample to which 3 mass% is added is “3In”
- 4 The sample added with 4% by mass is “4In”
- the sample with 5% by mass added is “5In”
- the sample with 6% by mass added is “6In”
- the sample with 7% by mass added is “7In”
- the added sample is referred to as “10In”.
- Such a sample was prepared by the above-described method, and the prepared sample was subjected to aging treatment at 150 ° C. for 0 hour and 500 hours, and then the tensile strength was measured by the above-described method.
- Table 9 is a table showing the measurement results of the tensile strength for the samples with different In addition amounts (hereinafter simply referred to as In changed samples). “A” in Table 9 is a measurement result of tensile strength after aging for 0 hour, and “C” in Table 9 is a measurement result of tensile strength after aging for 500 hours. FIG. 7 is a graph summarizing the measurement results of tensile strength of samples with different amounts of In.
- Table 10 is a table showing the measurement results of the elongation rate with respect to the In change sample.
- “A” is the measurement result of the elongation after 0-hour aging
- “C” in Table 10 is the measurement result of the elongation after 500-hour aging
- the elongation change rate is the value after 500-hour aging. It is the result which showed the change of elongation rate in percentage (%).
- FIG. 8 is a graph summarizing the measurement results of the elongation rate of the In change sample.
- the elongation is obtained by the following equation.
- ⁇ is the elongation
- Lo is the distance between the gauge points before measuring the tensile strength
- L is the distance between the gauge points after measuring the tensile strength.
- ⁇ (%) (L ⁇ Lo) / Lo ⁇ 100
- the elongation rate is the distance between the marks when a predetermined distance between test points (50 mm (Lo)) is marked on the test piece before measuring the tensile strength and the fractured test piece is abutted after measuring the tensile strength.
- the length (L) was measured and calculated using the above formula.
- the transformation start temperature may decrease.
- the amount of In added is more preferably 0.1% by mass to 6% by mass.
- the amount of In added can be 0.1% by mass to 10.0% by mass.
- Table 11 is a table showing the measurement results of the tensile strength of the samples to which such additive elements are added.
- “A” in Table 11 is a measurement result of tensile strength after aging for 0 hour
- “C” in Table 11 is a measurement result of tensile strength after aging for 500 hours.
- FIG. 9 is a graph summarizing the measurement results of the tensile strength of the sample to which such an additive element is added.
- Table 12 shows the composition of the sample to which such an additive element was added.
- SAC305 has the same composition as “SAC305” (manufactured by Nippon Superior Co., Ltd.) in Table 4 above, and the composition of “+1.5 Bi” (I) is already shown in Table 2, so detailed composition display Is omitted.
- Samples II to XIV contain Cu, Ni, and Bi, respectively, at 0.7% by mass, 0.05% by mass, and 1.5% by mass, respectively.
- such contents of Cu, Ni, and Bi are also referred to as a basic composition.
- Samples II and III in addition to the basic composition, Ge is further contained in an amount of 0.001% by mass or 0.1% by mass, respectively, and the balance is Sn.
- Samples IV to XIV contain 0.006% by mass of Ge together with the basic composition, and further contain such additive elements.
- Ge and P have a unique effect of preventing oxidation of Sn and solder components by an oxide film.
- Ti and Ga have an intrinsic effect of an auto-oxidation effect and an increase in bulk strength.
- In has an inherent effect of lowering the liquid phase temperature and increasing strength
- Ag has an inherent effect of increasing strength before aging due to dispersion and precipitation strengthening.
- Co has a unique effect of making the intermetallic compound layer finer
- Al has a unique effect of making the intermetallic compound finer, suppressing a decrease in strength after aging, and an auto-oxidation effect.
- Table 13 is a table comparing the tensile strengths of “SAC305” and samples I to XIV before and after aging. More specifically, the ratios of the tensile strengths of Samples I to XIV with respect to “SAC305” and the tensile strengths of “SAC305” and Samples II to XIV with respect to Sample I are shown as percentages. In other words, the relative tensile strength with respect to “SAC305” and Sample I before and after aging is shown.
- the lead-free solder alloy having the basic composition of Sn-Cu-Ni-Bi of the present invention is not limited in shape and usage within the range having the effects of the present invention, and can be used for flow and reflow soldering.
- the bar-type solder shape for flow it can be processed into various forms such as solder paste, solder containing solder, powder, preform, and ball depending on the application.
- solder joint part soldered using the lead-free solder alloy of this invention processed into various shapes is also the object of this invention.
- the present invention is a general-purpose lead-free solder alloy that is not limited to the form of a solder product, and since there is little decrease in the joint strength of the solder joint even when exposed to high temperatures for a long time, The reliability of the part is high over a long period of time, and it can be widely applied to devices / equipment having solder joints where a large current flows as well as devices / equipment exposed to high temperature as well as solder joining of electronic devices.
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Abstract
Description
近年、Sn-Ag-Cu系はんだ合金及びSn-Cu-Ni系はんだ合金に加え、BiやIn、Sb等を添加した鉛フリーはんだ合金やSn-Zn系はんだ合金等の接合用途や特性に対応した鉛フリーはんだ合金が提案されている。
例えば、特許文献1では、Sn-Cu-Ni基本組成に0.01~3重量%のBiを添加し、はんだの融点制御を容易にした鉛フリーはんだ合金が開示されている。
また、特許文献2では、Sn-Cu-Sb基本組成に1重量%以下の割合でBiを添加し、機械的強度を向上させた鉛フリーはんだ合金が開示されている。
そして、特許文献3では、SnにCu、Ni、及びBiを0.001~5重量%添加し、接着強度の向上と固相線温度を下げる効果を有する鉛フリーはんだ合金が開示されている。
更に、出願人は、特許文献4に於いて、Sn-Bi共晶組成に一定量のNi及びCuを添加することにより、はんだ接合部及びはんだ接合界面に六方最密充填構造を有する金属間化合物を形成させて、はんだ接合時の強固な接合強度を有する鉛フリーはんだ合金を開示している。
また、特許文献2で開示されているはんだ合金組成は基本組成にSbが10重量%以上配合されているため、実施例にあるように固相線温度が230℃以上であり、特許文献1同様に従来の代表的な鉛フリーはんだ組成に比べ、高い温度でのはんだ付け工程が必要となる。
そして、特許文献3で開示されている技術は極細線はんだに限定したはんだ合金組成であり、種々のはんだ接合に対応するものではなく、汎用性に課題が残っている。
一方、特許文献4で開示されている技術は、接合界面にNiAs型結晶構造を有する金属間化合物を形成させることにより強固な接合を目的とした技術であり、配合するSn及びBiの比率が、Sn:Bi=76~37原子量%:23~63原子量%であり、共晶付近を対象としている。
更に、特許文献5で開示されている技術は、極低温で錫ペストの発生が防止され、かつ濡れ性及び耐衝撃性の良好なSn-Cu-Ni-Biからなるはんだ合金組成であり、当該発明の目的から、Cu配合量が0.5~0.8質量%、Ni配合量が0.02~0.04質量%、Bi配合量が0.1質量%以上、1質量%未満と限定された数値となっている。
そこで、はんだ接合の信頼性には、はんだ接合時の接合強度は勿論のこと、高温に曝された場合での接合強度も重要になってくる。
ところが、特許文献1~特許文献5で開示されている技術には高温で長時間曝された場合の接合強度に関して何らの示唆もない。
そして、電子機器の長期使用に十分に耐えられる高い信頼性を有するはんだ接合が可能な、且つ、はんだ接合に於いて汎用性のある鉛フリーはんだ合金が求められている。
従来、電子機器等のはんだ接合には、重要項目として、はんだ接合時の接合強度が挙げられており、はんだ接合時の接合強度を向上させたはんだ合金の開発や提供がなされている。
しかし、電子機器等に使用されるはんだ接合部は、電子機器の使用には特に電流が流れた状態になることや高温に曝される場合も多く、また、外部の環境によってはんだ接合部の温度上昇が加速される場合もあり、高温状態でのはんだ接合部の経時劣化を抑制することも、はんだ接合部の信頼性を高めるためには必要である。
一方、はんだ接合部の評価として、はんだ接合部を冷温状態及び高温状態に一定時間放置することを繰り返すヒートサイクル試験と言われる試験方法を用いて評価する方法が一般的に用いられているが、この方法は高温状態の後に冷温状態にて一定時間放置するため、高温状態のままで長時間放置するエージング試験の場合とは、試験後のはんだ接合部の状態が異なるとも知られている。
本発明は、実際の電子機器の使用実態に応じた状況の一例を示す環境である高温状態に連続してはんだ接合部が曝されることによる、はんだ接合部の接合強度の低下を抑制するはんだ合金組成に関する発明である。
そして、本発明のSn-Cu-Ni-Biを基本組成とする鉛フリーはんだ合金には、本発明の効果を有する範囲に於いて、P、Co、Al、Ti、Ag等の元素を任意に添加することも可能である。
また、Inを添加した場合、CuやSbの含有量が1質量%を超えて当該はんだ合金に配合された場合でも、本発明の効果を有しながら固相線温度を下げる効果をも有し、電子機器に接合する電子部品等やはんだ付け作業の負荷低減効果が期待できる。
そして、GeやGaを添加した場合は、本発明の効果を有しながらはんだ接合部の酸化を抑制することや濡れ性の向上が可能となり、はんだ接合部の長期信頼性やはんだ接合特性を相乗的に向上することが期待できる。
本発明の鉛フリーはんだ合金について、以下に説明するエージング試験を行い評価した。
〔エージング試験〕
(方法)
1)表1に示す組成のはんだ合金を調製し、溶解させた後、10mm×10mmの断面を有するdog-bone形状の鋳型に鋳込み、測定用サンプルを作製する。
2)測定サンプルを150℃に500時間放置し、エージング処理を行う。
3)島津製作所製試験機AG-ISを用いて、エージング処理を行わないサンプルと行ったサンプルを、室温(20℃~25℃)10mm/分の条件にて、各サンプルが切断するまで引っ張り、サンプルの引張強度を測定する。
(結果)
結果を図1に示す。
本発明のサンプルは、No.2~5であり、エージング処理を行った場合でも未処理品と比較しても引張強度の低下が少ないことがわかる。
これに対して、比較品であるサンプルNo.1及びサンプルNo.6~9は、エージング未処理品に対してエージング処理品の引張強度の低下が著しい。
この結果から、Sn-Cu-Ni-Biを基本組成とする本発明の鉛フリーはんだ合金は、150℃という高温に500時間曝されながら、他の鉛フリーはんだ合金組成に比べて引張強度の低下が抑制されていることが明確にわかる。
表2は、前記引張強度の測定に用いられたサンプルの組成を示す組成表である。
比較例(サンプルi:サンプル名をSN2)として、Biを配合しないSn-Cu-Ni組成も含む。また、Biを含有したサンプルを、サンプルii「サンプル名:+0.1Bi*」、サンプルiii「サンプル名:+0.5Bi*」、サンプルiv「サンプル名:+1.0Bi*」、サンプルv「サンプル名:+1.5Bi*」、サンプルvi「サンプル名:+2.0Bi*」、サンプルvii「サンプル名:+3.0Bi*」、サンプルviii「サンプル名:+4.0Bi*」、サンプルix「サンプル名:+5.0Bi*」及びサンプルx「サンプル名:+6.0Bi*」と称する。サンプルi~xは夫々Biが0.1質量%、0.5質量%、1.0質量%、1.5質量%、2.0質量%、3.0質量%、4.0質量%、5.0質量%及び6.0質量%含まれている。
また、Biの添加量が0.1質量%以上であるサンプルii~xにおいては、Biが添加されていないサンプルiに対して、500時間のエージング処理の場合、該サンプルi以上の高い引張強度を表している。更にBiの添加量が1.0質量%から3.0質量%であるサンプルiv~viiにおいては、強度変化率が98%以上であり、500時間エージング後の引張強度の変化率が極めて小さいこと、取分けサンプルv~viiにおいては500時間エージング後の引張強度がエージングしなかった場合よりも向上していることがわかる。
一方、Bi添加量が6質量%のサンプルxに至ってはBi無添加サンプルiの引張強度の変化率85.2%を下回る71.8%となり、好ましい配合量とは言えない。
また、Biの添加量が0.5質量%以上であるサンプル4~11においては、Biが添加されておらず、Agが添加されているサンプル1に対して、500時間のエージング処理の場合、該サンプル1以上の引張強度を表している。更にBiの添加量が1.0質量%から3.0質量%であるサンプル5~8においては、強度変化率が98%以上であり、500時間エージング後の引張強度の変化率が極めて少ないことがわかる。
従って、サンプル4~11においては、Agを使用しないことからコストダウンを図ることができるうえ、引張強度の向上の効果を奏する。
σ(%)=(L-Lo)/Lo×100
そして、種々の形状に加工された本発明の鉛フリーはんだ合金を用いてはんだ接合したはんだ接合部も本発明の対象である。
Claims (8)
- Snが76.0~99.5質量%、Cuが0.1~2.0質量%、Niが0.01~0.5質量%、Biが0.1~5.0質量%、及び不可避不純物を含有することを特徴とする鉛フリーはんだ合金。
- Sbが0.1~5.0質量%、Inが0.1~10.0質量%、Geが0.001~1.0質量%、及びGaが0.001~1.0質量%から選択される1種又は2種以上添加したことを特徴とする請求項1記載の鉛フリーはんだ合金。
- Biを0.5質量%~4質量%含有することを特徴とする請求項1又は2に記載の鉛フリーはんだ合金。
- Biを1質量%~3質量%含有することを特徴とする請求項1から請求項3の何れかに記載の鉛フリーはんだ合金。
- Geを0.001質量%~0.1質量%含有することを特徴とする請求項1から4の何れかに記載の鉛フリーはんだ合金。
- Inを0.1質量%~6質量%含有することを特徴とする請求項1から5の何れかに記載の鉛フリーはんだ合金。
- P、Co、Ti、Al、Agのうち、少なくとも1つを更に含有することを特徴とする請求項1から請求項6に記載の鉛フリーはんだ合金。
- 請求項1から請求項7の何れかに記載の鉛フリーはんだ合金を用いることを特徴とするはんだ接合部。
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RU2016146520A RU2662176C2 (ru) | 2014-04-30 | 2015-04-28 | Бессвинцовый припой |
MX2016014012A MX2016014012A (es) | 2014-04-30 | 2015-04-28 | Aleacion de soldadura libre de plomo. |
AU2015254179A AU2015254179B2 (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
BR122021001612-7A BR122021001612B1 (pt) | 2014-04-30 | 2015-04-28 | Liga de solda isenta de chumbo e isenta de prata, e junta soldada que utiliza a mesma |
EP15785689.9A EP3138658B1 (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
CA2946994A CA2946994C (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
KR1020167033604A KR20160147996A (ko) | 2014-04-30 | 2015-04-28 | 무연솔더합금 |
CN202111526384.7A CN114161023A (zh) | 2014-04-30 | 2015-04-28 | 无铅焊料合金 |
EP20170413.7A EP3708292A1 (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
MYPI2016001916A MY188657A (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
US14/901,638 US10286497B2 (en) | 2014-04-30 | 2015-04-28 | Lead-free solder alloy |
CN201580001155.XA CN105339131A (zh) | 2014-04-30 | 2015-04-28 | 无铅焊料合金 |
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JP2015524557A JP5872114B1 (ja) | 2014-04-30 | 2015-04-28 | 鉛フリーはんだ合金 |
PH12016502152A PH12016502152B1 (en) | 2014-04-30 | 2016-10-27 | Lead-free solder alloy |
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