WO2006131979A1 - 無電解Niめっき部のはんだ付け方法 - Google Patents
無電解Niめっき部のはんだ付け方法 Download PDFInfo
- Publication number
- WO2006131979A1 WO2006131979A1 PCT/JP2005/010660 JP2005010660W WO2006131979A1 WO 2006131979 A1 WO2006131979 A1 WO 2006131979A1 JP 2005010660 W JP2005010660 W JP 2005010660W WO 2006131979 A1 WO2006131979 A1 WO 2006131979A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- electroless
- solder
- mass
- lead
- soldering
- Prior art date
Links
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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/34—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
- H05K3/3457—Solder materials or compositions; Methods of application thereof
- H05K3/3463—Solder compositions in relation to features of the printed circuit board or the mounting process
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/10—Details of components or other objects attached to or integrated in a printed circuit board
- H05K2201/10613—Details of electrical connections of non-printed components, e.g. special leads
- H05K2201/10621—Components characterised by their electrical contacts
- H05K2201/10734—Ball grid array [BGA]; Bump grid array
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/072—Electroless plating, e.g. finish plating or initial plating
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
Definitions
- the present invention relates to a soldering method for improving joint strength by performing soldering on a portion subjected to electroless Ni plating with lead-free solder.
- Cu is used for a soldering portion of an electronic device. Since Cu is easily wetted by molten solder, there are few soldering defects such as voids when soldering. However, if the soldering part of Cu, for example, the electrode of an electronic component such as a BGA substrate, is left in the atmosphere for a long time after the manufacture of the electronic component, the Cu surface will be exposed to atmospheric oxygen. It is oxidized or sulfurized with the exhaust gas of automobiles using fossil fuel or the combustion gas of heating with burning fossil fuel. As a result of such acid or sulfur, if the Cu surface is covered with oxides or sulfides, the molten solder becomes difficult to wet during soldering, causing the above-mentioned poor soldering. End up.
- Methods for applying Ni plating to the Cu surface include an electrolytic plating method and an electroless plating method.
- the electrolytic plating method In the electrolytic plating method, a cathode and an anode are placed in an electrolytic solution, and a metal plating layer is formed on the cathode surface by an electrolytic reaction.
- the electrolytic plating method has problems such as special wiring for the purpose of conduction to the plating part, restrictions on the electrolytic current density, corrosion of the metal part in the plating equipment, and the use of a soluble anode as the anode.
- the deposition rate of Ni which can be reduced by force, was slow, that there were few deposits at locations far from the anode and in the recesses, and that almost no metal was deposited on the back of the cathode.
- the electroless plating method simply immerses the material in the plating solution and can obtain a uniform Ni plating thickness regardless of the type and shape of the material without conducting electricity.
- electroless plating is often used for Ni plating on the electrodes of electronic equipment.
- the plating solution used for electroless Ni plating is a Ni-P plating solution that combines nickel sulfate as the Ni source and sodium hypophosphite as the reducing agent to keep the pH of the plating solution constant.
- sodium hydroxide is used. Therefore, the electroless Ni plating having a thickness of about 0.5 to 10 / ⁇ ⁇ obtained with such an M-P plating solution usually contains about 2 to 15% by mass of P.
- solder bumps are formed in advance on the electrodes, and when mounting the BGA board on a printed board, the solder bumps are melted to print the BGA board and the printed board. Make sure to solder the board.
- first apply adhesive flux to the electrodes of the BGA substrate mount a solder ball on it, heat the BGA substrate in a reflow furnace, and then solder it. Melt the ball. The molten solder balls are wetted and soldered to the electrodes on the BGA board, and solder bumps are formed on the electrodes.
- the electroless Ni plating containing P is applied to the BGA electrode as described above.
- the flash plating thinness improves the familiarity with the solder on the electroless Ni plating. Therefore, the molten solder ball becomes wetted with the electrode without causing poor soldering.
- solder used to form solder bumps on BGA substrates has been Pb-Sn solder.
- Pb-Sn solder has a composition near the eutectic, that is, when Sn is around 63% by mass, the melting point is relatively low at 183 ° C, so heating during solder bump formation in a reflow furnace and subsequent BGA substrate Heating during soldering between PCB and printed circuit board has little effect on the BGA board and the elements inside BGA.
- Pb-Sn solder is not preferred because Pb is harmful to the environment!
- Lead-free solder is mainly composed of Sn. Lead-free solder is also used for soldering to electroless Ni-plated parts. It is used.
- Patent Document 1 when lead-free soldering is used for the electroless Ni-plated part, the adhesion strength is reduced and the Ni plating layer is dissolved and lost when the reflow is repeated. Electroless gold plating as the second metal plating after electroless Ni plating on the electrode, because the conventional Au flash plating has a large adhesion thickness and the adhesion strength is not sufficient. It is disclosed that the thickness is 0.005 to 0.04 i um.
- Patent Document 1 Japanese Patent Laid-Open No. 14-327279
- the present inventors have intensively studied the cause of easy peeling when an electroless Ni-plated portion is soldered with lead-free solder.
- the Sn-based lead-free solder contains a large amount of Sn, and the soldering temperature is higher than that of Pb-Sn solder, so a large amount of Ni in electroless Ni plating and a large amount of lead-free solder.
- a SnNi intermetallic compound layer that reacts with Sn and has brittle properties grows thick.
- M escapes from the surface of the electroless Ni plating, and a concentrated layer with a large amount of P is formed on the surface of the electroless Ni.
- the concentrated P layer remaining on this surface is also brittle, and coupled with the growth of the large SnNi reaction layer, the soldered part becomes even more brittle and easy to peel off. is there.
- FIG. 1 is an electron micrograph of a conventional solder joint showing the above-described state.
- the surface of the Cu electrode of a BGA substrate (not shown) is applied by an electroless plating method.
- Ni plating layer 1 is provided.
- solder bump 5 is formed by soldering with Sn-4Ag-0.5Cu lead-free solder solder ball on Ni plating layer 1
- solder bump 6 A thickly grown SnNi intermetallic compound layer 6 is formed, and an electroless Ni plating force M is released between the intermetallic compound layer 6 and the electroless Ni plating layer 1 to generate a large amount of P.
- SnNi intermetallic compounds having brittle properties grow to a thickness of 1 to 2 m.
- the lead-free solder that is soldered to the electroless Ni-plated portion and has such an inhibitory effect is a solid phase rate power mass% or less of P-compound at 250 ° C.
- This P-compound is a compound formed by reacting with components in lead-free solder.
- the present invention was also selected from Sn-PA g-based and Sn-P-Cu-based forces with Sn as the main component, with a loading force of 0.03 to 0.1% by mass added P / S! Soldering an electroless Ni-plated part characterized by improving the joint strength of the soldered part by soldering the soldered part with electroless Ni plating with such lead-free solder Is the method.
- the SnNi intermetallic compound having brittle properties is thinned, and the electroless Ni-plated surface P-concentrated layer can also be thinned. Therefore, according to the present invention, since the bonding strength of the electroless Ni-plated part can be sufficiently increased, the soldered part will be peeled off even if the electronic device is subjected to a large external impact, and reliability is improved. An excellent soldering part can be obtained.
- FIG. 1 is an electron micrograph of a cross section of a solder joint when an electroless Ni-plated part is soldered with P-free lead-free solder in the prior art.
- FIG. 2 is an electron micrograph of a cross section of a solder joint when an electroless Ni-plated part is soldered with lead-free solder to which a large amount of P is added according to the present invention.
- FIG. 3 is a schematic explanatory view showing a state where a solder bump is peeled off at a joint portion with an electrode in a pull strength test.
- FIG. 4 is a schematic explanatory view showing a state where the solder bump itself is broken.
- FIG. 5 is a schematic explanatory view showing a state where the electrode is peeled off together with the substrate.
- solder used in the present invention either Sn-P-Ag or Sn-P-Cu is suitable.
- the expected effects can be expected even with Sn-P-Zn and Sn-P-Sb systems.
- Sn-P-Ag is Sn-P-Ag-Cu alloy, Sn-P-Ag-Cu-Ni alloy, Sn-P-Ag-Sb alloy, Sn-P-Ag-Ni alloy, Sn -P-Ag-In alloy, Sn-P-Ag-Bi alloy, Sn-P-Ag-Bi-In alloy, etc.
- Sn-P-Cu type is Sn-P-Cu-Ni alloy, Sn-P P-Cu-In alloy, Sn-P-Cu-Bi alloy, Sn-P-Cu-1n-Bi alloy, etc.
- Sn-P-Zn series is Sn-P-Zn-Ni alloy, Sn-P -Zn-Ag alloy, Sn-P-Zn-Sb alloy, Sn-P-Zn
- the lead-free solder used in the present invention has a liquidus temperature of 250 ° C or higher and a solid phase ratio of P-compound of 0.2 mass% or lower at 250 ° C. In other words, when soldering at 250 ° C using the lead-free solder, even if the compound consisting of P and the component power of lead-free solder is present in the solid state up to about 0.2% by mass, There will be no obstacles.
- FIG. 2 is a micrograph of a cross section of an example of a solder joint when soldering is performed according to the present invention in the examples described later.
- the surface of the electrode is provided with a Ni plating layer 1 applied by electroless plating.
- solder bump 2 is formed by soldering with a lead-free solder ball of Sn-0.03P-4Ag-0.5Cu on Ni plating layer 1, electroless Ni plating layer 1 and solder bump 2
- the growth of the SnNi intermetallic compound layer 3 is suppressed at the joint, and as a result, between the intermetallic compound layer 3 and the electroless Ni plating layer 1, conventionally, the above-described FIG.
- the intermetallic compound layer 3 of SnNi does not grow.
- the presence of layer 4 is as small as possible, and even if the electroless Ni-plated part is soldered with lead-free solder, the joint shows excellent adhesion strength against a large external impact.
- the means for applying electroless Ni plating is not particularly limited, but electroless plating using a reducing agent such as sodium hypophosphite is exemplified as in the prior art. If the plating thickness is the conventional one, usually 0.5-10 ⁇ m is sufficient.
- the lead-free solder used in the present invention is one containing various elements with Sn as a main component, and preferably contains at least 80% by mass of Sn. If the Sn content is less than 80% by mass, wetting of the electroless Ni-plated part will be poor. Sn lead When P added to lead solder is less than 0.03% by mass, SnNi intermetallic compound growth suppression effect and electroless Ni plating surface force Ni do not sufficiently escape, and 0.1 mass by mass. If it exceeds 50%, the solid phase ratio of the P compound in the molten state at 250 ° C will exceed 0.2%, and this will interfere with soldering. Therefore, the amount of P applied should be 0.03 to 0.1 mass%. A preferred lower limit is 0.04% by mass and an upper limit is 0.08% by mass.
- the lead-free solder used in the present invention includes one or more elements selected from Ni, Cr, Fe, Mn, Co, Sb, and Ti having an effect of improving mechanical strength in total 1 You may add below mass%. These elements that have an effect of improving mechanical strength generally have a high melting point, so if adding more than 1% by mass in total, the liquidus temperature of lead-free solder becomes higher and the soldering temperature must be increased. This will cause thermal damage to electronic components.
- the lead-free solder used in the present invention contains a total of 15 masses of one or more elements selected from Ag, Cu, Bi, In, Zn, Ge, and Ga, which are melting point lowering elements. % Or less can be added. Some of these elements, if many added than 15 mass 0/0, excessively lower the solidus temperature, it takes a long time until the molten solder during soldering solidified, the soldering portion Causes cracks. Therefore, the total amount of melting point depressing elements added to the lead-free solder used in the present invention is up to 15% by mass.
- solder alloys used in the present invention Sn-P-Ag alloy, Sn-P-Cu alloy, Sn-P-Ag-Cu alloy, Sn-P- Ag-Sb alloy and Sn-P-Ag-Cu-In (Ni) alloy.
- the preferred composition range in these alloys is Sn: 80% by mass or more, Ni and Sb are 1% by mass or less in total, and Ag, Cu and In are 15% by mass or less in total. Further preferred ranges of alloying elements are summarized as follows.
- solder balls are suitable for forming solder bumps on BGA and CSP substrates.
- a solder ball having a diameter of 0.04 to 1.0 mm is preferable.
- solder balls when forming a solder bump on a BGA substrate or CSP substrate, it is also possible to use solder balls with a diameter of 0.04 to 1.0 mm.
- an electroless Ni-plated BGA substrate with a thickness of 5 ⁇ m is soldered with a solder ball with a diameter of 0.76 mm to form a solder bump.
- the pull strength is taken as the pull strength.
- the pull strength test does not cut from the solder joint portion, that is, most of the cut portion breaks the solder itself or the BGA substrate force.
- the breaking strength at this time is 40-euton (N) or more. This is because when an electronic device such as a mobile phone or a personal computer is dropped from the height of lm, the soldered part of the electronic component incorporated in these electronic devices is subjected to a strong impact. Under the same conditions, the strength of general lead-free solder is about 25N, and the strongest possible joint strength is required. Suppressing delamination at the soldering interface when an electronic device is subjected to a strong impact gives a great degree of freedom to the design of the component or solder composition and significantly improves reliability.
- the present invention is a method for joining solder noves showing a joining strength of 40 N or more.
- BGA substrate electrodes on which electroless Ni plating was applied were soldered using solder balls of lead-free solder alloys having the compositions shown in Table 1. Electroless Ni plating can be performed by conventional methods using nickel sulfate containing nickel sulfate as the Ni source and sodium hypophosphite as the reducing agent. The plating solution was used until the plating layer thickness became 5 ⁇ m.
- a circular electrode 11 is formed on the BGA substrate 10, and its periphery is covered with a resist 12.
- the electrode 11 is soldered with a solder ball having a diameter larger than that of the electrode to form a solder bump 13.
- the solder bump 13 formed on the electrode 11 of the BGA substrate 10 is sandwiched between a pair of clampers 14 and 14 and pulled up at a high speed to peel off the solder bump 13 from the electrode 11, and the pull strength (N) at that time Measure.
- the average pull strength (50 samples) of the lead-free solder used in the present invention was 40 N or more.
- the measurement conditions at this time were as follows.
- Solder ball Diameter 0.76mm Electrode: 0.61mm diameter
- FIG. 4 shows the solder bump 13 in the middle, that is, the solder itself is broken, and this is referred to as B mode.
- B mode the solder joint portion is stronger than the solder bump itself, and is a preferable fracture state.
- Fig. 5 shows the electrode peeled off together with the solder bump, and this is called C mode.
- the C mode is also a preferable peeled state because the solder joint is stronger than the joint between the electrode and the substrate.
- the peel rate (number of samples: 50) is calculated by the following formula, and this value must be 10% or less.
- the peeling rate of the lead-free solder used in the present invention was 10% or less.
- the BGA substrate on which suitable lead-free solder bumps containing 0.03 to 0.1% by mass of P have excellent bonding strength at the joints, and the peel rate is all 10 % Or less and excellent reliability.
- a lead-free solder with a P content of less than 0.03 mass%, or a BGA board that does not contain P at all and is formed of solder bumps with lead-free solder has a low bonding strength and a peeling rate of 60% or more. It was easy to peel off.
- Fig. 2 shows an electron micrograph of the joint when the electroless Ni-plated part is soldered with the preferred solder No. 6 lead-free solder (Sn-0.03P-4Ag-0.5Cu) in Table 1.
- Ni plating 1 is applied to the surface of the Cu electrode on the BGA substrate (not shown) by the electroless method.
- solder bump 2 is formed on the Ni plating with a solder ball of Sn-0.03P-4Ag-0.5Cu lead-free solder, the joint between electroless Ni plating 1 and solder bump 2 S without P SnNi intermetallic compound 3 thinner than SnNi intermetallic compound layer 4 when soldered with n-4Ag-0.5Cu lead-free solder was formed.
- the force described above for the soldering method of the BGA substrate, particularly the electroless Ni-plated electrode, in addition to the BGA substrate is applicable to CSP and MCM that are soldered using lead-free solder balls. It can be applied to any soldered part that has electroless Ni plating.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
- Chemically Coating (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007520005A JP4811403B2 (ja) | 2005-06-10 | 2005-06-10 | 無電解Niめっき部のはんだ付け方法 |
EP05750722A EP1894667A4 (en) | 2005-06-10 | 2005-06-10 | METHOD FOR BRAZING A UNLIMITED NICKEL PART |
US11/921,861 US8887980B2 (en) | 2005-06-10 | 2005-06-10 | Method of soldering portions plated by electroless Ni plating |
PCT/JP2005/010660 WO2006131979A1 (ja) | 2005-06-10 | 2005-06-10 | 無電解Niめっき部のはんだ付け方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2005/010660 WO2006131979A1 (ja) | 2005-06-10 | 2005-06-10 | 無電解Niめっき部のはんだ付け方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2006131979A1 true WO2006131979A1 (ja) | 2006-12-14 |
Family
ID=37498191
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2005/010660 WO2006131979A1 (ja) | 2005-06-10 | 2005-06-10 | 無電解Niめっき部のはんだ付け方法 |
Country Status (4)
Country | Link |
---|---|
US (1) | US8887980B2 (ja) |
EP (1) | EP1894667A4 (ja) |
JP (1) | JP4811403B2 (ja) |
WO (1) | WO2006131979A1 (ja) |
Cited By (6)
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JP2010129664A (ja) * | 2008-11-26 | 2010-06-10 | Fujitsu Ltd | 電子装置及びその製造方法 |
JP2013193092A (ja) * | 2012-03-16 | 2013-09-30 | Panasonic Corp | はんだ材料および実装体 |
JP5349703B1 (ja) * | 2012-07-19 | 2013-11-20 | ハリマ化成株式会社 | はんだ合金、ソルダペーストおよび電子回路基板 |
JP5578301B1 (ja) * | 2013-04-18 | 2014-08-27 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
WO2015019966A1 (ja) * | 2013-08-05 | 2015-02-12 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
US9428674B2 (en) | 2013-03-19 | 2016-08-30 | Nippon A & L Inc. | Copolymer latex for adhesives and adhesive composition |
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CN103299406A (zh) * | 2007-09-21 | 2013-09-11 | 艾格瑞系统有限公司 | 用于改善耐脆性断裂的焊接方法及相关器件 |
US9780055B2 (en) * | 2012-06-30 | 2017-10-03 | Senju Metal Industry Co., Ltd. | Lead-free solder ball |
KR101514529B1 (ko) * | 2013-07-09 | 2015-04-22 | 삼성전기주식회사 | 인쇄회로기판 및 그 제조방법 |
JP6369994B2 (ja) * | 2015-09-02 | 2018-08-08 | 田中電子工業株式会社 | ボールボンディング用銅合金細線 |
CN111052510B (zh) * | 2018-03-16 | 2021-05-25 | 富士电机株式会社 | 半导体装置 |
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- 2005-06-10 US US11/921,861 patent/US8887980B2/en active Active
- 2005-06-10 WO PCT/JP2005/010660 patent/WO2006131979A1/ja active Application Filing
- 2005-06-10 JP JP2007520005A patent/JP4811403B2/ja active Active
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Cited By (11)
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JP2010129664A (ja) * | 2008-11-26 | 2010-06-10 | Fujitsu Ltd | 電子装置及びその製造方法 |
JP2013193092A (ja) * | 2012-03-16 | 2013-09-30 | Panasonic Corp | はんだ材料および実装体 |
JP5349703B1 (ja) * | 2012-07-19 | 2013-11-20 | ハリマ化成株式会社 | はんだ合金、ソルダペーストおよび電子回路基板 |
WO2014013632A1 (ja) * | 2012-07-19 | 2014-01-23 | ハリマ化成株式会社 | はんだ合金、ソルダペーストおよび電子回路基板 |
KR101538293B1 (ko) * | 2012-07-19 | 2015-07-20 | 하리마카세이 가부시기가이샤 | 땜납 합금, 솔더 페이스트 및 전자 회로 기판 |
US9445508B2 (en) | 2012-07-19 | 2016-09-13 | Harima Chemicals, Incorporated | Solder alloy, solder paste, and electronic circuit board |
US9428674B2 (en) | 2013-03-19 | 2016-08-30 | Nippon A & L Inc. | Copolymer latex for adhesives and adhesive composition |
JP5578301B1 (ja) * | 2013-04-18 | 2014-08-27 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
WO2014170994A1 (ja) * | 2013-04-18 | 2014-10-23 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
WO2015019966A1 (ja) * | 2013-08-05 | 2015-02-12 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
JP5679094B1 (ja) * | 2013-08-05 | 2015-03-04 | 千住金属工業株式会社 | 鉛フリーはんだ合金 |
Also Published As
Publication number | Publication date |
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EP1894667A1 (en) | 2008-03-05 |
US20090218387A1 (en) | 2009-09-03 |
JPWO2006131979A1 (ja) | 2009-01-08 |
US8887980B2 (en) | 2014-11-18 |
EP1894667A4 (en) | 2009-12-02 |
JP4811403B2 (ja) | 2011-11-09 |
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