WO2009104338A1 - Etain, alliage à souder, et dispositif à semi-conducteurs - Google Patents

Etain, alliage à souder, et dispositif à semi-conducteurs Download PDF

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Publication number
WO2009104338A1
WO2009104338A1 PCT/JP2008/073145 JP2008073145W WO2009104338A1 WO 2009104338 A1 WO2009104338 A1 WO 2009104338A1 JP 2008073145 W JP2008073145 W JP 2008073145W WO 2009104338 A1 WO2009104338 A1 WO 2009104338A1
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WO
WIPO (PCT)
Prior art keywords
tin
solder alloy
molten
acid
lead
Prior art date
Application number
PCT/JP2008/073145
Other languages
English (en)
Japanese (ja)
Inventor
石川　久雄
正徳 横山
Original Assignee
日本ジョイント株式会社
ホライゾン技術研究所株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日本ジョイント株式会社, ホライゾン技術研究所株式会社 filed Critical 日本ジョイント株式会社
Publication of WO2009104338A1 publication Critical patent/WO2009104338A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B25/00—Obtaining tin
    • C22B25/08—Refining
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40—Making wire or rods for soldering or welding
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • 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

Definitions

  • the present invention relates to a printed circuit board saddle land and a semiconductor package when a mounting member such as a semiconductor package or an electronic device is joined to the printed circuit board or the like using tin or solder for circuit formation.
  • a mounting member such as a semiconductor package or an electronic device is joined to the printed circuit board or the like using tin or solder for circuit formation.
  • it relates to semiconductor devices. More specifically, it is far more flexible and stretchable as a physical and mechanical property than current tin or solder alloys, has high toughness, has low viscosity in the molten state, and has good wettability.
  • tin or solder alloy The amount of tin or solder alloy covered is unlikely to become over volume, and tin or solder alloy bridges into adjacent lead circuit parts at narrow intervals.
  • tin or a solder alloy that enables joining with high joining reliability of the joined micro-joint part, and a printed circuit board / semiconductor package that is joined using the tin or solder alloy And a technology for the same.
  • the tin or solder alloy side used for the bonding is also required to have a bonding strength, in particular, a bonding area of the electronic device and electronic component leads and a high reliability of the bonding portion due to the finer pitch.
  • Patent Document 3 Japanese Patent Laid-Open No. 5-0 2 8 6 (Patent 3 0 2 7 4 4 1)
  • Patent Document 2 JP-A-11 1 7 7 3 6 6 (Patent 3 2 9 6 2 8 9)
  • Patent Document 3 Japanese Patent Laid-Open No. 9-9 4 6 8 8 (Patent 3 2 9 9 0 9 1)
  • the present invention provides a mounting member such as a printed circuit board, a semiconductor package, and an electronic element using tin, a tin ship solder alloy, a lead-free solder alloy, etc., which are currently in practical use,
  • a mounting member such as a printed circuit board, a semiconductor package, and an electronic element using tin, a tin ship solder alloy, a lead-free solder alloy, etc., which are currently in practical use
  • mounting members such as printed circuit boards, semiconductor packages, and electronic devices for the purpose of solving the problem of continuity failure due to time-dependent fatigue fracture due to repeated heat cycles of the above-mentioned joints)
  • mounting members such as printed circuit boards, semiconductor packages, and electronic devices for the purpose of solving the problem of continuity failure due to time-dependent fatigue fracture due to repeated heat cycles of the above-mentioned joints
  • a printed circuit board, a semiconductor package, a mounting member such as an electronic element, and a semiconductor device including these electronic components are provided.
  • the present invention relates to an organic compound having at least a carbocycle group (-COOH) which is soluble in an oil-based solvent at a liquid temperature of 180 to 300 and is stable in terms of molecular structure.
  • a solution containing 80% by weight, ordinary tin, tin-lead solder alloy, lead-free solder alloy, which is currently widely used that is, molten tin, or tin as a main component, lead, silver , Copper, zinc, bismuth, antimony, nickel, germanium, or a molten solder alloy containing one or more metals and stir vigorously, in the molten tin or molten solder alloy
  • it has unprecedented physical properties, that is, it has a very low melt viscosity and good wettability, and it is flexible and excellent in elongation and toughness as physical and mechanical properties.
  • Bonded parts especially lead widths of 0.05 mm or less , Tin or solder alloy that enables highly reliable joining of fine joints in microcircuits with a lead interval (pitch) of 0.1 mm or less, and solder joint reliability of minute parts by using it TECHNICAL FIELD
  • the present invention relates to a semiconductor device including a mounting member such as a Z circuit package / electronic element, and its technology.
  • an organic compound having at least a carbonyl group that is dissolved in an oil-based solvent having a liquid temperature of 180 to 300,000 and stable in molecular structure is used in the present invention.
  • Methanoic acid formic acid
  • ethanoic acid succinic acid
  • propionic acid butyric acid, isobutyric acid, ⁇ -methyl-j8-oxybutyric acid, valeric acid, isovaleric acid, active valeric acid, piperic acid (trimethylacetic acid)
  • Force bromic acid 2-ethylbutyric acid, caproic acid, force prillic acid, 2-ethyl hexyl acid, nonanoic acid, force puric acid, undecanoic acid, myristic acid, palmitic acid, margaric acid, stearic acid, oleic acid, Linoleic acid, linolenic acid, arachidic acid, arachidonic acid, pehenic acid,
  • an organic compound having a low boiling point it can be used at a high pressure, but it is not preferred in practice.
  • industrially more suitable for practical use are, for example, oxalic fatty acids having 13 to 20 carbon atoms, that is, myristic acid, palmitic acid, margaric acid, stearic acid, oleic acid, linol. Acids, linolenic acid, arachidic acid, arachidonic acid, etc., which have a great effect in accordance with the object of the present invention and are useful.
  • ffl fatty acids can be used even with carbon numbers of 12 or less, they have water absorbency and are not so preferred because they are used at high temperatures.
  • organic fatty acids having 21 or more carbon atoms can be used, they have a high melting point, poor permeability and are difficult to handle, and the antifouling effect of the treated tin or solder alloy is somewhat insufficient.
  • panolemitic acid having 16 carbon atoms and stearic acid having 18 carbon atoms which are both industrially produced and used in large quantities, are most suitable.
  • the molten tin or molten solder is contained in a solution having a liquid temperature of 180 to 30, which is composed of an oil-based solvent that is stable in a low temperature range of 80 to 80% by weight and the balance from 180 to 350.
  • a solution having a liquid temperature of 180 to 30, which is composed of an oil-based solvent that is stable in a low temperature range of 80 to 80% by weight and the balance from 180 to 350 By immersing and vigorously stirring the alloy, the fine tin or impure metal present inside the molten tin or molten solder alloy is removed, and unprecedented physical, mechanical and chemical properties, especially flexible and stretched, 3 ⁇ 49 rich, low viscosity when melted (apparently there is also a “smooth” feeling compared to conventional tin and solder alloys), excellent wettability and good clean tin or solder An alloy is obtained.
  • the liquid temperature is determined by the melting point of the molten tin or molten solder alloy to be used, and is dissolved in an oil-based solvent having a liquid temperature of 180 to 300 3 ⁇ 4 at least in a high temperature region above the melting point and stable in molecular structure. It is necessary to vigorously agitate the molten tin or molten solder alloy with an organic compound solution having at least a carbon tomb (-COOH).
  • the upper limit temperature is about 300 ° from the viewpoints of smoke and odor and energy saving, and is preferably about 270 ° C. or higher than the melting point of the tin or solder alloy used.
  • a solvent that is stable in the high temperature range any of mineral oil, vegetable oil, and synthetic oil may be used as long as it dissolves the organic compound. However, stability, safety, economy, and handling are particularly good. In this respect, ester synthetic oil is most suitable.
  • the purpose and reason for using a solvent that is stable at high temperature is to lower the viscosity of the liquid and to perform more uniform agitation treatment, and to control the high temperature smoke generation and odor of the organic compound. .
  • the stirring method is as follows. Put the above # ⁇ compound and a high-temperature stable solvent in a stainless steel container equipped with a heating device, and stir using a normal batch-type stainless steel impeller stirrer while heating to a specified temperature.
  • the solution may be uniformly made into a solution, and tin or solder alloy solution previously melted in a separate tank may be poured into the solution while vigorously stirring. Stirring can efficiently remove oxides and impurities present in tin or solder alloy in a short time using a static mixer.
  • 3 ⁇ 4 IS verification example of the present invention mainly includes a tin 'silver' copper-based alloy and a commercially available alloy obtained by adding nickel and germanium thereto, and a commercially available alloy obtained by adding nickel and silver to a tin-zinc alloy.
  • the above-mentioned organic compound and the ester-saponified oil solution of the present invention were immersed and stirred, and the effect was verified.
  • Other lead-free solder alloys, pure tin, and tin-lead solder alloys It is estimated that the same effect can be obtained by applying the processing. This is because there are oxides and impurities including tin oxide in common with the examples.
  • refined pure tin itself an industrial raw material, contains a very small amount of acid with an oxygen concentration of 80 to several 100 ppm. Since commercially available pure tin and various solder alloys are generally used as raw materials, the same very small amount of oxide exists in a molecular or ultrafine granular state.
  • the stirring time depends on the amount of tin or solder alloy added, the structure of the stirrer, and the stirring conditions, but generally strong stirring for about 10 to 60 minutes is sufficient. Then, using the specific gravity difference, the lower layer tin or solder alloy from which the above oxides and most of the impurities have been separated and removed from the bottom of the reaction tank and cleaned is taken out in a molten state, and the storage tank of the molten tin or molten soldering device It is poured into a tin or soldering tank that is circulated into a tin or soldering tank and poured into a vertical mold, and then solidified, and the ingot is poured into a normal molten tin or solder storage tank or tin or soldering device.
  • flux When flux is used for tin / solder alloy coating / joining, flux residue and reaction decomposition decomposition impurities are mixed in the molten tin or molten solder alloy.
  • the decomposition products also move naturally to the upper organic compound layer due to the above specific gravity difference, and are separated from the molten tin or molten solder alloy.
  • the same effect can be obtained even when the tin or solder alloy of the present invention is used as a powder for tin or solder-coated solder joint. Furthermore, even if the tin or solder alloy of the present invention is processed and used as a solder cream, or processed into a solder ball and used for forming a bump for BG ⁇ or CSP, the above-mentioned physical properties are maintained. So the same effect can be obtained.
  • the viscosity at the time of melting of the tin or solder alloy of the present invention is simply that the tin or solder coating and over-volume and bridge-over are not applied to the minute parts of minute circuit printed circuits and electronic elements and electronic parts. In addition to enabling bonding, for example, it is possible to manufacture high-precision fine solder balls with a diameter of 80 ⁇ or less used for BGA ⁇ CSP bumps.
  • FIG. 1 is an example of a cross-sectional crystal structure of the solder alloy of the examples and comparative examples of the present invention.
  • 1a is Example 1
  • 1b is Comparative Example 1
  • 1c is Example 2
  • 1d is Comparative Example 2.
  • FIG. 2 shows the application of the lead-free solder alloy of Example 2 of the present invention and conventional comparative example 2 to a narrow pitch printed circuit board having a very small width of 20 ⁇ m and a distance of 60 ⁇ m between adjacent circuits.
  • 2a is an external view of Example 2 taken from the top, and 2b is taken from the top.
  • An appearance photograph of Comparative Example 2 and 2c are photographs obtained by enlarging the above 2a from an oblique upper part.
  • FIG. 3] 3a and 3b are photographs obtained by enlarging the cross section of [Fig. 2] 2a.
  • FIG. 4 Industry in which lead-free solder alloy (Example 2) according to the present invention is directly applied to the formation of solder bumps on a silicon wafer plate having a circuit width of 80 ⁇ m and an interval of 32.0 ⁇ m between adjacent circuits. It is the photograph which enlargedly photographed the appearance of the state of soldering of a typical application example.
  • FIG. 5 is a graph showing the relationship between the temperature and viscosity of a lead-free solder alloy of the present invention (Example 2) and a conventional lead-free solder (Comparative Example 2).
  • FIG. 6 A diagram showing an example of thermal analysis results of the lead-free solder alloy of the present invention and a conventional lead-free solder, 6a is Example 2 and 6b is Example 2 of Comparative Example 2. .
  • Comparative Example 1 a commercially available lead-free solder alloy consisting of 2.5% by weight of silver, 0.5% by weight of copper, and the balance tin was used.
  • Example 1 of the present invention 2.5% by weight of silver having the same composition as Comparative Example 1 above, copper
  • a lead-free solder alloy consisting of 0.5% by weight and the remaining tin is melted in advance and added dropwise to a solution of stearic acid and 50% by weight of the remaining ester synthesis solution at a temperature of 260 ° C. While stirring vigorously with a rotary agitator with a stainless impeller installed in two stages, the cleaned lead-free solder is taken out from the bottom of the treatment tank 30 minutes later and used for evaluation tests. did.
  • Comparative Example 2 a lead-free solder alloy composed of 2.5% by weight of silver, 0.5% by weight of copper, 0.1% by weight of Eckenole, 0.05% by weight of germanium, and the balance tin It was used.
  • Example 2 2.5% by weight of silver having the same composition as that of Comparative Example 2 was used.
  • a lead-free solder alloy consisting of 0.05% by weight of germanium and the balance of tin is melted in advance, and a small amount is shifted into the solution at a liquid temperature of 25% consisting of 40% by weight of palmitic acid and the balance of ester. While dripping, the cleaned lead-free solder is taken out from the bottom of the treatment tank after 60 minutes while stirring vigorously with a rotary impeller with a stainless steel impeller installed in two stages. Provided.
  • Example 3 is composed of the following composition of Comparative Example 3 and containing 8.0% by weight of nickel, 0.05% by weight of nickel, 1.0% by weight of silver, and the balance tin.
  • a lead-free solder alloy is melted in advance, and stainless steel is installed in two stages at the top and bottom while dripping slightly into the solution at a liquid temperature of 280 consisting of 40% by weight palmitic acid, 20% by weight stearic acid and the remaining ester. While vigorously stirring with a rotary impeller equipped with a less impeller, the cleaned bell-free solder was taken out from the bottom of the treatment tank 20 minutes later and subjected to an evaluation test.
  • Viscosity was measured by placing each solder separately in an alumina crucible, dissolving in an argon atmosphere, gradually decreasing the temperature from 300 to the freezing point using an alumina vibrating piece type viscometer.
  • the results are shown in [Table 1] below.
  • the cleaned lead-free solder alloy of the example has a physical mechanical property that is 1.5 times or more larger than the comparative example, and is less likely to break. It suggests. Also, it is overwhelmingly easy to wet even with solder wettability, its viscosity in the molten state (viscosity) is much lower than that of comparative examples, and it has a low viscosity that is not found in conventional solder alloys. This is because, in the case of the solder internal crystal structure after solidification, in the case of the solder alloy subjected to the processing method of the present invention, the crystal grains are small ([Fig. 1] la, 1 c).
  • Comparative Examples 1 to 3 existed at 70 to 270 ppm, whereas Examples 1 to 3 were all verified to be over 5 ppm and the oxygen concentration was overwhelmingly low. ([Table 1]).
  • the viscosity was measured by gradually decreasing the temperature from 30 to around the freezing point and measured every 5th.
  • the comparative example was from 0.0051 to 0.0067 Pa ⁇ S. Examples are found to have an overwhelmingly low viscosity at 0. 0034 to 0. 0038 P a 'S, which improves “solder wettability” and contributes significantly to the suppression of “over volume” and “bridge bar”. (Fig. 5)).
  • Example 2 the results of analysis with the differential thermal analyzer for Example 2 and Comparative Example 2 showed that the melting point at the time of temperature increase was 217, both of which were almost the same in the vicinity, but the solidification characteristics at the time of temperature decrease were compared.
  • the solidification was completed at 217 to 214 3 ⁇ 4, whereas in Example 2 of the present invention, a part started to solidify at 218 to 215, and even when it dropped to around 204 ° C, it still solidified only about half.
  • the coagulation was finally completed at around 189, which clearly showed a significant difference in physical properties ([Fig. 6] 6a, 6b).
  • the technology of the present invention clearly has excellent physical properties such as high elongation and toughness, low viscosity, and high wettability that are not found in conventional tin or solder alloys.
  • This is an epoch-making technology with high industrial value that makes it possible to manufacture highly reliable electronic components and semiconductor devices without bridging over an extremely narrow pitch circuit junction.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Connection Of Electric Components To Printed Circuits (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne l'étain ou un alliage à souder, qui a des propriétés non conventionnelles, à savoir une très faible viscosité à l'état fondu pour offrir de bonnes propriétés d'étalement par voie humide, qui a d'excellentes propriétés physiques et mécaniques, à savoir une flexibilité, un allongement et une résistance excellents, et qui permet de réaliser un assemblage de soudure dans lequel la fiabilité de l'assemblage au niveau du joint par recouvrement ou assemblage à l'aide d'étain ou d'alliage à souder est élevée, et un composant électronique et un dispositif à semi-conducteurs utilisant l'étain ou l'alliage à souder. De l'étain conventionnel, un alliage à souder à base d'étain et de plomb, un alliage à souder sans plomb, lesquels sont actuellement largement utilisés, c'est-à-dire un étain fondu, ou un alliage à souder fondu composé principalement d'étain et contenant l'un quelconque ou au moins deux des métaux choisis parmi le plomb, l'argent, le cuivre, le zinc, le bismuth, l'antimoine, le nickel, et le germanium est immergé dans une solution contenant 5 à 80 % en poids d'un composé organique contenant au moins un groupe carbonyle (-COOH), qui est soluble dans un solvant à base d'huile ayant une température à l'état liquide allant de 180 °C à 300 °C et qui a une structure moléculaire stable, puis le tout est agité vigoureusement pour éliminer les oxydes et les impuretés présents dans l'étain fondu ou dans l'alliage à souder fondu.
PCT/JP2008/073145 2008-02-22 2008-12-12 Etain, alliage à souder, et dispositif à semi-conducteurs WO2009104338A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008-72364 2008-02-22
JP2008072364A JP4375485B2 (ja) 2008-02-22 2008-02-22 鉛フリーはんだ合金の製造方法及び半導体装置の製造方法

Publications (1)

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WO2009104338A1 true WO2009104338A1 (fr) 2009-08-27

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PCT/JP2008/066018 WO2009104294A1 (fr) 2008-02-22 2008-08-29 Alliage à souder sans plomb et dispositif à semi-conducteurs
PCT/JP2008/073145 WO2009104338A1 (fr) 2008-02-22 2008-12-12 Etain, alliage à souder, et dispositif à semi-conducteurs

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WO (2) WO2009104294A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111009798A (zh) * 2019-12-20 2020-04-14 中国科学院电工研究所 一种多芯铁基超导接头及其制备方法
TWI760476B (zh) * 2017-04-10 2022-04-11 比利時商梅泰洛比利時公司 用於製造粗製焊料之改良製法

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KR101686312B1 (ko) * 2012-04-17 2016-12-13 가부시키가이샤 다니구로구미 땜납 범프 및 그 형성방법과 땜납 범프를 구비한 기판 및 그 제조방법
CN107245602B (zh) * 2017-06-09 2019-03-22 升贸科技股份有限公司 无铅锡合金及使用其的镀锡铜线
JP7026907B2 (ja) * 2020-04-08 2022-03-01 石川技研株式会社 はんだ製品の製造方法、プリント回路板、線材、フレキシブルプリント基板および電子部品
SG11202111303WA (en) * 2019-04-09 2021-11-29 Ishikawa Technology Laboratory Co Ltd Method for manufacturing solder product, solder, soldered component, solder product, printed wiring board, printed circuit board, wire, soldered product, flexible printed board, electronic component, method for manufacturing tin article, method for manufacturing tin intermediate product, tin article, tin intermediate product, and conductive member
TWI799696B (zh) * 2020-03-12 2023-04-21 石川久雄 焊料製品之製造方法、焊料、焊接部件、焊料製品、印刷線路板、印刷電路板、線材、焊接製品、可撓印刷電路板、電子部件、錫成品之製造方法、錫半成品之製造方法、錫成品、錫半成品及導電構件

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JPS5040103B1 (fr) * 1969-10-08 1975-12-22
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JPH0563349A (ja) * 1991-09-04 1993-03-12 Sony Corp 噴流半田槽
JP2006045676A (ja) * 2004-08-03 2006-02-16 Wc Heraeus Gmbh 微細ろう粉末を製造する際に、合金成分を精製しそして均一分布させ並びに軟ろうから不所望の反応生成物およびスラッジを除く方法
JP2007532321A (ja) * 2004-04-16 2007-11-15 ピー．ケイ メタル，インコーポレイティド はんだ付け方法および装置

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JPS5040103B1 (fr) * 1969-10-08 1975-12-22
JPH02118003A (ja) * 1988-10-26 1990-05-02 Mitsubishi Metal Corp はんだ合金微粉末の製造方法
JPH0563349A (ja) * 1991-09-04 1993-03-12 Sony Corp 噴流半田槽
JP2007532321A (ja) * 2004-04-16 2007-11-15 ピー．ケイ メタル，インコーポレイティド はんだ付け方法および装置
JP2006045676A (ja) * 2004-08-03 2006-02-16 Wc Heraeus Gmbh 微細ろう粉末を製造する際に、合金成分を精製しそして均一分布させ並びに軟ろうから不所望の反応生成物およびスラッジを除く方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI760476B (zh) * 2017-04-10 2022-04-11 比利時商梅泰洛比利時公司 用於製造粗製焊料之改良製法
CN111009798A (zh) * 2019-12-20 2020-04-14 中国科学院电工研究所 一种多芯铁基超导接头及其制备方法

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WO2009104294A1 (fr) 2009-08-27
JP2009197315A (ja) 2009-09-03
JP4375485B2 (ja) 2009-12-02

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