JP2013231228A - めっき部材、コネクタ用めっき端子、めっき部材の製造方法、及びコネクタ用めっき端子の製造方法 - Google Patents
めっき部材、コネクタ用めっき端子、めっき部材の製造方法、及びコネクタ用めっき端子の製造方法 Download PDFInfo
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- JP2013231228A JP2013231228A JP2012188457A JP2012188457A JP2013231228A JP 2013231228 A JP2013231228 A JP 2013231228A JP 2012188457 A JP2012188457 A JP 2012188457A JP 2012188457 A JP2012188457 A JP 2012188457A JP 2013231228 A JP2013231228 A JP 2013231228A
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- Prior art keywords
- silver
- layer
- tin
- plating
- plating layer
- Prior art date
- Legal status (The legal status 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 status listed.)
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/615—Microstructure of the layers, e.g. mixed structure
- C25D5/617—Crystalline layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
【解決手段】銅又は銅合金よりなる母材1の表面にスズめっき層31と銀めっき層21とを交互に積層して最表面を銀めっき層22とした後に、加熱を行うことで、母材の表面を被覆する銀−スズ合金層4と、銀−スズ合金層を被覆し、最表面に露出する銀被覆層5とを同時に形成し、めっき部材を得る。
【選択図】図1
Description
本発明にかかるめっき部材は、図1の(b)及び(d)に示すように、銅又は銅合金からなる母材1の表面が、銀−スズ合金層4により被覆され、さらにその表面が銀被覆層5により被覆されたものである。
本発明にかかるめっき部材の製造方法においては、まず銅、銅合金又はそれらにニッケル下地めっきを施した母材の表面に、銀めっき層とスズめっき層が交互に積層された、複数のめっき層よりなる積層構造を作成する。次に、それを加熱することで、銀−スズ合金層と、銀−スズ合金層を被覆して最表面に露出する銀被覆層とを同時に形成する。上記積層構造においては、最表層がスズめっき層ではなく、銀めっき層とされる。
清浄な銅基板の表面に、厚さ0.5μmのニッケル下地めっきを形成した。この表面に、目標値で厚さ1μmの軟質銀めっき層を形成した。その上に、目標値で厚さ1μmのスズめっき層を形成し、さらにその上に厚さ2μmの軟質銀めっき層を形成した。この材料を大気中において200℃で60分間加熱した。これを実施例1にかかるめっき部材とした。軟質銀めっき層及びスズめっき層の具体的な形成条件は以下のとおりであった。
・Ag濃度45g/Lのめっき浴を使用
・操作温度:30℃
・電流密度:5ASD(2.5μm/分)
・めっき時間: 20〜30秒(めっき層の厚さ:1μm)、40〜60秒(めっき層の厚さ:2μm)
・Sn濃度60g/Lのめっき浴を使用
・添加剤:40mL/L
・操作温度:40℃
・電流密度:5ASD(2.5μm/分)
・めっき時間:20〜30秒(めっき層の厚さ:1μm)
実施例1と同様に、ニッケルめっきを施した銅基板の表面に目標値で厚さ1μmの軟質銀めっき層、厚さ1μmのスズめっき層、厚さ2μmの軟質銀めっき層をこの順に積層しためっき部材を、290℃で1分間加熱した。
[実施例3]
ニッケルめっきを施した銅基板の表面に厚さ1.5μmの軟質銀めっき層、厚さ1.0μmのスズめっき層、厚さ2.5μmの軟質銀めっき層をこの順に積層しためっき部材を、290℃で1分間加熱した。
実施例1と同様のニッケル下地めっきを形成した銅基板に、厚さ8μmの軟質銀めっき層を形成し、比較例1にかかるめっき部材とした。
実施例1と同様のニッケル下地めっきを形成した銅基板に、厚さ8μmの銀−スズ合金層を形成し、比較例2にかかるめっき部材とした。銀−スズ合金層は、銀−スズ合金めっき液(大和化成社製、商品名「ダイシンスター」)を使用して形成した。Ag濃度は35g/Lとし、温度25℃、電流密度1〜2ASD(0.3μm/分)の条件で、30分程度めっきを行った。
[比較例3]
実施例1と同様のニッケル下地めっきを形成した銅基板に、厚さ8μmの硬質銀めっき層を作成し、比較例1にかかるめっき部材とした。
(層構造の評価)
実施例1〜3のめっき部材において、加熱前及び加熱後の層構造を評価するため、集束イオンビーム−走査イオン顕微鏡(FIB−SIM)を用いて、加熱前及び加熱後の実施例にかかるめっき部材の断面の観察を行った。
実施例1〜3にかかるめっき部材の加熱後における構成層の化学組成を調べるため、微小領域に対するオージェ電子分光(AES)測定を行い、めっき層中における元素の存在量比を見積もった。
実施例1及び比較例1にかかるめっき部材の銀めっき層について、硬さの指標として、銀微結晶の平均粒径を見積もった。見積もりは、得られたFIB−SIM像を解析することによって行った。
実施例1及び各比較例のめっき部材について、動摩擦係数を評価した。つまり、平板型のめっき部材と半径3mmのエンボス形のめっき部材を鉛直方向に接触させて保持し、ピエゾアクチュエータを用いて鉛直方向に5Nの荷重を印加しながら、10mm/min.の速度でエンボス型のメッキ部材を水平方向に引張り、ロードセルを使用して接点部に働く摩擦力を測定した。摩擦力を荷重で割った値を摩擦係数とした。
加熱環境下での端子の使用に伴う接触抵抗の上昇の程度を見積もるため、荷重−抵抗特性の評価を行った。実施例1及び各比較例にかかるめっき部材について、接触抵抗を四端子法によって測定した。この際、開放電圧を20mV、通電電流を10mA、荷重印加速度を0.1mm/min.とし、0〜40Nの荷重を往復で印加した。また、電極として、板状のめっき部材と半径3mmのエンボス形のめっき部材を使用した。この荷重−抵抗特性の評価を、作成直後のめっき部材に対して行った。次いで、めっき部材を大気中150℃で120時間放置し(以下、この条件を「高温放置」と称する場合がある)、放置後のめっき部材に対しても室温に放冷後、同様に荷重−抵抗特性の評価を行った。さらに、荷重10Nにおける接触抵抗値について、初期(高温放置前)から高温放置後に上昇した値を、抵抗上昇値とした。比較例1〜3のめっき部材についても、同様の測定を行った。ここで、10Nという荷重は、一般的な大電流用端子において接点部に及ぼされる荷重を近似した値である。
本発明にかかるめっき部材の硬さが、初期値としてどの程度であり、高温放置によってどのように変化するのかを調べるための測定を行った。実施例1にかかるめっき部材について、大気中150℃で120時間放置する前と後の硬さを、ビッカース硬さ計を用いて測定した。比較例1〜3のめっき部材についても、同様の測定を行った。
(加熱前のめっき部材の層構造の評価)
図3(a)に、実施例1にかかるめっき部材の加熱前の断面のFIB−SIM像を示す。めっき層が、下から1.9μm、1.9μm、2.9μmの厚さを有する3層よりなっている。それぞれ、銀めっき層、スズめっき層、銀めっき層に対応するものであり、加熱前においては、合金化等が進行せず、作成した積層構造が維持されている。これらの層の厚さは、上記で過不足なく合金化反応が進行するスズめっき層と銀めっき層の厚さの比に基づいて導出した理想的な各層の厚さの関係にほぼ合致するものである。
加熱した後の実施例1にかかるめっき部材について、断面のFIB−SIM像を図3(b)に示す。断面の層構造の構成は、加熱前と比べて大きく変化している。下から、厚さ1.1μm、3.4μm、1.9μmの層が形成されている。後に示す化学組成の分析結果と合わせて、中層に位置して最も大きな割合を占める厚さ3.4μmの層は、銀−スズ合金層である。最表面の厚さ1.9μmの層は、銀よりなる銀被覆層である。銀−スズ合金層と銀被覆層の間には、明確な界面が形成されている。また、最下層の1.1μmの層は、化学組成分析の結果によると、ニッケル−スズ合金よりなる。ニッケル−スズ合金層と、銀−スズ合金層の間にも、明確な界面が形成されている。界面においてニッケル−スズ合金層と銀−スズ合金層は強固に密着している。
図3(c)は、実施例1のめっき部材について、加熱後に得られた銀被覆層の中の箇所を拡大観察したFIB−SIM像である。これを見ると、銀被覆層が、粗大な結晶粒の集合体よりなっていることが分かる。
表1に、実施例1及び各比較例のめっき部材について、摩擦係数の測定結果を示す。
表2に、実施例1及び最表面に銀−スズ合金が露出した比較例2にかかるめっき部材の高温放置前後の荷重10Nで測定した接触抵抗値と、その上昇値を示す。
高温放置の前後で測定した実施例1のめっき部材についてのビッカース硬さを測定した。1000mNの試験荷重において、初期(高温放置前)のめっき部材では、ビッカース硬さが155Hvであった。
銀めっき層とスズめっき層を最表層を銀めっき層として交互に積層し、加熱することで、銀−スズ合金層と銀被覆層を有するめっき部材が形成されることが明らかになった。
21、22 銀めっき層
31、32 スズめっき層
4 銀−スズ合金層
5 銀被覆層
Claims (14)
- 銅又は銅合金よりなる母材の表面が銀−スズ合金層により覆われ、前記銀−スズ合金層の表面が銀被覆層により覆われ、前記銀被覆層が最表面に露出していることを特徴とするめっき部材。
- 前記母材の表面に接触してニッケル又は銅よりなる下地めっきが形成され、前記下地めっきの表面に前記銀−スズ合金層が形成されていることを特徴とする請求項1に記載のめっき部材。
- 前記銀被覆層は、前記銀−スズ合金層よりも薄いことを特徴とする請求項1又は2に記載のめっき部材。
- 前記銀−スズ合金層の厚さが1〜45μmの範囲内にあり、前記銀被覆層の厚さが0.5〜15μmの範囲内にあることを特徴とする請求項1〜3のいずれかに記載のめっき部材。
- 請求項1〜4のいずれかに記載のめっき部材よりなることを特徴とするコネクタ用めっき端子。
- 銅又は銅合金よりなる母材の表面にスズめっき層と銀めっき層とを交互に積層して最表面を銀めっき層とした後に、加熱を行い、前記母材の表面を被覆する銀−スズ合金層と、前記銀−スズ合金層を被覆し、最表面に露出する銀被覆層とを形成することを特徴とするめっき部材の製造方法。
- 前記母材に接触させてニッケル下地めっき層を形成し、前記スズめっき層と前記銀めっき層よりなる積層構造のうちの最下層を銀めっき層として前記ニッケル下地めっき層に接触させて形成することを特徴とする請求項6に記載のめっき部材の製造方法。
- 前記スズめっき層と前記銀めっき層よりなる積層構造は、最下層の銀めっき層と、中間層のスズめっき層と、最表層の銀めっき層の3層よりなることを特徴とする請求項7に記載のめっき部材の製造方法。
- 前記最表層の銀めっき層は、前記最下層の銀めっき層よりも厚いことを特徴とする請求項8に記載のめっき部材の製造方法。
- 前記最表層の銀めっき層は、前記中間層のスズめっき層よりも厚いことを特徴とする請求項8又は9に記載のめっき部材の製造方法。
- 前記最下層の銀めっき層の厚さは0.5〜15μmの範囲内にあり、前記中間層のスズめっき層の厚さは0.5〜15μmの範囲内にあり、前記最表層の銀めっき層の厚さは1〜30μmの範囲内にあることを特徴とする請求項8〜10のいずれかに記載のめっき部材の製造方法。
- 前記スズめっき層と前記銀めっき層よりなる積層構造の加熱を、180℃以上かつスズの融点以下の温度で行うことを特徴とする請求項6〜11のいずれかに記載のめっき部材の製造方法。
- 銅又は銅合金よりなる母材の表面にスズめっき層と銀めっき層とを交互に積層して最表面を銀めっき層とした後に、加熱を行い、前記母材の表面を被覆する銀−スズ合金層と、前記銀−スズ合金層を被覆し、最表面に露出する銀被覆層とを形成することを特徴とするコネクタ用めっき端子の製造方法。
- 前記スズめっき層と前記銀めっき層よりなる積層構造の加熱を、180℃以上かつスズの融点以下の温度で行うことを特徴とする請求項13に記載のコネクタ用めっき端子の製造方法。
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PCT/JP2012/083055 WO2013150690A1 (ja) | 2012-04-06 | 2012-12-20 | めっき部材、コネクタ用めっき端子、めっき部材の製造方法、及びコネクタ用めっき端子の製造方法 |
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US14/390,108 US9755343B2 (en) | 2012-04-06 | 2012-12-20 | Plated member and plated terminal for connector |
CN201280072161.0A CN104204310B (zh) | 2012-04-06 | 2012-12-20 | 镀敷部件、连接器用镀敷端子、镀敷部件的制造方法以及连接器用镀敷端子的制造方法 |
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JP5819547B2 (ja) * | 2013-06-11 | 2015-11-24 | 株式会社Kanzacc | 接触端子構造 |
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JP2016015224A (ja) * | 2014-07-01 | 2016-01-28 | 日本航空電子工業株式会社 | コネクタ |
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JP2016056422A (ja) * | 2014-09-11 | 2016-04-21 | 株式会社オートネットワーク技術研究所 | 端子用部材およびその製造方法ならびにコネクタ用端子 |
DE112015005914B4 (de) | 2015-01-09 | 2022-05-25 | Autonetworks Technologies, Ltd. | Verbindungsanschlusspaar |
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WO2017068974A1 (ja) * | 2015-10-20 | 2017-04-27 | 株式会社オートネットワーク技術研究所 | 端子用金属板、端子及び端子対 |
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JP2017079143A (ja) * | 2015-10-20 | 2017-04-27 | 株式会社オートネットワーク技術研究所 | 端子用金属板、端子及び端子対 |
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US11088482B2 (en) | 2019-01-18 | 2021-08-10 | Autonetworks Technologies, Ltd. | Metallic material and connection terminal |
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Also Published As
Publication number | Publication date |
---|---|
CN104204310B (zh) | 2016-11-23 |
DE112012006189T5 (de) | 2014-12-24 |
WO2013150690A1 (ja) | 2013-10-10 |
US20150079422A1 (en) | 2015-03-19 |
CN104204310A (zh) | 2014-12-10 |
JP5387742B2 (ja) | 2014-01-15 |
US9755343B2 (en) | 2017-09-05 |
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