JPWO2017150118A1 - 研磨用組成物およびこれを用いた研磨方法 - Google Patents
研磨用組成物およびこれを用いた研磨方法 Download PDFInfo
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- JPWO2017150118A1 JPWO2017150118A1 JP2018502985A JP2018502985A JPWO2017150118A1 JP WO2017150118 A1 JPWO2017150118 A1 JP WO2017150118A1 JP 2018502985 A JP2018502985 A JP 2018502985A JP 2018502985 A JP2018502985 A JP 2018502985A JP WO2017150118 A1 JPWO2017150118 A1 JP WO2017150118A1
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- APBDREXAUGXCCV-UHFFFAOYSA-L tetraethylazanium;carbonate Chemical compound [O-]C([O-])=O.CC[N+](CC)(CC)CC.CC[N+](CC)(CC)CC APBDREXAUGXCCV-UHFFFAOYSA-L 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- WJZPIORVERXPPR-UHFFFAOYSA-L tetramethylazanium;carbonate Chemical compound [O-]C([O-])=O.C[N+](C)(C)C.C[N+](C)(C)C WJZPIORVERXPPR-UHFFFAOYSA-L 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本発明の一形態は、砥粒と、水溶性高分子と、アニオン性界面活性剤と、塩基性化合物と、水と、を含み、前記アニオン性界面活性剤がオキシアルキレン単位を有し、前記アニオン性界面活性剤の前記オキシアルキレン単位の平均付加モル数が3を超えて25以下である、研磨用組成物である。本発明の一形態に係る研磨用組成物によれば、研磨対象物のヘイズを低減することができると共に、研磨速度にも優れる研磨用組成物が提供される。
本発明の一形態に係る研磨用組成物は、特定のアニオン性界面活性剤を必須に含む。ここで、「アニオン性界面活性剤」とは、水中で解離して陰イオンとなる官能基および疎水性基を有し、界面活性作用を有する化合物をいう。本発明に係る研磨用組成物に含まれるアニオン性界面活性剤は、水溶性高分子と共にヘイズを低減する働きを有する。さらに、アニオン性界面活性剤の添加により、研磨後の研磨表面に親水性を付与して研磨後の洗浄効率を良くし、汚れの付着等を防いだり、研磨用組成物の分散安定性を向上させたりする効果が期待できる。
本発明の一形態に係る研磨用組成物は、水溶性高分子を必須に含む。水溶性高分子は、研磨対象物の表面に水溶性高分子膜を形成するため、ヘイズを低減することができる。また、水溶性高分子は、上記アニオン性界面活性剤と共に、研磨対象物のヘイズを低減する働きを有する。本明細書中、「水溶性高分子」とは、水(25℃)に対する溶解度が0.01g/100mL以上である高分子をいう。また、「高分子」とは、重量平均分子量が5,000以上のものをいう。重量平均分子量は、ゲルパーミエーションクロマトグラフィー(GPC)により測定することができ、より詳細には、実施例に記載の方法により測定される値を採用する。
本発明の一形態に係る研磨用組成物は、砥粒を必須に含む。砥粒は、研磨対象物の表面を機械的に研磨する働きをする。
本発明の一形態に係る研磨用組成物は、塩基性化合物を必須に含む。ここで塩基性化合物とは、研磨用組成物に添加されることによって該組成物のpHを上昇させる機能を有する化合物を指す。塩基性化合物は、研磨対象物の面をエッチングにより化学的に研磨する働き、および砥粒の分散安定性を向上させる働きを有する。また、塩基性化合物は、pH調整剤として用いることができる。
本発明の一形態に係る研磨用組成物は、水を必須に含む。水は、他の成分を溶解させる溶媒または分散させる分散媒としての働きを有する。
本発明の一形態に係る研磨用組成物は、砥粒、水溶性高分子、アニオン性界面活性剤、塩基性化合物および水以外にも、必要に応じて他の成分を含有してもよい。しかし、一方で、本発明に係る研磨用組成物は、酸化剤を実質的に含まないことが好ましい。研磨用組成物中に酸化剤が含まれていると、当該組成物が研磨対象物(例えばシリコンウェハ)に供給されることにより、該研磨対象物の表面が酸化されて酸化膜が形成され、これにより研磨速度が低下しうる。ここでいう酸化剤の具体例としては、過酸化水素(H2O2)、過硫酸ナトリウム、過硫酸アンモニウム、ジクロロイソシアヌル酸ナトリウム等が挙げられる。なお、研磨用組成物が酸化剤を実質的に含まないとは、少なくとも意図的には酸化剤を含有させないことをいう。したがって、原料や製法等に由来して微量(例えば、研磨用組成物中における酸化剤のモル濃度が0.0005モル/L以下、好ましくは0.0001モル/L以下、より好ましくは0.00001モル/L以下、特に好ましくは0.000001モル/L以下)の酸化剤が不可避的に含まれている研磨用組成物は、ここでいう酸化剤を実質的に含有しない研磨用組成物の概念に包含されうる。
本発明の一形態に係る研磨用組成物は、キレート剤を含有していてもよい。キレート剤は、研磨用組成物中に元々含まれている金属不純物や研磨中に研磨対象物や研磨装置から生じる、あるいは外部から混入する金属不純物を捕捉して錯体を形成することで、研磨対象物への金属不純物の残留を抑制する。特に、研磨対象物が半導体の場合、金属不純物の残留を抑制することで半導体の金属汚染を防止し、半導体の品質低下を抑制する。
本発明の一形態に係る研磨用組成物は、防腐剤・防カビ剤をさらに含んでいてもよい。
本発明の一形態に係る研磨用組成物は、オキシアルキレン単位の平均付加モル数が特定の範囲内であるアニオン性界面活性剤を必須に含むが、本発明の効果を損なわない限りにおいて、その他の、上記アニオン性界面活性剤以外の界面活性剤をさらに含んでいてもよい。かような界面活性剤は、研磨後の研磨表面に親水性を付与することにより、研磨後の洗浄効率をより向上させ、汚れの付着等を防ぐことを目的として添加されうる。
研磨用組成物は、必要に応じて研磨用組成物に一般に含有されている公知の添加剤、例えば有機酸、有機酸塩、無機酸、無機酸塩等をさらに含有してもよい。
本発明に係る研磨用組成物の製造方法は特に制限されない。例えば、砥粒と、水溶性高分子と、アニオン性界面活性剤と、塩基性化合物と、必要に応じて添加される他の成分を順次添加し、水中で撹拌することにより製造することができる。
本発明に係る研磨用組成物は、一剤型であってもよいし、二剤以上から構成する多剤型であってもよい。また、上記で説明した研磨用組成物は、そのまま研磨に使用されてもよいし、研磨用組成物の濃縮液を、水を加えて希釈する、あるいは多剤型の研磨用組成物の場合は水と構成成分の一部を含有する水溶液で希釈することにより調製して研磨に使用されてもよい。例えば、研磨用組成物の濃縮液を保管または輸送した後に、使用時に希釈して研磨用組成物を調製することができる。すなわち、ここに開示される技術における研磨用組成物の概念には、研磨対象物に供給されて該研磨対象物の研磨に用いられる研磨液(ワーキングスラリー)と、希釈して研磨液として用いられる濃縮液(研磨液の原液)との双方が包含される。
本発明の一形態に係る研磨用組成物を用いて研磨する研磨対象物は、特に制限されず、種々の材質および形状を有する研磨対象物の研磨に適用され得る。研磨対象物の材料は、例えば、シリコン材料、アルミニウム、ニッケル、タングステン、鋼、タンタル、チタン、ステンレス鋼等の金属もしくは半金属、またはこれらの合金;石英ガラス、アルミノシリケー卜ガラス、ガラス状カーボン等のガラス状物質;アルミナ、シリカ、サファイア、窒化ケイ素、窒化タンタル、炭化チタン等のセラミック材料;炭化ケイ素、窒化ガリウム、ヒ化ガリウム等の化合物半導体基板材料;ポリイミド樹脂等の樹脂材料;等が挙げられる。また、研磨対象物は、上記材料のうち、複数の材料により構成されていてもよい。
本発明のその他の形態としては、上記研磨用組成物を用いて研磨対象物を研磨することを含む、研磨方法が提供される。本発明に係る研磨用組成物は、ヘイズの低減効果に優れるため、仕上げ研磨工程において特に好適に用いられる。すなわち、本発明に係る研磨方法は、仕上げ研磨工程において好適に用いられる。したがって、本発明によれば、上記研磨用組成物を用いた仕上げ研磨工程を含む研磨物の製造方法(例えば、シリコンウェハの製造方法)もまた提供される。なお、仕上げ研磨工程とは、目的物の製造プロセスにおける最後の研磨工程(すなわち、その工程の後にはさらなる研磨を行わない工程)を指す。本発明に係る研磨用組成物は、また、仕上げ研磨工程よりも上流の研磨工程(粗研磨工程と最終研磨工程との間の工程を指す)、例えば仕上げ研磨工程の直前に行われる研磨工程に用いられてもよい。
<実施例1〜4および比較例1〜5>
表1に示される組成となるように以下の材料を脱イオン水中で混合することにより、pHが10.0である実施例1〜4および比較例1〜5の研磨用組成物をそれぞれ調製した(混合温度:約20℃、混合時間:約5分)。なお、研磨用組成物(液温:20℃)のpHは、pHメータ(株式会社堀場製作所製 商品名:LAQUA(登録商標))により確認した。このとき、標準緩衝液(フタル酸塩pH緩衝液 pH:4.01(25℃)、中性リン酸塩pH緩衝液 pH:6.86(25℃)、炭酸塩pH緩衝液 pH:10.01(25℃))を用いて3点校正した後で、ガラス電極を研磨用組成物に挿入し、2分以上経過し、安定した後の値を測定した。
・水溶性高分子(ヒドロキシエチルセルロース(HEC)、重量平均分子量:25万)
・塩基性化合物(アンモニア水(29質量%))
・界面活性剤
各研磨用組成物の特徴を表1にまとめる。
表2に示される組成となるように添加した材料の種類および添加量を変更したこと以外は、上記実施例1と同様にして、実施例5および比較例6〜7の研磨用組成物をそれぞれ調製した。使用した材料は、以下の通りである。
・水溶性高分子(ポリビニルアルコール・ポリビニルピロリドン ランダム共重合体(PVA−PVP;PVA:PVP(モル比)=90:10)、重量平均分子量:1.5万)
・塩基性化合物(アンモニア水(29質量%))
・界面活性剤
各研磨用組成物の特徴を表2にまとめる。
表3に示される組成となるように添加した材料の種類および添加量を変更したこと以外は、上記実施例1と同様にして、実施例6および比較例8の研磨用組成物をそれぞれ調製した。使用した材料は、以下の通りである。
・水溶性高分子(ヒドロキシエチルセルロース(HEC)、重量平均分子量:25万)
・水溶性高分子(ポリビニルピロリドン(PVP)、重量平均分子量:5万)
・塩基性化合物(アンモニア水(29質量%))
・界面活性剤
各研磨用組成物の特徴を表3にまとめる。
表4に示される組成となるように添加した材料の種類および添加量を変更したこと以外は、上記実施例1と同様にして、実施例7および比較例9の研磨用組成物をそれぞれ調製した。使用した材料は、以下の通りである。
・水溶性高分子(ビニルアルコール単位とn−プロピルビニルエーテル単位とを85:15(モル比)で有するランダム共重合体(疎水変性PVA)、重量平均分子量:1.6万)
・塩基性化合物(アンモニア水(29質量%))
・界面活性剤
各研磨用組成物の特徴を表4にまとめる。
カラム:TSKgel GMPWxl×2+G2500PWxl(φ7.8mm×300mm×3本)(東ソー株式会社製)
溶離液:200mM 硝酸ナトリウム水溶液
試料濃度:0.05質量%
流量:1.0mL/min
注入量:200μL
標準物質:ポリエチレンオキサイド
カラム温度:40℃
検出器:示差屈折計(RI)。
カラム:TSKgel G2500PWX(東ソー株式会社製)
溶離液:水/メタノール=70/30(0.5%酢酸ナトリウム)
試料濃度:0.25質量%
流量:1.0mL/min
注入量:200μL
標準物質:ポリエチレンオキサイド
カラム温度:40℃
検出器:示差屈折計(RI)。
<ヘイズ(相対値)の評価>
≪前処理≫
1質量%の砥粒(コロイダルシリカ、一次粒子径:35nm、二次粒子径:70nm)および0.07質量%の水酸化カリウム(KOH)を含むスラリー(分散媒:水)を用い、単結晶シリコン基板(直径:300mm、p型、結晶方位<100>、抵抗率:0.1Ω・cm以上100Ω・cm未満、COPフリー)を以下の研磨条件(条件I)で前処理した。
研磨機:枚葉研磨機 PNX−322(株式会社岡本工作機械製作所製)
研磨パッド:POLYPAS(登録商標) FP55(不織布タイプ、厚さ約2mm、密度約0.3g/cm3、圧縮率約7%、圧縮弾性率約90%、硬度約50°、フジボウ愛媛株式会社製)
研磨荷重:15kPa
プラテン(定盤)回転数:30rpm
ヘッド(キャリア)回転数:30rpm
研磨用組成物の供給速度:0.5L/min
研磨時間:3min
定盤冷却水の温度:20℃
研磨用組成物の保持温度:20℃。
次に、上記(1)で得られた各研磨用組成物を用い、前処理した単結晶シリコン基板を以下の研磨条件(条件II)で研磨した。
研磨機:枚葉研磨機 PNX−322(株式会社岡本工作機械製作所製)
研磨パッド:POLYPAS(登録商標) 27NX(スウェードタイプ、厚さ約1.5mm、密度約0.4g/cm3、圧縮率約20%、圧縮弾性率約90%、硬度約40°、平均開孔径約45μm、開孔率約25%、フジボウ愛媛株式会社製)
研磨荷重:15kPa
プラテン(定盤)回転数:30rpm
ヘッド(キャリア)回転数:30rpm
研磨用組成物の供給速度:0.4L/min
研磨時間:4min
定盤冷却水の温度:20℃
研磨用組成物の保持温度:20℃。
上記研磨後の単結晶シリコン基板を、さらに洗浄液(NH4OH(29質量%):H2O2(31質量%):脱イオン水(DIW)=1:1:15(体積比))を用いて洗浄した(SC−1洗浄)。より具体的には、洗浄槽を2つ用意し、それら第1および第2の洗浄槽の各々に上記洗浄液を収容して60℃に保持し、研磨後の単結晶シリコン基板を第1の洗浄槽に5分、その後超純水による周波数950kHzの超音波発振器を取り付けたリンス槽を経て、第2の洗浄槽に5分、それぞれ上記超音波発振器を作動させた状態で浸漬した。その後、スピン乾燥を行った。
上記のように処理した単結晶シリコン基板について、上記条件IIによる研磨を行った後単結晶シリコン基板表面におけるヘイズレベルを測定した。ヘイズレベルの測定は、ウェハ検査装置「Surfscan SP2」(ケーエルエー・テンコール社製)を用いて、DWOモードでヘイズ(ppm)を測定した。得られた結果を、実施例1〜4および比較例1〜4については、比較例5のヘイズ値を100%とする相対値に換算して表1に示した。また、実施例5および比較例6については比較例7のヘイズ値を、実施例6については比較例8のヘイズ値を、実施例7については比較例9のヘイズ値を、それぞれ100%とする相対値に換算して表2、表3および表4にそれぞれ示した。なお、ヘイズ比が100%未満である場合に、ヘイズ低減効果が有意に確認できるものとする。
上記<ヘイズ(相対値)の評価>と同様に前処理および研磨を行い、研磨前後の研磨対象物(単結晶シリコン基板)の質量をそれぞれ測定した。これらの差分から、研磨前後の研磨対象物の質量変化量を求め、実施例1〜4および比較例1〜4については、比較例5の質量変化量を100%とする相対値に換算して表1に示した。また、実施例5および比較例6については比較例7の質量変化量を、実施例6については比較例8の質量変化量を、実施例7については比較例9の質量変化量を、それぞれ100%とする相対値に換算して表2、表3および表4にそれぞれ示した。なお、研磨速度比が100%を超える場合に、研磨速度向上効果が有意に確認できるものとする。
Claims (6)
- 砥粒と、水溶性高分子と、アニオン性界面活性剤と、塩基性化合物と、水と、を含み、
前記アニオン性界面活性剤がオキシアルキレン単位を有し、
前記アニオン性界面活性剤の前記オキシアルキレン単位の平均付加モル数が3を超えて25以下である、研磨用組成物。 - 前記アニオン性界面活性剤が、硫酸エステルおよびその塩、スルホン酸およびその塩、カルボン酸およびその塩、ならびにリン酸エステルおよびその塩からなる群から選択される、請求項1に記載の研磨用組成物。
- 前記アニオン性界面活性剤の含有量が、1×10−6質量%以上1質量%以下である、請求項1または2に記載の研磨用組成物。
- 前記水溶性高分子が、窒素原子を含有するポリマー、セルロース誘導体およびビニルアルコールに由来する構成単位を含むポリマーからなる群から選択される少なくとも一種を含む、請求項1〜3のいずれか1項に記載の研磨用組成物。
- 研磨対象物が単結晶シリコン基板である、請求項1〜4のいずれか1項に記載の研磨用組成物。
- 請求項1〜5のいずれか1項に記載の研磨用組成物を用いて研磨対象物を研磨することを含む、研磨方法。
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JP2009218558A (ja) * | 2008-02-12 | 2009-09-24 | Hitachi Chem Co Ltd | Cmp用研磨液、基板の研磨方法及び電子部品 |
JP2010095650A (ja) * | 2008-10-17 | 2010-04-30 | Hitachi Chem Co Ltd | 研磨剤組成物及びこの研磨剤組成物を用いた基板の研磨方法 |
JP2010153626A (ja) * | 2008-12-25 | 2010-07-08 | Fujifilm Corp | 研磨液 |
JP2015007236A (ja) * | 2010-03-12 | 2015-01-15 | 日立化成株式会社 | スラリ、研磨液セット、研磨液及びこれらを用いた基板の研磨方法 |
WO2014196299A1 (ja) * | 2013-06-07 | 2014-12-11 | 株式会社フジミインコーポレーテッド | シリコンウエハ研磨用組成物 |
WO2015146282A1 (ja) * | 2014-03-28 | 2015-10-01 | 株式会社フジミインコーポレーテッド | 研磨用組成物 |
JP2016009759A (ja) * | 2014-06-24 | 2016-01-18 | 株式会社フジミインコーポレーテッド | シリコンウェーハ研磨用組成物 |
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US20190062595A1 (en) | 2019-02-28 |
EP3425016A1 (en) | 2019-01-09 |
WO2017150118A1 (ja) | 2017-09-08 |
KR102645587B1 (ko) | 2024-03-11 |
EP3425016B1 (en) | 2021-01-27 |
KR20180113198A (ko) | 2018-10-15 |
TW201734160A (zh) | 2017-10-01 |
US11332640B2 (en) | 2022-05-17 |
EP3425016A4 (en) | 2019-03-13 |
TWI719144B (zh) | 2021-02-21 |
JP6892434B2 (ja) | 2021-06-23 |
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