TWI436881B - 芯材料用的改良對接頭 - Google Patents
芯材料用的改良對接頭 Download PDFInfo
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- TWI436881B TWI436881B TW097125899A TW97125899A TWI436881B TW I436881 B TWI436881 B TW I436881B TW 097125899 A TW097125899 A TW 097125899A TW 97125899 A TW97125899 A TW 97125899A TW I436881 B TWI436881 B TW I436881B
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- Prior art keywords
- foam
- weight
- meth
- fiber
- layer
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- 125000000217 alkyl group Chemical group 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- DZBOAIYHPIPCBP-UHFFFAOYSA-L magnesium;2-methylprop-2-enoate Chemical compound [Mg+2].CC(=C)C([O-])=O.CC(=C)C([O-])=O DZBOAIYHPIPCBP-UHFFFAOYSA-L 0.000 description 1
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
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- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/06—Fibrous reinforcements only
- B29C70/08—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers
- B29C70/086—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers and with one or more layers of pure plastics material, e.g. foam layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/06—Fibrous reinforcements only
- B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
- B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
- B29C70/24—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in at least three directions forming a three dimensional structure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
- B29K2033/04—Polymers of esters
- B29K2033/12—Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate
-
- 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
- B32B2305/00—Condition, form or state of the layers or laminate
- B32B2305/02—Cellular or porous
- B32B2305/022—Foam
-
- 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
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/16—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
- B32B37/22—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of both discrete and continuous layers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
本發明之目的係經由在夾心結構的厚度方向(z方向)引入強化元件來改良對接頭在夾心結構中的機械性質。本發明可用於製造夾心元件、這些元件應用於太空及造船中、建造電動車及軌道車、建造動力產生系統、及建造運動設備。
對眾多應用而言,聚甲基丙烯醯亞胺發泡體配置纖維強化層,以得到具有極佳性質的複合材料。這些複合材料特別係用於旋轉葉片之製造(US 5547629)。亦描述黏合至熟知的熱塑料,一個實例為聚甲基丙烯醯亞胺發泡體壓合至聚甲基丙烯酸甲酯(EP 736 372)。聚甲基丙烯醯亞胺發泡體的另一個應用係在發泡體中摻入導電顆粒,以使發泡體吸收電磁輻射(DE 38 264 69 A1)。亦描述於汽車工業之應用(JP 63315229 A2)。其他相關的專利為DE3304882 A、GB 1547978 A、DE 2822881、DE 2235028及DE 2114524。
當製造由複合材料組成的組件時,一個經常發生的問題係芯材料(發泡體,例如Rohace11型的發泡體,其可得自Rhm GmbH,或者其他發泡體,例如由聚氯乙烯(PVC)或PU組成的發泡體)無法以需要或希望的尺寸供應。舉例而言,現今高載量航空器的尾翼(fin)需要尺寸
之截面約為6米×5米,但是,因為製造技術的原因,發泡體片僅能以較小的尺寸製造。
除了提供具所須尺寸之芯材料的需求之外,另一需求是將適於阻斷發泡體內裂紋擴大之強化材料摻至複合組件中。由於外層為不透明,使得裂紋無法由外部查覺,所以此為特別重要的作用。
在接頭(例如對接頭(或芯接點))區域中,剛度(stiffness)的突然改變會產生集中應力,其可能會使強度降低。接頭處鄰接的芯材料可以相同或相異。
一目的係開發改良的對接頭。
具有獨立產品項之所有特性的對接頭達成以上討論之目的,並且亦達成其他目的,雖然未個別提及這些目的,但是嫻於本技藝之人士可由概述中的討論輕易推衍而得。本發明之薄片的較佳實施例係藉由附屬項提供,該附屬項參照獨立產品項。獨立方法項保障本發明之接頭的製法。附屬方法項提供該方法的較佳修飾。該目的之達成方式在於,在夾心元件之對接頭的區域內強化元件被引至厚度方向。不同或完全相同的芯材料或其他材料可在此處對接。
強化元件可以較低及/或較高密度或硬度引至芯材料的過渡區中(見圖1)。可以使用的強化元件之實例為碳纖維棒。強化元件亦可穿透兩個外層,例如,以改善層離性質、衝擊性質及裂紋擴大性質,此處的結果為對接頭及
整個夾心結構對損害更具容忍性。使用傳統的縫紉法或分束法、釘連法(如Airbus使用之基於Aztex原理或TFC原理者)可將強化元件引至芯材料或夾心結構中。
將強化元件引至芯材料中的作法首先可以降低硬度的突然改變,產生較少的集中應力,其次提高機械性質(例如抗張強度、壓縮性質、剪力性質及層離性質)的水平。此有利的效應可以提高對接頭的靜態及循環強度。
強化元件亦可作為裂紋終止物,因此可以防止裂紋由對接頭的一側不受阻地擴張至另一側。
結果:.強化造成組件重量增加約7%,並且此可以藉由使用諸如ROHACELLRIMA替代ROHACELLWF而再降低,藉此而降低總重量,.靜態切變強度提高約26%,.循環切變強度提高,.壽命較長。
與本發明之方法有關的芯材料包含聚(甲基)丙烯醯亞胺發泡體。
括號內的文字係用以表現可選擇的特性。舉例而言,(甲基)丙烯酸系意指丙烯酸系、甲基丙烯酸系及二者組
成的混合物。
由本發明之組成物製得的聚(甲基)丙烯醯亞胺發泡體包含可以式(I)表示的重覆單元
其中R1
及R2
相同或相異且可為氫或甲基,且R3
可為氫或具有至多20個碳原子的烷基或芳基部分。
結構(I)的單元以佔聚(甲基)丙烯醯亞胺發泡體之超過30重量%為佳,超過50重量%較佳,超過80重量%更佳。
剛性聚(甲基)丙烯醯亞胺發泡體的製造已為習知,且揭示於如GB專利案1 078 425、GB專利案1 045229、DE專利案1 817 156(=US專利案3 627 711)或DE專利案27 26 259(=US專利案4 139 685)中
特別地,結構式(I)的單元可由(甲基)丙烯酸與(甲基)丙烯腈的鄰近單元經環化異構化反應在加熱到150℃至250℃的條件下形成(參考DE-C 18 17 156、DE-C 27 26 259、EP-B 146 892)。前驅物通常是先在自由基起始劑存在時,於低溫(例如,30℃至60℃)下,經單體的
聚合作用製得,其後續加熱至60℃至120℃,之後使用發泡劑,藉由加熱至約180℃至250℃而發泡(見EP-B 356 714)。
舉例而言,此可藉由先形成包含莫耳比以1:3至3:1為佳的(甲基)丙烯酸和(甲基)丙烯腈之共聚物而達成。
這些共聚物可進一步包含其他的單體單元,例如自丙烯酸或甲基丙烯酸之酯類(特別是與具有1至4個碳原子的低碳醇類(如,甲醇、乙醇、丙醇、異丙醇、正丁醇、異丁醇或第三丁醇)之酯類)衍生而得者,或衍生自苯乙烯及苯乙烯衍生物者(如,α-甲基苯乙烯),或衍生自馬來酸或其酐類、衣康酸或其酐類者,或衍生自乙烯基吡咯烷酮、氯乙烯或1,1-二氯乙烯者。無法環化或者僅能以高困難度環化之共聚單體的比例不超過單體重量的30重量%,以20重量%為佳,10重量%更佳。
習知之可以類似方式有利地使用的其他單體為少量的交聯劑,如,丙烯酸烯丙酯、甲基丙烯酸烯丙酯、二丙烯酸乙二醇酯或二甲基丙烯酸乙二醇酯;或丙烯酸或甲基丙烯酸的多價金屬鹽,如,甲基丙烯酸鎂。以可聚合的單體總量計,這些交聯劑的定量比例通常在0.005重量%至5重量%的範圍內。
可進一步使用添加的金屬鹽且通常會降低煙霧量。這些尤其是丙烯酸或甲基丙烯酸的鹼金屬鹽或鹼土金屬鹽或鋅鹽、鋯鹽或鉛鹽。較佳者為(甲基)丙烯酸鈉、(甲基
)丙烯酸鉀、(甲基)丙烯酸鋅及(甲基)丙烯酸鈣。2至5重量份的單體量顯著降低FAR 25.853a防火試驗中的煙霧密度。
所用的聚合起始劑包含習用於(甲基)丙烯酸酯之聚合反應者,其例為偶氮化合物(如,偶氮二異丁烯腈)和過氧化物(如,過氧化二苯甲醯或過氧化二月桂醯)或其他的過氧化物(如,過氧辛酸第三丁酯或過氧縮酮)及,適當時,氧化還原引發劑(此可參考如H.Rauch-Puntigam,Th.Vlker,Acryl-und Methacrylverbindungen[Acrylic and methacrylic compounds],Springer,Heidelberg,1967,或Kirk-Othmer,Encyclopedia of Chemical Technology,Vol.1,pages 286 et seq.,John Wiley & Sons,New York,1978)。以起始物計,聚合反應引發劑用量以0.01至0.3重量%為佳。
視時間和溫度而定,亦可有利地合併具有不同分解性質之聚合起始劑。例如,非常適當地,同時使用過氧新戊酸第三丁酯、過氧苯甲酸第三丁酯和2-乙基過氧己酸第三丁酯,或同時使用過氧苯甲酸第三丁酯、2,2-偶氮雙異-2,4-二甲基戊腈、2,2-偶氮雙異丁腈及二-第三丁基過氧化物。
聚合反應以藉整體聚合的變體來實施為佳,其例為習知之細胞法,但不在此限。
聚合物的重均分子量 w
以大於106
克/莫耳為佳,特別是大於3×106
克/莫耳,但不在此限。
用以在轉換成含有醯亞胺基團之聚合物的期間使共聚物發泡,發泡劑係以習知的方式使用,並在150℃至250℃經由分解作用或蒸發作用形成氣相。具有醯胺結構之發泡劑(如,尿素或者一甲基-或N,N-二甲基脲或甲醯胺或一甲基甲醯胺)之分解作用釋出氨或胺,其有助於醯亞胺基團的進一步形成。但亦可使用無氮發泡劑,例如甲酸、水、或具有3至8個碳原子的一羥基脂族醇(如,1-丙醇、2-丙醇、正丁-1-醇、正丁-2-醇、異丁-1-醇、異丁-2-醇、戊醇及/或己醇)。發泡劑的用量視發泡體所欲密度而定,但此處,以所用單體計,發泡劑在反應混合物中的用量通常由約0.5重量%至15重量%。
前驅物可進一步包含習知的添加劑。這些尤其是抗靜電劑、抗氧化劑、脫模劑、潤滑劑、染料、阻燃劑、流動改良劑、填料、光安定劑及有機磷化合物(如,亞磷酸鹽或膦酸鹽)、顏料、天候安定劑及塑化劑。
抑制發泡體帶靜電的導電顆粒是另一類較佳的添加劑種類。這些尤其是鹼金屬粒子及碳黑粒子,此二者亦可以纖維的形態存在,其尺寸在10奈米至10毫米的範圍內,如EP 0 356 714 A1所述者
舉例而言,以下步驟可以製得具有特佳用途之聚甲基丙烯醯亞胺發泡體:
1.經由包含以下組份之組成物的自由基聚合反應,製得聚合物片
(a)單體混合物,其包含20重量%至60重量%之甲基丙烯腈、80重量%至40重量%之甲基丙烯酸及,適當時,至多20重量%(以甲基丙烯酸及甲基丙烯腈總量計)之具有乙烯系不飽和性的單官能單體(b)0.5重量%至15重量%之發泡劑混合物,其包含甲醯胺或一甲基甲醯胺及分子中具有3至8個碳原子的一羥基脂族醇(c)交聯劑系統,其由下列者所構成(c.1)0.005重量%至5重量%之分子中具有乙烯系不飽和性並具有至少2個雙鍵且能夠進行自由基聚合反應之化合物,及(c.2)1重量%至5重量%之溶解於單體混合物中的氧化鎂(d)引發劑系統(e)慣用的添加劑。
2.此混合物於30℃至45℃下在由尺寸為50×50公分的兩片玻璃板和邊緣密封厚度為2.2公分所形成的槽室中聚合數日。之後,此聚合物於40℃至130℃熱調節約20小時,以完成聚甲基丙烯醯亞胺之聚合反應。於200℃至250℃數小時進行後續的發泡。
具有高耐熱性的聚甲基丙烯醯亞胺可以再藉由聚甲基丙烯酸甲酯或其共聚物與一級胺的反應製得,其亦可依據本發明使用。以下者可以作為此聚合物-類似醯亞胺化反
應之各式實例的代表:US 4 246 374、EP 216 505 A2、EP 860 821。高耐熱性在此處可以經由使用芳基胺(JP 05222119 A2)或者經由使用特定共聚單體(EP 561 230 A2、EP 577 002 A1)而達成。但是,這些反應皆製得固態聚合物而非發泡體,且若要製得發泡體,其必須在分離的第二步驟中發泡。此技術亦為嫻於本技藝之人士所習知。
剛性聚(甲基)丙烯醯亞胺發泡體亦可以商業上取得,其例為Rhm GmbH生產的Rohacell,其可以多種密度和尺寸供應。
聚(甲基)丙烯醯亞胺發泡體的密度以在20公斤/立方米至320公斤/立方米的範圍內為佳,在50公斤/立方米至110公斤/立方米的範圍內更佳。
無意於造成任何限制,芯層的厚度在1毫米至200毫米的範圍內,特別是在5毫米至100毫米的範圍內,在10毫米至70毫米的範圍內特別佳。
芯層內部亦可具有其他層。但在本發明之方法中,聚(甲基)丙烯醯亞胺發泡體連接至纖維強化層。但在本發明之方法的特別體系中,所使用的芯層由聚(甲基)丙烯醯亞胺發泡體所構成。
所用的纖維強化層可以包含任何已知的片狀結構,該結構在製造複合材料所需的加工條件(如,壓力及溫度)下呈安定性。具有多層結構的織物亦可作為纖維強化層。
這些尤其是,例如,纖維強化的薄片,其中有聚丙烯
、聚酯、聚醯胺、聚脲、聚氯乙烯及/或聚(甲基)丙烯酸甲酯的存在。
此纖維強化層亦可經由包含纖維之已知樹脂之固化而製得,其例子為環氧樹脂(EP樹脂)、甲基丙烯酸酯樹脂(MA樹脂)、不飽和聚酯樹脂(UP樹脂)、酚系樹脂、異氰酸酯樹脂、雙馬來醯亞胺樹脂及苯丙烯酸酯樹脂(PHA樹脂)。
可以使用的纖維強化物尤其是碳纖維、玻璃纖維、聚芳基胺纖維、聚丙烯纖維、聚酯纖維、聚醯胺纖維、聚脲纖維、聚(甲基)丙烯酸甲酯纖維、聚氯乙烯纖維和/或金屬纖維。
也可能且較佳地使用,如,預浸物(其亦可為SMC(板材模塑化合物)),以在芯層上得到纖維強化層。SMC和預浸物係以可固化塑料預先浸潤的網,大部分是玻璃纖維蓆、玻璃絲梭織物或者包含碳纖維和/或包含芳醯胺纖維束,其可熱壓加工成模製品或半成品。在可使用的SMC中,特別者是SMCR(具有隨機指向纖維的SMC)、SMCO(具有定向纖維的SMC)、SMCCR(具有一些定向程度之纖維的SMC)、XMC(具有網絡狀纖維強化的SMC)及HMC(具有高纖維含量的SMC)。
這些材料為目前已知者且述於如,Ullmann’s Encyclopedia of Industrial Chemistry,5th
edition,其標題為”Fabrication of Polymer Composites”。
沿著纖維強化層,亦可使得由金屬所構成的層經由本
發明之方法極為牢固地連結至芯層。這些的例子尤其是,由鋁所構組成的薄片或板。欲製得複合材料,金屬層可以單獨使用或者與纖維強化層一起使用。特別佳的金屬層尤其是被稱為鋁預浸物的材料。
在以有機溶劑處理之後,芯層對纖維強化層或金屬層的連結取決於欲施用的層之種類。已經知道適當的方法。
舉例而言,由包含由聚(甲基)丙烯醯亞胺發泡體所構成的芯和纖維強化層或金屬層之複合材料通常可藉習稱的熱壓法得到。這些方法為嫻於本技藝之人士習知者,且本發明亦含括特定體系,如,雙帶加壓法、SMC加壓法及GMT加壓法。
欲進一步強化複合材料,芯層可在熱壓期間內壓實。就此而言,可在壓製過程使用習稱為限位器(stops)的定距片(spacers)。其將比較容易將芯層緻密度設定於所欲程度,但此處無意以此對本發明造成任何限制。
欲改善黏著性,亦可使用膠黏劑,其可在表面以有機溶劑處理之後施用。但是對某些纖維強化層材料而言,並無此需要。
舉例而言,用以製造複合材料,SMC層或預浸物層的量(就重量而言,此量為適當量)可置於模具內之適當尺寸的發泡體片上並以壓製機施加壓力。
使預浸物或SMC開始流動及固化的典型條件為壓力高於1牛頓/平方毫米及溫度在60℃至180℃之範圍內。這些參數亦可用於梯次階段以避免熱的累積。壓製時間通常
為5分鐘至6小時,以達成纖維強化層的功能。10至120分鐘為一個特別有利的範圍。
前述樹脂及纖維強化亦可以人工的方式施用至聚(甲基)丙烯醯亞胺發泡體。此處,樹脂層及纖維網交替放置。在施用纖維強化樹脂層之後,樹脂係以已知的方式固化。適當的系統如West System,其得自M.u.H.von der Linden GmbH,P.O.Box 100543,D-46465 Wesel/Rhein,Germany。
外層的厚度以在0.1至100毫米的範圍內為佳,0.5至50毫米較佳,1至5毫米更佳。
本發明之強化可用於太空船的建造,其中特別著重接頭為輕但安定,並且亦可用於航空器的建造,特別是高載客量的航空器或者高載貨量的航空器,或者用於船舶或水翼艇或氣墊船的建造,及用於陸地車輛的建造,例如用於軌道車的建造。本發明之改良對接頭的另一個優勢的應用為建造風力渦輪的葉片。
圖1顯示強化接頭的結構。
圖2顯示非強化對接頭的常見作用力及失效模式。
圖3為藉本發明之對接頭之強化而獲得的改善。
Claims (6)
- 一種夾心結構中相同或不同芯材料的改良對接頭,其特徵為一或多個強化元件被引至芯材料中鄰接欲改良之對接頭的區域內。
- 如申請專利範圍第1項之改良對接頭,其中Rohacell發泡體係作為芯材料。
- 如申請專利範圍第1項之改良對接頭,其中碳纖維材料零件係作為強化元件。
- 一種如申請專利範圍第1至3項中任一項之改良對接頭在建造太空船、航空器、船舶及陸地車輛中的用途。
- 一種如申請專利範圍第1至3項中任一項之改良對接頭在建造風力渦輪中的用途。
- 一種如申請專利範圍第1至3項中任一項之改良對接頭在建造運動設備中的用途。
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DE102007033120A DE102007033120A1 (de) | 2007-07-13 | 2007-07-13 | Verbesserte Stumpfstoßverbindungen für Kernwerkstoffe |
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EP2176056B1 (de) | 2015-08-05 |
CN101743116A (zh) | 2010-06-16 |
ES2549729T3 (es) | 2015-11-02 |
HK1141492A1 (zh) | 2010-11-12 |
AU2008277848A1 (en) | 2009-01-22 |
JP2010533216A (ja) | 2010-10-21 |
US20100189954A1 (en) | 2010-07-29 |
BRPI0813721A2 (pt) | 2014-12-30 |
KR20100032892A (ko) | 2010-03-26 |
DK2176056T3 (en) | 2015-11-02 |
WO2009010316A9 (de) | 2009-12-17 |
DE102007033120A1 (de) | 2009-01-15 |
EP2176056A1 (de) | 2010-04-21 |
PL2176056T3 (pl) | 2015-12-31 |
ZA201000234B (en) | 2010-09-29 |
WO2009010316A1 (de) | 2009-01-22 |
TW200918771A (en) | 2009-05-01 |
CN101743116B (zh) | 2014-12-24 |
CA2693889A1 (en) | 2009-01-22 |
CA2693889C (en) | 2016-01-05 |
JP5586459B2 (ja) | 2014-09-10 |
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