TW200806718A - Composites - Google Patents

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TW200806718A
TW200806718A TW096112076A TW96112076A TW200806718A TW 200806718 A TW200806718 A TW 200806718A TW 096112076 A TW096112076 A TW 096112076A TW 96112076 A TW96112076 A TW 96112076A TW 200806718 A TW200806718 A TW 200806718A
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nylon
particles
composition
clay
nanoparticle comprises
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TW096112076A
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Dongsheng Mao
Zvi Yaniv
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Nano Proprietary Inc
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/203—Solid polymers with solid and/or liquid additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/04—Polyamides derived from alpha-amino carboxylic acids

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Description

200806718 (1) 九、發明說明 【發明所屬之技術領域】 本專利申請案係主張美國臨時專利申請案案號 60/789,3 00及60/810,394優先權，該二案件並因此倂屬本 案之參考文獻。 【先前技術】 Φ 奈米複合材料係指包含粒徑範圍介於1-100 nm之粒 子的複合材料，這些材料發揮分子的次微米結構特性。這 些粒子’例如黏土及奈米碳管（earb〇n nanotubes，CNT)， 一般而言具有優異的特性、高深寬比及層狀結構，致使高 分子與粒子間的鍵結最大化。少量添加這些添加物（0.5-5%)可增加高分子材料許多特性，包括強度更高、剛性更 佳、高抗熱性、抗紫外線性更高、低吸水率、低氣體穿透 率及其他改良特性（T. D. Forties，D. L. Hunter及D. R. • Paul，“Nylon-6 nanocomposites from Alkylammonium-modified clay: The role of Alkyl tails on exfoliation/5 Macromolecules 37， pp. 1793-1798 (2004))。 然而，奈米粒子的分散對於強化以高分子爲基質之奈 米複合材料十分重要。高分子基質中之奈米粒子的分散係 爲難題。此係爲何那些以奈米粒子強化之奈米複合材料並 未如預期地達到傑出的性質（Shamal K· Mhetre，Yong K· Kim, Steven B. Warner, Prabir K. Patra, Phaneshwar Katangur ? and Autumn Dhanote “Nanocomposites with •4- .200806718 (2) functionalized carbon nanotubes,” Mat. Res. Soc. Symp Proc· Vol· 788(2004))。有硏究宣稱奈米複合材料之原位 聚合可促進奈米粒子的分散。奈米複合材料的較佳特性也 因此不知所以然地獲得。但在高分子製程中，原位聚合並 未被證實可當作令人滿意的製造方法。也有利用較爲普遍 及可量產製造的熱熔加工方法來製備那些以奈米粒子強化 高分子之奈米複合材料。但其結果不甚令人滿意。 【發明內容】 經黏土及奈米碳管強化之高分子基質奈米複合材料兩 者增進之機械性質係可藉由奈米粒子與高分子顆粒熱熔加 工前之前處理來獲得。藉由球磨加工可將奈米粒子披覆至 高分子顆粒表面。奈米粒子薄膜於混合物經一定時間之硏 磨後形成至高分子顆粒表面。 球磨製程： 1. 允許奈米粒子貼附至高分子顆粒表面上；及 2. 藉由高分子顆粒之轟擊粉碎奈米粒子之大群簇，並 進一步在熱熔加工製程後分散高分子基質中之奈米粒子。 除了黏土及奈米碳管外，也可使用其他的塡充劑，例 如石墨粒子、碳纖維、碳簇、奈米碳管及陶瓷粒子。 【實施方式】 以下二例係可供闡明本發明之實施態樣。 -5- 200806718 (3) 實施例1 :尼龍1 1 /黏土奈米複合材料 尼龍1 1顆粒係獲自日本 Arkema 公司（商品名： RILSAN BMV-P20 PA11)。黏土係由美國 S o u t h e r n C 1 ay Products 所提供（商品名：Cloisite® series 93A)。其係爲 經三銨鹽修飾之天然蒙脫土。 參考第2圖，在步驟2 0 1中，黏土與尼龍1 1顆粒兩者皆 於80°C之真空爐中乾燥至少1 6小時，藉以完全消除水分。 φ 接著將其置於玻璃容器中進行步驟202之球磨製程。第1圖 係爲典型球磨裝置之示意圖。機器之速度係約每分鐘50〜 60轉。在此方法中係選用 5 wt·%及1〇 wt. %之黏土粉末來 進行測試。混合物至少硏磨半小時，藉此令所有的黏土粒 子被貼附至尼龍11顆粒之表面上。可將溶劑，例如異丙醇 、水或丙酮加入混合物中。另外也使用直接混合法以進行 比較。黏土與尼龍11接著被置入塑膠袋中，並以手搖動至 少半小時。 # 混合物經球磨及直接混合製程混合後，步驟203係利 用一部HAKKE Rheomex CTW 1〇〇雙螺桿押出機（德國）混 融尼龍1 1/黏土 / SEBS。以下參數係用於此步驟 旋擰區域1溫度-23 0°C ; 旋擰區域1溫度-220°C ; 旋摔區域1溫度_ 2 2 0 C ; 壓鑄溫度-230°C ; 旋擰速度-1 00 rpm。 因爲在每次收集複口材料樹脂前，需要使用混合物清 -6 - (4) 200806718 潔雙螺桿押出機，因此每次操作的尼龍1 1與黏土的量係爲 1磅。合成的樹脂可於後續的射出成形步驟製成20個條狀 物。在步驟2 04中，奈米複合材料纖維在押出步驟後係以 水冷卻並利用一部Haake PP1造粒機p〇STEX製成顆粒。 在步驟205中’奈米複合材料顆粒在進行射出成行步驟製 成樣品前係先以70 °C乾燥。在步驟206中，一部]^^-Jector(Model 55, Mini-Jector Machinery Corp. Newbury, φ Ohio, US A)實驗室級射出成形機係用來製造步驟207中物 性測試用之衝擊棒。樣品係利用ASTM指定鑄模（衝擊強 度測試用之ASTM D256，抗彎模數測試用之ASTM D790) 賦予特定尺寸。以下係爲使用之參數： 射出壓力-70 bar ; 保壓壓力-35 bar ; 保壓時間-40秒； 加熱區域1溫度-220°C ; # 加熱區域2溫度—220 °C ; 噴嘴溫度-23(TC ; 鑄模溫度-60-80 °C。 樣品在進行測試前係於乾燥器中乾燥至少40小時。抗 彎模數與樣品衝擊係利用標準三點彎曲法量測。 表1呈現不同重量比例之尼龍11/黏土/SEBS複合材料 之機械特性（抗彎模數與衝撃強度）。 ‘200806718 (5) 表1 樣品序號 前處理 抗彎模數(GPa) 衝擊強度 (kgf cm/cm) 純尼龍11 0.553 尼龍11/黏土 5 wt.% 直接混合 0.928 21·2 尼龍11/黏土 5 wt.% 球磨 1.04 30.3 尼龍11/黏土 10 wt.% 直接混合 1.33 20.4 尼龍11/黏土 10 wt.% 球磨 1.35 27.8
其係可清楚呈現以球磨前處理之尼龍1 1 /黏土奈米複 合材料之機械特性優於那些在塡充相同黏土時採直接混合 之材料。 實施例2 :尼龍6/奈米碳管奈米複合材料 尼龍6顆粒係獲自日本UBE公司（商品名：SF1018A) 。黏土係由美國Southern Clay Products所提供（商品名： Cloisite® series 93 A)。本例中所使用之奈米碳管係爲雙壁 奈米碳管（double wall nanotubes，DWNTs)係獲自比利時 Nanocyl 公司 ° 使用類似上述關於第2圖之製程。奈米碳管與尼龍6顆 粒兩者皆於80°C之真空爐中乾燥至少1 6小時，藉以完全消 除水分。接著將其至於玻璃容器中進行球磨製程。在本例 中，使用於尼龍6基質中之奈米碳管係0.4 wt. %。 -8- .200806718 (6) 第3圖係爲純尼龍6顆粒（左）與尼龍6/奈米碳管（右）之 影像。純尼龍6係爲透明，當其與奈米碳管進行球磨步驟 後係爲黑色，其係由於奈米碳管係爲黑色。此係顯示奈米 碳管均勻地披覆至尼龍6顆粒之表面上。 混合物經球磨及直接混合製程混合後，利用一部 HAKKE Rheomex CTW 100雙螺桿押出機（德國）混融尼龍6/ 黏土/SEBS。以下參數係用於此步驟 φ 旋擰區域1溫度-240°C ; 旋擰區域1溫度-230°C ; 旋擰區域1溫度_230°C ; 壓鑄溫度-220°C ; 旋擰速度-100 rpm。 因爲在每次收集複合材料樹脂前，需要使用混合物清 潔雙螺桿押出機，因此每次操作的尼龍6與奈米碳管的量 係爲1磅。合成的樹脂可於後續的射出成形步驟製成20個 φ 條狀物。奈米複合材料纖維在押出步驟後係以水冷卻並利 用一部Haake PP1造粒機POSTEX製成顆粒。奈米複合材 料顆粒在進行射出成形步驟製成樣品前係先以70 °C乾燥。 利用]\^11卜16〇1:〇1*(]\/1〇(161 555 ]\/[1111-^〇1:〇1]\4&。111116^0；〇巧· Newbury，Ohio，USA)實驗室級射出成形機製造物性測試 用之衝撃棒。樣品係利用ASTM指定鑄模（衝撃強度測試 用之ASTM D63 8，抗彎模數測試用之ASTM D790)賦予特 定尺寸。以下係爲使用之參數： 射出壓力-70 bar ; -9- (7) 200806718 保壓壓力-35 bar ; 保壓時間-40秒； 加熱區域1溫度-23(TC ; 加熱區域2溫度-230°C ; 噴嘴溫度-240°C ; 鑄模溫度-6 0 - 8 0 °C。 爲進行比較，也取純尼龍6樣品並將其成形。樣品在 φ 進行測試前係於乾燥器中乾燥至少40小時。 表2呈現尼龍6/奈米碳管複合材料之機械特性（抗張強 度與抗彎模數）。 表2 樣品序號 抗張強度（MPa) 抗彎模數（GPa) 純尼龍6 7 6 2.5 尼龍6 /奈米碳管（〇 . 4 wt. % ) 8 1 3.0 其係可清楚呈現以球磨前處理之尼龍6/奈米碳管奈米 複合材料之機械特性優於那些純尼龍6。以熱熔加工製程 合成之尼龍6/奈米碳管奈米複合材料之機械特性劣於純尼 ft 6(Dhanote, “Nanocomposites with functionalized carbon nanotubes”，Mat. Res. Soc. Symp. Proc. Vol. 788，Lll.17.1-LI 1·17_6)。 【圖式簡單說明】 -10- 200806718 (8) 第1圖係爲球磨裝置之示意圖。 第2圖係爲製造尼龍1 1/黏土 /SEBS/複合材料樹脂之流 程圖。 第3圖左係爲純尼龍6顆粒之影像，其相較於右側之尼 龍6/奈米碳管顆粒呈現透明。 【主要元件符號說明】 2〇1 :尼龍11顆粒與黏土（於真空爐中，80它，16小時） 2〇2 :乾燥混合 2〇3 :以雙螺桿押出機熱熔加工 2 04 :擠出物以水冷卻並顆粒化 2〇5 :尼龍11奈米複合材料顆粒於真空爐中，8(Γ(：，16小時 2〇6 ·將用以射出成形製成測試樣品之顆粒進行前乾燥 207 :抗彎模數，衝擊強度測試
-11 ·

Claims (1)

  1. .200806718 (1) 十、申請專利範圍 1. 一種方法，其包含利用一球磨裝置混合奈米粒子與 尼龍顆粒。 2. 如申請專利範圍第1項所述之方法，其中前述尼龍 顆粒係尼龍11顆粒。 3. 如申請專利範圍第1項所述之方法，其中前述尼龍 包含尼龍6顆粒。 φ 4.如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含黏土奈米粒子。 5 .如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含奈米碳管。 6. 如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含石墨粒子。 7. 如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含碳纖維。 φ 8 .如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含碳簇。 9.如申請專利範圍第1項所述之方法，其中前述奈米 粒子包含陶瓷粒子。 1 〇.如申請專利範圍第1項所述之方法，其中以球磨裝 置混合後之尼龍顆粒被奈米粒子覆蓋。 11. 一種物質組合物’其包含表面附著有奈米粒子之 尼龍顆粒。 12. 如申請專利範圍第11項所述之組合物，其中前述 -12- ‘200806718 (2) 尼龍顆粒係尼龍Π顆粒。 1 3 .如申請專利範圍第1 1項所述之組合物，其中前述 尼龍顆粒包含尼龍6顆粒。 1 4 .如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含黏土奈米粒子。 1 5 .如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含奈米碳管。 φ 1 6 .如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含石墨粒子。 1 7.如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含碳纖維。 1 8 .如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含碳簇。 1 9 .如申請專利範圍第1 1項所述之組合物，其中前述 奈米粒子包含陶瓷粒子。 φ 20.如申請專利範圍第1 1項所述之組合物，其中前述 尼龍顆粒以球磨裝置混合後被奈米粒子覆蓋。 -13-
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