TW202300338A - 複合材料以及用於形成該複合材料之方法 - Google Patents

複合材料以及用於形成該複合材料之方法 Download PDF

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TW202300338A
TW202300338A TW111107553A TW111107553A TW202300338A TW 202300338 A TW202300338 A TW 202300338A TW 111107553 A TW111107553 A TW 111107553A TW 111107553 A TW111107553 A TW 111107553A TW 202300338 A TW202300338 A TW 202300338A
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composite material
pfa
layer
mold
ptfe
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宮内卓也
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美商杜邦聚合物股份有限公司
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Abstract

揭露了一種複合材料，其具有(A)含有全氟烷氧基烷烴和碳纖維的基底層、(B)中間層以及(C)聚四氟乙烯覆蓋層，其中該中間層含有全氟烷氧基烷烴。

Description

複合材料以及用於形成該複合材料之方法
本發明關於一種具有全氟烷氧基烷烴(PFA)基底層和聚四氟乙烯(PTFE)覆蓋層的複合材料，該等層藉由PFA中間層彼此結合。
已知纖維增強的PFA係用於半導體製造設備的結構材料。可以將這種纖維增強的PFA模製以獲得對設備有用的任何形狀。在WO2011/002883A中揭露了一種獲得纖維增強的PFA的實用方法，其揭露了一種包含氟聚合物和碳纖維的複合製品，以及一種用於製造該複合製品之方法。
雖然纖維增強的PFA因其機械性能、耐熱性和耐化學性係優異的材料，但是當材料暴露於強酸時，裸露在材料表面上的增強纖維被強酸氧化並降解。這導致材料性能劣化。降解的增強纖維可以容易地從材料上脫落並導致污染問題。此外，藉由氧化產生的氣體在高溫下使材料的表面膨脹。
WO2009/110341A揭露了一種由包含碳粉或碳纖維作為增強材料的PFA和PTFE製成的構件，其中藉由使構件與氧化氣體接觸，與構件的內部相比，構件表面上的碳粉/纖維被去除。然而，該方法在零件加工後需要若干個附加的步驟，如浸入氧化氣體中並重新加熱材料至軟化溫度或超過軟化溫度。
因此，在半導體技術中仍然需要纖維增強的PFA材料就耐酸性而言的進一步改進。
因此，本發明之一個方面係一種複合材料，其包含(A)包含全氟烷氧基烷烴和碳纖維的基底層、(B)中間層以及(C)聚四氟乙烯覆蓋層，其中該中間層包含全氟烷氧基烷烴。
本發明之其他方面係兩種用於製備以上所揭露的複合材料之方法。第一種方法包括以下步驟：(a)製備包含PFA和碳纖維的固結墊，(b)在模具中放置覆蓋層、中間層以及該多個固結墊，然後(c)在該模具中熱壓這三個組份以形成複合材料。
第二種用於製備以上所揭露的複合材料之方法包括以下步驟：(d)製備包含PFA和碳纖維的固結墊，(e)在模具中放置多個固結墊，(f)熱壓該多個固結墊以形成模製的材料，(g)在模具中放置覆蓋層、中間層和藉由步驟(f)獲得的該模製的材料，然後(h)在該模具中熱壓這三個組份以形成複合材料。
本發明之另外的方面係一種由以上所描述的複合材料形成的製品。
本發明關於一種複合材料，其包含：(A)包含全氟烷氧基烷烴(PFA)和碳纖維的基底層、(B)中間層以及(C)聚四氟乙烯(PTFE)覆蓋層，其中該中間層包含全氟烷氧基烷烴。
(A)PFA基底層
PFA基底層包含PFA和碳纖維。它還被稱為碳纖維增強的PFA。這種材料在本領域中是已知的並且可以用於本發明。例如，WO2011/002883A揭露了一種包含氟聚合物和碳纖維的固結複合製品。在該揭露中，首先製備含有碳纖維的PFA墊，然後將PFA墊堆疊，然後模製以形成複合製品。
可以使用任何種類的PFA。一般地，PFA具有藉由ASTM E831的120至200×10-6/℃的線膨脹係數，以及藉由ASTM D1238的2至17g/分鐘的熔體流動指數(MFI)。PFA可以在商業上獲得，例如由科慕-三井氟產品有限公司(Chemours-Mitsui Fluoroproducts Co.,Ltd.)提供的具有2至15g/分鐘的MFI的TeflonTM PFA。
在本發明中，碳纖維用作PFA基底層的增強材料。碳纖維比由無機化學材料如SiC製成的其他纖維材料具有優勢，由於與這種無機纖維相比，它的更柔軟的特性並且更容易在商業上獲得。
碳纖維可以在商業上獲得，例如由東麗公司(Toray)提供的TORAYCATM或由帝人公司(Teijin)提供的TenaxTM。典型的短切碳纖維具有3至25mm的長度以及500至5,000的縱橫比。
PFA基底層中的碳纖維的含量係基於PFA基底層的總重量較佳的是從5至50wt%、更較佳的是從10至30wt%。
PFA基底層可以進一步含有任何其他添加劑，如碳奈米管、石墨粉和奈米金剛石。
PFA基底層的厚度例如是從1至50mm、較佳的是從15至35mm。
藉由ASTM E831，PFA基底層的垂直於模製方向的平面內線膨脹係數較佳的是從1至20×10-6/℃、更較佳的是從2至10×10-6/℃，溫度範圍為從25至260℃。
(B)中間層
基底層和覆蓋層藉由中間層相互附著，並且中間層係本發明之關鍵。中間層包含全氟烷氧基烷烴(PFA)。
用作本發明之中間層的PFA可以是與PFA基底層中使用的相同的PFA，但可以是不同的PFA，其具有數十萬的分子量，藉由ASTM D1238的2至17g/分鐘的MFI。
中間層可以進一步含有本領域已知的添加劑，但不需要含有其他添加劑。
中間層的厚度較佳的是從10至2,000微米、更較佳的是100至2,000微米。
(C)PTFE覆蓋層
本發明所用的PTFE具有數百萬至一千萬的分子量作為模製等級。
在本說明書中，PTFE包括改性的PTFE。改性的PTFE的實例係例如用全氟(烷基乙烯基醚)(PAVE)改性的PTFE、用六氟丙烯(HFP)改性的PTFE等。
一般地，藉由ASTM E831，PTFE覆蓋層的線膨脹係數為從120至220×10-6/℃。
PTFE覆蓋層的厚度較佳的是從0.1至10mm、更較佳的是從0.5至5mm。
製備複合材料之方法
有兩種製備本發明之複合材料之方法。第一種方法係一步熱壓法，而第二種方法係兩步熱壓法。第一種方法還揭露為同時模製法。
第一種方法(方法1)具有在下文中揭露的以下步驟(a)至(c)。
(a)製備包含PFA和碳纖維的固結墊：
首先，製備包含PFA和碳纖維的固結墊。可以藉由將包含PFA和碳纖維的墊加熱至高於兩者的軟化溫度的溫度，然後將其冷卻至低於所述軟化溫度的溫度來製備固結墊。可以根據WO2011/002883A、WO1993/011450和US5506052A中揭露之方法獲得包含PFA和碳纖維的固結墊。
(b)在模具中放置覆蓋層、中間層以及多個固結墊。
在下一步驟中，將固結墊切成模具形狀並在模具中按特定數量堆疊。然後將中間層和覆蓋層按順序放置在模具中的堆疊的固結墊的頂部上。在模具中放置這三層的順序可以顛倒。
(c)在模具中熱壓這三個組份以形成複合材料。
下一步驟係熱壓步驟以形成複合材料。對模具施加熱量和壓力持續足夠量的時間以形成最終的複合材料。這樣做所需的溫度、壓力和時間將隨MFI、厚度和纖維負載量等因素而變化。示例性地，將模具在低於0.5MPa的壓力下加熱至高於327℃(高於PTFE的熔融溫度)，持續30至60分鐘。然後將模具在比初始壓力更高的壓力下冷卻至室溫，並且獲得複合材料。
第二種方法(方法2)具有在下文中揭露的以下步驟(d)至(h)。
(d)製備包含PFA和碳纖維的固結墊，如以上所提及的與步驟(a)相同之方法，
(e)在模具中放置多個固結墊，與以上所提及的步驟(b)相同，除了中間層和覆蓋層不放置在堆疊的固結墊上之外。
(f)熱壓以上所揭露的多個固結墊以形成模製的材料。以與以上所揭露的(c)相同的方式熱壓堆疊的固結墊。該步驟後，獲得模製的材料，即模製的PFA-碳纖維材料，沒有上層和中間層。
(g)在模具中放置覆蓋層、中間層以及該模製的材料。
然後在模具中放置藉由步驟(f)獲得的該模製的材料。在模具中放置之前，可以將該模製的材料加工成適合模具尺寸的特定形狀。然後，將中間層和覆蓋層按順序放置在模具中的該模製的材料的頂部上。
(h)在模具中熱壓這三個組份以形成複合材料。
與提及的步驟(C)相同的條件適用於複合材料的模製。這樣做所需的溫度、壓力和時間將隨複合材料的形狀而變化。
(D)製品
該複合材料的顯著特性係優異的耐酸性與良好的抗熱衝擊性結合，儘管層狀結構的多種材料具有各自的線膨脹係數。
該複合材料可用作用於半導體製造設備、尤其是用於暴露於酸性液體的該等設備的部件，例如晶圓清洗機、泵和閥門。並且它還可以用於化學加工工業如CPL生產、HF生產、TiO2生產以及用於金屬精煉的高壓酸浸，其中在該等方法中使用了硫酸。
實例
US2011/0001082 A、WO2011/002867A、WO2011/002877A和WO2011/002883A中詳述了與以下類似的材料，以及用於製造類似的材料和製品之方法，所有該等專利都以其全文藉由援引併入。
原料
PFA(片狀)
使用具有約305℃的熔點、藉由ASTM D1505約2.12至2.17的比重以及藉由ASTM D882約31.4至41.2MPa的拉伸強度的片狀的PFA。
PTFE(片狀)
使用具有約327℃的熔點、藉由ASTM D1505約2.13至2.20的比重以及藉由ASTM D882約20至35MPa的拉伸強度的片狀的PTFE。
改性的PTFE(片狀)
使用具有約327℃的熔點、藉由ASTM D1505約2.13至2.20的比重以及藉由ASTM D882約20至35MPa的拉伸強度的片狀的改性的PTFE。
實例1至33(同時模製法、一步模製法)
根據WO2011/002883 A1之方法製備固結墊，切割的直徑為91.5mm。一個固結墊的厚度約為0.3mm，並且它由20重量%的CF和80重量%的PFA製成。
在模具中一個接一個地堆疊約60個固結墊。然後，將表1中揭露的PFA和PTFE或改性的PTFE按順序放置在堆疊的固結墊上。之後，將堆疊件(即堆疊的固結墊、PFA和PTFE)放入模具中。
將基本上在環境溫度下的模具放置在溫度受控的壓板式壓機中並加熱，以使整個堆疊件的溫度大於327℃，同時在小於0.5MPa的壓力下沿厚 度方向最低程度地壓縮堆疊件，而在長度和寬度方向上不受任何附加壓力的約束。保持該溫度和壓力持續大於30分鐘。然後在結束加熱的同時沿厚度方向進一步壓縮完全加熱的模具。然後在2.3至6.0MPa的壓力下冷卻模具。因此，堆疊件被固結成約16mm厚度的基底層，並且整個製品的溫度降低至低於290℃。然後將堆疊件的溫度和壓力降低至環境條件，以獲得複合材料。模製的複合材料具有91.5cm的直徑，約16.0mm的堆疊的固結墊(基底層)厚度，0.1至1.0mm的PFA(中間層)厚度，以及0.5至5.0mm的PTFE或改性的PTFE(覆蓋層)厚度。
實例34至66(兩步模製法)
除了PFA(中間層)和PTFE或改性的PTFE(覆蓋層)沒有放入模具中之外，進行與實例1至33相同之方法。在與實例1至33中揭露的相同條件下熱壓(模製)堆疊的固結墊。獲得沒有中間層和覆蓋層的模製的固結墊。
將表2中揭露的PTFE或改性的PTFE(覆蓋層)和PFA(中間層)按順序放入模具中。然後將獲得的模製的固結墊放置在PFA上。在與實例1至33中揭露的相同條件下熱壓堆疊件(即PTFE或改性的PTFE、PFA和模製的固結墊)。
模製的複合材料具有91.5cm的直徑，約16.0mm的堆疊的固結墊(基底層)厚度，0.1至1.0mm的PFA(中間層)厚度，以及0.5至5.0mm的PTFE或改性的PTFE(覆蓋層)厚度。
分析方法
1.熱衝擊試驗
藉由切片和切割從獲得的模製的複合材料製備測試件。將模製的複合材料的基底層切成4.0mm的厚度。然後，從10mm的寬度切割模製的材料，並在測試件的平面的中心鑽兩個孔(直徑為3mm)。
熱衝擊試驗，也稱為溫度衝擊試驗，將產品暴露於交替的冷和熱溫度循環。熱衝擊試驗用於評估物品是否能夠承受周圍環境溫度的突然變化，而不會出現物理損傷或性能劣化。測試件反復浸入熱矽油中加熱，並且拿起用風扇冷卻。使用50℃為冷和200℃為熱的溫度設置，持續2,000個循環，以評估基底層、中間層與覆蓋層之間的附著性。
螢光滲透探傷用於評估熱衝擊試驗前後的附著情況。在評估中，將螢光滲透劑黏貼在測試件上並用溶劑(乙醇)擦拭。然後使用黑光，評估測試件的層之間是否存在任何間隙。結果在表1和2中示出。
外觀
○：良好(無剝離)
△：一般(部分剝離)
×：不好(剝離)
螢光滲透探傷
○：良好(無間隙)
△：一般(約10至100微米的微小間隙)
×：不好(顯著的間隙)
Figure 111107553-A0202-12-0010-1
Figure 111107553-A0202-12-0011-2
Figure 111107553-A0202-12-0012-3
Figure 111107553-A0202-12-0013-4
結果表明，如果不施加中間層，則覆蓋層可以容易地剝離，並且與在模製的複合材料上附加的模製相比，與固結墊同時模製顯示出優異的附著性。

Claims (9)

  1. 一種複合材料，包含：
    (A)基底層，包含全氟烷氧基烷烴及碳纖維的，
    (B)中間層以及
    (C)聚四氟乙烯覆蓋層，
    其中，該中間層包含全氟烷氧基烷烴。
  2. 如請求項1所述之複合材料，其中，該基底層(A)的線膨脹係數為從3至15×10-6/℃，並且該PTFE覆蓋層的線膨脹係數為120至220×10-6/℃。
  3. 如請求項1所述之複合材料，其中，在熱衝擊試驗後該基底層與PTFE覆蓋層係結合的，該熱衝擊試驗係藉由將該複合材料置於50℃下接著置於200℃下加熱作為一個循環，重複2,000次。
  4. 如請求項1所述之複合材料，其中層(B)的厚度為從10至2,000微米。
  5. 一種用於製備如請求項1所述之複合材料之方法，包含以下步驟：
    (a)製備包含PFA和碳纖維的固結墊，以及
    (b)在模具中放置覆蓋層、中間層以及該多個固結墊，然後
    (c)在該模具中熱壓這三個組份以形成複合材料。
  6. 一種用於製備如請求項1所述之複合材料之方法，其包括以下步驟：
    (d)製備包含PFA和碳纖維的固結墊，
    (e)在模具中放置多個固結墊，
    (f)熱壓該多個固結墊以形成模製的材料，
    (g)在模具中放置覆蓋層、中間層以及該模製的材料，
    (h)在該模具中熱壓這三個組份以形成複合材料。
  7. 一種製品，其由如請求項1所述之複合材料形成。
  8. 如請求項7所述之製品，其使用於半導體製造方法。
  9. 如請求項7所述之製品，其使用於化學加工方法。
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