TW202406986A - 石墨片、製造其的方法以及用於製造其之聚醯亞胺膜 - Google Patents
石墨片、製造其的方法以及用於製造其之聚醯亞胺膜 Download PDFInfo
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- TW202406986A TW202406986A TW112125450A TW112125450A TW202406986A TW 202406986 A TW202406986 A TW 202406986A TW 112125450 A TW112125450 A TW 112125450A TW 112125450 A TW112125450 A TW 112125450A TW 202406986 A TW202406986 A TW 202406986A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 124
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- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 238000000034 method Methods 0.000 title claims description 22
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 6
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- CKOFBUUFHALZGK-UHFFFAOYSA-N 3-[(3-aminophenyl)methyl]aniline Chemical compound NC1=CC=CC(CC=2C=C(N)C=CC=2)=C1 CKOFBUUFHALZGK-UHFFFAOYSA-N 0.000 claims description 3
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- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本發明公開一種按聚醯亞胺膜包含的醯亞胺化催化劑的總重量100重量%基準,包含1.5重量%以上、8重量%以下的磷類化合物的用於製造石墨片之聚醯亞胺膜及由此製得之石墨片。
Description
本發明係關於用於石墨片之聚醯亞胺膜及由此製得之石墨片。
最近,電子設備正在實現輕量化、小型化、超薄化和高積體化,因而在電子設備中產生大量的熱。這種熱會縮短製品壽命或誘發故障、失靈等。因此,對電子設備的熱管理正成為重要關注點。
石墨片具有比銅或鋁等金屬片更高的導熱率,作為電子設備的散熱構件而受到關注。
石墨片可以多樣方法製造,例如可使高分子膜碳化並石墨化而製造。特別是聚醯亞胺膜,由於優異的力學、熱尺寸穩定性、化學穩定性等,作為用於製造石墨片的高分子膜正在受到關注。
在用於製造石墨片之聚醯亞胺膜中使用了多樣的添加劑,其中,可塑劑廣泛用於提高聚醯亞胺膜的物性,但在將包含可塑劑的聚醯亞胺膜轉換成石墨片時,發生熱擴散係數和外觀品質低下等問題,因而要求針對此的解決方案。
另外,最近為了將石墨片應用於實現小型化和複雜化的電子製品,要求石墨片具有優異的耐折特性,而耐折特性和熱擴散特性通常表現出相反的傾向。
因此,要求開發一種耐折特性和熱擴散特性均優異的石墨片。
[技術課題]
本發明的目的係提供一種在製造石墨片時,機械特性和熱特性不低下特別是耐折特性優異的可製造石墨片之聚醯亞胺膜。
本發明的另一目的係提供一種由前述聚醯亞胺膜製造石墨片之方法及由此製得之品質優異的石墨片。
[技術方案]
為實現如上所述目的,本發明一實施形態提供一種用於製造石墨片之聚醯亞胺膜,按聚醯亞胺膜包含的醯亞胺化催化劑的總重量100重量%基準,包含1.5重量%以上、8重量%以下的磷類化合物。
本發明另一實施形態提供一種石墨片的製造方法,包括將前述聚醯亞胺膜進行碳化、石墨化或碳化及石墨化的步驟。
本發明又一實施形態提供一種根據前述石墨片之製造方法製造且MIT折疊次數為50,000次以上的石墨片。
[發明效果]
本發明具有的效果係提供一種包含磷類化合物的聚醯亞胺膜、由前述聚醯亞胺膜製造石墨片之方法及由此製得之特性優異的石墨片。
下文對本發明的實現例和實施例進行詳細描述,以便本發明所屬技術領域的一般技藝人士可以容易地實施。但是,本發明可以以多種不同形態體現,不限定於在此描述的實現例和實施例。在本說明書通篇中,當提到某部分「包括」某構成要素時,除非另有特別說明,意指不排除其他構成要素,可以還包括其他構成要素。
只要上下文未明確表示不同,本說明書中單數的表達包括複數的表達。
在解釋構成要素方面,即使沒有另外的明確記載,也解釋為包括誤差範圍。
在本說明書中,在表示數值範圍的「a至b」中,「至」定義為≥a且≤b。
本發明一個態樣的用於製造石墨片之聚醯亞胺膜,按前述聚醯亞胺膜包含的醯亞胺化催化劑的總重量100重量%基準,可包括1.5重量%以上、8重量%以下的磷類化合物。
例如,前述磷類化合物的含量按前述聚醯亞胺膜包括的前述醯亞胺化催化劑的總重量100重量%基準,可為2重量%以上、6重量%以下,3重量%以上、6重量%以下,或4重量%以上、6重量%以下。
當磷類化合物含量超出前述範圍時,利用前述用於製造石墨片之聚醯亞胺膜製造的石墨片的耐折特性(MIT折疊次數)會低下,伸長率會低下。
如將包括磷類化合物的聚醯亞胺膜煆燒以製造石墨片,則各石墨烯層不均一,形成皺褶形態的層疊形態,藉由後續軋製製程,在石墨烯層間形成細微皺褶。
形成的細微皺褶提高了最終製造的石墨片的耐折特性(MIT折疊次數)。
相反,若煆燒不含磷類化合物的聚醯亞胺膜以製造石墨片,則各石墨烯層均一,形成按既定間隔層疊的形態,為了應用於可折疊設備,在軋製製程之後藉由補充製程,形成人為皺褶或折疊區域。
形成的人為皺褶或折疊區域相比在石墨烯層間形成的細微皺褶,無法極大提高石墨片的耐折特性。
在一實現例中,前述用於製造石墨片之聚醯亞胺膜的磷(P)元素含量可為1,200 ppm以上、5,000 ppm以下。
例如,磷(P)元素的含量可為2,500 ppm以上、3,000 ppm以上、3,500 ppm以上或4,000 ppm以上、4,500 ppm以上。
在一實現例中,前述磷類化合物可為選自由三苯基磷酸酯(triphenyl phosphate)、磷酸三甲苯酯(tricresyl phosphate)、三苯基膦(triphenylphosphine)、間苯二酚雙(二苯基磷酸酯)(resorcinol bis(diphenyl phosphate))、雙酚A雙(磷酸二苯酯)(bisphenol A bis(diphenyl phosphate))、磷酸三乙酯(triethyl phosphate)、三異丙基磷酸酯(trixylyl phosphate)和磷酸甲苯二苯酯(cresyl diphenyl phosphate)構成的組的任一種。
例如,前述磷類化合物可為三苯基磷酸酯(triphenyl phosphate)或磷酸三甲苯酯(tricresyl phosphate)。
在一實現例中,用於製造前述用於製造石墨片之聚醯亞胺膜的聚醯胺酸溶液的固形物含量可為15重量%以上、20重量%以下。
在前述固形物的範圍內,固形物含量越低,利用前述用於製造石墨片之聚醯亞胺膜製造的石墨片的耐折特性(MIT折疊次數)和伸長率特性越提高。
另一方面,當固形物含量超出前述範圍時,利用前述用於製造石墨片之聚醯亞胺膜製造的石墨片的耐折特性(MIT折疊次數)會低下,伸長率會低下。
在一實現例中,前述用於製造石墨片之聚醯亞胺膜係將藉由二酐單體和二胺單體的反應而形成的聚醯胺酸實現醯亞胺化而製造,前述聚醯胺酸可以具有100,000至300,000的重均分子量。
在前述範圍內製造石墨片時,會容易石墨化。其中,「重均分子量(weight-average molecular weight)」可使用凝膠色譜法(GPC),將聚苯乙烯用作標準樣品進行測量。聚醯胺酸的重均分子量例如可為100,000至300,000,又例如可為150,000至250,000,再例如可為200,000至250,000,但不限於此。
作為用於形成前述用於製造石墨片之聚醯亞胺膜的二酐單體和二胺單體,可使用聚醯亞胺膜製造領域通常使用的多樣單體。
例如,前述用於製造石墨片之聚醯亞胺膜的二酐單體可為芳族二酐單體,二胺單體可為芳族二胺單體。作為二酐單體,可使用但不限於均苯四甲酸二酐、3,3',4,4'-聯苯四甲酸二酐、2,3,3',4'-聯苯四羧酸二酐、氧二鄰苯二甲酸二酐、二苯碸-3,4,3',4'-四甲酸二酐、雙(3,4-二羧基苯基)硫醚二酐、2,2-雙(3,4-二羧基苯基)-1,1,1,3,3,3-六氟丙烷二酐、2,3,3',4'- 二苯甲酮四甲酸二酐、3,3',4,4'-二苯甲酮四甲酸二酐、雙(3,4-二羧基苯基)甲烷二酐、2,2-雙(3,4-二羧基苯基)丙二酐、對亞苯基雙(偏苯三酸單酯酐)、對亞聯苯雙(偏苯三酸單酯酐)、間三聯苯3,4,3',4'-四甲酸二酐、對三聯苯-3,4,3',4'-四甲酸二酐、1,3-雙(3,4-二羧基苯氧基)苯二酐、1,4-雙(3,4-二羧基苯氧基)苯二酐、1,4-雙(3,4-二羧基苯氧基)聯苯二酐、2,2-雙[(3,4-二羧基苯氧基)苯基]丙烷二酐、2,3,6,7-萘四甲酸二酐、1,4,5,8-萘四甲酸二酐、4,4'-(2,2-六氟異丙叉)二鄰苯二甲酸二酐或其組合。作為二胺單體,可使用但不限於包含1個苯環的二胺單體(例如,1,4-二胺基苯、1,3-二胺基苯、2,4-二胺基甲苯、2,6-二胺基甲苯、3,5-二胺基苯甲酸等)、包含2個苯環的二胺單體(例如,4,4'-二胺基二苯醚、3,4'-二胺基二苯醚等二胺基二苯醚,4,4'-二胺基二苯甲烷、3,3'-二甲基-4,4'-二胺基聯苯、2,2'-二甲基-4,4'-二胺基聯苯、2,2'-雙(三氟甲基)-4,4'-二胺基聯苯、3,3'-二甲基-4,4'-二胺基二苯甲烷、3,3'-二羧基-4,4'-二胺基二苯甲烷、3,3',5,5'-四甲基-4,4'-二胺基二苯甲烷、雙(4 -胺基苯)硫醚、4,4'-二胺基苯甲醯苯胺、3,3'-二甲基聯苯胺、2,2'-二甲基聯苯胺、3,3'-二甲氧基聯苯胺、2,2'-二甲氧基聯苯胺、3,3'-二胺基二苯醚、3,4'-二胺基二苯醚、4,4'-二胺基二苯醚、3,3'-二胺基二苯硫醚、3,4'-二胺基二苯硫醚、4,4'-二胺基二苯硫醚、3,3'-二胺基二苯碸、3,4'-二胺基二苯碸、4,4'-二胺基二苯碸、3,3'-二胺基二苯甲酮、4,4'-二胺基二苯甲酮、3,3'-二胺基-4,4'-二氯二苯甲酮、3,3'-二胺基-4,4'-二甲氧基二苯甲酮、3,3'-二胺基二苯甲烷、3,4'-二胺基二苯甲烷、4,4'-二胺基二苯甲烷、2,2-雙(3-胺基苯基)丙烷、2,2-雙(4-胺基苯基)丙烷、2,2-雙(3-胺基苯基)-1,1,1,3,3,3-六氟丙烷、2,2-雙(4-胺基苯基)-1, 1,1,3,3,3-六氟丙烷、3,3'-二胺基二苯亞碸、3,4'-二胺基二苯亞碸、4,4'-二胺基二苯亞碸等)、包含3個苯環的二胺單體(例如,1,3-雙(3-胺基苯基)苯、1,3-雙(4-胺基苯基)苯、1,4-雙(3-胺基苯基)苯、1,4-雙(4-胺基苯基)苯、1, 3-雙(4-胺基苯氧基)苯、1,4-雙(3-胺基苯氧基)苯、1,3-雙(3-胺基苯氧基)-4-三氟甲基苯、3,3'-二胺基-4-(4-苯基)苯氧基二苯甲酮、3,3'-二胺基4 ,4'-二(4-苯基苯氧基)二苯甲酮、1,3-雙(3-胺基苯硫醚)苯、1,3-雙(4-胺基苯硫醚)苯、1,4-雙(4-胺基苯硫醚)苯、1,3-雙(3-胺基苯碸)苯、1,3-雙(4-胺基苯碸)苯、1,4-雙(4-胺基苯碸)苯、1,3-雙[2-(4-胺基苯基)異丙基]苯、1, 4-雙[2-( 3-胺基苯基)異丙基]苯、1,4-雙[2-(4-胺基苯基)異丙基]苯等)、包含4個苯環的二胺單體(例如,3,3'-雙(3-胺基苯氧基)聯苯、3,3'-雙(4-胺基苯氧基)聯苯、4,4'-雙(3-胺基苯氧基)聯苯、4, 4'-雙(4-胺基苯氧基)聯苯、雙[3-(3-胺基苯氧基)苯基]醚、雙[3-(4-胺基苯氧基)苯基]醚、雙[4-(3-胺基苯氧基)苯基]醚、雙[4-(4-胺基苯氧基)苯基]醚、雙[3-(3-胺基苯氧基)苯基]酮、雙[3-(4-胺基苯氧基)苯基]酮、雙[4-(3-胺基苯氧基)苯基]酮、雙[4-(4-胺基苯氧基)苯基]酮、雙[3-(3-胺基苯氧基)苯基]硫醚、雙[3-(4-胺基苯氧基)苯基]硫醚、雙[4-(3-胺基苯氧基)苯基]硫醚、雙[4-(4-胺基苯氧基)苯基]硫醚、雙[3-(3-胺基苯氧基)苯基]碸、雙[3-(4-胺基苯氧基)苯基]碸、雙[4-(3-胺基苯氧基)苯基]碸、雙[4-(4-胺基苯氧基)苯基]碸、雙[3-(3-胺基苯氧基)苯基]甲烷、雙[3-(4-胺基苯氧基)苯基]甲烷、雙[4-(3-胺基苯氧基)苯基])苯基]甲烷、雙[4-(4-胺基苯氧基)苯基]甲烷、2,2-雙[3-(3-胺基苯氧基)苯基]丙烷、2,2-雙[3-(4-胺基苯氧基)苯基]丙烷、2,2 -雙[4-(3-胺基苯氧基)苯基]丙烷、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷、2,2-雙[3-(3-胺基苯氧基)苯基]-1,1 ,1,3,3,3-六氟丙烷、2,2-雙[3-(4-胺基苯氧基)苯基]- 1,1,1,3,3,3-六氟丙烷、2,2-雙[4-(3-胺基苯氧基)苯基]-1,1, 1,3,3,3-六氟丙烷、2,2-雙[4-(4-胺基苯氧基)苯基]-1,1,1,3,3,3-六氟丙烷等)或其組合。
特別是作為二酐單體,可使用均苯四甲酸二酐、3,3',4,4'-聯苯四甲酸二酐、2,3,3',4-聯苯四羧酸二酐、氧雙鄰苯二甲酸酐、雙(3,4-二羧基苯基)碸二酐、3,3',4,4'-二苯甲酮四甲酸二酐或其組合,作為二胺單體,可使用4,4'-二胺基二苯醚、3,4'-二胺基二苯醚、對苯二胺、間苯二胺、4,4'-亞甲基二苯胺、3,3'-二胺基二苯甲烷或其組合。
例如,作為二酐單體,可使用均苯四甲酸二酐,作為二胺單體,可使用4,4'-二胺基二苯醚。
前述用於製造石墨片之聚醯亞胺膜的厚度可為25至250 μm。用於製造石墨片之聚醯亞胺膜的厚度例如可為25至250 μm,又例如可為40至200 μm,但不限於此。
前述用於製造石墨片之聚醯亞胺膜可以藉由聚醯亞胺膜製造領域通常使用的多樣方法製造。例如,用於製造石墨片之聚醯亞胺膜可以但不限於如下製造,即,將1種以上二酐單體和1種以上二胺單體在溶劑中聚合而製造聚醯胺酸溶液後,在前述聚醯胺酸溶液中添加醯亞胺化催化劑、脫水劑及可選的昇華性無機填充劑、溶劑等,形成用於聚醯亞胺膜的組合物,將前述組合物製膜而製造。
使前述聚醯胺酸溶液實現醯亞胺化的過程可以藉由熱醯亞胺化法、化學醯亞胺化法或並用前述熱醯亞胺化法和化學醯亞胺化法的複合醯亞胺化法等公知的醯亞胺化法執行。
前述用於製造石墨片之聚醯亞胺膜中包含的昇華性無機填充劑總平均粒徑(D50)可為1至20 μm,昇華性無機填充劑總含量按聚醯亞胺膜總重量100重量%基準可為0.15至0.25重量%。
前述昇華性無機填充劑在聚醯亞胺膜的碳化和/或石墨化時可以昇華而誘導既定的發泡現象。這種發泡現象可使得碳化和/或石墨化時發生的昇華氣體順利排氣以能夠收得優質石墨片,隨著發泡而形成的既定空隙還可以提高石墨片的耐折性(「可撓性」)。
不過,過度發泡現象和由此導致的大量空隙會極大惡化石墨片的導熱性和機械物性,會在石墨片表面導致缺陷,因而昇華性無機填充劑的種類、含量和顆粒大小應慎重選擇。
對於「平均粒徑(D50)」,可將昇華性無機填充劑在二甲基甲醯胺溶劑中,在25℃下超聲波分散5分鐘後,利用粒度測量儀(laser diffraction particle size analyzer)(SALD-2201,日本島津公司)測量。
用於製造石墨片之聚醯亞胺膜中的昇華性無機填充劑總平均粒徑(D50)例如可為0.5至4.0 μm,又例如可為1.0至5.0 μm,再例如可為1.5至5.0 μm,再例如可為1.5 μm至小於2.5 μm,但不限於此。以聚醯亞胺膜總重量為基準,聚醯亞胺膜中的昇華性無機填充劑總含量例如可為0.07至0.35重量%,又例如可為0.1至0.3重量%,再例如可為0.15至0.3重量%,但不限於此。
前述昇華性無機填充劑可包括平均粒徑(D50)為0.1至2.0 μm的第一昇華性無機填充劑和平均粒徑(D50)為大於2.0 μm至5.0 μm的第二昇華性無機填充劑。
前述昇華性無機填充劑中的第一昇華性無機填充劑和第二昇華性無機填充劑的含量不特別限定,例如以昇華性無機填充劑總重量為基準,第一昇華性無機填充劑可以包含10至90重量%,第二昇華性無機填充劑可以包含10至90重量%。例如,以昇華性無機填充劑總重量為基準,第一昇華性無機填充劑的含量例如可為15至85重量%,又例如可為20至80重量%,再例如可為30至80重量%,再例如可為50至80重量%,第二昇華性無機填充劑的含量例如可為85至15重量%,又例如可為80至20重量%,再例如可為70至20重量%,再例如可為50至20重量%,但不限於此。
作為前述昇華性無機填充劑的示例,可以例如但不限於碳酸鈣、磷酸氫鈣、硫酸鋇等。
作為前述溶劑,只要是能夠溶解聚醯胺酸的,則不特別限定。例如,溶劑可包括非質子極性溶劑(aprotic polar solvent)。
特別是可以單獨使用二甲亞碸、二乙亞碸等亞碸類溶劑,N,N-二甲基甲醯胺、N,N-二乙基甲醯胺等甲醯胺類溶劑,N,N-二甲基乙醯胺、N,N-二乙基乙醯胺等乙醯胺類溶劑,N-甲基-2-吡咯啶酮、N-乙烯基-2-吡咯啶酮等吡咯啶酮類溶劑,苯酚、鄰、間、對甲酚、二甲酚、鹵代苯酚、兒茶酚等酚類溶劑,六甲基磷醯胺、γ-丁內酯等非質子極性溶劑等,或組合2種以上使用,但不限於此。
作為前述脫水劑,可以單獨使用乙酸酐、丙酸酐、丁酸酐、苯甲酸酐等,或組合2種以上使用,但不限於此。
前述製膜可以但不限於如下執行,即,將聚醯胺酸溶液在基材上塗成膜狀,在30至200℃溫度下加熱乾燥15秒至30分鐘而製造凝膠膜後,將去除了基材的凝膠膜在250至600℃溫度下熱處理15秒至30分鐘。
利用本申請的用於製造石墨片之聚醯亞胺膜製造石墨片時,能夠製造特性優異的石墨片。
本發明另一態樣的石墨片之製造方法包括:使本申請的用於製造石墨片之聚醯亞胺膜進行碳化、石墨化或碳化及石墨化的步驟。
前述碳化是使用於製造石墨片之聚醯亞胺膜的高分子鏈熱分解而形成包括非晶碳、非結晶碳和/或無定形碳的初級石墨片的製程,例如可包括但不限於將聚醯亞胺膜在減壓條件下或惰性氣體氣氛下,經10小時至30小時從常溫升溫至最高溫度1,000℃至1,500℃範圍的溫度並保持的步驟。視情況,為了碳的高取向性,亦可在碳化時利用熱壓機等對聚醯亞胺膜施加壓力,此時的壓力例如可為5kg/cm
2以上,又例如可為15kg/cm
2以上,再例如可為25kg/cm
2以上,但不限於此。
前述石墨化是對非晶碳、非結晶碳和/或無定形碳的碳元素進行重排以形成石墨片的製程,例如可包括但不限於將初級石墨片視情況在惰性氣體氣氛下,經2小時至30小時從常溫升溫至最高溫度2,500℃至3,000℃範圍的溫度並保持的步驟。視情況,為了碳的高取向性,亦可在石墨化時利用熱壓機等對初級石墨片施加壓力,此時的壓力例如可為100kg/cm
2以上,又例如可為200kg/cm
2以上,再例如可為300kg/cm
2以上,但不限於此。
本發明又一態樣的石墨片根據前述石墨片之製造方法而製造,MIT折疊次數可為50,000次以上。
例如,可為60,000次以上、70,000次以上、80,000次以上、90,000次以上、100,000次以上、150,000次以上、200,000次以上、250,000次以上、300,000次以上。在一實現例中,前述石墨片的密度可為2.00g/cm
3以上,伸長率可為2%以上。例如,前述石墨片的密度可為2.10g/cm
3以上、2.20g/cm
3以上、2.30g/cm
3以上。另外,前述石墨片的伸長率可為2.5%以上、3.0%以上、3.5%以上、4.0%以上、4.5%以上、5.0%以上、5.5%以上。
在一實現例中,前述石墨片的動態折疊次數可為210,000次以上。
另一方面,前述石墨片的強度和模數可以分別為41.3~84.9MPa、2.2~3.3Gpa,熱擴散係數和導熱係數可以分別為590~710mm
2/s和1,118~1,226W/(m*K)。下文藉由實施例,更詳細描述本發明。不過,這只是提出本發明較佳示例,不得從任何意義上解釋為本發明由此限定。
製造例1(聚醯亞胺膜的製造)
向反應器中投入二甲基甲醯胺205.0 g作為溶劑,將溫度調節為20℃。在其中添加作為二胺單體的4,4'-二胺基二苯醚(ODA) 21.5 g,接著添加作為二酐單體的均苯四甲酸二酐(PMDA) 23.4 g,製造了黏度為230,000cP的聚醯胺酸溶液。
接著,向所製造的聚醯胺酸溶液中混合作為脫水劑的乙酸酐39.5g、作為醯亞胺化劑的β-ficolin 4.8 g、作為昇華性無機填充劑的磷酸氫鈣(平均粒徑(D50):2.5 μm) 0.12 g和二甲基甲醯胺30.4 g。
另外,如下表1所示,添加適量磷酸三甲苯酯(tricresyl phosphate、TCP),製造了實施例1至7和比較例1至6的聚醯亞胺膜前驅物溶液。不過,比較例7使用了喹啉替代TCP。
使用刮刀將準備的聚醯亞胺膜前驅物溶液在SUS板(100SA,Sandvik)上流延38 μm並在100℃至200℃的溫度範圍下乾燥而製造了具有自支撐性的凝膠膜。
接著,將凝膠膜從SUS Plate剝離,固定至針架,並轉移至高溫拉幅機。將膜在高溫拉幅機中從200℃加熱至700℃後,冷卻至25℃,從針架分離,得到聚醯亞胺膜。
根據製造例1的製造方法所製造的實施例1至7和比較例1至7的聚醯亞胺膜的TCP含量、固形物含量、磷(P)元素含量、膜厚度和發泡厚度示出於下表1。
表1中過量使用TCP的比較例4,由於無法製膜而未能製造聚醯亞胺膜,無法測量磷含量、膜厚度和發泡厚度。
發泡厚度藉助數顯千分尺(標準型、三豐公司)進行了測量。
另外,磷(P)元素含量使用ICP-OES(Inductively Coupled Plasma Optical Emission Spectrometry,電感耦合電漿發射光譜法)進行了測量。
[表1]
TCP重量 (重量%) | 固形物含量 (重量%) | 磷(P)含量 (ppm) | 膜厚度 ( μm) | 發泡厚度 ( μm) | |
實施例1 | 1.50 | 18.5 | 1772 | 38 | 48 |
實施例2 | 2.00 | 18.5 | 3440 | 38 | 59 |
實施例3 | 3.00 | 18.5 | 2600 | 38 | 54 |
實施例4 | 4.00 | 18.5 | 3390 | 38 | 59 |
實施例5 | 6.00 | 18.5 | 4720 | 38 | 61 |
實施例6 | 4.00 | 15 | 3754 | 38 | 54 |
實施例7 | 4.00 | 20.0 | 2916 | 38 | 51 |
比較例1 | 0 | 18.5 | 592 | 38 | 34 |
比較例2 | 0.30 | 18.5 | 708 | 38 | 34 |
比較例3 | 1.00 | 18.5 | 1090 | 38 | 42 |
比較例4 | 10.00 | 18.5 | - | - | - |
比較例5 | 4.00 | 10 | 5630 | 38 | 30 |
比較例6 | 4.00 | 25 | 2252 | 38 | 62 |
比較例7 | 使用喹啉(Quinoline) 1.0 mol% | 18.5 | 590 | 38 | 39 |
可以確認,隨著TCP含量的增加,磷含量和發泡厚度增加。
製造例2(石墨片的製造)
將根據製造例1製造的實施例1至7和比較例1至3及比較例5至7的聚醯亞胺膜,使用可碳化的電爐,在氮氣氣氛下以3.3℃/min的速度升溫至1,210℃,在1,210℃下保持了約2小時(碳化)。
無法製造聚醯亞胺膜的比較例4,當然也無法製造石墨片,無法測量石墨片的特性。
接著,使用可石墨化的電爐,在氬氣氣氛下以2.5℃/min的升溫速度從1,210℃升溫至2,200℃,執行了第一煆燒步驟。
達到2,200℃後,將升溫速度變更為1.25℃/min的升溫速度,連續升溫至2,500℃,執行了第二煆燒步驟。
達到2,500℃後,將升溫速度變更為10℃/min的升溫速度,連續升溫至2,800℃,執行了第三煆燒步驟,在2,800℃下靜置數分鐘後,完成石墨化,以10℃/min速度進行了冷卻。
然後,經軋製製造了石墨片。
將根據製造例2製造的石墨片的軋製厚度和密度示出於下表2。
密度是針對將所製造的石墨片截斷成15mmХ300mm(橫向Х縱向)大小的試片,使用比重瓶(AccuPyc 1340、Micromeritics),在常溫條件下使用氦氣進行了測量。
[表2]
用於製造石墨片之聚醯亞胺膜 | 軋製厚度 (μm) | 密度 (g/cm 3) |
實施例1 | 18 | 2.13 |
實施例2 | 2.24 | |
實施例3 | 2.18 | |
實施例4 | 2.30 | |
實施例5 | 2.23 | |
實施例6 | 2.02 | |
實施例7 | 2.05 | |
比較例1 | 1.84 | |
比較例2 | 1.96 | |
比較例3 | 2.06 | |
比較例4 | - | |
比較例5 | 1.71 | |
比較例6 | 2.31 | |
比較例7 | 1.93 |
使用實施例1至7的聚醯亞胺膜製造的石墨片的密度均為2.00g/cm
3以上。
另一方面,使用比較例1、2、5及7的聚醯亞胺膜製造的石墨片的密度不足2.00g/cm
3。
實驗例1
測量了使用實施例1至實施例7和比較例1至3及比較例5至7的聚醯亞胺膜並根據製造例2製造的石墨片的伸長率、強度和模數。
具體地,伸長率和強度使用Autograph萬能試驗機(日本島津公司,AG-IS),以根據ASTM D882的方法進行了測量。另外,利用英斯特朗5564型,以ASTM D882方法測量了模數。
實驗例1的測量結果示出於下表3。
[表3]
用於製造石墨片之聚醯亞胺膜 | 強度 (MPa) | 模數 (GPa) | 伸長率 (%) |
實施例1 | 41.3 | 2.2 | 2.6 |
實施例2 | 58.4 | 2.3 | 4.3 |
實施例3 | 72.9 | 3.3 | 4.8 |
實施例4 | 66.3 | 2.3 | 5.1 |
實施例5 | 84.9 | 2.9 | 5.6 |
實施例6 | 64.3 | 2.5 | 4.5 |
實施例7 | 46.8 | 2.7 | 3.1 |
比較例1 | 42.6 | 5.9 | 1.0 |
比較例2 | 64.5 | 10.3 | 1.0 |
比較例3 | 39.1 | 2.8 | 1.9 |
比較例4 | - | - | - |
比較例5 | 52.4 | 2.1 | 2.8 |
比較例6 | 43.6 | 2.6 | 2.9 |
比較例7 | 45.4 | 5.2 | 1.4 |
使用實施例1至實施例7的聚醯亞胺膜並根據製造例2製造的石墨片的強度、模數和伸長率,分別測量為41.3~84.9MPa、2.2~3.3Gpa和2.6~5.6%。
另一方面,使用比較例1至3、5和7的聚醯亞胺膜製造的石墨片,相比使用實施例1至實施例7的聚醯亞胺膜製造的石墨片,強度、模數和伸長率中任一項以上的特性低下。
大體上,隨著用於石墨片製造的聚醯亞胺膜包括的TCP含量增加,石墨片的伸長率表現出增加傾向。
比較在相同條件下,使用僅固形物含量不同的實施例4和實施例7的聚醯亞胺膜製造的石墨片,若固形物含量減少,則強度和伸長率升高,模數降低。
實驗例2
測量了使用實施例1至實施例7的聚醯亞胺膜並根據製造例2製造的石墨片的熱擴散係數和導熱係數。
具體地,對於熱擴散係數,將石墨片截斷成直徑1吋、厚度18μm大小而準備了樣品,使用測量裝置(耐馳公司、LFA 467),以激光閃光法測量了平面方向熱擴散係數。將如此測量的熱擴散係數值(在25℃溫度下分別測量5次的平均值)乘以密度(重量/體積)及比熱(理論值為0.85kJ/(kg•K))後算出了導熱係數。
實驗例2的測量結果示出於下表4。
[表4]
用於製造石墨片之聚醯亞胺膜 | 熱擴散係數 (mm 2/s) | 導熱係數 (W/(m*K)) |
實施例1 | 678 | 1,226 |
實施例2 | 621 | 1,183 |
實施例3 | 636 | 1,176 |
實施例4 | 625 | 1,220 |
實施例5 | 590 | 1,118 |
實施例6 | 601 | 1,032 |
實施例7 | 685 | 1,190 |
使用實施例1至實施例7的聚醯亞胺膜並根據製造例2所製造的石墨片的熱擴散係數和導熱係數,分別測量為590~685mm
2/s和1,032~1,226W/(m*K)。
比較在相同條件下,使用僅固形物含量不同的實施例4和實施例7的聚醯亞胺膜製造的石墨片,若固形物含量減少,則熱擴散係數降低,導熱係數升高。
實驗例3
測量了使用實施例1至實施例7和比較例1至7的聚醯亞胺膜並根據製造例2製造的石墨片的耐折特性(MIT折疊(folding)次數)。
具體地,使用MIT萬能試驗機,以每分鐘90次的速度實施左右135°(曲率:0.38R、Load:405.5g)彎曲試驗,測量了耐折特性。
若石墨片折斷,則將臨折斷前折疊次數作為表示石墨片耐折特性的MIT折疊(folding)次數。
實驗例3的測量結果示出於下表5。
[表5]
用於製造石墨片之聚醯亞胺膜 | MIT折疊次數 |
實施例1 | 54,061 |
實施例2 | 62,965 |
實施例3 | 98,331 |
實施例4 | 426,080 |
實施例5 | 105,381 |
實施例6 | 65,926 |
實施例7 | 252,375 |
比較例1 | 13,240 |
比較例2 | 29,434 |
比較例3 | 10,373 |
比較例4 | - |
比較例5 | 89,113 |
比較例6 | 45,610 |
比較例7 | 13,200 |
使用實施例1至實施例7的聚醯亞胺膜並根據製造例2製造的石墨片的MIT折疊次數,分別測量為54,061~426,080次,均為50,000次以上。
另一方面,使用比較例1至3、6和7的聚醯亞胺膜製造的石墨片,MIT折疊次數降低為不足50,000次。
大體上,隨著用於製造石墨片之聚醯亞胺膜包括的TCP含量的增加,石墨片的MIT折疊次數呈現增加後減少的傾向。
特別是使用實施例4(TCP包含4重量%)的聚醯亞胺膜製造石墨片時,石墨片的耐折特性最優異。
比較在相同條件下,使用僅固形物含量不同的實施例4和實施例7的聚醯亞胺膜製造的石墨片,確認了若固形物含量減少,則耐折特性提高。
實驗例4
測量了使用實施例1至實施例7和比較例1的聚醯亞胺膜並根據製造例2製造的石墨片的動態折疊(Dynamic folding)次數。
為了測量動態折疊次數,首先在所製造的石墨片的一面附著厚度為5μm的雙面膠,在相向面上貼合厚度為10 μm的保護膜,準備了測量樣品。
將所準備的測量樣品如圖1所示固定於作為測量裝置的動態折疊試驗機(Dynamic folding tester),按每分鐘60次的速度和0.5R或1.0的曲率半徑條件進行折疊實驗,如圖1的最左側測量樣品所示,若測量樣品折斷,則將臨折斷之前的折疊次數作為石墨片的動態折疊次數。
按大致每5萬次折疊次數區間確認了石墨片是否折斷。
示例性地,如圖1所示,以0.5R曲率半徑進行21萬次折疊,結果顯示,使用不含TCP的比較例1(原有)的聚醯亞胺膜製造的石墨片,在15萬次~20萬次折疊次數區間折斷,而使用實施例2(TCP包含2重量%)和實施例4(TCP包含4重量%)的聚醯亞胺膜製造的石墨片完全未發生損傷。
即,使用本申請實施例的聚醯亞胺膜製造的石墨片,均以0.5R的曲率半徑執行動態折疊測量,結果確認了動態折疊次數均超過21萬次。
即,顯示了使用本申請實施例1至實施例7的聚醯亞胺膜製造的石墨片具有優異的機械特性和熱特性。特別是顯示了極大提高的耐折特性。
本發明的製造方法的實施例只是用於使本發明所屬技術領域的一般技藝人士可以容易地實施本發明的較佳實施例,不限定於前述實施例,因此本發明的範圍不由此限定。因此,本發明真正的技術保護範圍應根據附帶的申請專利範圍的技術思想確定。另外,在不超出本發明的技術精神的範圍內可以進行多種置換、變形和變更,這是從業人員不言而喻的,可以由從業人員容易地變更的部分也包括於本發明的範圍內,這是不言而喻的。
無
圖1係示出本申請的石墨片的動態折疊次數測量裝置、以0.5R曲率半徑折疊21萬次後測量樣品的狀態及測量樣品折疊時的形態的照片。
Claims (9)
- 一種用於製造石墨片之聚醯亞胺膜,其按前述聚醯亞胺膜包含的醯亞胺化催化劑的總重量100重量%基準,包含1.5重量%以上、8重量%以下的磷類化合物。
- 如請求項1所述之用於製造石墨片之聚醯亞胺膜,其中,前述聚醯亞胺膜的磷(P)元素的含量為1,200 ppm以上、5,000 ppm以下。
- 如請求項1所述之用於製造石墨片之聚醯亞胺膜,其中,前述磷類化合物為選自由三苯基磷酸酯(triphenyl phosphate)、磷酸三甲苯酯(tricresyl phosphate)、三苯基膦(triphenylphosphine)、間苯二酚雙(二苯基磷酸酯)(resorcinol bis(diphenyl phosphate))、雙酚A雙(磷酸二苯酯) (bisphenol A bis(diphenyl phosphate))、磷酸三乙酯(triethyl phosphate)、三異丙基磷酸酯(trixylyl phosphate)和磷酸甲苯二苯酯(cresyl diphenyl phosphate)構成的組的任一種。
- 如請求項1所述之用於製造石墨片之聚醯亞胺膜,其中,用於製造前述用於製造石墨片之聚醯亞胺膜的聚醯胺酸溶液的固形物含量為15重量%以上、20重量%以下。
- 如請求項1所述之用於製造石墨片之聚醯亞胺膜,其中,前述聚醯亞胺膜由二酐單體和二胺單體形成,前述二酐單體包括均苯四甲酸二酐、3,3',4,4'-聯苯四羧酸二酐、2,3,3',4-聯苯四羧酸二酐、氧雙鄰苯二甲酸酐、雙(3,4-二羧基苯基)碸二酐、3,3',4,4'-二苯甲酮四甲酸二酐或其組合,前述二胺單體包括4,4'-二胺基二苯醚、3,4'-二胺基二苯醚、對苯二胺、間苯二胺、4,4'-二胺基二苯甲烷、3,3'-二胺基二苯甲烷或其組合。
- 一種石墨片之製造方法,其包括將如請求項1至5中任一項所述之聚醯亞胺膜進行碳化、石墨化或碳化及石墨化的步驟。
- 一種石墨片,其係如請求項6所述之石墨片之製造方法製造,前述石墨片的MIT折疊次數為50,000次以上。
- 如請求項7所述之石墨片,其中,前述石墨片的密度為2.00 g/cm 3以上,伸長率為2%以上。
- 如請求項7所述之石墨片,其中,前述石墨片的動態折疊次數為210,000次以上。
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