TWI601689B - 含氮之多孔性碳材料及其電容與製造方法 - Google Patents

含氮之多孔性碳材料及其電容與製造方法 Download PDF

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TWI601689B
TWI601689B TW105103168A TW105103168A TWI601689B TW I601689 B TWI601689 B TW I601689B TW 105103168 A TW105103168 A TW 105103168A TW 105103168 A TW105103168 A TW 105103168A TW I601689 B TWI601689 B TW I601689B
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nitrogen
porous carbon
containing porous
carbon material
group
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TW105103168A
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TW201728530A (zh
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李光哲
廖泊彥
彭志偉
蔡群賢
蔡群榮
李庭鵑
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台灣奈米碳素股份有限公司
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Priority to TW105103168A priority Critical patent/TWI601689B/zh
Priority to CN201610410863.5A priority patent/CN107021468A/zh
Priority to JP2016131365A priority patent/JP2017137229A/ja
Priority to US15/402,487 priority patent/US20170221646A1/en
Publication of TW201728530A publication Critical patent/TW201728530A/zh
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Description

含氮之多孔性碳材料及其電容與製造方法
本發明為有關一種多孔性碳材料，尤指一種含氮之多孔性碳材料及其電容與製造方法。
多孔碳材料是指具有不同孔徑大小的碳材料，其孔徑大小的範圍可以從具有相當於分子大小的奈米級孔徑，一直到適於微生物增殖及活動的微米級孔徑，且多孔碳材料又具有耐高溫、耐酸鹼、導電、傳熱等一系列優點，因此已廣泛的應用於氣體和液體的精製、水處理、空氣淨化、催化材料、電子能源材料、生物工程材料等方面。
多孔碳材料如美國發明專利公開第US 2014/0118884號之「Porous carbon material and manufacturing method thereof and supercapacitor」，其揭露了一種多孔性碳材料，包含有複數個大孔洞、複數個中孔洞與複數個微孔洞，其中各該大孔洞的孔徑大於50奈米，各該中孔洞的孔徑為2~50奈米，各該微孔洞的孔徑小於2奈米，該些大孔洞的孔洞體積的分布比例為10~25%，該些中孔洞的孔洞體積的分布比例為20~80%，該些微孔洞的孔洞體積的分布比例為0.01~20%。藉由調整該些大孔洞、該些中孔洞與該些微孔洞的孔洞體積的分布比例，可以使比表面積達到一最佳值，而可提高該多孔性碳材料的導電、導熱、氧化還原等性質。
然而，當比表面積達到一最佳值時，其導電、導熱、氧化還原等性質便會達到一定值，而無法更進一步的提升，因此，如何更進一步的提升多孔性碳材料的性質，使其在應用上更具有優勢，實為相關業者共同努力的目標。
本發明的主要目的，在於解決傳統多孔性碳材料的性質難以更進一步提升的問題。
為達上述目的，本發明提供一種含氮多孔性碳材料的製造方法，包含有以下步驟：
S1：將一碳材料、一高分子材料以及一改質材料混合形成一預成形體，該改質材料包含一氮，且該改質材料選自於由胺類、醯胺、含氮雜環有機化合物以及銨鹽所組成之群組，其中，於該預成形體中，該碳材料的重量百分比介於30%至85%，該高分子材料的重量百分比介於10%至60%，該改質材料的重量百分比介於3%至40%；
S2：對該預成形體進行一成形製程而得一成形體；以及
S3：對該成形體進行一高溫燒結，使一部分的該高分子材料被分解而去除，另一部分的該高分子材料和該碳材料共同形成一包含複數孔隙的骨幹結構，並使該改質材料中的該氮能附著於該骨幹結構形成一含氮官能基，而得到一含氮多孔性碳材料。
為達上述目的，本發明還提供一種含氮多孔性碳材料，係以前述方法製成，包含有該骨幹結構，大部分地由碳所組成並包含有該些孔隙以及與該骨幹結構鍵結的該含氮官能基。
為達上述目的，本發明更提供一種用於海水的儲能電容，包括一第一含氮多孔性碳板以及、一和該第一含氮多孔性碳板相隔設置的第二含氮多孔性碳板、一與該第一含氮多孔性碳板接觸的第一集流板以及一與該第二含氮多孔性碳板接觸的第二集流板，該第一含氮多孔性碳板、該第二含氮多孔性碳板、該第一集流板與該第二集流板設置於一海水中，且該第一含氮多孔性碳板和該第二含氮多孔性碳板並以申請專利範圍第1項之方法製成，其中，該海水中的氯化鈉解離為鈉離子和氯離子並分別進入該第一含氮多孔性碳板和該第二含氮多孔性碳板而儲能。
綜上所述，本發明具有以下特點：
一、 進行高溫燒結時，一部分的該高分子材料被分解而去除，另一部分的該高分子材料和該碳材料共同形成該骨幹結構和該些孔隙；搭配該改質材料因高溫而形成的該含氮官能基，而可進一步提高該含氮多孔性碳材料的導電、導熱、氧化還原、離子氧化還原、催化效率等等的性質，使該含氮多孔性碳材料在應用上更具有優勢。
二、 傳統的儲能電容，由於電極並非塊材的形式，故需要塗布於金屬集流板來形成層狀或片狀結構而被使用，又由於此種電極的厚度增加不易，當需要較大體積的電極時，只能增加電極的面積，此時金屬集流板的面積也需要相應增加；相較之下，利用本發明之方法所得到的含氮多孔性碳材料，係具有剛性，屬於塊材的形式，當用於儲能電容做為電極時，可以利用增加厚度的方式達到較大體積，以減少該第一集流板與該第二集流板的使用面積，進而減少材料的使用，因此，可以大量減少金屬集流板的使用和成本。
三、 藉由該第一含氮多孔性碳板和該第二含氮多孔性碳板具有含氮官能基，可以獲得一定量的贗電容，提高儲能能力。
有關本發明的詳細說明及技術內容，現就配合圖式說明如下：
請參閱「圖1」，本發明為一種含氮之多孔性碳材料及其電容與製造方法，其製造方法包含有以下步驟：
S1：將一碳材料、一高分子材料以及一改質材料混合形成一預成形體，該碳材料可以為碳黑、碳纖維、奈米碳管、氣相生長碳纖維、活性碳、石墨、石墨烯、中空碳、軟碳、硬碳或其組合，該高分子材料可以為酚醛樹脂(Phenol formaldehyde resin)、環氧樹脂(Epoxy)、聚丙烯腈(Polyacrylonitrile，簡稱PAN)、呋喃樹脂(Furan resin)、聚乙烯醇(Polyvinyl alcohol，簡稱PVA)、聚氯乙烯(Polyvinyl chloride，簡稱PVC)、纖維素(Cellulose)、聚偏二氟乙烯(Polyvinylidene fluoride，簡稱PVDF)、聚四氟乙烯(Polytetrafluoroethene，簡稱PTFE)、氟化乙烯丙烯共聚物(Fluorinated ethylene propylene，簡稱FEP)或其組合等，而該改質材料則可以為胺類、醯胺、含氮雜環有機化合物、銨鹽等等，且該改質材料包含有一氮，其中，胺類之通式為R1-NH 2或NH 2-R1-NH 2，其中R1可為C3-C24烷基，例如：丙胺、異丙胺、己胺、辛胺、十二烷基胺、3-甲基-2-氨戊烷、乙二胺等，R1也可為芳香基，例如：苯胺、甲苯胺、萘胺、聯苯胺、聯苯二胺、苯二胺、甲苯二胺、苯二胺、2,6-甲苯二胺等；醯胺之通式為R2-CONH 2，其中R2可為C1-C18烷基、環烷基，也可為芳香基，例如：苯基、萘基，R2還可為氨基，醯胺類可為乙醯胺、尿素、乙醯苯胺等；含氮雜環有機化合物可為五元雜環或六元雜環，五元雜環的實例如：吡咯烷、吡咯，六元雜環的實例如：吡啶、六氫吡啶、4-氨基-2-氧嘧啶、2,4-二氧嘧啶、三聚氰胺、5-甲基-2,4-二氧嘧啶；銨鹽之通式為NH 4COO-R3，其中R3可以為羥基，例如：碳酸氫銨，也可以為氨基，例如：氨基甲酸銨，R3亦可以直接由氫或甲基取代，例如：碳酸銨、乙酸銨，R3本身也可為銨基，例如：碳酸銨。
而於該預成形體中，該碳材料的重量百分比介於30%至85%，該高分子材料的重量百分比介於10%至60%，該改質材料的重量百分比介於3%至40%。
S2：對該預成形體進行一成形製程而得一成形體，於本實施例中，該成形製程係使該預成形體處於一介於100℃至220℃之間的受熱溫度以及一介於5 Kgf/cm 2至200 Kgf/cm 2之間的成形壓力，藉由該受熱溫度以及該成形壓力，調整該預成形體的緻密度以及立體結構，進而形成塊狀的該成形體。於本發明之一實施例中，該成形製程可為一熱壓製程，即同時施予該受熱溫度以及該成形壓力，但本發明並不以此為限，舉例來說，亦可先對該預成形體施予該受熱溫度，再施予該成形壓力，例如一模壓製程。
S3：對該成形體進行一高溫燒結，使一部分的該高分子材料被分解而去除，另一部分的該高分子材料和該碳材料共同形成一包含複數孔隙的骨幹結構，並使該改質材料中的該氮能附著於該骨幹結構形成一含氮官能基，而得到一含氮多孔性碳材料。於本發明中，當進行該高溫燒結時，另一部分的該高分子材料將扮演黏結劑的功能(Binder)，將該碳材料燒結為呈三維立體網狀的該骨幹結構，換句話說，該骨幹結構係大部分地由碳所組成。本實施例之高溫燒結為使該成形體處於一還原氣氛之中，該還原氣氛可以為氬氣或氮氣等，並處於一介於400℃至1200℃之間的加熱溫度，使該高分子材料於該成形體之中燃燒裂解，而使該含氮多孔性碳材料具有一介於10 % 至85 % 之間的孔隙率，該些孔隙的形成，使得該碳材料的表面積以及內部空間增加，並藉由形成該含氮官能基，而可進一步的提高該含氮多孔性碳材料的導電、導熱、氧化還原、離子氧化還原、催化效率等等的性質，使該含氮多孔性碳材料在應用上更具有優勢。
此外，於該高溫燒結的過程中，將可進一步產生一附著於該碳材料之間的外加碳材料，該外加碳材料可能為由該高分子材料或該改質材料燃燒裂解後而殘留於該碳材料之間，或可以由額外通入之含碳氣氛所提供，因此，最終所得之該含氮多孔性碳材料中，該碳材料的重量百分比會較剛添加時高，使導電性優良。
續搭配參閱「圖2」及「圖3」所示，為用於海水的儲能電容，其包含有一第一含氮多孔性碳板10、一第二含氮多孔性碳板20、一第一集流板40、一第二集流板50以及一海水30，該第一含氮多孔性碳板10與該第一集流板40接觸，該第二含氮多孔性碳板20與該第二集流板50接觸，且該第一含氮多孔性碳板10和該第二含氮多孔性碳板20為利用前述之製造方法所製作而成，並彼此相隔設置於做為電解質之用的該海水30之中，當外接一電源時，該海水30中的氯化鈉會解離為鈉離子和氯離子並分別進入該第一含氮多孔性碳板10和該第二含氮多孔性碳板20而儲能。
如「圖2」所示，為本發明的第一實施例，該第一集流板40與該第二集流板50為分別設置於該第一含氮多孔性碳板10與該第二含氮多孔性碳板20之內，而如「圖3」所示，為第二實施例，該第一集流板40為設置於該第一含氮多孔性碳板10遠離該第二含氮多孔性碳板20之一側，該第二集流板50為設置於該第二含氮多孔性碳板20遠離該第一含氮多孔性碳板10之一側，但設置方式不以此為限。
由於將該第一含氮多孔性碳板10和該第二含氮多孔性碳板20做為電容的電極使用，而可以不使用傳統電容中的隔離膜，以降低電容的製造成本，並可提高工作電壓，並可以長時間儲存能量，而由於該第一含氮多孔性碳板10和該第二含氮多孔性碳板20具有含氮官能基，可以獲得一定量的贗電容，提高儲能能力。此外，利用本發明之方法所得到的含氮多孔性碳材料，係具有剛性，屬於塊材的形式，而習知技術的電極為片狀，並為堆疊式結構，在相同體積電極的條件下，本發明可以利用增加該第一含氮多孔性碳板10和該第二含氮多孔性碳板20的厚度的方式達到較大體積，以減少該第一集流板40與該第二集流板50的使用面積，進而減少材料的使用，因此，可以大量減少金屬集流板的使用和成本。
綜上所述，本發明具有以下特點：
一、 進行高溫燒結時，一部分的該高分子材料被分解而去除，另一部分的該高分子材料和該碳材料共同形成該骨幹結構和該些孔隙；搭配該改質材料因高溫而形成的該含氮官能基，而可進一步提高該含氮多孔性碳材料的導電、導熱、氧化還原、離子氧化還原、催化效率等等的性質，使該含氮多孔性碳材料在應用上更具有優勢。
二、 傳統的儲能電容，由於電極並非塊材的形式，故需要塗布於金屬集流板來形成層狀或片狀結構而被使用，又由於此種電極的厚度增加不易，當需要較大體積的電極時，只能增加電極的面積，此時金屬集流板的面積也需要相應增加；相較之下，利用本發明之方法所得到的含氮多孔性碳材料，係具有剛性，屬於塊材的形式，當用於儲能電容做為電極時，可以利用增加厚度的方式達到較大體積，因此，可以大量減少金屬集流板的使用和成本。
三、 藉由該第一含氮多孔性碳板和該第二含氮多孔性碳板具有含氮官能基，可以獲得一定量的贗電容，提高儲能能力。
以上已將本發明做一詳細說明，惟以上所述者，僅爲本發明的一較佳實施例而已，當不能限定本發明實施的範圍。即凡依本發明申請範圍所作的均等變化與修飾等，皆應仍屬本發明的專利涵蓋範圍內。
10：第一含氮多孔性碳板 20：第二含氮多孔性碳板 30：海水 40：第一集流板 50：第二集流板 S1~S3：步驟
「圖1」，為本發明含氮多孔性碳材料的製作流程示意圖。 「圖2」，為本發明第一實施例的局部剖面應用示意圖。 「圖3」，為本發明第二實施例的應用示意圖。
S1~S3：步驟

Claims (12)

  1. 一種含氮多孔性碳材料的製造方法，包含有以下步驟：S1：將一碳材料、一高分子材料以及一改質材料混合形成一預成形體，該改質材料包含一氮，且該改質材料選自於胺類、醯胺、含氮雜環有機化合物、銨鹽所組成之群組，其中，於該預成形體中，該碳材料的重量百分比介於30%至85%，該高分子材料的重量百分比介於10%至60%，該改質材料的重量百分比介於3%至40%；S2：對該預成形體進行一成形製程而得一成形體，該成形製程係使該預成形體處於一介於100℃至220℃之間的受熱溫度以及一介於5Kgf/cm2至200Kgf/cm2之間的成形壓力；以及S3：對該成形體進行一高溫燒結，使一部分的該高分子材料被分解而去除，另一部分的該高分子材料和該碳材料共同形成一包含複數孔隙的骨幹結構，並使該改質材料中的該氮能附著於該骨幹結構形成一含氮官能基，而得到一含氮多孔性碳材料。
  2. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該碳材料選自於碳黑、碳纖維、奈米碳管、氣相生長碳纖維、活性碳、石墨、石墨烯、中空碳、軟碳及硬碳所組成的群組。
  3. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該高分子材料為選自酚醛樹脂、環氧樹脂、聚丙烯腈、呋喃樹脂、聚乙烯醇、聚氯乙烯、纖維素、聚偏二氟乙烯、聚四氟乙烯及氟化乙烯丙烯共聚物所組成之群組。
  4. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S3步驟中，該高溫燒結使該成形體處於一介於400℃至1200℃之間的加熱溫度。
  5. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S3步驟中，該含氮多孔性碳材料具有一介於10%至85%之間的孔隙率。
  6. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該胺類選自於由丙胺、異丙胺、己胺、辛胺、十二烷基胺、3-甲基-2-氨戊烷、乙二胺、苯胺、甲苯胺、萘胺、聯苯胺、聯苯二胺、苯二胺、甲苯二胺、苯二胺及2,6-甲苯二胺所組成之群組。
  7. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該醯胺選自於由乙醯胺、尿素及乙醯苯胺所組成之群組。
  8. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該含氮雜環有機化合物選自於由吡咯烷、吡咯、吡啶、六氫吡啶、4-氨基-2-氧嘧啶、2,4-二氧嘧啶、三聚氰胺及5-甲基-2,4-二氧嘧啶所組成之群組。
  9. 如申請專利範圍第1項所述之含氮多孔性碳材料的製造方法，其中於S1步驟中，該銨鹽選自於由氨基甲酸銨、碳酸氫銨、乙酸銨及碳酸銨所組成之群組。
  10. 一種如申請專利範圍第1項之製作方法而製成的含氮多孔性碳材料，包含有：該骨幹結構，大部分地由碳所組成並包含有該些孔隙；以及與該骨幹結構鍵結的該含氮官能基。
  11. 如申請專利範圍第10項所述之含氮多孔性碳材料，其中該骨幹結構具有一介於10%至85%之間的孔隙率。
  12. 一種用於海水的儲能電容，包括一第一含氮多孔性碳板、一和該第一含氮多孔性碳板相隔設置的第二含氮多孔性碳板、一與該第一含 氮多孔性碳板接觸的第一集流板以及一與該第二含氮多孔性碳板接觸的第二集流板，該第一含氮多孔性碳板、該第二含氮多孔性碳板、該第一集流板與該第二集流板設置於一海水中，且該第一含氮多孔性碳板和該第二含氮多孔性碳板以申請專利範圍第1項之方法製成。
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