TW201421781A - 石墨烯電極、包含其之能量儲存裝置、及其製造方法 - Google Patents
石墨烯電極、包含其之能量儲存裝置、及其製造方法 Download PDFInfo
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Abstract
本發明提供一種石墨烯電極、包含其之能量儲存裝置、及其製造方法。其中,該石墨烯電極包含一金屬箔;一未摻雜石墨烯層;以及、一異原子摻雜石墨烯層,其中該異原子摻雜石墨烯層與該金屬箔係被該未摻雜石墨烯層隔開。
Description
本發明係有關於一種石墨烯電極結構及其製造方法,且特別是有關於一種可應用於能量儲存裝置之石墨烯電極結構及其製造方法。
隨著綠色環保議題受到世界各國的重視,電動車的開發已成為目前最熱門的研究課題之一。然而,傳統鋰離子電池無法滿足電動車對於所使用之電池的高電容量、高功率以及快充等需求。為改善傳統鋰離子電池,業界目前亟需能夠取代石墨的新世代負極材料。
石墨烯因具備優異的電子導電度和多孔性結構,使得電子的傳導以及鋰離子的擴散都相當快速。另外,由於石墨烯的不規則結構,使其具備比石墨更高的電容量。然而,由於石墨烯的不可逆電容太大及導電度較低,使得石墨烯負極在鋰電池的應用遲遲無法商業化。
本發明提供一種石墨烯電極及其製造方法,係利用一乾式表面改質處理,在低溫下對石墨烯表面進行異原子摻雜,可提昇石墨烯電極的電容量、以及降低不可逆電容。此外,所得之石墨烯電極適合應用於能源儲存系統中。
本發明所述之石墨烯電極,包含:一金屬箔;一未摻雜石墨烯層;以及,一異原子摻雜石墨烯層,其中該異原
子摻雜石墨烯層與該金屬箔係被該未摻雜石墨烯層隔開。
本發明亦提出一種石墨烯電極的製造方法,用以形成上述之石墨烯電極。該方法包含,提供一金屬箔;形成一石墨烯層於該金屬箔之上;以及,對該石墨烯層進行一乾式表面改質處理,以將異原子摻雜至該石墨烯層表面。
根據本發明一實施例,本發明亦提供一種能量儲存裝置,其中該能量儲存裝置包含上述石墨烯電極作為一第一電極、一第二電極、以及一隔離膜配置於該第一電極與該第二電極之間。
為讓本發明之上述和其他目的、特徵、和優點能更明顯易懂,下文特舉出較佳實施例,並配合所附圖式,作詳細說明如下:
請參照第1圖,本發明所述之石墨烯電極100,可具有一金屬箔(metal foil)10,其上具有一石墨烯層20。其中,該石墨烯層20包含一未摻雜石墨烯層24,以及一異原子摻雜石墨烯層22。值得注意的是,該異原子摻雜石墨烯層22與該金屬箔10係被該未摻雜石墨烯層24所隔開。該金屬箔10之材質可為一導電金屬,例如為一銅箔。該金屬箔10的厚度並無限制,可例如介於0.1至200μm之間。該異原子摻雜石墨烯層22係為該石墨烯層20的表面21經一異原子23摻雜後所得,而該石墨烯層20未被摻雜的部份則被定義為該未摻雜石墨烯層24。該異原子23可為氮原子、磷原子、硼原子、或其組合,例如為氮原子。該異原子摻
雜石墨烯層22可具有一異原子摻雜量介於0.1-3 atom%(原子百分比)之間,上述原子百分比的分母係為該異原子摻雜石墨烯層22的總原子數。該未摻雜石墨烯層24可為單層石墨烯(graphene)、多層石墨烯(graphene nanosheets、GNS)、或上述之組合;且該異原子摻雜石墨烯層22可為異原子摻雜單層石墨烯(graphene)、異原子摻雜多層石墨烯(graphene nanosheets、GNS)、或上述之組合。
本發明亦提供上述石墨烯電極的製造方法,請參照第2圖,係為本發明一實施例所述石墨烯電極的製造方法之步驟流程圖。首先,提供一金屬箔(步驟101),該金屬箔可例如為一銅箔。接著,形成一石墨烯層於該金屬箔上(步驟102)。最後,對該石墨烯層進行一乾式表面改質處理,以將異原子摻雜至該石墨烯層表面(步驟103)。該乾式表面改質處理之目的在於將一異原子摻入該石墨烯層表面,以使該石墨烯層的一部份形成一異原子摻雜石墨烯層,而該石墨烯層其他未被異原子所摻雜的部份則定義為一未摻雜石墨烯層。該乾式表面改質處理可例如一電漿改質製程,值得注意的是,由於本發明僅需將異原子摻雜至該石墨烯層的表面,不需要使其擴散致整層石墨烯層,因此在進行該乾式表面改質處理時,不需要額外對該石墨烯層或金屬箔進行加熱。此外,在該電漿改質製程中通入一反應氣體,以使異原子摻入石墨烯層中。舉例來說,該反應氣體包含所欲摻雜之異原子的氣體(例如氮氣、氨氣、空氣、或其組合),或是含所欲摻雜之異原子的氣體(例如氮氣、氨氣、
空氣、或其組合)與其他氣體(例如氫氣、氬氣、氧氣、或其組合)的混合。根據本發明另一實施例,電漿改質製程中可進一步通入一承載氣體以穩定該電漿改質製程,該承載氣體可包含氦氣、氬氣、氮氣、氖氣、或其組合。本發明所述之電漿改質製程,所使用的反應器可為低壓(low pressure)操作之電漿反應器或是常壓(atmospheric pressure)操作之電漿反應器。在進行電漿改質製程時,由於所使用的機台不同,製程參數會有所改變,因此本發明在進行該進行電漿改質製程時,可依實際需要調整該反應氣體的流量、該承載氣體流量、反應壓力、功率、反應時間、以及石墨烯層與電漿反應器電極間的距離,以使異原子摻雜石墨烯層可具有一異原子摻雜量介於0.1-3 atom%(原子百分比)之間。
根據本發明一實施例,石墨烯層的形成方式可包含以下步驟。首先,在該金屬箔上形成一由一含石墨烯之組合物所構成之塗層,其中形成該塗層的方法可例如為網印、旋轉塗佈法(spin coating)、棒狀塗佈法(bar coating)、刮刀塗佈法(blade coating)、滾筒塗佈法(roller coating)、或浸漬塗佈法(dip coating)。接著,對該塗層進行一烘乾製程,得到一石墨烯層。該烘乾製程的溫度可介於40-150℃之間,烘烤時間可介於1分鐘至10小時。在此,該含石墨烯之組合物可包含一石墨烯、以及一增黏劑。根據本發明其他實施例,該含石墨烯之組合物可更包含一助導劑。該增黏劑可為水系複合增黏劑、有機增黏劑、或其組合,例如羧甲
基纖維素鈉鹽(CMC)、苯乙烯-丁二烯橡膠(styrene butadiene rubber、SBR)、或是聚偏氟乙烯(PVdF)。該助導劑可例如為石墨、碳黑、或其組合。
請參照第3圖,本發明亦提供一種能量儲存裝置(例如:鋰電池、或燃料電池)200,包含上述之石墨烯電極100。該能量儲存裝置200可包含一石墨烯電極作為第一電極202(例如負極)、一第二電極206(例如正極)、以及一隔離膜204,配置於該第一電極202與該第二電極206之間。值得注意的是,該石墨烯電極係以該異原子摻雜石墨烯層與該隔離膜接觸。該石墨烯電極係以。該第二電極206之材質係為一鋰或含有鋰的金屬氧化物,例如為鋰、LiCoO2、LiFePO4、LiCo1/3Ni1/3Mn1/3O2、LiMn2O4或其他正極材料及其組合。該隔離膜之材質係為一高分子,例如聚乙烯、聚丙烯、或其組合,且可具有複數之孔洞。該隔離膜204內可具有一電解質(未圖示),例如乙二醇碳酸酯(ethylene carbonate,EC)、碳酸丙烯(propylene carbonate,PC)、與丁酸內酯(gamma-butyrolactone,GBL)、碳酸二乙酯(diethyl carbonate,DEC)、碳酸二甲酯(dimethyl carbonate,DMC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)、與碳酸甲基丙基酯(methyl propyl carbonate、MPC)、碳酸亞乙烯酯(vinylene carbonate、VC)、鋰鹽或其組合。
為了讓本發明之上述和其他目的、特徵、和優點能更明顯易懂,下文特舉數實施例及比較實施例,來說明本發明所述之石墨烯電極、及包含其裝置。
首先取5.3571g的去離子水、以及0.0337g羧甲基纖維素鈉鹽(CMC,作為增黏劑)置入一反應瓶中,以均質機在2000 rpm的轉速下攪拌20分鐘。之後,加入0.0056g乙炔黑(由Timcal製造及販售,商品號為Super P,作為助導劑)、以及0.5g石墨烯(graphene)於反應瓶中,並攪拌20分鐘。接著,加入0.0562g苯乙烯-丁二烯橡膠(styrene butadiene rubber、SBR,作為增黏劑)於反應瓶中,並攪拌30分鐘,得到一含石墨烯之組合物。
接著,將上述含石墨烯之組合物以150μm的刮刀塗佈於一銅箔上形成一塗層,並在120℃烘乾,得到一具有石墨烯層之石墨烯電極(I)。
值得注意的是,石墨烯電極(I)的石墨烯層並未摻雜有任何之異原子。
將實施例所得之石墨烯電極(I)置於一電漿反應器內,其中該石墨烯電極(I)係以該銅箔部份置於一電漿反應器內的支撐基板(石墨烯層與電漿反應器電極間的距離為2.2mm)。接著,在通入氮氣(流量為5sccm)及氦氣(電漿反應器內5.88 L/min)於該電漿反應器後,在操作壓力為1atm、及射頻(RF)功率65W下對石墨烯極板表面進行電漿改質製程以將氮元素摻雜至該石墨烯層表面(此製程中不需要加
溫)。在反應6秒後,得到石墨烯電極(II)。
接著,以X光光電子光譜儀(X-ray Photoelectron Spectrometer、XPS)對所得之石墨烯電極(II)的表面進行分析,以統計石墨烯層表面的氮元素含量,結果請參照第4圖。
如實施例2之相同方式進行,但將實施例2所述之氮氣流量由5sccm增加至30sccm,得到石墨烯電極(III)。
接著,以X光光電子光譜儀(X-ray Photoelectron Spectrometer、XPS)對所得之石墨烯電極(III)的表面進行分析,以統計石墨烯層表面的氮元素含量,結果請參照第4圖。
如實施例2之相同方式進行,但將實施例2所述之反應時間由6秒增加至18秒,得到石墨烯電極(IV)。
接著,以X光光電子光譜儀(X-ray Photoelectron Spectrometer、XPS)對所得之石墨烯電極(IV)的表面進行分析,以統計石墨烯層表面的氮元素含量,結果請參照第4圖。
由該圖可知,在經電漿處理後,本發明所述之石墨烯電極(II)-(IV)的石墨烯層表面含有氮原子,証實氮原子確實摻入該石墨烯層表面。
如實施例2之相同方式進行,但將實施例2所述之之氮氣流量由5sccm增加至15sccm、且反應時間由6秒增加至18秒,得到石墨烯電極(V)。
如實施例2之相同方式進行,但將實施例2所述之之氮氣流量由5sccm增加至30sccm、且反應時間由6秒增加至18秒,得到石墨烯電極(VI)。
請參照表1,係顯示實施例2-6所述之電漿改質製程的製程參數。
將實施例1所述之石墨烯電極(I)經裁切成適當大小(直徑13mm)作為負極,搭配聚乙烯/聚丙烯(PE/PP)複合膜(厚度為20μm)作為隔離膜(注入乙二醇碳酸酯(ethylene carbonate、EC)、碳酸乙基甲基酯(ethyl methyl carbonate、EMC)、碳酸亞乙烯酯(vinylene carbonate、VC)以及1M的LiPF6作為電解液)、以及鋰金屬層作為正極,進行組裝,得到鈕釦型鋰電池(I)。
將實施例4所述之石墨烯電極(IV)經裁切成適當大小(直徑13mm)作為負極,搭配聚乙烯/聚丙烯(PE/PP)複合膜(厚度為20μm)作為隔離膜(注入乙二醇碳酸酯(ethylene carbonate,EC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)以及1M的LiPF6作為電解液)、以及鋰金屬層作為正極,進行組裝,得到鈕釦型鋰電池(II)。
將實施例5所述之石墨烯電極(I)經裁切成適當大小(直徑13mm)作為負極,搭配聚乙烯/聚丙烯(PE/PP)複合膜(厚度為20μm)作為隔離膜(注入乙二醇碳酸酯(ethylene carbonate,EC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)、碳酸乙基甲基酯(ethyl methyl
carbonate,EMC)以及1M的LiPF6作為電解液)、以及鋰金屬層作為正極,進行組裝,得到鈕釦型鋰電池(III)。
將實施例6所述之石墨烯電極(I)經裁切成適當大小(直徑13mm)作為負極,搭配聚乙烯/聚丙烯(PE/PP)複合膜(厚度為20μm)作為隔離膜(注入乙二醇碳酸酯(ethylene carbonate,EC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)、碳酸乙基甲基酯(ethyl methyl carbonate,EMC)以及1M的LiPF6作為電解液)、以及鋰金屬層作為正極,進行組裝,得到鈕釦型鋰電池(IV)。
將實施例7所得之電池(I)及實施例8所得之電池(II)進行充放電測試,得到充放電曲線圖如第5圖所示。
接著,對實施例7所得之電池(I)及實施例8所得之電池(II)在不同的充电率(C-rate)下評估其放電電容,結果請參照第6圖。由圖可知,電池(II)(具有經電漿改質製程摻入氮原子的石墨烯電極)在不同的充电率(C-rate)下,其電容量皆大於電池(I)(石墨烯電極未摻雜氮原子)的電容量。
將實施例7所得之電池(I)、實施例9所得之電池(III)、以及實施例10所得之電池(IV)進行電池循環壽命測試,結果如第7圖所示。由該圖可知,電池(III)及電池(IV)(具有經電漿改質製程摻入氮原子的石墨烯電極)其電容量都比
具有未進行電漿改質製程之石墨烯電極的電池(I)來得高。尤其是電池(III),其電容量足足高出電池(I)1倍之多,效果相當優異。此外,由電池循環壽命測試的結果可知,電池(III)及電池(IV)在使用數次後其效能仍維持一定的水準。
將實施例7所得之電池(I)、實施例8所得之電池(II)、及實施例9所得之電池(III)進行充放電循環測試,並量測其不可逆電容與庫侖效率,結果如表2所示。
由表2可知,具有本發明所述石墨烯電極的電池,無論是在第1循環充放電測試或第2循環充放電測試,其庫侖效率明顯增加,且不可逆電容大幅下降,這表示經過電漿改質製程的石墨烯電極在電性表現上更加穩定。
基於上述,本發明所述之石墨烯電極,由於其石墨烯層表面經過一乾式表面改質處理,提升了石墨烯的電化學特性(電容量與載子遷移率增加、不可逆電容下降),因此非常適合應用於能源儲存裝置中。
雖然本發明已以數個較佳實施例揭露如上,然其並非
用以限定本發明,任何所屬技術領域中具有通常知識者,在不脫離本發明之精神和範圍內,當可作任意之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
10‧‧‧金屬箔
20‧‧‧石墨烯層
21‧‧‧表面
22‧‧‧異原子摻雜石墨烯層
23‧‧‧異原子
24‧‧‧未摻雜石墨烯層
100‧‧‧石墨烯電極
101、102、103‧‧‧步驟
200‧‧‧能量儲存裝置
202‧‧‧第一電極
204‧‧‧隔離膜
206‧‧‧第二電極
第1圖係為一剖面示意圖,說明本發明一實施例所之石墨烯電極。
第2圖係為本發明一實施例所述之石墨烯電極製造方法之步驟流程圖。
第3圖係為一剖面示意圖,說明本發明一實施例所之能量儲存裝置。
第4圖係說明石墨烯電極(II)、石墨烯電極(III)、及石墨烯電極(IV)其異原子摻雜石墨烯層之氮元素含量。
第5圖係為電池(I)及電池(II)之充放電曲線圖。
第6圖係說明電池(I)及電池(II)不同的充电率(C-rate)下的放電電容。
第7圖係為電池(I)、電池(III)、以及電池(IV)其充放電次數及放電電容關係圖。
10‧‧‧金屬箔
20‧‧‧石墨烯層
21‧‧‧表面
22‧‧‧異原子摻雜石墨烯層
23‧‧‧異原子
24‧‧‧未摻雜石墨烯層
100‧‧‧石墨烯電極
Claims (21)
- 一種石墨烯電極,包含:一金屬箔;一未摻雜石墨烯層;以及一異原子摻雜石墨烯層,其中該異原子摻雜石墨烯層與該金屬箔係被該未摻雜石墨烯層隔開。
- 如申請專利範圍第1項所述之石墨烯電極,其中該異原子摻雜石墨烯層所摻雜之異原子包含氮原子、磷原子、硼原子、或其組合。
- 如申請專利範圍第1項所述之石墨烯電極,其中該異原子摻雜石墨烯層之異原子摻雜量係介於0.1-3atom%,以該異原子摻雜石墨烯層的總原子數為基準。
- 如申請專利範圍第1項所述之石墨烯電極,其中該未摻雜石墨烯層係為單層石墨烯、多層石墨烯、或上述之組合。
- 如申請專利範圍第1項所述之石墨烯電極,其中該異原子摻雜石墨烯層係為異原子摻雜單層石墨烯、異原子摻雜多層石墨烯、或上述之組合。
- 一種石墨烯電極之製造方法,包含:提供一金屬箔;形成一石墨烯層於該金屬箔之上;以及對該石墨烯層進行一乾式表面改質處理,以將異原子摻雜至該石墨烯層表面。
- 如申請專利範圍第6項所述之石墨烯電極之製造方法,其中該異原子包含氮原子、磷原子、硼原子、或其組 合。
- 如申請專利範圍第6項所述之石墨烯電極之製造方法,其中該異原子摻雜至該石墨烯層表面,形成一異原子摻雜石墨烯層。
- 如申請專利範圍第6項所述之石墨烯電極之製造方法,其中該石墨烯層至少一部份未摻雜該異原子。
- 如申請專利範圍第9項所述之石墨烯電極之製造方法,其中該石墨烯層未摻雜該異原子的部份係定義為一未摻雜石墨烯層。
- 如申請專利範圍第6項所述之石墨烯電極之製造方法,其中該石墨烯層的形成方式包含:在該金屬箔上形成一由一含石墨烯之組合物所構成之塗層;以及對該塗層進行一烘乾製程,得到一石墨烯層。
- 如申請專利範圍第11項所述之石墨烯電極之製造方法,其中該含石墨烯之組合物包含:一石墨烯;以及一增黏劑。
- 如申請專利範圍第12項所述之石墨烯電極之製造方法,其中該增黏劑包含水系複合增黏劑、有機增黏劑、或其組合。
- 如申請專利範圍第12項所述之石墨烯電極之製造方法,其中該含石墨烯之組合物更包含一助導劑。
- 如申請專利範圍第14項所述之石墨烯電極之製造 方法,其中該助導劑包含石墨、碳黑、或其組合。
- 如申請專利範圍第6項所述之石墨烯電極之製造方法,其中該乾式表面改質處理包含一電漿改質製程。
- 如申請專利範圍第16項所述之石墨烯電極之製造方法,其中在該電漿改質製程中通入一反應氣體,且該反應氣體包含氮氣、氨氣、空氣、或其組合。
- 如申請專利範圍第17項所述之石墨烯電極之製造方法,其中該反應氣體更包含氬氣、氫氣、氧氣、或其組合。
- 如申請專利範圍第17項所述之石墨烯電極之製造方法,其中在該電漿改質製程中進一步通入一承載氣體,且該承載氣體包含氦氣、氬氣、氮氣、氖氣、或其組合。
- 一種能量儲存裝置,包含:一第一電極,其中該第一電極係為申請專利範圍第1項所述之石墨烯電極;一第二電極;以及一隔離膜,配置於該第一電極與該第二電極之間。
- 如申請專利範圍第20項所述之能量儲存裝置,其中該能量儲存裝置係為一鋰電池、或一燃料電池。
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CN201210528039.1A CN103840129A (zh) | 2012-11-21 | 2012-12-10 | 石墨烯电极、包含它的能量储存装置、及其制造方法 |
US13/949,732 US20140141355A1 (en) | 2012-11-21 | 2013-07-24 | Graphene electrode, energy storage device employing the same, and method for fabricating the same |
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CN106033808B (zh) * | 2015-03-17 | 2019-08-13 | 石东益 | 硅基电极及其制作工艺 |
CN106033807B (zh) * | 2015-03-17 | 2019-08-13 | 石东益 | 硅基电极制作工艺及其储能装置 |
CN104953102A (zh) * | 2015-06-29 | 2015-09-30 | 北京理工大学 | 一种适用于工业化生产的锂硫电池的制备 |
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CN109987597B (zh) * | 2018-12-25 | 2020-10-30 | 宁波大学 | 一种异性堆叠石墨烯的制备方法 |
US10431811B1 (en) * | 2018-12-31 | 2019-10-01 | Sf Motors, Inc. | Electric vehicle battery cell having water-based Li-ion anode slurry and process of preparing same |
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US20140030590A1 (en) * | 2012-07-25 | 2014-01-30 | Mingchao Wang | Solvent-free process based graphene electrode for energy storage devices |
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