TWI500206B - 共擠壓多層式電池隔離件 - Google Patents
共擠壓多層式電池隔離件 Download PDFInfo
- Publication number
- TWI500206B TWI500206B TW096138213A TW96138213A TWI500206B TW I500206 B TWI500206 B TW I500206B TW 096138213 A TW096138213 A TW 096138213A TW 96138213 A TW96138213 A TW 96138213A TW I500206 B TWI500206 B TW I500206B
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- TW
- Taiwan
- Prior art keywords
- polymer
- film
- improving
- battery separator
- layer
- Prior art date
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C48/32—Extrusion nozzles or dies with annular openings, e.g. for forming tubular articles
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- B29C48/08—Flat, e.g. panels flexible, e.g. films
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Description
本發明的電池隔離件為一共擠壓多層式電池隔離件。此隔離件之一實施例可用於鋰離子電池。
多層式電池隔離件揭露於例如,美國專利第4,650,730、5,240,655、5,281,491、5,691,047、5,691,077、6,080,507、6,878,226及美國專利公開案第20020136945號中。
雖然某些前述參考資料提及多層式隔離件可由共擠壓製程製造,但在商業實施上,此共擠壓製程不易施行於商業準則上。特別是,前述共擠壓試驗的產品伴隨著均勻度的問題,其約束這些製程所製造產品的商業化。這些問題相信是由於伴隨同時擠壓至少兩個相異聚合物經過一狹窄的孔洞模之複雜性而引發的。於是,先前技術對製造共擠壓多層式電池隔離件的嘗試仍產生不均勻產物。因此,無共擠壓多層式電池隔離件為可商業取得的。
因此,對於具有均勻物理性質的共擠壓多層式電池隔離件存有一需求。
一電池隔離件包括共擠壓、微孔隙膜,該膜具有至少
二由可擠壓聚合物製成的層且具有:標準偏差小於0.8微米(μm)的一均勻厚度;或剝離強度大於60克的層間黏合性。
即時電池隔離件的描述為有關在二次鋰離子電池(如:使用於行動電話、膝上型電腦及其他需要輕量充電儲存裝置的裝置)中的使用。然而,其可理解本發明並未因此受限,且即時電池隔離件可使用在其他電池系統(例如:NiMH、NiCd、鹼性、一次鋰離子、等)。
一般而言,用於鋰離子電池的電池隔離件為微孔隙膜,其具有下列物理性質:厚度-小於5密耳(125μm),或小於2密耳(50μm),或小於1密耳(25μm),可實施的最低限度為1/3密耳(8μm);擊穿強度-大於400克,或大於550克;平均孔徑-0.005-10.000μm,或0.01-5.00μm,或0.05-2.00μm;Gurley值(ASTM-D726(B))-5-100秒,或10-60秒。
此即時電池隔離件為共擠壓多層式電池隔離件。共擠壓意指聚合物同時一起置於一擠壓模中並由為一型式的模中擠出,此處該型式通常為一平面結構,且該型式具有藉由聚合物形成不連續層介面的摻混將至少二不連續層於不連續層的介面接合一起。擠壓模可以是平坦片材狀(或溝槽)模或吹膜(或環狀)模。此共擠壓製程將於後詳述。多層為指具有至少兩層之隔離件。多層也可為3、4、5、6、7或更多層的結構。每一層是經由分離的聚合物進料注入擠壓模形成。這些層可能是不同的厚度。更通常是,這些進料流的至少兩個為相異聚合物。相異聚合物為:聚合物具有不同的化學本質(如:PE與PP,或PE與及PE之一共聚物為具有不同化學性質之聚合物);及/或具有相同化學本質但不同的性質(如:密度、分子量、分子量分佈、流變學、添加劑(組成及/或百分比)等)之聚合物。然而,這些聚合物可為相同或一致。
可用於即時電池隔離件的聚合物為可擠壓的。這些聚合物一般稱為熱塑性聚合物。熱塑性聚合物的範例包括但未限制為聚烯烴、聚縮醛(或聚氧甲烯)、聚醯胺、聚酯、聚硫化物、聚乙烯醇、聚乙烯酯及聚偏乙烯。聚烯烴包括但未限制為聚乙烯(包括,例如LDPE、LLDPE、HDPE、UHDPE)、聚丙烯、聚丁烯、聚甲基戊烷、其等之共聚物及其等之摻合物。聚醯胺(尼龍)包括但未限制為聚醯胺6、聚醯胺66、尼龍10,10、聚鄰苯二甲醯胺(PPA)、其等之共聚物及其等之摻合物。聚酯包括但未限制為聚鄰苯二甲酸酯、聚鄰苯二甲酸丁酯、其等之共聚物及其等之摻合物。聚硫化物包括但未限制為聚苯基硫化物、其共聚物及其摻合物。聚乙烯醇包括但未限制為乙烯-乙烯醇,其共聚物及其摻合物。聚乙烯酯包括但未限制為聚醋酸乙烯、乙烯-醋酸乙烯酯,其共聚物及其摻合物。聚偏乙烯包括但未限制為氟化聚偏乙烯(例如,聚偏二氯乙烯、聚偏二氟乙烯),其共聚物及其摻合物。
多種材料可加進該些聚合物。這些材料係加入以改質或加強單一層或整體隔離件的性能或性質。這些材料包括,但未限制為:可加入降低聚合物熔點的材料。基本上,此多層式隔離件包括一層,其設計為在預定溫度封閉孔隙以阻礙介於電池電極間的離子流動。此功能通常稱為“不啟動”。在一實施例中,一三層隔離件具有一中間不啟動層。為降低該層的不啟動溫度,具有熔點比與其混合的聚合物低的材料可加進此聚合物。這些材料包括但未限制為:熔點低於125℃的材料,例如,聚烯烴或聚烯寡聚物。這些材料包括但未限制為聚烯烴蠟(聚乙烯蠟、聚丙烯蠟、聚丁烯蠟、及其等之摻合物)。這些材料可在聚合物重量百分比5-50%的比例填入聚合物中。在一實施例中可獲得低於140℃的不啟動溫度。從其他實施例可獲得低於130℃的不啟動溫度。
可加入可促進膜熔融完整性的材料。熔融完整性為指膜在高溫下限定其實體尺寸減少或破壞的能力,以致電極維持實體上的分離。這些材料包括礦物性填充劑。礦物性填充劑包括但未限制為滑石、高嶺土、合成矽土、矽藻土、雲母、奈米黏土、氮化硼、二氧化矽、二氧化鈦、硫酸鋇、碳酸鈣、氫氧化鋁、氫氧化鎂及其相似物、及其摻合物。這些材料也可包括但未限制為精密纖維。精密纖維包括玻璃纖維及短切聚合物纖維。填入比例範圍為該層聚合物1-60重量百分比。這些材料也可包括高熔點或高黏度的有機材料,例如PTFE及UHMWPE。這些材料也可包括交聯或偶合劑。
可加入可改良膜強度或韌度的材料。這些材料包括彈性體。彈性體包括但未限制為乙烯-丙烯(EPR)、乙烯-丙烯-二烯(EPDM)、苯乙烯-丁二烯(SBR)、苯乙烯異戊二烯(SIR)、乙烯新戊二烯(ENB)、環氧化物、聚胺甲酸酯及其等摻合物。這些材料也可包括但未限制為精密纖維。精密纖維包括玻璃纖維及短切聚合物纖維。填入比例範圍為該層聚合物之2-30重量百分比。這些材料也可包括交聯或偶合劑或高黏度或高熔點材料。
可加入改良膜抗靜電性質的材料。這些材料包括例如,抗靜電劑。抗靜電劑包括但未限制為丙三醇單硬脂酸酯、氧乙基化胺、聚醚(如Pelestat 300,可從日本三洋化學取得)。填入比例範圍為該層聚合物0.001-10重量百分比。
可加入改良隔離件表面可濕性的材料。這些材料包括例如潤濕劑。潤濕劑包括但未限制為:氧乙基化醇、第一級聚羧酯、乙二醇(如聚丙二醇及聚乙二醇)、以順丁烯二酸酐聚烯、丙烯酸、甲基丙烯酸環氧丙酯官能化之聚烯烴。填入比例範圍為該層聚合物之0.01-10%重量百分比。
可加入改良隔離件表面磨潤效能的材料。這些材料包括例如,潤滑劑。潤滑劑包括例如氟聚合物(如,聚偏二氟乙烯、聚四氟乙烯、低分子量氟聚合物)、增滑劑(如油醯胺、硬脂醯胺、芥子醯胺、Kemamide®、硬脂酸鈣、聚矽氧)。填入比例範圍為該層聚合物之0.001-10重量百分比。
可加進改良聚合物可處理性的材料。這些材料包括例如,氟聚合物、氮化硼、聚烯烴蠟。填入比例範圍為100ppm至該層聚合物之10重量百分比。
可加入改良膜難燃本質的材料。這些材料包括例如溴化阻燃劑、磷酸銨、氫氧化銨、氫氧化鋁及磷酯。
可加進促進聚合物成核作用的材料。這些材料包括成核劑。成核劑包括但未限制為:苯甲酸鈉、二苯亞甲基山梨糖醇(DBS)、及其化學衍生物。填入比例為習知的。
可加入染色該些層的材料。這些材料為習知的。
在即時電池隔離件製造中,共擠壓該些聚合物以形成多層式、非孔洞前驅物,且接著處理此前驅物以形成微孔。微孔可由“濕製程”或“乾”製程形成。濕製程(亦指溶劑萃取、相反轉、熱誘導相分離(TIPS)、膠質萃取)一般包含:在形成前驅物前添加可移除性材料,及接續藉由例如萃取製程,移除該材料以形成孔洞。乾製程(亦指Celgard製程)一般包含:擠壓一前驅物(不包括任何為形成孔洞的可移除性材料);退火前驅物,及拉伸前驅物以形成孔洞。本發明將於後討論相關乾製程。
為獲得此即時共擠壓多層式電池隔離件的均勻尺寸特性,使用一具有特定剪切速率的擠壓模。其確定模的剪切速率在產量18-100 lbs/hr(8.2-45.4 Kg/hr)/每層下必須為最小值4/秒。在一實施例,在一產量為18-100 lbs/hr(8.2-45.4 Kg/hr)/每層時,剪切速率大於8/秒。所有其他參數為傳統習知。
前述發明將進一步描述於後續範例中。表1說明依據本發明前述討論製造的11個樣本。表2說明使用不同材料以改進之隔離件的熔融完整性與無該些材料的隔離件。表3說明使用其他前述材料以改進隔離件的不同性質。用於收集各表資料的測試程序描述如下。
Gurley:藉由兩種方式測量Gurley。在第1種由日本工業標準Gurley(JIS Gurley)定義的方法中,Gurley使用OHKEN透氣測試機測量。JIS Gurley定義為在4.8英吋H2
O的固定壓力下100 cc空氣穿透一平方英吋薄膜所需的時間,以秒為單位。在第二方法中,依據ASTM D-726程序測量Gurley且定義為在4.8英吋H2
O的固定壓力下10 cc空氣穿透一平方英吋薄膜所需的時間,以秒為單位。
拉伸性質:MD及TD拉伸強度係使用Instron Model 4201依據ASTM-882程序測量。
擊穿強度:擊穿強度係使用Instron Model 4442依據ASTM D3763測量。擊穿強度單位為牛頓。測量橫越拉伸產品的整個寬度,且平均擊穿能量(擊穿強度)定義為擊穿測試樣本所需的力。
剝離強度或黏著性:內層黏著性使用Chatillon TCD-200剝離強度測試機測試。
收縮量:使用修改過的ASTM D-2732-96程序在90℃測量收縮量60分鐘。
厚度:膜厚度值使用Emveco Microgage 210-A精密測微計依據ASTM D374測量。厚度值使用微米(μm)單位。為20個各別取自橫越樣本整個寬度的測微計讀數的平均。
孔隙度:微孔隙膜的孔隙度以ASTM D2873方法測量。
高溫熔解完整性:高溫溶解完整性使用熱機械分析儀(TMA)測量。當溫度在5℃/分鐘的比例下從25℃掃描至300℃,在固定負載為125克的壓擠下,使用TMA壓縮探針測量隔離件厚度變化。殘留在250℃的厚度百分比定義為高溫熔融完整性。
可濕性:一滴典型的鋰離子電解液置於一膜的樣本上。記錄樣本外觀從不透光至可透光的改變。對可濕性的隔離件來說,外觀應該是近乎均勻透光,沒有不透光的區域。非可濕性的樣本維持其不透光性。
ER(電阻):電阻的單位為Ω-cm2
。隔離件電阻特性為從最終材料剪下小塊的隔離件,且接著放置於兩阻隔電極之間。隔離件以在體積比為3:7的EC/EMC溶劑中為1.0M LiPF6
鹽的電池電解液完全飽和。隔離件的電阻R(Ω)以4-探針AC阻抗技術測量。為降低電極/隔離件介面上的測量錯誤,經由增加更多的隔離件層而需要多次測量。根據多次測量,電(離子)阻,與電解液飽和的隔離件的Rs
(Ω)接著由公式計算出,
其中ρ s
為隔離件的離子電阻(Ω-cm),A為電極面積(cm2
)及l
為隔離件膜的厚度(cm)。ρ s /A
比為計算隔離件電阻(ΔR
)與多個隔離件層(Δδ)差異的斜率,其為,
亦參考於2006年4月7日申請的美國專利申請案序號第11/400,465號,關於‘離子電阻’的測試程序,其併入本文以供參考。
銷移除:銷移除測試模擬電池的捲繞製程。銷移除力為公克的力,其為由捲繞後的膠狀捲中央拉出銷的力量。電池捲繞機用來沿銷(或核心或心軸)捲繞隔離件。此銷為一具有0.16英吋直徑及一光滑外表面的二(2)件式圓柱形心軸。每一件具有一半圓橫切面。隔離件在捲繞在銷上,討論於後文下。此在隔離件上的起始力(正切)為0.5 kgf,且之後隔離件以24秒10英吋的比例捲繞。在捲繞中,一張力滾筒接合至被捲撓在心軸上之隔離件。張力滾柱包括一位於相對隔離件進料側的5/8英吋直徑滾筒,一(當接合時)施用1巴空氣壓力的英吋氣力汽缸,及一英吋的桿互相連接滾筒汽缸。隔離件由兩片30 mm(寬度)x 10英吋的測試膜組成。測試5組隔離件,平均其結果,並紀錄平均值。每一片疊接以1英吋重疊在一捲繞機上疊接於隔離件進料捲上。由隔離件的進料自由端,亦即,疊接端的遠端,在吋及7吋製作一墨印標記。此英吋的標記與銷的遠側(亦即,張力滾筒相鄰側)對齊,此隔離件在銷的二件間接合,且在滾筒接合下開始捲繞。當7英吋標記距膠狀捲(隔離件捲繞在銷上)為英吋時,此隔離件在標記處切除,而此的隔離件自由端以一片膠帶(1英吋寬,英吋重疊)固定於膠狀捲上。此膠狀捲(亦即,具有隔離件捲繞的銷)由捲嬈機移除。一可接受膠狀捲無皺摺且未縮短。此膠狀捲置於一拉伸強度測試機(亦即,美國北卡羅來納州Greensboro市Chatillon公司之Chatillon Model TCD 500-MS)之承載室(50磅x 0.02磅;Chatillon DFGS 50)中。此應變速率為每分鐘2.5英吋且得自承載室的數據以每秒10點的速率記錄。記錄峰值為銷移除力。亦可參閱美國專利第6,692,867號,該專利併入本案參考。
介電質破壞:提高樣本上的電壓直到觀察到材料的介電質破壞。介電質破壞以伏特表示。隔離件放置於兩電極之間,且供應一電壓穿越該些電極。提高電壓直到觀察到隔離件的介電質破壞。強隔離件表現高失效電壓。任何非均勻度會導致低失效電壓。
Aqua孔徑:使用PMI(Porous Materials Inc.)的Aquapore測量孔徑。孔徑以微米(μm)表示。
混合滲透性:混合滲透性為需要藉由隔離件產生一短路的力並以公斤-力(kilogram-force,kgf)表示。混合滲透性為需要藉由隔離件歸因於混合滲透性而產生一短路的力。在此測試中,以一第一金屬平板基材開始,一陰極材料片材放置於此平板上,一隔離件置於陰極上,及一陽極材料片材至於該隔離件上。然後提供一3 mm球尖接觸至一測力計。此球尖經由一電阻計連接至一第一金屬板。施加力於此球尖,其記錄於測力計上。一旦施加力,在隔離件的二側建立一陽極混合及一陰極混合。當電阻戲劇性的下降,其象徵由於混合滲透性之隔離件的短路。混合滲透性量測隔離件強度與朝向混合滲透性的電阻。已發現此為更精準的模擬真實電池芯的性能。此為比擊穿強度更佳適宜說明隔離件如何在電池芯中運轉。此測試用來指出隔離件的傾向以容許在電池組裝時的短路。亦參考於2006年4月7日申請的美國專利申請案序號第11/400,465號,其併入本文以供參考。
本發明在不偏離其精神及必要特性下可以其他形式實施,且因此可參考做為說明本發明範疇之後附申請專利範圍,而非前述之說明書。
Claims (22)
- 一種電池隔離件,其包含:一共擠壓微孔隙膜,其厚度範圍為4-50μm,該共擠壓微孔隙膜具有至少兩層,其中兩層係各由不同的可擠壓之聚合物製成;並具有一標準偏差小於0.8微米(μm)的一均勻厚度。
- 如申請專利範圍第1項之電池隔離件,其中:該共擠壓微孔隙膜具有一定義為剝離強度大於60克的層間黏合性。
- 如申請專利範圍第1或2項之電池隔離件,其中一該可擠壓的聚合物為一熱塑性聚合物。
- 如申請專利範圍第1或2項之電池隔離件,其中一該可擠壓的聚合物係選自於下列群組:聚烯烴、聚縮醛、聚醯胺、聚酯、聚硫化物、聚乙烯醇、聚乙烯酯及聚偏乙烯、前述之共聚合物、及其等之摻合物。
- 如申請專利範圍第1或2項之電池隔離件,其中一該層更包含一被添加之材料。
- 如申請專利範圍第5項之電池隔離件,其中該材料選自於適用於下列各情況之材料之組群:降低該聚合物之熔點;改良該膜之熔融完整性;改良該膜之韌度之強度;改良該膜之抗靜電性質;改良該隔離件之表面可濕性;改良該隔離件之表面磨潤效能;改良該聚合物之可處理性;改良該膜之難燃本質;促進該聚合物之成核作用;染色該膜之層;及其等之組合。
- 如申請專利範圍第1或2項之電池隔離件,其中一該可擠壓的聚合物為聚乙烯,另一者為聚丙烯。
- 如申請專利範圍第1或2項之電池隔離件,其中一該聚合物選自於下列組成之群組:聚甲基戊烷、聚縮醛、聚醯胺、聚酯、聚乙烯醇、聚乙烯酯、聚硫化物、聚偏乙烯。
- 如申請專利範圍第1或2項之電池隔離件,其包含由一可擠壓之聚合物製成的第三層,且該第三層的該聚合物為與前述兩層的該等聚合物為相同或不同。
- 如申請專利範圍第1或2項之電池隔離件,其中該膜為一乾拉伸膜。
- 一種製造微孔隙多層式膜之方法,該膜具有一4-50μm的厚度範圍,並具有至少兩層,其中兩層係各由不同的可擠壓之聚合物製成,且該膜具有由標準偏差小於0.8μm所界定的一均勻厚度,該方法包含步驟:共擠壓一無孔隙的多層式前驅物穿過一擠壓模,該共擠壓具有最小剪切速率4sec-1 及一產量為18-100lbs/hr(8.2-45.4Kg/hr)/每層;及處理該無孔隙的多層式前驅物以獲得該微孔隙多層式膜。
- 如申請專利範圍第11項之方法,其中該剪切速率為8/sec。
- 如申請專利範圍第11項之方法,其中處理更包含:退火該無孔隙多層式前驅物;及 拉伸該經退火之無孔隙的多層式前驅物。
- 如申請專利範圍第11項之方法,其中該共擠壓更包含:添加一材料於至少一層中。
- 如申請專利範圍第14項之方法,其中該材料選自於適用於下列各情況之材料之組群:降低該聚合物之熔點;改良該膜之熔融完整性;改良該膜之韌度之強度;改良該膜之抗靜電性質;改良該隔離件之表面可濕性;改良該隔離件之表面磨潤效能;改良該聚合物之可處理性;改良該膜之難燃本質;促進該聚合物之成核作用;染色該膜之層;及其等之組合。
- 如申請專利範圍第11項之方法,其中該微孔隙多層式膜所具一該可擠壓的聚合物為一熱塑性聚合物。
- 如申請專利範圍第11項之方法,其中該微孔隙多層式膜所具一該可擠壓的聚合物係選自於下列群組:聚烯烴、聚縮醛、聚醯胺、聚酯、聚硫化物、聚乙烯醇、聚乙烯酯及聚偏乙烯、前述之共聚合物、及其等之摻合物。
- 如申請專利範圍第11項之方法,其中該共擠壓微孔隙膜具有一定義為剝離強度大於60克的層間黏合性。
- 如申請專利範圍第11~18項中任一項之方法,其中該微孔隙多層式膜所具一該可擠壓的聚合物為聚乙烯,另一者為聚丙烯。
- 如申請專利範圍第11至18項中任一項之方法,其中該微孔隙多層式膜含有由一可擠壓之聚合物製成的第三層,且該第三層的該聚合物為與前述其他兩層的該等聚 合物為相同或不同。
- 如申請專利範圍第11至18項中任一項之方法,其中該膜為一乾拉伸膜。
- 一種電池隔離件,其係由申請專利範圍第11至21項中任一項之方法所製成。
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