TW200537726A - Method of forming an electrode structure useful in energy storage devices - Google Patents
Method of forming an electrode structure useful in energy storage devices Download PDFInfo
- Publication number
- TW200537726A TW200537726A TW094108276A TW94108276A TW200537726A TW 200537726 A TW200537726 A TW 200537726A TW 094108276 A TW094108276 A TW 094108276A TW 94108276 A TW94108276 A TW 94108276A TW 200537726 A TW200537726 A TW 200537726A
- Authority
- TW
- Taiwan
- Prior art keywords
- energy storage
- electrode structure
- binder
- current collector
- carbon
- Prior art date
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Classifications
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H01M4/0435—Rolling or calendering
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Description
200537726 九、發明說明: 【發明所屬之技術領域] ’更特定言之, 之電極結構的方 本發明係關於-種形成電極結構的方法 本發明係關於-種形成用於能量儲’ 法。 【先前技術】 能量儲存裝置之電極結構習知係由包 材料、黏合劑及溶劑的漿液製備。此漿液二 :方法塗覆於金屬㈣電器以提供激液的薄、均= 集電器,該經塗覆集電器接著於 曰、 目τ乾燥以移除溶顏及 熟化黏合劑。該電極結構可接著選 ^ 按者選擇性地砑光以藉由減少 體積或電化學活性材料的填充分率 機夕電極結構的整體 孔隙度以硬化塗覆於集電器的電化學活性材料。 伴隨關連於方法中使用溶劑形成電極裝置的此種習知方 法存在種種缺點,例如使用溶劑於這些習知方法會造成關 於揮發性有機化合物(V0Cs)釋入環境中的環境議伴隨 此種溶劑的使用之增加成本(包括確保溶劑自該電極結構 的足夠移除所需的增加烤箱乾燥次數所造成的增加能量成 本)〇 克服伴11¾習知電極組裝方法的缺點之一個企圖揭示於頒 予Firsich的美國專利第5,993,996號,Firsich揭示,尤其是, 藉由喷霧塗覆碳化黏合劑及碳化聚合物前軀體於可移動背 材上形成碳電極單晶片。該經喷霧塗覆材料可在碳化前或 後自背材移除,經碳化材料可經由後續酸處理活化及官能 99230.doc 200537726 化。然而,希望具一種直接沉積經活化碳材料於集電器之 方法,其不需如Firsich所揭示的後續碳化及其最小化或、、肖 除溶劑之需求。 【發明内容】 在本發明一個方向提供一種形成電極結構的方法,其包 括(a)藉由喷霧一種混合物至集電器而沉積多孔電極於集電 器,混合物包括:⑴碳;(Π)黏合劑;及,選擇性地,(^1) ® 電傳導添加劑;(b)加熱(a)的產物以熟化黏合劑;及,選擇 W 性地,(c)砑光(b)的產物。 在本發明另一個方向提供一種形成電極結構的方法,其 包括:(a)藉由靜電喷霧沉積一種混合物至集電器而沉積多 孔電極於集電器,混合物包括··⑴碳;(ii)黏合劑,·及,= 擇性地,(iii)電傳導添加劑;(b)加熱(_產物以熟化黏2 劑,及’選擇性地,(c)砑光(b)的產物。 在本發明另一個方向提供一種形成電極結構的方法,其 J &括、a)預處理集電器以改良其表面能;⑻藉由噴霧一種 混合物至該集電器而沉積多孔電極於該經改良集電器,混 合物包括:⑴碳;⑼黏合劑;及,選擇性地,㈣電傳; 添加劑;(b)加熱⑷的產物以熟化黏合劑;及,選擇性地, (c)石牙光(b)的產物。 在本發明另一個方向’提供一種長壽命雙層電容写,立 包括:⑷至少兩個由本發明方法製備的電極結構;⑻置: 該至少兩個電極結構之間的至少—個多孔分離器該 至少兩個電極結構及該至少一個多孔分離器解 99230.doc 200537726 溶液。 在本發明另一個 的電極結構之能量儲存裳:供一種包含由本發明方法製備 在本發明另_個 系統之用* in提供本發明能量儲存裝置於各種 光電池的能量儲存|電力質系統、引擎啟動系統、 ^ ώ Μ ^ A ”統、風車的能量儲存系統、醫筚卒% 八車推進糸統、軍用啻2么 酋杀糸統、 消費者用電子以、” 輸系統、商用電子系統、 裝置。 、’帶式電子系統、音聲系統及消費者 本舍明沉積方沐认 的使用係使用為使用者及環境皆 材料,在習知液體涂灣庙衣兄^友善的 劑載體之需求幾乎被消除, =有機冷 %疋本發明》儿積方法產生此
微(右存在)揮發性物質進人環境的排放;由此,減輕空氣;; 染及伴隨此種揮發性物質的健康議題。而且,本發明方法 ^現非吊w的塗覆效率,其係部分基於過噴霧材料的易循 壞性,例如’在本發明-個具體實施例中,至少75重量% 的經喷霧粉末:或者是至少85重量%的經喷霧粉末轉移至 集電器及保留於JL卜,甘從 、八上八餘如末可容易地被回收及以9〇重 量%或更高的速率循環。 &適用於本發明的沉積技術包括如,粉末火焰喷塗、火 焰喷塗熱解、燃燒化學氣相沉積、高速火焰熱噴、空氣電 聚喷霧、靜電喷霧、電弧喷霧及流體化浸人。在本發明一 個具體實施例中,使用靜電喷霧沉積技術。在此具體實施 例的一個方面,微細磨碎碳及黏合劑的混合物被施以靜電 99230.doc 200537726 荷及推進至集電器。在此具體實施例的另一個方面,可使 用標準負電暈靜電喷搶以沉積碳及黏合劑的混合物於連接 至接地的集電器。此種喷霧搶的一個實例為購自N0rds0n
Cwp01^1011 of Amherst俄亥俄的 VersaSprayll。 :炭、黏合劑及,選擇性的,電傳導添加劑的經噴霧混合 物藉由如傳導、對流、輻射、電感熱能量、電磁輻射鮮 或其組成而熟化。在一個具體實施例中,碳、黏合劑及, 選擇性的,電傳導添加劑的經噴霧混合物加熱至高於黏合 劑的玻璃態化溫度,但低於黏合劑的分解溫度之溫度2至 120分鐘的期間;或是2至6〇分鐘;或是2至3〇分鐘。 ;本發明方法可選擇性地包括集電器預處理操L, 5亥集電器可進行表面處理以改盖i 及/或其黏著性質。 I"表以以增進其可濕性 適合用於本發明的集電器,表面預處理操作包括,如, 電軍二:、機械磨,、化學㈣、熱處理及化學處理。 【實施方式】 在一個具體實施例中,由本 方法所沉積的多孔電極 顯現在25及500微米之間的平均孰 ^ 7…化;度;或是在50及250 U木之間,或疋在50及150微米之間。 在一個具體實施例中,由本發 铟相檄儿, 月方法所形成的多孔電極 顯現變化少於10%的均勻厚 2%;或是少於1%。 次疋少於5%;或是少於 制^適用於本發明電極結構的集電器可由幾乎任何電導體 1仏熟知本技藝者知道選擇已知 應、用的集電器的適當建 99230.doc 200537726 造材料,例如,熟知本技藝者可認知要併入雙層超級電容 器的電極結構的集電器應由顯現對用於該裝置的電解材料 具電化學及化學抗腐蝕的電傳導材料製造。在一個具體實 施例中’該集電器可由自鋁、不鏽鋼、辞、鈦、鈕、銅、 金、鎳、或其組合所選出材料製造;或是自銅及鋁所選出 材料;或是鋁。 在一個具體實施例中,該集電器可為一種包括,如,荡、 /具三度空間結構的泡殊金屬、冷服金屬、網狀物、網、毛 織物及其組合之型式。在此具體實施例的一個方向,該集 電器可由鋁箔製造。 一在個具體實施例中,本發明集電器顯現一種5至5〇〇微 米的平均厚度;或是在5至100微米;或是在5及5〇微米。 在本發明一個具體實施例中,碳、黏合劑及,選擇性的, 電傳導添加劑的混合物可包含5〇至98重量%的碳;或是 至95重量%的碳,或是5〇至90重量%的碳,或是50至85重量 • %的碳,或是50至80重量%的碳。 在本發明一個具體實施例中,碳、黏合劑及,選擇性的, 電傳導添加劑的混合物可包含不超過5〇重量%的黏合劑, ^疋0.5至5〇重量%的黏合劑,或是2至5〇重量%的黏合劑, =疋)於15重量%的黏合劑,或是〇5至1〇重量%的黏合 劑,或是少於5重量%的黏合劑。 在本發明一個具體實施例中,碳、黏合劑及,選擇性的, 電傳導添加劑的混合物可包含少於或等於10重量%的電傳 導】加背i ’或是少於5重量%的電傳導添加劑;或是少於2 99230.doc 200537726 重量。/〇的電傳導添加劑。 合適用於本發明的碳包括,如,活性碳、大網狀碳、碳 奈米管及富勒烯。 在一個具體實施例中,碳為活性碳及顯現大於10F/g的電 容。 在另一具體實施例中,碳為活性碳及顯現使用
Brunauer、Emmett、Teller(BET)分析方法所決定的表面積 為至少50 m2/g ’或是50至3,000 m2/g,或是至少5〇〇 m2/g, 或是 500 至 2,500 m2/g,或是 8〇〇 至 2,500 m2/g,或是 ι〇〇〇 至 2,5〇〇 m%,或是M00 至 2,500 m2/g,或是 Μ。。至 25〇〇 m /g。 在另-具體實施例中’碳為顯現由氮吸附技術的大於〇ι m3/g的細孔容積之活性碳。 在另一具體實施例中,碳為顯現由 H〇rVath-Kawaz〇e(H-K)方法的孔徑分佈具至少一個尖峰在 〇·1及5.0奈米之間之活性碳。 在另一具體實施例中,碳顯現由Barrett-J0yner_
Halenda(B JH)方法的孔徑分佈具至少一個尖峰在2 〇奈米及 50.0奈米之間。 在另-具體實施例中,碳顯現具至少一個第一明顯高峰 於少於或等於2.0奈米的孔徑之孔徑分佈當利用Η_κ dv/d1〇g(W)孔徑分佈測量時及至少一個第二明顯高峰,利 用BJH dv/dlog⑼孔徑分布測量,於大於2〇奈米的孔徑, 或是大於3奈米,或是大於5奈米,或是大於1〇奈米,或是 99230.doc 200537726 大於12.5奈米。 在另—具體實施例中,碳為顯現少於5〇微米的體積平均 粒子大小之活性碳。 在另-具體實施例中,碳為顯現微孔、介孔及大孔的分 布及至少500 V/g的而表面積,且邮㈣的順表面積 貢獻至具自1.7至10,000奈米直徑的孔之活性碳。 在另一具體實施例中,碳為一種活性碳其顯現大於1〇?/§ 的電容;BET表面積大於50m2/g,或是5(^3,〇〇〇m2/g,或 是2 至少 500 m2/g,或是 500 至 2,5〇〇 m2/g,或是 8〇〇 至 2,5〇〇 m /g,或是1,〇〇〇至2,500 m2/g,或是以⑽至“⑽^化或 是1,500至2,500 m2/g;細孔容積大於〇1 cm3/g;至少一個 尖峰在0.1及50奈米之間的孔徑分布及少於5〇微米的體積 平均粒子大小。在此具體實施例的方向,該碳為大網狀碳 質材料,在此具體實施例的另一個方向,該碳為粉末。 適合用於本發明的活性碳可由數種起始材料製造包括, 如,酚-甲醛聚合物、三聚氰醯胺_甲醛聚合物、間苯二酚-甲醛聚合物、聚苯胺、聚丙烯腈、kynel、嫘縈、椰殼、碳 水化合物(如蔗糖)、瀝青、木材及其混合物。 適合用於本發明的黏合劑包括,如,聚醯胺、聚酯、纖 維素酯、曱基纖維素、甲基丙烯酸酯、聚曱基丙烯酸酯、 聚乙烯、聚丙烯、聚氯乙烯(PVC)、聚偏乙烯二氟(pvdf)、 聚苯砜、聚乙烯吡咯烷酮、聚四氟乙烯(PTFE)、泡沫聚四 氟乙烯(ePTFE)、乙烯丙烯雙烯單體(EPDM)、高分子量聚 乙烯(UHMWPE)、苯乙烯系及其組合。適合用於本發明的 99230.doc -12 - 200537726 商業可提供黏合劑包括購自Atofina Chemicals af
Phlladelphla,賓州的Kynar® 761 及 Kynar® 28(H。熟知本技 藝者知道選擇適合用於包含本發明電極結構的已知裝置的 黏合劑材料,例如,對用於雙層的電極結構、超級電容器, 熟知本技藝者知道選擇與要用於該裝置的電解質相容的黏 合劑材料。 在一個具體實施例中,該黏合劑顯現少於或等於5微米的 體積平均粒子大小。在另一個具體實施例中,該黏合劑顯 現不大於由碳所顯現的體積平均粒子大小的5〇%的 均粒子大小。 斤適合用於本發明的電傳導添加劑包括,如,炭黑、石墨、 〃鈦1化釕及其混合物,在一個具體實施例中,談電 傳導添加劑包括傳導性碳,在此具體實施例的一個方二 ==碳為炭黑、石墨及其混合物,適合用於本發明的 ” &供厌黑包括,如,分別得自Azk〇 N〇beaCab〇t C〇rP〇ratlon的科琴黑及 目 "、在另一具體實施例中, :電傳導添加劑顯現少於或等於50微米的體積平均粒子大 =明電極結構可用於多種能量館存裝置包括,如 亦已知為超級電容器)、電池、燃料電池 穩疋化裝置及電容去離;#恶 a, 电力 量儲存裝置可用於多m包。纟發明電極結構的能 動系統、光電池的能量 醫_、汽一,電子 99230.doc 200537726 用電子系統、消螫古田+ 7/ 、 電子糸統、攜帶式電子系統、音聲 系統及消費者裝置。 日耳 在個具體貫施例中,本發明電極結構可用於電容器, 在此具體實施例的—個方向,該電容器為包含至少兩個由 本發明方法所製備的電極結構,置於該至少兩個電極結構 之間的至少一個多孔分離器及與該至少兩個電極結構及該 至> ㈤多孔分離器接觸的電解質溶液之雙層電容器。 適合用於本發明的電解質溶液包括,如,有機電解質溶 液及水相電解質溶液。在一個具體實施例中,該電解質溶 液為有機電解質溶液’在此具體實施例的一個方向,該有 機電解質洛液可藉由溶解電解質於有機溶劑或有機混 合物而得到。 適口用於本發明的電解質溶液的有機溶劑包括,如,電 化于i定的奴酸乙烯酯;碳酸丙烯酯;碳酸丁烯酯;τ _ 丁 内曰衣丁石馬,J衣丁碼衍生物,· 3-甲基環丁石風;ι,2-二甲氧 基^烷’乙腈’戊二腈;戊腈;二甲替甲醯胺;二甲亞砜; 四氫夫南’一甲氧基乙& ;甲酸甲酯;碳酸二曱酯;碳酸 一乙酉曰,甲基乙基碳酸酯及其混合物。 、適合用於有機溶劑的電解質包括,如,具以RimN+ 或表示的季鏽陽離子之鹽類,其中n R3 及R4的每一個獨立地為Cm烷基及陰離子係選自,如, BF4 PF6、C104、CF3S〇3i(s〇2R5) (s〇2r眞其中 R5 及R6的每個獨立地為Cw烷基、亞烴基及統稱為環狀結 構在個具體實施例中,電解質係選自包含 99230.doc -14- 200537726 (C2H5)4NBF4 λ (C2H5)3(CH3)NBF4 ^ (C2H5)4PBF4 A (C2H5)3 (CH3)PBF4的族群。在一個具體實施例中,著名的鹽類之一 以 0 1 $ 9 < • · m〇1/L,或0·5至2 mol/L的濃度溶解於有機溶 液0 適合用於本發明的分離器可由,如,聚丙烯纖維的非織 造織物、玻璃纖維的非織造織物、合成纖維、天然纖維或 其組合物所製造。
現在在下列實例中詳細敘述一些本發明具體實施例,在 下列實例中說明的所有分率及百分率係以重量表示除非另 外訂定。 實例1 電極結構的製備 三種不同活性碳使用於實例i_36。 在表I中標示,,BP-15”的碳可購自日本Kuraray Chemical 的 BP-15。 在表I中標示為”EGL-572”的碳係由將購自賓州費城
Rohm and Hass Company 的產品 AmbersorbTM 572碟碎為少 於30微米粒子大小而製備。 在表I中標示為”EGL-923"的碳係由將購自賓州費城
Rohm and Haas Company 的產品 AmberliteTM XAD-761 於 1,000QC下碳化及在二氧化碳下活化而製備。接著將在這些 條件下產生的大網狀碳碾碎為少於30微米粒子大小。 六種不同黏合劑使用於實例1-36。 在表I中標示為"PVDF”的黏合劑可購自賓州費城At〇fina 99230.doc -15- 200537726
Chemicals 的 Kynar® 711。 在表I中標不為"PTFE’’的黏合劑可講自紐澤西州Dayton
Shamrock Technologies,Inc·,的 FluoroTM C-369。 在表I中標示為”AP”的黏合劑為藉由自實例2所敘述乳液 聚合物乾燥為粉末形式而製備的12重量❻/σ的聚(丙稀酸丁 醋)/88重量%的聚(甲基丙烯酸甲酯)乳液聚合物的丙烯酸系 粉末。
在表I中標示為"AE”的黏合劑為使用實例2所敘述步驟製 備的水相12重量。/〇的聚(丙烯酸丁酯)/88重量%的聚(甲基丙 烯酸甲酯)乳液聚合物之丙烯酸乳液。 在表I中標示為Epoxy的黏合劑可購自紐約州(Tarryt〇wn)
Ciba Specialty Chemicals 的 Araldite® GT 7013。 在實例2-19及27-29的每一個實例中,乾燥粉末活性碳與 AP以表I所說明分率混合。 在實例20-26及30-36的每一個實例中,乾燥粉末活性碳 與AE以表1所說明分率混合及接著在真空下於60。(:乾燥24 小時。 在實例2-36的每一個實例中,活性碳與黏合劑的混合物 使用IKA® All攪拌器機械攪拌30秒至5分鐘。 在貫例1-36中,三種不同金屬用做集電器,表j標示為"A1 箔”的集電器材料係購自得自Reynolds Consume Pr〇ducts, a Dwmon 〇f Alco Inc·,〇f Richmond,Virginia的心则以 Aluminum FoU。表”票示為"Cuig,,的集電器材料係購自紐約 Hoosick Fall的 0ak Mitsui c〇mpany,表鳩示為”Au绪"的集 99230.doc -16- 200537726 電器材料係購自俄亥俄州Cleveland All-Foils的鋁箱。 在貫例1-36的每一個實例中,活性碳/黏合劑混合物係使 用講自俄亥俄Amberst Nordson Corporation的重力進料
VersaSparyll ’標準負電暈靜電噴霧搶而靜電喷霧沉積於在 表I所標不的75 mm X 125 mm集電器材料片。在靜電喷霧沉 積J間10亥集電器材料收集於接地,及該靜電噴霧搶的控 制參數如下··進料空氣壓力1〇psi,喷嘴空氣壓力i〇psi, 及電壓100 kv。 在實例1-36中,具碳/黏合劑混合物沉積於其上的集電器 …、二化於購自伊利諾州Blue Island Blue M Electric 型號 〇V-58〇C_2對流爐。對每一個個別實驗,該爐子加熱至表! 所標示溫度。具碳/黏合劑混合物沉積於其上的集電器接著 於爐子熟化並於表!所說明時間期間保持爐子溫度於所標 不溫度。 : 例1-36的每一個結果係提供於表I,每-個實例所產生 :句勾多孔電極之沉積在表j的”均句多孔電極"的核對標示辨 硪。均勻多孔電極係定羞糸 、 电位係疋義“全覆盍及黏著於集電器(由目 視檢查決定)的均勻碳/黏合劑声 ^。剤層表1亦包括相對黏著強度 的才曰示’其係由在實例9、1 〇、Μ λα 〇 j 10 15、2〇-26 及 30-26 所沉積多 孔電極顯現’(亦即,對每—個 ㈣、"”主 才母個產生均句多孔電極之沉積的 貫例)。1表示多孔電極顯現相 片几仰田是的黏著,,丨2”矣 電極顯現相當良好的黏著,,, 、 表不多孔電極顯現相當強的 黏者。夕孔電極的相對黏 沒係由人工刮除決定。 99230.doc 200537726
表I 樣品 號碼 集電器 碳 黏合劑 型式 碳分率 (重量 %) 黏合劑 分率 (重量 %) 熟化溫 度(〇F) 熟化時 間(分 鐘) 均勻多 孔電極 相對黏 著強度 1 A1箔 EGL-572 - 100 0 450 10 2 EGL-572 PVDF 95 5 450 10 3 EGL-572 PVDF 95 5 500 15 4 EGL-572 PVDF 95 5 450 10 5 EGL-572 PVDF 85 15 450 10 6 EGL-572 PVDF 85 15 500 15 7 EGL-572 Epoxy 85 15 450 10 8 EGL-572 PVDF 85 15 450 5 9 EGL-572 PVDF 50 50 450 10 V 2 10 Cu箔 EGL-572 PVDF 50 50 450 10 V 1 11 EGL-923 PTFE 50 50 350 10 12 EGL-923 PTFE 50 50 500 5 13 EGL-923 PVDF 95 5 500 10 14 EGL-923 PVDF 85 15 500 10 15 EGL-923 PVDF 50 50 500 10 V 2 16 EGL-923 PVDF 95 5 500 105 17 EGL-923 AP 50 50 400 15 18 EGL-923 AP 85 15 400 15 19 EGL-923 AP 95 5 400 15 20 EGL-923 AE 50 50 400 15 V 3 21 EGL-923 AE 85 15 400 15 V 1 22 EGL-923 AE 95 5 400 15 V 1 23 BP-15 AE 50 50 400 15 V 3 24 BP-15 AE 85 15 400 15 V 1 25 EGL-923 AE 50 50 400 15 V 3 26 EGL-923 AE 95 5 400 15 V 3 27 All-箔 EGL-923 AP 50 50 400 15 28 EGL-923 AP 85 15 400 15 29 EGL-923 AP 95 5 400 15 30 EGL-923 AE 50 50 400 15 V 3 31 EGL-923 AE 85 15 400 15 V 1 32 EGL-923 AE 95 5 400 15 V 1 33 BP-15 AE 50 50 400 15 V 3 34 BP-15 AE 85 15 400 15 V 1 35 EGL-923 AE 50 50 400 15 V 3 36 EGL-923 AE 95 5 400 15 V 3 99230.doc -18- 200537726 實例2 BA/MMA乳液聚合物黏合劑之製備 12重量%的聚(丙烯酸丁酯)及88重量%的聚(丙烯酸甲g| ) 聚合物組合物係使用下列步驟製備: (A) 於配備漿式攪拌器,加熱架及溫度計的5公升,4_頸, 圓底燒瓶加入: (i) 1267份去離子水;
(ii) 0.20份酒石酸; (iii) 0.018份硫酸亞鐵;及 (iv) 17.8份月桂硫酸鈉於水的28%溶液; (B) 接著加熱圓底燒瓶的内容物至48°C並以氮氣喷佈; (c)藉由合併下列製備第一乳化單體混合物(EMM); (i) 117.4份曱基丙烯酸甲酯; (ii) 16.0份丙烯酸丁酯; (iii) 99·5份去離子水;及 (iv) 3.46份月桂硫酸納於水的28%溶液; (D) 接著以高速機械攪拌器乳化(c)的產物; (E) 接著將(D)的產物加至圓底燒瓶内容物; (F) 將圓底燒瓶内容物的反應溫度調整至45〇c ; (G) 將0.072份曱醛合次硫酸氫鈉二水合物溶解於3·53份 去離子水; (Η)接著將(G)的產物加至圓底燒瓶内容物; (I)接著將0.074份第三丁基過氧化氫及〇〇74份第三丁基 過氧化氫(70%於水中)加至圓底燒瓶内容物; 99230.doc -19- 200537726 (J) 接著由合併234.8份曱基丙烯酸甲酯、32.0份丙烯酸丁 酯、144.2份去離子水及1.62份月桂硫酸鈉於水的28%溶液 製備第二EMM ; (K) 接著將(J)的產物加至圓底燒瓶内容物; (L) 接著將圓底燒瓶内容物的溫度調整至57°C ; (Μ)接著將0.309份月桂硫酸鈉於水的28%溶液及0.3 14份 70%第三丁基過氧化氫接著加至圓底燒瓶内容物; (Ν)接著由合併352.2份甲基丙烯酸甲酯、48.0份丙烯酸丁 酯、193.4份去離子水及2.38份28%月桂硫酸鈉溶液製備第 三 EMM ; (〇)接著將(N)的產物加至圓底燒瓶内容物; (P) 接著將反應溫度調整至52QC ; (Q) 將0.464份28%月桂硫酸鈉溶液(溶解於22.7份去離子 水)及接著0.460份70%第三丁基過氧化氫接著加至圓底燒 瓶内容物;
(R) 接著藉由合併下列製備第四EMM ; (i) 469.7份甲基丙烯酸甲酯; (ii) 64.0份丙烯酸丁酯; (iii) 259.5份去離子水;及 (iv) 3.40份28%月桂硫酸鈉於水; (S) 接著將(R)的產物加至圓底燒瓶内容物; (T) 接著將反應溫度調整至49QC ; (U) 接著將2· 14份月桂硫酸鈉(溶解於104.6份去離子水) 及2.14份過硫酸鉀(溶解於104.6份去離子水)加至圓底燒瓶 99230.doc -20- 200537726 内容物; (V) 將0.21 3份28%月桂硫酸鈉(溶解於10.4份去離子水)及 接著0.322份70%第三丁基過氧化氫接著加至圓底燒瓶内容 物; (W) 15分鐘後,0.213份28%月桂硫酸鈉(溶解於10.4份去 離子水)及接著0.322份70%第三丁基過氧化氫接著加至圓 底燒瓶内容物;及 (X) 15分鐘後,冷卻圓底燒瓶内容物至30°C以提供聚合物 產物。 99230.doc •21 -
Claims (1)
- 200537726 十、申請專利範圍: ‘ 1 · 一種形成電極結構的方法,其包括 ⑷沉積多孔電極於集電器,其係藉 -種混合物,其包括: 4“上噴霧 ⑴碳; (ii) 黏合劑;及, (出)選擇性地,電傳導添加劑;及, (b)加熱(a)的產物以熟化該黏合劑。 2 ·根據請求項1的方法,直中 /、亥此合物進一步包括一種電僂 導添加劑。 裡电得 3 ·根據ό月求項1的方法,盆中 夕 ^ ^ ^ ^ ’、 μ夕1電極係藉由靜電喷霧沉 積方法/儿積於該集電器。 (c)砑光(b)的產物 4·根據請求項1的方法,其進一步包括 5 ·根據清求項1的方法,盆推一 jk > 進一 v包括預處理該集電器以名 沉積該多1電極前改善其表面能。 6·根據請求項1的方法,1 具中黏合劑於該混合物的數量係在 2至5 0重量%的範圍。 其中該黏合劑的體積平均粒子大4 7 ·根據清求項1的方法 係少於或等於5微米 8·根據請求項1的方法,1 八T该黏合劑顯現不大於5〇0/〇由磅 所顯現的體積平均# 十吟叔子大小之體積平均粒子大小。 9. 一種能量儲存裝置,jl白赵士 ▲主4 八匕栝由请求項1的方法所製備的電 極結構。 99230.doc 200537726 10. —種請求項9的能量儲存裝置於汽車、電力品質、引擎啟 動、光電池的能量儲存、風車的能量儲存、醫藥系統、 汽車推進系統、軍用電子、傳輸系統、商用電子、消費 者用電子、攜帶式電子、音聲系統及消費者裝置之用途。99230.doc 200537726 七、指定代表圖: (一) 本案指定代表圖為:(無)。 (二) 本代表圖之元件符號簡單說明: 八、本案若有化學式時,請揭示最能顯示發明特徵的化學式: (無) 99230.doc ·' 200537726 _ 1-^發明專利說明書 (本說明書格式、順序及粗體字’請勿任意更動,※記號部分請勿填寫) ※申請案號:1^0 ※申請日期:0 來1卩(:分類: 一、發明名稱:(中文/英文) 用於能量儲存裝置之電極結構的形成方法 METHOD OF FORMING AN ELECTRODE STRUCTURE USEFUL IN ENERGY STORAGE DEVICES 一、申請人:(共1人) 姓名或名稱··(中文/英文) 羅門哈斯公司 ROHM AND HAAS COMPANY 代表人:(中文/英文) 愛德樂馬可S ADLER, MARC S. ^ 住居所或營業所地址:(中文/英文) 美國•賓州19106-2399 ·費城·獨立大道西區1〇〇號 100 Independence Mall West, Philadelphia, Pennsylvania 19106-2399, U.S.A. 國籍:(中文/英文) 美國 U. S. A. 93026L
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| US7419745B2 (en) | 2008-09-02 |
| CN1677722A (zh) | 2005-10-05 |
| EP1583169A2 (en) | 2005-10-05 |
| TWI264845B (en) | 2006-10-21 |
| EP1583169B1 (en) | 2015-10-21 |
| JP2005294832A (ja) | 2005-10-20 |
| KR100703628B1 (ko) | 2007-04-06 |
| AU2005201234B2 (en) | 2010-09-09 |
| US20050220989A1 (en) | 2005-10-06 |
| AU2005201234A1 (en) | 2005-10-20 |
| EP1583169A3 (en) | 2006-05-17 |
| KR20060045064A (ko) | 2006-05-16 |
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