TWI484273B - 電泳粒子 - Google Patents

電泳粒子 Download PDF

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TWI484273B
TWI484273B TW099103772A TW99103772A TWI484273B TW I484273 B TWI484273 B TW I484273B TW 099103772 A TW099103772 A TW 099103772A TW 99103772 A TW99103772 A TW 99103772A TW I484273 B TWI484273 B TW I484273B
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electrophoretic
electrophoretic medium
particle
black pigment
display
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TW201042351A (en
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Jason D Feick
Michael D Walls
Michael D Musick
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E Ink Corp
Shepherd Color Co
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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/165—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on translational movement of particles in a fluid under the influence of an applied field
    • G02F1/166—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect
    • G02F1/167—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on translational movement of particles in a fluid under the influence of an applied field characterised by the electro-optical or magneto-optical effect by electrophoresis
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/34—Compounds of chromium
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/165—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on translational movement of particles in a fluid under the influence of an applied field
    • G02F1/1675—Constructional details
    • G02F1/16757—Microcapsules
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/165—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on translational movement of particles in a fluid under the influence of an applied field
    • G02F1/1675—Constructional details
    • G02F2001/1678—Constructional details characterised by the composition or particle type
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/04—Materials and properties dye
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/36—Micro- or nanomaterials

Description

電泳粒子
本申請案關於：
(a)　美國專利第6,822,782號；
(b)　美國專利第7,411,720號；
(c)　美國專利第7,002,728號；及
(d)　美國專利第7,247,379號。
本發明關於電泳粒子(即用於電泳介質之粒子)及此電泳粒子之製造方法。本發明亦關於電泳介質及加入此粒子之顯示器。更特定言之，本發明關於新穎之黑色或暗色電泳粒子。
關於電光顯示器之背景術語及技藝狀態詳細地討論於美國專利第7,012,600號，其給予讀者進一步資訊。因而將此術語及技藝狀態簡要地歸納於下。
粒子為主電泳顯示器(其中帶電粒子在電場影響下移動通過介質)近年來已成為深入硏發之標的。相較於液晶顯示器時，此顯示器可具有良好之亮度與對比、寬視角、狀態雙穩定性、及低電力消耗的屬性。
名詞「雙穩定」及「雙穩定性」在此係以其在此技藝之習知意義使用而指稱包含具有第一與第二顯示狀態(至少一種光學性質不同)之顯示元件的顯示器，及使得在已藉有限期間之定址脈衝驅動任何指定元件後，假定為其第一或第二顯示狀態在終止定址脈衝後此狀態持續至少數次(例如至少4次)，改變顯示元件之狀態所需定址脈衝之最小期間。美國專利第7,170,670號證明一些可為灰階之粒子為主電泳顯示器不僅在其極端黑白狀態，亦在其中間灰階狀態穩定，而且亦適用於一些其他型式之電光顯示器。此型顯示器被適當地稱為「多穩定」而非雙穩定，雖然為了方便而在此使用名詞「雙穩定」涵蓋雙穩定與多穩定顯示器。
儘管如此，電泳顯示器之長期影像品質問題使其無法普及地使用。例如組成電泳顯示器之粒子趨於沉降，造成這些顯示器之不當使用壽命。
如上所示，電泳介質需要流體。在大部分先行技藝電泳介質中，此流體為一種液體，但是電泳介質可使用氣態流體製造；參見例如Kitamura,T.等人之”Electrical toner movement for electronic paper-like display”,IDW Japan,2001,Paper HCS1-1，及Yamaguchi,Y.等人之”Toner display using insulative particles charged triboelectrically”,IDW Japan,2001,Paper AMD4-4)。亦參見美國專利公告第2005/0259068、2006/0087479、2006/0087489、2006/0087718、2006/0209008,2006/0214906、2006/0231401、2006/0238488、2006/0263927號、及美國專利第7,321,459與7,236,291號。此氣體為主電泳介質顯然易有如液體為主電泳介質由於粒子沉降造成之相同型式問題，例如將介質分配於垂直面之跡象。事實上，由於氣態懸浮流體相較於液體之較低黏度使電泳粒子更快速地沉降，粒子沉降顯然在氣體為主電泳介質中為較液體為主嚴重之間題。
讓渡予或麻省理工學院(MIT)與E Ink Corporation擁有之許多專利及申請案敘述各種用於封包電泳與其他電光介質之技術。此封包介質包含許多小囊，其本身各包含一種在流體介質中含電泳地移動粒子之內相、及包圍此內相之囊壁。一般而言，此囊本身係保持在聚合黏合劑內而形成位於兩個電極間之內聚層。這些專利及申請案所述之技術包括：
(a)　電泳粒子、流體與流體添加劑；參見例如美國專利第5,961,804；6,017,584；6,120,588；6,120,839；6,262,706；6,262,833；6,300,932；6,323,989；6,377,387；6,515,649；6,538,801；6,580,545；6,652,075；6,693,620；6,721,083；6,727,881；6,822,782；6,870,661；7,002,728；7,038,655；7,170,670；7,180,649；7,230,750；7,230,751；7,236,290；7,247,379；7,312,916；7,375,875；7,411,720號；及美國專利申請案公告第2005/0012980；2006/0202949；2007/0146310；2007/0200795；2008/0013155；與2008/0013156號；
(b)　囊、黏合劑與封包方法；參見例如美國專利第6,922,276與7,411,719號；
(c)　含電光材料之膜與次組件；參見例如美國專利第6,982,178號；及美國專利申請案公告第2007/0109219號；
(d)　背板、黏著層與其他輔助層、及用於顯示器之方法；參見例如美國專利第7,116,318號；及美國專利申請案公告第2007/0035808號；
(e)　顏色形成與顏色調整；參見例如美國專利第7,075,502號；及美國專利申請案公告第2007/0109219號；
(f)　驅動顯示器之方法；參見例如美國專利第7,012,600號；及美國專利申請案公告第2006/0262060號；及
(g)　顯示器之應用；參見例如美國專利第7,312,784號；及美國專利申請案公告第2006/0279527號。
已知之電泳介質(封包與未封包)可分成兩種主要型式，為了方便而在以下各稱為「單粒子」與「雙粒子」。此單與雙粒子之說明參見美國專利第6,870,661號。
許多上述專利及申請案認為在封包電泳介質中包圍不連續微囊之壁可被連續相取代，如此製造所謂之聚合物分散電泳顯示器，其中電泳介質包含多個不連續電泳流體滴、及聚合物材料之連續相，而且此聚合物分散電泳顯示器內之不連續電泳流體滴可視為囊或微囊，即使個別液滴均不附帶不連續囊膜；參見例如上述美國專利第6,866,760號。因而對於本申請案之方法，此聚合物分散電泳介質係視為封包電泳介質之次物種。
一種相關型式之電泳顯示器為所謂之「微管電泳顯示器」。在微管電泳顯示器中，帶電粒子與流體均不封包於微囊內，而是保留在多個於載體介質(一般為聚合物膜)內形成之穴內。參見例如美國專利第6,672,921與6,788,449號，其均讓渡予Sipix Imaging,Inc.。以下可使用名詞「微穴電泳顯示器」涵蓋封包與微管電泳顯示器。
雖然電泳介質經常為不透明(由於例如在許多電泳介質中，粒子實質上阻擋可見光穿透顯示器)且以反射模式操作，其可使許多電泳顯示器以所謂之「快門模式」操作，其中一種顯示狀態為實質上不透明及一種為透光性。參見例如美國專利第5,872,552；6,130,774；6,144,361；6,172,798；6,271,823；6,225,971；與6,184,856號。類似電泳顯示器但依賴電場強度變化之二電泳顯示器可以類似模式操作；參見美國專利第4,418,346號。其他型式之電光顯示器亦可以快門模式操作。以快門模式操作之電光介質可用於全彩顯示器之多層結構；在此結構中，相鄰顯示器之觀看表面的至少一層係以快門模式操作而暴露或隱藏距觀看表面較遠之第二層。
封包電泳顯示器一般不遭受傳統電泳顯示器之簇聚與沉降失敗模式，及提供進一步之優點，如在廣泛種類之撓性與剛性基板上印刷或塗覆顯示器之能力。(使用文字「印刷」係意圖包括全部之印刷與塗覆形式，其包括但不限於：前計量塗覆，如補片模塗覆、縫式或幾壓塗覆、滑動或串接塗覆、簾式塗覆；輥式塗覆，如刮刀輥式塗覆、正反輥式塗覆；凹版塗覆；浸式塗覆；噴灑塗覆；彎式塗覆；旋轉塗覆；刷式塗覆；空氣刀塗覆；絲網印刷法；靜電印刷法；熱印刷法；噴墨印刷法；電泳沉積(參見美國專利第7,339,715號)；及其他類似技術。)因此所得顯示器可為撓性。此外因為可印刷(使用各種方法)顯示介質，其可使顯示器本身不昂貴。
然而封包電泳顯示器之電光性質仍待改良。一般而言，電泳顯示器係設計成具有黑白極端光學狀態；然後可藉由相鄰電泳介質提供濾色片而產生顏色。許多先行技藝雙粒子顯示器使用鈦氧作為白色顏料及碳黑作為黑色顏料。然而如上述美國專利第7,002,728號所討論，碳黑在電泳顯示器引起許多問題，而且此專利教示以亞鉻酸銅，較佳為以聚合殼，及視情況地在亞鉻酸銅核與聚合殼之間具矽石層而取代碳黑。
在雙粒子顯示器中使用亞鉻酸銅作為黑色顏料確實解決許多碳黑顏料附帶之問題。然而用於電泳顯示器之顏料要求持續增加；特別是已發現，達成顯示器之非常低暗態反射性極為重要而確保使用濾色片陣列之彩色電泳顯示器的良好顏色飽和度，即使由亞鉻酸銅顏料提供之暗態對此目的較不理想。因而需要可提供較由亞鉻酸銅所提供暗之狀態的黑色顏料，及本發明尋求提供此黑色顏料。本發明提供之特定顏料具有無鉻之額外優點，如此排除可能存在於含亞鉻酸銅介質中成為污染物之六價鉻。
因而在一個態樣中，本發明提供一種電泳介質，其包含至少一種帶電粒子分散於流體，而且在對流體施加電場時可移動通過流體。依照本發明，此至少一種帶電粒子包含表面積為至少7平方米/克之無機黑色顏料。
用於本發明之較佳無機黑色顏料為表面積為至少10平方米/克，而且希望為15平方米/克者。如以下實例所證，實驗上發現平均顏料粒度與暗態性能之間有強烈之關聯，及顯示器之暗態反射性隨表面積增加而穩定地降低。因而希望使用一種表面積儘可能高之顏料，其當然有關處理及安全問題(在處理非常小之顏料粒子時可能遭遇)。較佳之黑色顏料為金屬氧化物(例如磁鐵礦(Fe3 O4 ))，及含鐵、鉻、鎳、錳、銅、鈷、可能與其他金屬之二或更多種的混合金屬氧化物。合適之顏料參見例如”Industrial Inorganic Pigments”,Gunter Buxbaum與Gerhard Pfaff(編者)，Wiley-VCH,2005。已發現得到良好結果之兩種指定顏料為銅鐵錳氧化物尖晶石(得自Ohio州Cincinnati之Shepherd Color Company的Shepherd黑444)與銅鉻錳氧化物尖晶石(得自同公司之黑20C920)。前者材料被製造者敘述為具有約0.5微米之平均粒度、5.3之比重、及22平方米/克之表面積，而後者被敘述為具有約1.0微米之平均粒度、5.1之比重、及11平方米/克之表面積。通常本發明之顏料粒子可具有0.1至2微米之平均直徑；如果粒子之平均粒度超過此範圍，則可使用硏磨或其他習知技術降低粒度。顏料粒子可塗有矽石及/或以聚合物化學地鍵結，或者圍繞顏料粒子交聯。通常較佳為聚合物化學地鍵結粒子。此聚合物可包含顏料粒子之1至15重量%，較佳為2至8重量%。此聚合物可包含帶電或可帶電基，例如胺基。此聚合物亦可包含一個主鏈及多個自主鏈延伸之側鏈，各側鏈包含至少4個碳原子。此聚合物可由丙烯酸酯或甲基丙烯酸酯形成。關於在顏料粒子上形成聚合物塗層之進一步細節參見美國專利第6,822,782；7,411,720與7,230,750號。
本發明之電泳介質可為任何上述型式，但是較佳為包含至少一種具有至少一種異於本發明顏料粒子之光學特徵的第二粒子，第二粒子亦具有異於本發明顏料粒子之電泳移動力。兩組粒子可帶有極性相反之電荷。第二粒子可為實質上白色，用於此目的之較佳白色顏料為鈦氧。在本發明之電泳介質中，懸浮流體可為液態或氣態，而且若為液體則可包含烴、或烴與氯化烴之混合物。
本發明之電泳介質可為封包型且包含囊壁，其內保留有流體與至少一種粒子。此封包介質可包含多個囊，其各包含囊壁與懸浮流體且將至少一個粒子保留於其中，此介質進一步包含聚合黏合劑包圍囊。
本發明延伸至一種電泳顯示器，其包含本發明電泳介質、及至少一個相鄰電泳介質而配置以對電泳介質施加電場之電極。在此電泳顯示器中，電泳介質可包含多個囊。或者電泳介質可為聚合物分散型且包含多個包含流體之液滴與包圍液滴之聚合材料連續相。此電泳顯示器亦可為微管型且包含其中形成多個密封穴之基板，流體與粒子係保留在密封穴內。
在另一個態樣中，本發明提供一種表面積為至少7平方米/克之無機黑色顏料，其具有聚合物化學地鍵結粒子或圍繞粒子交聯。較佳為此聚合物係化學地鍵結粒子。此聚合物可包含粒子之1至30重量%，較佳為4至25重量%。此聚合物可包含帶電或可帶電基，例如胺基。此聚合物可包含一個主鏈及多個自主鏈延伸之側鏈，各側鏈包含至少4個碳原子。此聚合物可由丙烯酸酯或甲基丙烯酸酯形成。
本發明之顯示器可用於任何其中已使用先行技藝電光顯示器之應用。因此例如本發明顯示器可用於電子書閱讀器、可攜式電腦、平板電腦、行動電話、智慧卡、信號、手錶、展示標籤、與記憶碟。
在另一個態樣中，本發明提供一種製造塗聚合物顏料粒子之方法；此方法包含：
(a)　反應表面積為至少7平方米/克之無機黑色顏料、與具有可與粒子反應及鍵結之官能基且亦具有可聚合或聚合引發基的試劑，因而引起官能基與粒子表面反應且對其附著可聚合基；及
(b)　在有效地引起粒子上可聚合或聚合引發基與至少一種單體或寡聚物間反應之條件下，反應步驟(a)之產物與至少一種單體或寡聚物，因而引起鍵結粒子之聚合物形成。
在此方法中，顏料粒子可在步驟(a)之前塗有矽石。用於步驟(a)之試劑可包含矽烷偶合基，例如三烷氧基矽烷偶合基。此試劑可進一步包含胺基。例如此試劑可包含N-[3-(三甲氧基矽烷基)丙基]-N’-(4-乙烯基苄基)-乙二胺鹽。此單體或寡聚物可包含至少一種丙烯酸酯或甲基丙烯酸酯，例如甲基丙烯酸月桂酯。
如上所示，本發明提供一種電泳介質，其使用一種包含表面積為至少7平方米/克之無機黑色顏料的帶電粒子。此粒子希望塗有聚合物。現已發現使用此無機黑色顏料粒子之電泳介質可強烈地顯示黑色暗態，L*值為約13至約22之範圍(其中L*具有一般CIE定義：
L*=116(R/R0 )1/3 -16，
其中R為反射度及R0 為標準反射值)，其實質上低於由亞鉻酸銅為主電泳介質得到之L*值。本發明電泳介質之白色狀態僅較亞鉻酸銅為主介質稍為不亮，使得本發明之介質具有較大之動態範圍(極端黑白狀態間之差，以L*單位表示)。此外對於在濾色片陣列為主顯示器中將顏色飽和最適化，由於模擬提示暗態改良較白色狀態改良重要，本發明之介質在此顯示器具有優異之顏色飽和，而且亦預期具有較悅人之顏色特徵。
以下為顯示用於本發明之方法及電泳介質的較佳試劑、條件及技術之實例，雖然僅為例證。
實例1：塗有聚合物的無機顏料粒子之製備
將原顏料(Shepherd黑444與Shepherd黑20C920)在水中硏磨以將前者顏料之平均粒度降至約0.3微米及後者為約0.5微米。然後利用如上述美國專利第6,822,782號的實例26之實質上相同步驟，使用N-[3-(三甲氧基矽烷基)丙基]-N’-(4-乙烯基苄基)-乙二胺貳鹽酸鹽(得自United Chemical Technologies)將經硏磨顏料表面官能化。完成之表面官能化量係藉熱重分析估計，其指示對黑444存在4-10%之揮發性(有機)材料，及對黑20C920為1.1-1.3%之揮發性(有機)材料。
實例2：含塗有聚合物的無機顏料粒子之電泳介質之製備
如下製備在實例1製造之兩種黑色顏料、及電泳介質內相之各種其他成分的標準溶液，而且在250毫升塑膠瓶中混合形成內相：
在裝有攪拌器與分液漏斗之500毫升外套反應器中製備明膠(10克)於溫度為42.5℃之去離子水(240克)的溶液。使用出口在明膠溶液表面下方之分液漏斗，在劇烈攪拌下將如上製備之內相經1分鐘加入。在此加入結束後立即將攪拌速率增至750 rpm以製造所需大小範圍之內相滴，而且將此攪拌程度維持1小時。在此時間結束後，將阿拉伯膠(10克)於溫度為40℃之去離子水(251.6克)的溶液加入內相分散液，及藉由加入10重量%之乙酸而將所得混合物之pH調整成4.9。然後將反應混合物之溫度分段降至8℃；在其溫度達到10℃時加入戊二醛(2.5克之50%水溶液)。然後將反應混合物加溫至25℃且維持在此溫度過夜而製造微囊於水性介質中之分散液。將微囊以澱積分隔，以去離子水清洗，及使用篩目為45與20微米之篩網篩選。所得囊之分析顯示平均大小為約40微米，超過97%之囊體積為直徑為20至60微米之囊。
實例3：囊成為實驗性顯示器之轉化
如下將在實例2製備之囊轉化成於聚合黏合劑之囊漿液。使囊沉降至少1小時，而且倒掉一些但非全部過量水。將含囊之瓶搖動以將囊在水中再分散，及以氫氧化銨將分散液之pH調整成9.0-9.5。將瓶再度搖動以再分散囊，而且藉熱重分析測量囊固體。將囊藉離子濃縮且倒掉上清液。加入足以製造且囊對黏合劑比例為8:1 w/w之聚合黏合劑、羥基丙基甲基纖維素(漿液質量之0.2%)、Triton X100界面活性劑(漿液質量之0.03%)、與水而製造含33重量%之囊固體的漿液，及將所得漿液劇烈地搖動以將濃縮囊自容器地部分散。然後將含漿液之瓶置於輥磨器上至少10小時。
然後在聚(對酞酸伸乙酯)(PET)/ITO膜之塗氧化銦錫(ITO)表面上使用4 mil(101微米)塗縫棒塗所得漿液，及將塗膜在60℃輸送器烤箱中乾燥約2分鐘而製造厚約18微米之囊(電光)層。分別地對脫模片以約25微米之厚度塗覆美國專利第7,012,735號所述型式之習用聚胺基甲酸酯層合黏著劑(摻雜180 ppm之六氟磷酸四丁銨)，及使用熱輥層合器將所得脫模片/層合黏著劑次組件層合至PET/ITO/囊層次組件(以層合黏著劑接觸囊層)。然後將所得前面層合物(參見上述美國專利第6,982,178號)切成二吋(51毫米)平方，去除脫模片，及將層合黏著劑熱輥層合至在撓性聚合物片上包含石墨電極之二吋(51毫米)平方背片。將合適之電導體附著至石墨與ITO電極而製造實驗性單像素顯示器。
使用15伏，240毫秒驅動脈衝測試如此製備之實驗性顯示器的電光性質。首先將各顯示器在其暗與白色狀態間重複地切換，然後最終使用單15伏，240毫秒驅動脈衝驅動至其暗與白色狀態之一。然後不施加驅動脈衝而使顯示器在相同狀態維持2分鐘(此2分鐘靜止期間係用以去除在一些電泳顯示器中出現之某些短期變化的影響)，然後測良其反射度且轉化成L*單位。暗態結果示於附圖之第1圖，及白態結果為第2圖。兩種情形均提供使用由亞鉻酸銅以相同方式製備之黑色顏料的對照顯示器之結果以比較。
由第1及2圖可知，本發明之兩種顏料產生實質上較先行技藝亞鉻酸銅顏料暗之暗態，同時僅遭受適度之白色狀態反射度降低。結果本發明之顯示器具有實質上較亞鉻酸銅為主顏料(8:1)大之對比比例(黑20C920為主顏料為14:1，及黑444為主顏料為20:1)。黑444為主顏料亦具有提供無鉻顏料之優點。
實例4：實驗性顯示器之暗態與顏料粒度之關聯
由Shepherd Color Company得到一系列具有大範圍每單位重量表面積測量之黑色顏料，而且其每單位重量表面積係藉習知BET(氮氣吸附)技術測量。然後以如實例1-3之相同方式將黑色顏料調配成實驗性單像素顯示器，及以如實例3之相同方式測量顯示器之暗態。第3圖為暗態相對每單位重量表面積之圖表(第3圖之橫座標為每克之平方米)。第3圖中最左之實驗點為亞鉻酸銅粒子，次兩組為表面積不同之黑20C920顏料樣品，及其餘均為表面積不同之黑444樣品。由第3圖提供之線性迴歸可知，增加表面積與改良暗態(即低L*值)間有強烈之關聯，而且此關聯顯然與顏料(至少對用於這些實驗之金屬氧化物顏料)之確實化學本性極為獨立。
附圖之第1及2圖各顯示在以上實例3所述實驗中得到之本發明特定實驗性顯示器及對照顯示器的暗及亮態反射值。
第3圖為在以上實例4所述實驗中得到之本發明特定實驗性顯示器的暗態相對暗色顏料之每單位重量表面積的圖表。

Claims (13)

  1. 一種電泳介質，其包含至少一種帶電粒子分散於流體，而且在對流體施加電場時可移動通過流體，此至少一種帶電粒子包含表面積為至少15平方米/克之無機黑色顏料，其中該無機黑色顏料包含磁鐵礦、或含鐵、鉻、鎳、錳、銅、與鈷之二或更多種的混合金屬氧化物。
  2. 如申請專利範圍第1項之電泳介質，其中該無機黑色顏料包含銅鐵錳氧化物尖晶石或銅鉻錳氧化物尖晶石。
  3. 如申請專利範圍第1項之電泳介質，其中無機黑色顏料具有化學地鍵結至該顏料粒子、或者在顏料粒子周圍交聯之聚合物。
  4. 如申請專利範圍第3項之電泳介質，其中該聚合物包含顏料粒子之1至15重量%。
  5. 如申請專利範圍第1項之電泳介質，其進一步包含至少一種具有至少一種異於無機黑色顏料粒子之光學特徵的第二粒子，該第二粒子亦具有異於無機黑色顏料粒子之電泳移動力。
  6. 如申請專利範圍第5項之電泳介質，其中兩組粒子可帶有極性相反之電荷。
  7. 如申請專利範圍第1項之電泳介質，其包含囊壁，該囊壁內保留有流體與無機黑色顏料粒子。
  8. 如申請專利範圍第7項之電泳介質，其進一步包含包圍該囊之聚合物黏合劑。
  9. 一種電泳顯示器，其包含如申請專利範圍第1項之電泳介質、及至少一個相鄰該電泳介質而配置以對該電泳介質施加電場之電極。
  10. 一種包含如申請專利範圍第9項之電泳顯示器之物品，其中該物品係電子書閱讀器、可攜式電腦、平板電腦、行動電話、智慧卡、信號(sign)、手錶、展示標籤、或記憶碟。
  11. 一種製造塗布有聚合物的顏料粒子之方法，此方法包含：(a)將表面積為至少15平方米/克之無機黑色顏料、與具有可與粒子反應及鍵結之官能基且亦具有可聚合或聚合引發基的試劑反應，因而引起官能基與粒子表面反應且對其附著可聚合基；及(b)在使粒子上可聚合或聚合引發基與至少一種單體或寡聚物之間有效地引起反應之條件下，將步驟(a)之產物與該至少一種單體或寡聚物反應，因而引起形成鍵結至該粒子之聚合物；其中該無機黑色顏料包含磁鐵礦、或含鐵、鉻、鎳、錳、銅、與鈷之二或更多種的混合金屬氧化物。
  12. 如申請專利範圍第11項之方法，其中用於步驟(a)之試劑包含矽烷偶合基。
  13. 如申請專利範圍第12項之方法，其中該試劑進一步包含胺基。
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