TWI549813B - 透明導電基材之製造方法及透明導電基材 - Google Patents
透明導電基材之製造方法及透明導電基材 Download PDFInfo
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- TWI549813B TWI549813B TW101143257A TW101143257A TWI549813B TW I549813 B TWI549813 B TW I549813B TW 101143257 A TW101143257 A TW 101143257A TW 101143257 A TW101143257 A TW 101143257A TW I549813 B TWI549813 B TW I549813B
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- film
- wet film
- transparent conductive
- conductive substrate
- metal nanowire
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Description
本發明係關於一種於基材薄膜上具有以配向狀態混亂之狀態包含金屬奈米線之導電層且表面電阻幾乎無異向性的透明導電基材之製造方法。詳細而言,係關於一種於塗佈包含金屬奈米線之塗佈液後進行乾燥之步驟中,變更金屬奈米線之朝向而使各金屬奈米線之配向狀態成為混亂之狀態的方法。
透明導電基材係用於平板型顯示器或觸控面板、電致發光器件用等。通常之透明導電性材料係基材薄膜/摻錫氧化銦(ITO,Indium Tin Oxide)等金屬氧化物之構成,且通常之製造方法係真空蒸鍍法、濺鍍法、離子電鍍法等氣相製膜法。然而,就ITO由於含有稀有金屬故而難以穩定地獲取、氣相製膜法之生產速度較慢等原因而言,代替品之開發盛行。
作為代替品之一,存在金屬奈米線(包含金屬且直徑為數十~數百nm、長度為1~百數十μm之線狀者)(專利文獻1、2)。金屬奈米線係由於纖維直徑充分小故而透明性不會降低,由於纖維長度充分長故而即便添加量較少亦可於基材上構建導電網。將水系溶劑中分散有金屬奈米線之塗佈液塗佈於基材上並進行乾燥,製造透明導電基材。
專利文獻1:日本專利特開2011-90879號公報
專利文獻2:日本專利特開2011-119142號公報
專利文獻3:日本專利特開2006-233252號公報
專利文獻4:日本專利特開2002-266007號公報
專利文獻5:日本專利特開2004-149871號公報
非專利文獻1:Adv. Mater., 2002, 14, 833~837
非專利文獻2:Chem. Mater., 2002, 14, 4736~4745
然而,作為使用有金屬奈米線之透明導電基材之課題,有金屬奈米線之長軸齊列於薄膜之搬送方向(搬送方向=長度方向=MD)上之情況。若金屬奈米線之長軸齊列於薄膜之MD上,則MD之表面電阻值、與垂直於MD之方向(寬度方向=短邊方向=TD)之表面電阻值會產生差異(異向性)。即,TD之電阻值變得大於MD之電阻值。其原因在於:MD之導電通道變密,TD之導電通道變疏。金屬奈米線之長軸齊列於薄膜之MD上之原因雖並未明確,但可認為係如下方面(參照圖5):i)於將塗佈液塗佈於基材薄膜上時,藉由擠出液體之力而將奈米線配向於液流(MD)上(奈米線齊列於最不受液流之
阻力之方向上);ii)將塗佈液塗佈於基材薄膜上之後,於搬送基材薄膜/塗佈液(濕膜)時,藉由基材薄膜於MD上移動而使濕膜中之奈米線排列於薄膜MD上。
為了解決此種課題,專利文獻1中指定剪切速度(薄膜搬送速度/狹縫式模具頭前端與薄膜之間隔)。然而,薄膜之搬送速度係由製造設備(尤其是乾燥設備)之能力所限制,狹縫式模具頭前端與薄膜之間隔係由模具之形狀或塗佈液之性質所限制,故而若並非符合液體之性質之狹縫式模具與具有充分之乾燥能力之製造設備,則可變更剪切速度之幅度較小,且因奈米線之配向狀態混亂而無法調整剪切速度。
因此,本發明之課題在於提供一種改善使用有金屬奈米線之透明導電基材之異向性的技術。即,其課題在於提供一種技術,其係以TD之表面電阻值(RTD)與MD之表面電阻值(RMD)無差異之方式變更各金屬奈米線之朝向,而成為金屬奈米線之配向狀態混亂之狀態。
本發明之目的在於提供一種於基材薄膜上具有以配向狀態混亂之狀態包含金屬奈米線之導電層且表面電阻幾乎無異向性的透明導電基材之製造方法、及以該製造方法所獲得之表面電阻幾乎無異向性之透明導電基材。
更具體而言,本發明之目的在於提供一種RTD/RMD=0.8~1.2、較佳為0.9~1.1之透明導電基材。
本發明者等人為了變更金屬奈米線之朝向,於剛塗佈塗佈液(奈米線+水系溶劑)後,自基材薄膜之TD進行送風(參照圖6)。將圖6之本發明之預試驗之結果示於表1及2中。可知藉由來自TD之送風而改善了RTD/RMD。
然而,並非為異向性之改善充分者(RTD/RMD=1.31)。認為其原因在於:由於基材上之塗佈液(濕膜)為較厚之15 μm左右,故而自濕膜突出(自濕膜表面露出面目)之奈米線之量較少,即便自TD進行送風,受到風影響而改變朝向之奈米線的量亦較少(參照圖1)。又,認為如下情況亦有影響,即,剛塗佈後之塗佈液係由於溶劑量較多且奈米線之自由度較高,故而藉由來自TD之送風而使配向暫且受到擾亂之奈米線亦於搬送步驟中再次排列於MD上。因此,本發明者等人係於濕膜厚度減少之乾燥步驟中進行送風(參照圖2)。於是,可明顯改善表面電阻值之異向性,以至完成本發明。
即,本發明係以如下(1)~(6)中記載之透明導電基材之製造方法作為主旨。
(1)一種透明導電基材之製造方法,其包括如下步驟:塗佈步驟,其係於基材薄膜上塗佈使金屬奈米線分散於溶劑中而成之塗佈液,形成濕膜;及乾燥步驟,其係乾燥去除上述濕膜中所含之溶劑;該製造方法之特徵在於:上述乾燥步驟包括如下步驟,即,自與形成有濕膜之基材薄膜之長度方向不同的方向朝向該濕膜進行送風,以輸送之風吹到自其表面突出之奈米線之方式變更各金屬奈米線之朝向,而成為各金屬奈米線之配向狀態混亂之狀態。
(2)一種透明導電基材之製造方法,其包括如下步驟:陸續送出步驟,其係陸續送出捲繞為捲筒狀之基材薄膜;塗佈步驟,其係於該基材薄膜上塗佈自狹縫式模具陸續送出之使金屬奈米線分散於溶劑中而成之塗佈液,形成濕膜;搬送步驟,其係將形成有濕膜之基材薄膜搬送至乾燥步驟;乾燥步驟,其係乾燥去除濕膜所含之溶劑;及捲取步驟,其係捲取所獲得之透明導電基材;該製造方法之特徵在於:上述乾燥步驟包括如下步驟,即,自與形成有濕膜之基材薄膜之長度方向不同之方向朝向該濕膜進行送風,以輸送之風吹到自其表面突出之奈米線之方式變更各金屬奈米線之朝向,而成為各金屬奈米線之配向狀態混亂之狀態。
(3)如上述(1)或(2)之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13 μm以下後朝向該濕膜進行送風。
(4)如上述(1)或(2)之透明導電基材之製造方法,其中,於
濕膜之膜厚減少至13 μm以下後自與基材薄膜之長度方向大致垂直的方向朝向該濕膜進行送風。
(5)如上述(1)或(2)之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13 μm以下後以4~20 m/s之風速朝向該濕膜進行送風。
(6)如上述(1)或(2)之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13 μm以下後以調整為30~60℃之送風朝向該濕膜進行送風。
又,本發明係以如下(7)中記載之透明導電基材作為主旨。
(7)一種透明導電基材,其係藉由如上述(1)或(2)之方法而製造,其特徵在於:於將基材薄膜之長度方向中之表面電阻值設為RMD、與長度方向垂直之方向中之表面電阻值設為RTD之情形時,以下述數學式1所表示。
[數1]RTD/RMD=0.8~1.2 (1)
根據本發明,於基材薄膜上具有包含金屬奈米線之導電層的透明導電基材之金屬奈米線之配向狀態之異向性有所改善。可提供一種表面電阻幾乎無異向性的透明導電基材之製造方法、及以該製造方法所獲得之表面電阻幾乎無異向性之透明導電基材。因此,本發明之透明導電基材可較佳地用於期待表面電阻值具有等向性的觸控面板之電極等中。
於本發明中,作為透明導電材料,金屬奈米線係作為主要之導電體發揮功能。金屬奈米線係可使用塊體狀態下之導電率為1×106 S/m以上的元素作為金屬元素。作為具體例,可列舉Ag、Cu、Au、Al、Rh、Ir、Co、Zn、Ni、In、Fe、Pd、Pt、Sn、Ti等。亦可組合使用2種以上之金屬奈米線,但自導電性之觀點出發,較佳為使用至少選自Ag、Cu、Au、Al、Co中之元素。
金屬奈米線之製造方法中並無特別限制,例如,可使用液相法或氣相法等公知之方法。例如,作為Ag奈米線之製造方法,可參考非專利文獻1、2等,作為Au奈米線之製造方法,可參考專利文獻3等,作為Cu奈米線之製造方法,可參考專利文獻4等,作為Co奈米線之製造方法,可參考專利文獻5等。尤其是上述非專利文獻1及2中提出報告的Ag奈米線之製造方法係因水系故而可簡便且大量地製造Ag奈米線,又,於金屬中Ag之導電率最大,故而可較佳地用作本發明之金屬奈米線之製造方法。
於本發明中,藉由使金屬奈米線彼此互相接觸而形成三維之導電網,顯現出較高之導電性並且光可穿透不存在金屬奈米線之導電網之窗部,從而可兼具較高之導電性與較高之穿透率。
於本發明中,就金屬奈米線之直徑而言,自透明性之觀點出發,較佳為200 nm以下,更佳為100 nm以下。作為金屬奈米線之平均長度,自導電性之觀點出發較佳為1 μm以上,考慮到因凝聚對透明性之影響,較佳為100 μm以下。更佳為1~50 μm,最佳為3~50 μm。
於本發明中,所謂「水系溶劑」係指50質量%以上為水之溶劑。當然亦可為不含有其他溶劑之純水,於考慮到乾燥時之金屬奈米線之分散穩定性之情形時,較佳為其他溶劑之含量少的水系溶劑。水系溶劑中之除水以外之成分只要為與水相溶之溶劑則並無特別限制,可較佳地使用醇系溶劑,其中,較佳為沸點相對較靠近水之異丙醇。
只要為透明樹脂薄膜,則可無特別限制地使用。較佳為,例如可列舉聚對苯二甲酸乙二酯(PET,Polyethylene terephthalate)、聚萘二甲酸乙二酯、改質聚酯等聚酯系樹脂薄膜,聚乙烯(PE,Polyethylene)樹脂薄膜、聚丙烯(PP,Polypropylene)樹脂薄膜、聚苯乙烯樹脂薄膜、環狀烯烴系樹脂等聚烯烴類樹脂薄膜,聚氯乙烯、聚偏二氯乙烯等乙烯系樹脂薄膜,聚醚醚酮(PEEK,Polyetheretherketone)樹脂薄膜,聚碸(PSF,Polysulfone)樹脂薄膜,聚醚碸(PES,Polyethersulphone)樹脂薄膜,聚碳酸酯(PC,Polycarbonate)
樹脂薄膜,聚醯胺樹脂薄膜,聚醯亞胺樹脂薄膜,丙烯酸系樹脂薄膜,三醋酸纖維素(TAC,Triacetyl cellulose)樹脂薄膜等;只要為可見光範圍內之波長(380~780 nm)下之穿透率為80%以上的樹脂薄膜,則可較佳地應用於本發明之透明樹脂薄膜中。其中,就透明性、耐熱性、使用之容易性、強度及成本之方面而言,較佳為聚對苯二甲酸乙二酯薄膜、聚碳酸酯薄膜。
就使金屬奈米線分散於溶劑、較佳為水系溶劑中而成之塗佈液而言,亦可含有添加劑及結合劑以調節黏度、腐蝕、黏著力、及奈米線分散。作為適當之添加劑及結合劑之例,可列舉羧甲基纖維素(CMC,Carboxymethyl cellulose)、2-羥乙基纖維素(HEC,2-Hydroxyethyl cellulose)、羥丙基甲基纖維素(HPMC,Hydroxypropyl methyl cellulose)、甲基纖維素(MC,Methyl cellulose)、聚乙烯醇(PVA,Polyvinyl alcohol)、三丙二醇(TPG,Tripropylene glycol)、及三仙膠(XG,Xanthan Gum)、及乙氧基化物、烷氧基化物、環氧乙烷及環氧丙烷及其等之共聚物般之界面活性劑,磺酸鹽、硫酸鹽、二磺酸鹽、磺基琥珀酸鹽、磷酸酯、及氟界面活性劑(例如Zonyl(註冊商標),Dupont公司),但並不限定於其等。
例如可使用模塗法、凹版塗佈法等,但因凹版塗佈法中版
眼會殘留於基材上而模塗法不會對基材施加損害之原因,模塗法最佳。
塗佈步驟:使用例如模塗機於基材上塗佈經調整之塗佈液。塗佈液之厚度並無特別限定,較理想為10~30 μm左右。
搬送步驟:將塗佈步驟中形成有濕膜之基材薄膜搬送至乾燥步驟。搬送方法並無特別限定,通常為輥搬送。於搬送步驟較長之情形時,會有於該步驟中濕膜厚度適當減少之情況。於此種情形時,亦可於下述乾燥步驟中立即進行變更奈米線之朝向的送風。又,於搬送步驟較短之情形時,較理想為於進行某種程度之乾燥而減少濕膜厚度之後,進行變更奈米線之朝向的送風。
乾燥步驟:乾燥方法並無特別限定,可例示使用IR(infrared,紅外線)加熱器等加熱之方法、藉由乾燥風加溫之方法等,但若乾燥爐內之空氣滯留則溶劑蒸氣濃度會上升而使乾燥耗費時間,故而較理想為使用乾燥風。作為乾燥風,為了防止塗佈面變粗糙,較佳為於與薄膜之前進方向相反方向上輸送。又,乾燥風較佳為於與薄膜表面相距十數~數十cm之位置流動(參照圖3)。再者,乾燥步驟中之乾燥風並非必須,可僅利用設置於乾燥步驟中之變更金屬奈米線之朝向之步驟中的風進行乾燥。於該情形時,變更奈米線之朝向之風對乾燥之影響大於乾燥風對乾燥之影響。
設置於乾燥步驟中。
作為具體之方法,自與MD不同之方向朝向基材上之濕膜送風。該風之朝向係TD,可以最佳的效率改善異向性。於自上方觀察基材薄膜之情形時,最理想為風自一側端向另一端(向TD)吹拂[參照圖4(a)]。較理想為,該風之中心於與基材平行之方向上吹拂濕膜表面之正上方(1~數cm)[參照圖4(b)]。若以噴附到濕膜上之方式吹拂,則有基材表面之平滑性紊亂之虞。該風之高度係以不擾亂基材表面(濕膜之表面)之平滑性、且使風吹到自基材表面突出之奈米線的方式進行適當調節。
該風之風速較佳為4~20 m/s,尤佳為8~12 m/s。若風速未達4 m/s則改變奈米線之配向狀態之效果不充分,若超過20 m/s則有基材表面之平滑性紊亂之虞。
該風之溫度較理想為30~60℃。若風之溫度較高則有塗膜變白等外觀惡化之虞。又,若風之溫度較高則乾燥時間變短,可變更奈米線之朝向之部位變窄。反之,若該風之溫度較低,則難以對濕膜之乾燥產生影響,故而可變更奈米線之朝向之部位變長而乾燥時間變長,因此,較理想為在環境溫度以上、尤其是30℃以上。再者,於在乾燥步驟中使用乾燥風之情形時,若該風(改變奈米線之朝向之風)之溫度與乾燥風之溫度為相同之溫度,則只要有一個調溫設備即可。
為了縮短送風時間或者增加線速,尤其較理想為在預先藉由乾燥風等使濕膜之厚度減少至13 μm以下後輸送改變奈米線之朝向的風,尤其較理想為於濕膜之厚度減少至10 μm以下後進行送風。又,送風亦可進行至濕膜完全乾燥為止,但即便稍微殘留有水系溶劑,只要濕膜厚度減少至奈米線之自由度被奪去之程度為止,則亦可停止送風。具體而言,於濕膜之厚度為5 μm以下之區域內亦可停止送風。其後,視需要亦可利用乾燥風等進行乾燥。
作為本發明之透明導電基材,當將基材薄膜之MD上之表面電阻值設為RMD、將TD上之表面電阻值設為RTD之情形時,以下述數學式1所表示。
[數1]RTD/RMD=0.8~1.2(尤佳為0.9~1.1) (1)
以下,藉由實施例更具體地說明本發明,但本發明之技術性範圍並不限定於該等例示。又,實施例中之%只要無特別記載則全部為質量%。
塗佈液:係由0.10重量%之金屬奈米線(纖維長:1~100 μm)、99.90重量%之溶劑(超純水)混合而成者。
塗佈步驟:利用模塗法。自狹縫式模具向經輥搬送之基材薄膜上擠出塗佈液。剛塗佈後之濕膜之厚度係15.0 μm。
搬送步驟:將自塗佈液擠出之基材薄膜輥搬送至乾燥爐。
乾燥步驟:於乾燥爐中使用乾燥風進行乾燥。具體而言係於與濕膜表面相距30 cm的上方,向與薄膜之前進方向相反的方向上輸送乾燥風(40℃,1 m/s),進行乾燥。再者,乾燥風係對未自TD送風之區域送風。即,於本實施例中不對自TD送風之區域吹拂乾燥風。
變更金屬奈米線之朝向之步驟:如以下圖示般,將乾燥步驟(乾燥爐)分割為4個區域,如表1所示自TD方向輸送風(40℃,10 m/s)。(實施例1~6)
於在基材薄膜上剛自狹縫式模具塗佈塗佈液後,在將基材薄膜搬送至乾燥步驟前與實施例相同地輸送來自TD之風,將此設為比較例1。
再者,實施例1~6、比較例1之薄膜之搬送速度係15 m/s。
準備兩個長度30 mm、寬度7 mm之金屬電極,以電極間距離成為24 mm之方式進行固定,以導線連接電極表面與測試器(A&D製造之數位萬用表AD-5536)之夾具,使用此種方式,對所獲得之透明導電基材測定電阻值。結果係示於表3中。
若於濕膜厚度為13 μm以下時吹拂來自TD之風則有RTD/RMD改善效果,尤其是於10 μm以下可看到改善效果。再者,實施例5、6中係於乾燥步驟中立即進行來自TD之送風,雖可確認有RTD/RMD改善效果,但可認為其原因在於:搬送至乾燥步驟之基材薄膜上之濕膜已經減少至13.1 μm。
繼而,使來自TD之風之速度發生變化而進行實驗。再者,設為0.18%之金屬奈米線、99.82%之溶劑(超純水),薄膜之搬送速度為10 m/s,且於第一至第二區域內吹拂來自TD之風。結果係示於表4中。
藉由增大來自TD之風之風速,而可看到RTD/RMD之改善。根據條件,亦有RMD超過RTD(RTD/RMD為1以下)之情況。
於與實施例8相同之條件下,僅將薄膜之搬送速度返回至15 m/s,製造透明導電基材。RTD/RMD係1.1。於在濕膜厚度之減少量相同之範圍內吹出變更奈米線之朝向的風之情形時,薄膜之搬送速度越慢則越可看到RTD/RMD改善效果。
圖1係說明圖6之預試驗中之金屬奈米線與送風的關係之圖式。
圖2係說明本發明之實施例中之金屬奈米線與送風的關係之圖式。
圖3係說明本發明之實施例中之乾燥爐內之送風與薄膜的關係之圖式。
圖4係說明本發明之實施例中之變更金屬奈米線之朝向之步驟的送風與薄膜的關係之圖式。(a)係說明朝TD送風之圖式,(b)係說明該風於與基材平行之方向上吹拂濕膜表面之正上方(風之中心為與濕膜表面相距1~數cm的上方)之圖式。
圖5係說明表面電阻之異向性之顯現的原因之流程圖。
圖6係說明為了變更金屬奈米線之朝向而於將塗佈液(奈米線+水系溶劑)塗佈後,自基材薄膜之TD進行送風的本發明之預試驗之圖式。
圖7係說明對變更金屬奈米線之朝向之步驟中使用之乾燥爐中、分割之4個區域的位置關係之圖式。
Claims (7)
- 一種透明導電基材之製造方法,其包括如下步驟:陸續送出步驟,其係陸續送出捲繞為捲筒狀之基材薄膜;塗佈步驟,其係於在長度方向上搬送之上述基材薄膜上塗佈使金屬奈米線分散於溶劑中而成之塗佈液,形成濕膜;搬送步驟,其係將上述基材薄膜於上述長度方向上搬送;及乾燥步驟,其係乾燥去除上述濕膜所含之溶劑;該製造方法之特徵在於:上述乾燥步驟包括如下步驟:自與形成有濕膜之基材薄膜之長度方向不同的方向,朝向該濕膜進行送風,以輸送之風吹到自其表面突出之奈米線之方式變更各金屬奈米線之朝向,而成為各金屬奈米線之配向狀態混亂之狀態。
- 一種透明導電基材之製造方法,其包括如下步驟:陸續送出步驟,其係陸續送出捲繞為捲筒狀之基材薄膜;塗佈步驟,其係於在長度方向上搬送之該基材薄膜上塗佈自狹縫式模具陸續送出之使金屬奈米線分散於溶劑中而成之塗佈液,形成濕膜;搬送步驟,其係將形成有濕膜之基材薄膜於上述長度方向上搬送至乾燥步驟;乾燥步驟,其係乾燥去除濕膜所含之溶劑;及捲取步驟,其係捲取所獲得之透明導電基材;該製造方法之特徵在於:上述乾燥步驟包括如下步驟:自與形成有濕膜之基材薄膜之長度方向不同之方向朝向該濕膜進行送風,以輸送之風吹 到自其表面突出之奈米線之方式變更各金屬奈米線之朝向,而成為各金屬奈米線之配向狀態混亂之狀態。
- 如申請專利範圍第1或2項之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13μm以下後,朝向該濕膜進行送風。
- 如申請專利範圍第1或2項之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13μm以下後,自與基材薄膜之長度方向大致垂直的方向朝向該濕膜進行送風。
- 如申請專利範圍第1或2項之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13μm以下後,以4~20m/s之風速朝向該濕膜進行送風。
- 如申請專利範圍第1或2項之透明導電基材之製造方法,其中,於濕膜之膜厚減少至13μm以下後,以調整為30~60℃之送風朝向該濕膜進行送風。
- 一種透明導電基材,其係藉由申請專利範圍第1或2項之方法而製造,其特徵在於:於將基材薄膜之長度方向中之表面電阻值設為RMD、與長度方向垂直之方向中之表面電阻值設為RTD之情形時,以下述數學式1所表示:[數1]RTD/RMD=0.8~1.2 (1)。
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