TWI675751B - 含有樹脂之薄片、以及使用其之構造體及配線板 - Google Patents
含有樹脂之薄片、以及使用其之構造體及配線板 Download PDFInfo
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- TWI675751B TWI675751B TW104136032A TW104136032A TWI675751B TW I675751 B TWI675751 B TW I675751B TW 104136032 A TW104136032 A TW 104136032A TW 104136032 A TW104136032 A TW 104136032A TW I675751 B TWI675751 B TW I675751B
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- Prior art keywords
- resin
- cellulose
- fixing agent
- fibers
- containing sheet
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Abstract
提供在提高纖維素奈米纖維不織布之力學強度的同時,基板的耐彎曲性亦提高的含有樹脂之薄片、以及使用其之構造體及配線板。
一種含有樹脂之薄片,其具有特定之纖維素奈米纖維不織布(11)、使纖維素奈米纖維不織布(11)中之纖維(1)彼此固著的固著劑(2)、與接觸於纖維素奈米纖維不織布(11)與固著劑(2)之樹脂(3),且固著劑(2)之儲存模數高於樹脂(3)之儲存模數。使該含有樹脂之薄片密合於基板而得到之構造體。具有該構造體之配線板。
Description
本發明係關於具有優良力學強度、彈性率、及耐彎曲性,適於電子機器用之配線板等的含有樹脂之薄片、以及使用其之構造體及配線板。
電子機器用之配線板,一般而言係使用將於由玻璃纖維或聚芳醯胺(aramid)纖維等所成之基材中含浸環氧樹脂等樹脂而得到之預浸物(半硬化狀態之樹脂絕緣層),與銅等之金屬箔密合,且以蝕刻法形成有電路者。又,為了防止零件構裝時之焊料流出,於配線板係設有阻焊劑。為了提高構裝信賴性,對配線板而言係期望高強度(高彈性率),對於其構成構件之預浸物或阻焊劑,亦同樣地謀求高彈性率化。又,於電子機器係有使用可撓配線板,由高密度化/薄型之要求而言,對可撓配線板亦有要求多層化。作為以往的可撓配線板之多層化材料,係有接合片或包覆層,要求作為配線板之耐彎曲性。
關於配線板材料之習知技術,例如專利文獻1中,記載為了得到絕緣信賴性及與配線之應力緩和的兩種
功能,而於核心層之兩面設置不同強度(彈性率)之樹脂層的預浸物。又,專利文獻2中,記載了具有特定彈性率之預浸物。此技術係以預浸物薄片與電路基板之臨時固定為目的,而藉由組成物來控制彈性率者。
進一步地,專利文獻3中,揭示了於預浸物中使用2種樹脂組成物的技術。於該預浸物中,係使2種樹脂組成物以越靠表面側彈性率越大的方式不平均存在。又進而,專利文獻4中記載為了改良與金屬箔之接著性,於預浸物表面設置接著層之技術。又進而,專利文獻5中記載了使用薄板玻璃、纖維素奈米纖維與樹脂之複合材料的配線板。
[專利文獻1]日本特開2008-088280號公報
[專利文獻2]日本特開2006-179716號公報
[專利文獻3]日本特開2010-095557號公報
[專利文獻4]日本特開2004-168943號公報
[專利文獻5]日本特開2008-242154號公報
但是,上述以往的預浸物及配線板,無法具有充分的力學強度與耐彎曲性。
因而,本發明之目的,係提供在提高力學強度的同時,耐彎曲性亦提高的含有樹脂之薄片、以及使用其之構造體及配線板。
本發明者等人為了解決上述課題而努力探討的結果,發現以下事實。
亦即,由微細之纖維所成的織布,例如纖維素奈米纖維不織布中,纖維彼此係藉由互相纏繞或相互作用而形成集合體。因此對纖維之集合體於一方向施加張力時,纖維彼此會於接點滑動而分離,於集合體產生跳紗,最終會斷裂。
如前所述,於配線板係使用玻璃布、或如由聚芳醯胺纖維與樹脂所成之預浸物般的含有樹脂之薄片,因此為了確保配線板之強度,如此之防止纖維之集合體中纖維彼此的滑動係重要的。另一方面,如前所述,對於含有樹脂之薄片,亦要求對可撓配線板所要求之耐彎曲性。
上述探討的結果,本發明者等人發現了藉由以下構成,可取得力學強度與耐彎曲性之平衡。
亦即,本發明之含有樹脂之薄片,其特徵為具有:由包含至少一層的含有70質量%以上之再生纖維素微細纖維的纖維素微細纖維層之單層或3層以下之複數層所構成,且滿足下述(1)~(3)之全部要件的纖維素奈米纖維不織布、
使前述纖維素奈米纖維不織布中之纖維彼此固著之固著劑、與鄰接於前述纖維素奈米纖維不織布與固著劑之樹脂,且前述固著劑之儲存模數,高於前述樹脂之儲存模數;(1)構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑為0.20μm以上且1.0μm以下、(2)透氣抵抗度為1s/100ml以上且40s/100ml以下、(3)膜厚為8μm以上且22μm以下。
本發明中,前述固著劑之玻璃轉移溫度,較佳為高於前述樹脂之玻璃轉移溫度或軟化溫度。本發明之含有樹脂之薄片,可藉由將前述纖維素奈米纖維不織布之纖維彼此藉由固著劑組成物固著後,使樹脂組成物含浸於該經固著之纖維素奈米纖維不織布而得到。此時,前述固著劑組成物之黏度,較佳為1Pa.s以下。
本發明之構造體,其特徵為將上述本發明之含有樹脂之薄片密合於基板而得到。
進一步地,本發明之配線板,其特徵為具有上述本發明之構造體。
依照本發明,可得到在提高力學強度的同時,提高耐彎曲性的含有樹脂之薄片。亦即,本發明中,係發現用以藉由作為纖維成分,使用再生纖維素微細纖維來構成具有特定物性之纖維素奈米纖維不織布,而且使固
著該纖維素奈米纖維不織布中之纖維彼此的固著劑之儲存模數,較接觸於纖維素奈米纖維不織布與固著劑之樹脂之儲存模數更高,而得到在實現高強度/高彈性率化的同時,亦提高耐彎曲性的含有樹脂之薄片的材料之條件。此係為對配線板用之樹脂絕緣材料係要求高強度化,但例如使用環氧樹脂等高彈性率材料時,耐彎曲性會惡化,於此,本發明係為在實現高彈性率化的同時,解決該耐彎曲性之問題者。
1‧‧‧纖維
2‧‧‧固著劑
3‧‧‧樹脂
11‧‧‧纖維素奈米纖維不織布
S‧‧‧空間
[圖1]示意性表示本發明之含有樹脂之薄片的構造之說明圖。
以下一邊參照圖式,一邊詳細說明本發明之實施形態。
圖1顯示表示本發明之含有樹脂之薄片的構造之說明圖。本發明之含有樹脂之薄片,主要係由纖維成分與樹脂成分所形成之薄片狀體,如圖所示,係具有纖維素奈米纖維不織布11、將纖維素奈米纖維不織布11中之纖維1彼此固著之固著劑2、與接觸於纖維素奈米纖維不織布11與固著劑2之樹脂3。再者,圖中之符號S,表示於纖維素奈米纖維不織布11內皆未含浸固著劑2及樹脂3的空
間。本發明之含有樹脂之薄片中,可說構成纖維素奈米纖維不織布11之纖維1、固著劑2、與樹脂3,全體係形成1個層者。本發明之含有樹脂之薄片中,固著纖維1彼此的固著劑2之儲存模數,於任一溫度中,較樹脂3之儲存模數更高的這點係重要的。
亦即,本發明者等人努力探討的結果,發現含有樹脂之薄片中所含之各種成分的角色係有2種,1種為作為用以抑制纖維彼此的滑動,使含有樹脂之薄片高強度及高彈性率化的固著劑之角色,另1種為提高耐彎曲性之角色。由該觀點,本發明者等人進一步探討的結果,發現含有樹脂之薄片中所含之樹脂成分的角色,關於確保高強度係由固著劑負責,而規定此等固著劑與樹脂之儲存模數或玻璃轉移溫度之關係,又,關於確保耐彎曲性,藉由存在有固著劑、樹脂與纖維素奈米纖維不織布,可一併良好地確保此等兩性能。如此地,將樹脂成分之角色分為2種,而兼顧高彈性率與良好的耐彎曲性之技術,係以往尚未為人所知。
概念性地說明本發明時,藉由將纖維素奈米纖維不織布中所含之纖維彼此的接點以固著劑固著,即使於一方向施加張力時,於接點亦不會產生滑動,因此可將纖維素奈米纖維不織布高強度/高彈性率化。進一步地,藉由以接觸於纖維素奈米纖維不織布與固著劑的方式含浸樹脂,亦可得到作為含有樹脂之薄片的良好之耐彎曲性。因而,依照本發明之含有樹脂之薄片,可一邊藉由固著劑
確保作為要求性能之高彈性率,一邊亦確保耐彎曲性,可得到單以使用環氧樹脂等高彈性率材料所無法得到之兼備高強度與良好之耐彎曲性兩者的含有樹脂之薄片。
本發明之含有樹脂之薄片所用之纖維素奈米纖維不織布,係由包含至少一層的含有70質量%以上之再生纖維素微細纖維的纖維素微細纖維層之單層或3層以下之複數層所構成。較佳為,再生纖維素微細纖維為75質量%以上。再生纖維素微細纖維未達70質量%時,由樹脂之含浸性觀點而言不佳。
首先,說明構成上述纖維素奈米纖維不織布之再生纖維素微細纖維。本發明中,再生纖維素,係指將天然纖維素予以溶解或結晶膨潤(絲光化)處理再生所得之物質,且係具有以粒子線繞射而獲得以相當於晶格面間隔0.73nm、0.44nm或0.40nm之繞射角為頂點的結晶繞射圖型(纖維素II型結晶)之分子序列的β-1,4鍵結葡聚醣(葡萄糖聚合物),例如意指縲縈、銅氨纖維(cupra)、天絲纖維(tencel)等之再生纖維素纖維。此等之中,就微細化之容易程度的觀點而言,尤以使用以對纖維軸方向之分子配向性高的銅氨纖維或天絲纖維為原料而經微細化之纖維較佳。
上述纖維素奈米纖維不織布中所含之構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑,必須
為1.0μm以下,較佳為0.7μm以下、最佳為0.5μm以下。此處,說明對應比表面積之纖維直徑。首先,使用氮吸附之BET法來評估比表面積,對此比表面積,以圓柱模式,來推導關於比表面積與纖維直徑之下述式;該圓柱模式,係假定表面係由假想構成含有樹脂之薄片的纖維係完全未發生纖維間融著的理想狀態,且纖維素密度為d(g/cm3)、L/D(L:纖維長,D:纖維直徑(單位均為:μm))為無限大之作為圓柱的纖維所構成;比表面積=4/(dD)(m2/g)將以BET法所得之比表面積作為上式之比表面積而代入,作為纖維素密度代入d=1.50g/cm3,將換算作為纖維直徑D之數值,定義為對應比表面積之纖維直徑。此處,係以比表面積/細孔分布測定裝置(Beckman Coulter公司製),遵照同裝置之程式測定對試樣約0.2g於液體氮之沸點的氮氣吸附量後,算出比表面積藉此來進行以BET法之比表面積測定。
本發明之含有樹脂之薄片,藉由選擇上述構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑為上述範圍,可成為具備均勻的厚度分布者。上述構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑超過1.0μm時,纖維直徑太粗,因此由微細纖維所形成之微多孔構造的分布變大,亦即,成為散佈有大孔徑的孔者,因
此變得無法得到薄且均勻性優良的含有樹脂之薄片。
另一方面,上述構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑,必須為0.20μm以上、較佳為0.25μm以上。上述構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑未達0.20μm時,纖維直徑太細,因此孔徑變小,樹脂之含浸性會惡化。
又,再生纖維素微細纖維之最大纖維粗細度較佳為3μm以下、更佳為2.5μm以下、最佳為2μm以下。此處,最大纖維粗細度為3μm以下,意指於由以下條件所測定之纖維素不織布於電子顯微鏡(SEM)中,於影像上完全無法確認到超過3μm之纖維直徑的纖維。
此處,以相當1萬倍之倍率採取纖維素奈米纖維不織布之表面SEM影像,關於此影像中所包含之所有的交織纖維其纖維直徑均為3μm以下、且同樣地以同一條件之SEM影像來觀察纖維素微細纖維層表面之任意部分,對於合計100根以上之纖維同樣地無法確認到超過3μm之纖維直徑的纖維時,即定義為最大纖維直徑為3μm以下。惟,影像中可明確確認數根的微細纖維多束化而形成超過3μm之纖維直徑時,則不認為其係具備超過3μm之纖維直徑的纖維。藉由使再生纖維素微細纖維之最大纖維粗細度為3μm以下,欲製造本發明規定之薄膜的含有樹脂之薄片,可容易確保孔徑等之均勻性而較佳。
上述纖維素奈米纖維不織布,透氣抵抗度必須為1s/100ml以上、且40s/100ml以下之範圍,較佳為
6s/100ml以上、且35s/100ml以下之範圍內。此處,透氣抵抗度,意指基於JIS P 8117記載之格利試驗機(Gurley tester)法所測定之數值。將以微細纖維構成同時無針孔且均勻之薄片,製造為透氣抵抗度低於1s/100ml之薄片係困難的,因而,透氣抵抗度低於1s/100ml時,作為含有樹脂之薄片的功能變得無法展現。又,透氣抵抗度超過40s/100ml時,纖維素奈米纖維不織布之空孔率顯著降低、或孔徑變得過小,樹脂之含浸性變差,因此作為本發明之含有樹脂之薄片所用的纖維素奈米纖維不織布而言係不佳的。
上述纖維素奈米纖維不織布,可將再生纖維素微細纖維加工為薄片狀而得到,因加工上及功能上的限制,膜厚必須為8μm以上、且22μm以下。此處,膜厚之測定,係使用面接觸型之膜厚計,例如Mitutoyo製之膜厚計(Model ID-C112XB)等,由含有樹脂之薄片切下10.0cm×10.0cm之正方形片,對各種位置求得5點測定值之平均值,作為膜厚T(μm)。又,可由膜厚之測定中切下的10.0cm×10.0cm之正方形片的膜厚T(μm)、與其重量W(g),使用以下之式算出膜的單位面積之重量(目付)W0(g/m2)。
W0=100×W
上述纖維素奈米纖維不織布,較佳為膜厚
9μm以上、且20μm以下,最佳為9μm以上且18μm以下。藉由使膜厚為上述範圍,可成為低內部電阻等之電特性(功能面)或纏繞含有樹脂之薄片以組裝裝置時的操作性極為良好的含有樹脂之薄片。厚度較8μm更薄時,裝置組裝步驟中操作變難,變得不適當,亦產生伴隨經時劣化之短路產生、或損及長期安定性之問題。又,厚度大於22μm時,於緊密化等之觀點而言不佳。
上述纖維素奈米纖維不織布所用之纖維素微細纖維層的單位面積之重量,較佳為4g/m2以上、且13g/m2以下,更佳為5g/m2以上、且12g/m2以下。單位面積之重量為4g/m2以上時,對各種裝置之組裝步驟中操作性成為良好,由長期安定性之觀點亦佳。單位面積之重量為13g/m2以下時,可薄膜化,作為含有樹脂之薄片可得到緊密化等之期望效果。
上述纖維素奈米纖維不織布所用之含再生纖維素微細纖維70質量%以上的纖維素微細纖維層中,於再生纖維素微細纖維以外,亦可進一步含有未達30質量%之天然纖維素微細纖維。藉由使用天然纖維素微細纖維,因其構成單位之微纖絲為細,故較容易得到未達0.20μm之纖維直徑的微細纖維素纖維,又,因摻混有更細且纖維長/纖維直徑比率大的天然纖維素微細纖維,可增大纖維素奈米纖維不織布之強度。藉由含有其未達30質量%,可得到纖維素微細纖維層之強度增加,組裝裝置時的操作性極良好之纖維素奈米纖維不織布。更佳為未達
20質量%。
上述纖維素奈米纖維不織布所用之纖維素微細纖維層中的天然纖維素微細纖維,較佳為最大纖維粗細度為2μm以下。藉由使最大纖維直徑為2μm以下,可利用基於微細纖維所造成之微多孔構造的高均勻性,良好地實現薄膜化。
纖維素之最大纖維直徑不超過2μm之天然纖維素微細纖維,包含由闊葉樹或針葉樹所得到之木漿、精製棉絨或將來自各種植物種(竹、麻系纖維、蔗渣、洋麻、棉絨等)之精製漿粕等予以高度微細化處理者,此外亦包含如纖維素生產菌(細菌)所生產之細菌纖維素(BC)之未曾乾燥且為微細纖維之集合體的天然纖維素微細纖維。
又,上述纖維素奈米纖維不織布所用之含有70質量%以上的再生纖維素微細纖維之纖維素微細纖維層中,於再生纖維素微細纖維以外,亦可進一步包含未達30質量%之由纖維素以外之有機聚合物所成之微細纖維。更佳為25質量%以下。作為該有機聚合物,只要係可製造微細纖維之有機聚合物,則任意者均可使用,可列舉例如芳香族系或脂肪族系之聚酯、耐綸、聚丙烯腈、纖維素乙酸酯、聚胺基甲酸酯、聚乙烯、聚丙烯、聚酮、芳香族系聚醯胺、聚醯亞胺、絹、羊毛等之纖維素以外的天然有機聚合物,但不限定於此等。由該有機聚合物所成之微細纖維,可列舉藉由將有機纖維打漿、或以高壓均質機等微細化處理而經高度地纖維化或微細化的微細纖維、以各種
聚合物為原料藉由電紡絲法所得之微細纖維、以各種聚合物為原料藉由熔噴(meltblown)法所得之微細纖維等,但不限定於此等。此等之中,特別地以將全芳香族聚醯胺之聚芳醯胺纖維藉由高壓均質機予以微細化的微小纖維狀聚芳醯胺、TIARA(註冊商標)(Daicel化學工業(股)製),為平均纖維直徑0.2~0.3μm、平均纖維長500~600μm,聚芳醯胺纖維之高耐熱性、高化學安定性亦相輔相成地,可適合作為上述微細纖維使用。
接著,記載纖維素微細纖維之製造方法。纖維素纖維之微細化,較佳為再生纖維素纖維及天然纖維素纖維均經前處理步驟、打漿處理步驟及微細化步驟。特別地,將再生纖維素纖維微細化的情況時,前處理步驟能夠以用以去除油劑之依情況使用界面活性劑之水洗步驟來實施,於天然纖維素纖維之前處理步驟中,藉由於100~150℃之溫度的水中含浸下之熱壓釜處理、酵素處理等、或此等之組合,而使原料漿粕預先成為於之後的步驟中容易微細化的狀態係有效的。上述前處理步驟時,添加1質量%以下之濃度的無機酸(鹽酸、硫酸、磷酸、硼酸等)或有機酸(乙酸、檸檬酸等)來進行熱壓釜處理,依情況亦為有效。此等前處理,不僅減輕微細化處理之負荷,將構成纖維素纖維之微纖絲表面或間隙所存在的木質素或半纖維素等雜質成分排出至水相,其結果,亦有提高經微細化之纖維的α-
纖維素純度之效果,因此亦有非常有效於提高纖維素奈米纖維不織布之耐熱性的情況。
打漿處理步驟以後,再生纖維素纖維及天然纖維素纖維一起地,由以下之內容製造。打漿處理步驟中,以原料漿粕成為0.5質量%以上且4質量%以下、較佳為0.8質量%以上且3質量%以下、更佳為1.0質量%以上且2.5質量%以下之固體成分濃度的方式分散於水中,以如打漿機或圓盤式精磨機(雙圓盤式精磨機)之打漿裝置來高度促進纖維化。使用圓盤式精磨機時,若將圓盤間之空隙極力設定為窄(例如0.1mm以下)來進行處理時,會進行極高度的打漿(纖維化),因此可緩和高壓均質機等之微細化處理的條件,而有有效的情況。
較佳之打漿處理之程度,係規定如下。根據本發明者等人之探討,隨著進行打漿處理,CSF值(表示纖維素之打漿程度。由以JIS P 8121所定義之漿粕的加拿大標準游離度試驗方法來評估)會經時地減少,一旦成為接近零後,進一步持續打漿處理時確認到有再度增大之傾向,為了配製微細纖維素纖維,已知作為前處理,較佳為於CSF值一旦成為接近零後,進一步持續打漿處理,打漿至CSF值增加之狀態為止。本說明書中,將自未打漿至CSF值減少之過程的CSF值標記為***ml↓、將成為零後於增大傾向之CSF值標記為***ml↑。於該打漿處理中,不管再生纖維素、天然纖維素,打漿步驟之CSF值較佳為打漿度至少比零高、更佳為打漿度比CSF30ml↑
高。配製為如此之打漿度的水分散體中,纖維化高度進行,特別是關於再生纖維素,藉由組合該打漿處理與後述之進一步的微細化處理,可得到對應比表面積之纖維直徑為0.20μm以上且0.70μm以下之微細纖維。CSF值具備至少零或其後增大之***ml↑之值的經高度打漿之水分散體,係有均勻性增大,可減輕其後之於高壓均質機等之微細化處理的堵塞之製造效率上的優點。進一步地,製造天然纖維素之微細纖維時,藉由組合上述打漿步驟與進一步的微細化處理,作為微細纖維之漿體,就纖維素奈米纖維不織布之強度補強的觀點而言,較佳為較CSF50ml↑更進一步被打漿,更佳為CSF100ml↑以上。
又,製造再生纖維素之微細纖維時,藉由組合上述打漿步驟與進一步的微細化處理,作為微細纖維之漿體,就纖維素奈米纖維不織布之強度補強的觀點而言,較佳為較CSF20ml↑更進一步被打漿,更佳為CSF50ml↑以上。
纖維素微細纖維之製造時,較佳為上述打漿步驟之後,以高壓均質機、超高壓均質機、研磨器等施以微細化處理。此時之水分散體中之固體成分濃度,根據上述之打漿處理,為0.5質量%以上且4質量%以下、較佳為0.8質量%以上且3質量%以下、更佳為1.0質量%以上且2.5質量%以下。若為此範圍之固體成分濃度,可不產生堵塞,而且達成有效率的微細化處理。
所使用之高壓均質機,可列舉例如Niro Soavi
公司(義大利)之NS型高壓均質機、(股)SMT之Lannier-type(R模式)壓力式均質機、三和機械(股)之高壓式均質機等,只要係以與此等裝置大致相同之機構來實施微細化之裝置,則此等以外之裝置亦可。就超高壓均質機而言,意指Mizuho工業(股)之Microfluidizer、吉田機械興業(股)Nanomizer、(股)SUGINO MACHINE之Ultimizer等之高壓碰撞型的微細化處理機,只要係以與此等裝置大致相同之機構來實施微細化之裝置,則此等以外之裝置亦可。研磨器型微細化裝置,可列舉以(股)栗田機械製作所之Pure Fine Mill、增幸產業(股)之Super masscolloider為代表之石臼式磨碎型,但只要係以與此等裝置大致相同之機構來實施微細化之裝置,則此等以外之裝置亦可。
纖維素微細纖維之纖維直徑,可藉由高壓均質機等之微細化處理的條件(裝置之選定或操作壓力及通過次數)或該微細化處理前之前處理的條件(例如熱壓釜處理、酵素處理、打漿處理等)來控制。
進一步地,作為本發明中可使用之纖維素微細纖維,亦可使用施加表面之化學處理的纖維素系之微細纖維、及6位之羥基藉由TEMPO氧化觸媒被氧化,變成羧基(包含酸型、鹽型)的纖維素系之微細纖維。前者的情況時,可依照目的,藉由施以各種表面化學處理,適當配製例如纖維素微細纖維之表面所存在之一部分或大部分的羥基被酯化為包含乙酸酯、硝酸酯、硫酸酯者;包含以甲基醚為代表之烷基醚、以羧基甲基醚為代表之羧基醚、氰
基乙基醚之經醚化者來使用。又,後者,亦即藉由TEMPO氧化觸媒使6位之羥基被氧化的纖維素微細纖維之配製時,並不一定必須使用如高壓均質機之需要高能源的微細化裝置,即可得到微細纖維素之分散體。例如,如文獻(A.Isogai et al.,Biomacromolecules,7,1687-1691(2006))所記載般,於天然纖維素之水分散體中使如2,2,6,6-四甲基哌啶基氧自由基之稱為TEMPO的觸媒與鹵化烷基共存,對其添加如次氯酸之氧化劑,進行一定時間之反應,藉此,於水洗等精製處理後施以通常之混合器處理,藉此可極為容易地得到微細纖維素纖維之分散體。
再者,本發明中,係有以本發明規定之量混合2種以上之上述原料相異的再生纖維素或天然纖維素系之微細纖維或纖維化度相異的天然纖維素之微細纖維、表面經化學處理之天然纖維素之微細纖維等,來形成纖維素微細纖維層亦為有效的情況。
上述纖維素奈米纖維不織布所用之纖維素微細纖維層,係有為了進行強度補強而含有反應性交聯劑10質量%以下亦為有效的情況。反應性交聯劑,係指來自多官能性異氰酸酯之反應體者,且係指藉由多官能性異氰酸酯化合物與含有活性氫之化合物之加成反應所生成之樹脂。藉由含有10質量%以下之反應性交聯劑,纖維素微細纖維層之強度會增加,成為組裝裝置時的操作性極為良好之纖維素奈米纖維不織布。反應性交聯劑之含量,更佳為6質量%以下。
作為形成上述纖維素奈米纖維不織布所用之纖維素微細纖維層中之反應性交聯劑的多官能性異氰酸酯化合物,可列舉例如芳香族多官能性異氰酸酯、芳香脂肪族多官能性異氰酸酯、脂環族多官能性異氰酸酯、脂肪族多官能性異氰酸酯等。由黃變性少之觀點而言,較佳為脂環族多官能性異氰酸酯及脂肪族多官能性異氰酸酯。又,多官能性異氰酸酯化合物亦可含有1種或2種以上。
芳香族多官能性異氰酸酯,可列舉例如2,4-甲苯二異氰酸酯、2,6-甲苯二異氰酸酯及其混合物(TDI)、二苯基甲烷-4,4’-二異氰酸酯(MDI)、萘-1,5-二異氰酸酯、3,3-二甲基-4,4-伸聯苯基二異氰酸酯、粗製TDI、聚亞甲基聚苯基二異氰酸酯、粗製MDI、伸苯基二異氰酸酯、伸二甲苯基二異氰酸酯等之芳香族多官能性異氰酸酯。
脂環族多官能性異氰酸酯,可列舉例如1,3-環戊烷二異氰酸酯、1,3-環戊烯二異氰酸酯、環己烷二異氰酸酯等之脂環族多官能性異氰酸酯。
脂肪族多官能性異氰酸酯,可列舉例如三亞甲基二異氰酸酯、1,2-伸丙基二異氰酸酯、伸丁基二異氰酸酯、五亞甲基二異氰酸酯、六亞甲基二異氰酸酯等之脂肪族多官能性異氰酸酯等。
含有活性氫之化合物,可列舉例如包含1元醇、多元醇及酚類之含有羥基之化合物、含有胺基之化合物、含有硫醇基之化合物、含有羧基之化合物等。又,亦包含於空氣中或反應場中存在的水或二氧化碳等。含有活
性氫之化合物,亦可含有1種或2種以上。
1元醇可列舉例如碳數1~20之烷醇(甲醇、乙醇、丁醇、辛醇、癸醇、十二烷基醇、肉豆蔻醇、鯨蠟醇及硬脂醇等)、碳數2~20之烯醇(油醇及亞麻醇等)及碳數7~20之芳香脂肪族醇(苄基醇及萘基乙醇等)等。
多元醇可列舉例如碳數2~20之2元醇[脂肪族二醇(乙二醇、丙二醇、1,3-或1,4-丁二醇、1,6-己二醇、新戊二醇及1,10-癸二醇等)、脂環式二醇(環己二醇及環己二甲醇等)及芳香脂肪族二醇{1,4-雙(羥基乙基)苯等}等]、碳數3~20之3元醇[脂肪族三醇(甘油及三羥甲基丙烷等)等]及碳數5~20之4~8元醇[脂肪族多元醇(季戊四醇、山梨醇、甘露醇、山梨醇酐、二甘油及二季戊四醇等)及糖類(蔗糖、葡萄糖、甘露糖、果糖、甲基糖苷及其衍生物)]等。
酚類可列舉例如1元酚(酚、1-羥基萘、蒽酚及1-羥基芘等)及多元酚[根皮三酚、五倍子酚、兒茶酚、氫醌、雙酚A、雙酚F、雙酚S、1,3,6,8-四羥基萘、1,4,5,8-四羥基蒽、酚與甲醛之縮合物(酚醛清漆)及美國專利3265641號說明書記載之多酚等]等。
含有胺基之化合物,可列舉例如碳數1~20之單氫胩[烷基胺(丁基胺等)、苄基胺及苯胺等]、碳數2~20之脂肪族多胺(乙二胺、六亞甲二胺及二乙三胺等)、碳數6~20之脂環式多胺(二胺基環己烷、二環己基甲二胺及異佛酮二胺等)、碳數2~20之芳香族多胺(苯二胺、甲苯二
胺及二苯基甲二胺等)、碳數2~20之雜環式多胺(哌嗪及N-胺基乙基哌嗪等)、烷醇胺(單乙醇胺、二乙醇胺及三乙醇胺等)、藉由二羧酸與過剩之多胺的縮合所得到之聚醯胺多胺、聚醚多胺、肼(肼及單烷基肼等)、二醯肼(琥珀酸二醯肼及對苯二甲酸二醯肼等)、胍(丁基胍及1-氰基胍等)及二氰二胺等。
含有硫醇基之化合物,可列舉例如碳數1~20之1價硫醇化合物(乙基硫醇等之烷基硫醇、苯基硫醇及苄基硫醇)及多價之硫醇化合物(伸乙基二硫醇及1,6-己烷二硫醇等)等。
含有羧基之化合物,可列舉1元之羧酸化合物(乙酸等之烷基羧酸、安息香酸等之芳香族羧酸)及多元之羧酸化合物(草酸或丙二酸等之烷基二羧酸及對苯二甲酸等之芳香族二羧酸等)等。
上述纖維素奈米纖維不織布,除了含有70質量%以上之再生纖維素微細纖維的纖維素微細纖維層以外,亦可含有單位面積之重量為3g/m2以上且15g/m2以下之不織布或紙的基材層,作為3層以下之複數層構造的一層。藉由含有單位面積之重量3g/m2以上且15g/m2以下之不織布或紙的基材層,即使薄膜之纖維素微細纖維層本身的強度不足,基材層為了補足強度,亦可在保持作為纖維素奈米纖維不織布之功能(作為含有樹脂之薄片之低內部電阻等)的同時,成為組裝裝置時之操作性極為良好的含有樹脂之薄片。
上述纖維素奈米纖維不織布所用之基材層,例如係由選自6-耐綸或6,6-耐綸等之聚醯胺纖維;聚對苯二甲酸乙二酯或聚對苯二甲酸丙二酯、聚對苯二甲酸丁二酯等之聚酯纖維;聚乙烯纖維、聚丙烯纖維、木漿或棉絨等之天然纖維素纖維;黏液縲縈或銅氨縲縈等之再生纖維素纖維及纖維素纖維或天絲纖維等之精製纖維素纖維之群的至少1種所成之不織布或紙。由電解液或複合化樹脂之含浸性的觀點而言,較佳為纖維素。又,上述基材層,由本發明中規定之膜厚範圍而言,可適合使用為熔噴(meltblown)或電紡絲系之不織布,進一步地,更佳為使用藉由壓延處理而薄膜化之基材。
又,上述纖維素奈米纖維不織布,依用途不同,作為含有金屬離子量之一個尺度的氯離子含有濃度較佳為40ppm以下。其係因氯離子含有濃度為40ppm以下時,Na、Ca等之金屬離子類亦變的含有相對低的濃度,其結果,例如可抑制如印刷配線板之裝置的電特性的阻礙之故。更佳為30ppm以下、最佳為25ppm以下時,會更適宜地展現耐熱性。氯離子濃度之評估可由離子層析法來進行。
作為形成固著劑2之固著劑組成物,只要係可附著於纖維素奈米纖維不織布11中之纖維1,使纖維1彼此固著者即可,可為僅固著纖維彼此互相接合的接點部者,亦
可為被覆纖維1之全體而固著者。固著劑組成物之使用量,只要係可使纖維1彼此固著,對耐彎曲性不造成不良影響之程度的量即可,於將纖維1藉由固著劑2固著之集合體中,以有機溶劑以外的固體成分計,纖維1與固著劑2之體積比以99:1~50:50之範圍、特別以99:1~60:40之範圍較佳。纖維1與固著劑2之體積比若於此範圍,纖維1彼此係變得藉由固著劑充分地固著而得到所期望之高強度,而且藉由其後之樹脂3的含浸可確保良好的耐彎曲性而較佳。特別地,固著劑2之使用量,較佳為於固著劑2之施用前後,纖維素奈米纖維不織布11之膜厚實質上不變化之程度的量。此處,膜厚實質上不變化,意指纖維素奈米纖維不織布11藉由固著劑組成物之溶劑成分等而膨潤,表觀上增大厚度之情況為不包含於膜厚的變化者。又,固著劑組成物,於附著於纖維時較佳為液體,亦可為藉由改變溫度或壓力而可成為液體來使用者。特別地,固著劑組成物於25℃以E型黏度計之轉子旋轉數5rpm所測定之黏度係以1Pa.s以下、例如1~0.0001Pa.s為佳,藉此,可使固著劑組成物含浸至纖維1之集合體的內部,可使纖維彼此更為確實地固著。
又,固著劑組成物係使用藉由熱或光而硬化者。此處所稱之硬化,意指藉由熱或光之能源由液體化學變化為固體。作為固著劑組成物,依其用途可使用慣用之成分,可1種單獨、或組合2種以上使用。固著劑組成物所用之慣用成分,可列舉例如熱硬化性樹脂、硬化劑、熱
硬化觸媒、光硬化性樹脂、光聚合起始劑、光酸產生劑、光鹼產生劑、有機溶劑等,具體而言,可使用以下所示者。
熱硬化性樹脂,只要係藉由加熱而硬化,顯示電絕緣性之樹脂即可,可列舉例如雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、雙酚E型環氧樹脂、雙酚M型環氧樹脂、雙酚P型環氧樹脂、雙酚Z型環氧樹脂等之雙酚型環氧樹脂;雙酚A酚醛清漆型環氧樹脂、酚酚醛清漆型環氧樹脂、甲酚酚醛清漆環氧樹脂等之酚醛清漆型環氧樹脂;聯苯基型環氧樹脂、聯苯基芳烷基型環氧樹脂、芳基伸烷基型環氧樹脂、四苯酚基乙烷型環氧樹脂、萘型環氧樹脂、蒽型環氧樹脂、苯氧基型環氧樹脂、二環戊二烯型環氧樹脂、降莰烯型環氧樹脂、金剛烷型環氧樹脂、茀型環氧樹脂、甲基丙烯酸縮水甘油酯共聚合系環氧樹脂、環己基馬來醯亞胺與甲基丙烯酸縮水甘油酯之共聚合環氧樹脂、環氧基改質之聚丁二烯橡膠衍生物、CTBN改質環氧樹脂、三羥甲基丙烷聚縮水甘油醚、苯基-1,3-二縮水甘油醚、聯苯基-4,4’-二縮水甘油醚、1,6-己二醇二縮水甘油醚、乙二醇或丙二醇之二縮水甘油醚、山梨醇聚縮水甘油醚、參(2,3-環氧基丙基)三聚異氰酸酯、三縮水甘油基參(2-羥基乙基)三聚異氰酸酯;酚酚醛清漆樹脂、甲酚酚醛清漆樹脂、雙酚A酚醛清漆樹脂等之酚醛清
漆型酚樹脂;未改質之甲階酚醛酚樹脂;經桐油、亞麻仁油、胡桃油等改質之油改質甲階酚醛酚樹脂等之甲階酚醛型酚樹脂等之酚樹脂;苯氧基樹脂、尿素(脲)樹脂、三聚氰胺樹脂等之含有三嗪環之樹脂;不飽和聚酯樹脂、雙馬來醯亞胺樹脂、鄰苯二甲酸二烯丙酯樹脂、聚矽氧樹脂、具有苯并噁嗪環之樹脂、降莰烯系樹脂、氰酸酯樹脂、異氰酸酯樹脂、胺基甲酸酯樹脂、苯并環丁烯樹脂、馬來醯亞胺樹脂、雙馬來醯亞胺三嗪樹脂、聚甲亞胺樹脂、聚醯亞胺樹脂等。此等之中特別以環氧樹脂或聚醯亞胺樹脂,由於作為絕緣層之信賴性優良,故較佳。
作為環氧樹脂,可使用1分子中具有至少2個環氧基之公知慣用的多官能環氧樹脂。環氧樹脂可為液狀、亦可為固體或半固體。其中尤特佳為雙酚A型環氧樹脂、萘型環氧樹脂、酚酚醛清漆型環氧樹脂或該等之混合物。此等之環氧樹脂,可1種單獨使用、亦可組合2種以上使用。環氧樹脂具體而言可列舉例如三菱化學(股)製之jER828等,但不限定於此。
使用環氧樹脂形成硬化物的情況時,於環氧樹脂以外,較佳為含有硬化劑。作為硬化劑,可使用2-乙基-4-甲基咪唑(2E4MZ)、2-苯基咪唑(2PZ)、2-苯基-4-甲基-5-羥基甲基咪唑(2P4MHZ)等之咪唑系硬化劑;二乙三胺、三乙四胺、四乙五胺、五乙六胺、間伸二甲苯二胺、異佛酮二胺、降莰烯二胺、1,3-雙胺基甲基環己烷、N-胺基乙基哌嗪等之胺系硬化劑;聚醯胺、乙烯基酚、芳烷基
型酚樹脂、酚苯基芳烷基樹脂、酚聯苯基芳烷基樹脂等之酚系硬化劑;鄰苯二甲酸酐、四氫鄰苯二甲酸、六氫鄰苯二甲酸、甲基四氫鄰苯二甲酸、甲基六氫鄰苯二甲酸、甲基降莰烯二酸酐、十二烷基琥珀酸酐、氯橋酸酐、苯均四酸酐、二苯甲酮四羧酸酐、乙二醇雙(偏苯三甲酸酐)、甲基環己烯四羧酸酐等之酸酐系硬化劑;氰酸酯樹脂、活性酯樹脂、脂肪族或芳香族之一級或二級胺、聚醯胺樹脂、多巰基化合物等之公知之硬化劑。硬化劑之摻合量,相對於上述環氧樹脂100質量份而言,較佳為0.1~150質量份、更佳為0.5~100質量份。藉由使硬化劑之摻合量為0.1質量份以上,可充分地硬化樹脂組成物,藉由為150質量份以下,可有效率地得到對應於摻合量的效果。
又,熱硬化觸媒可列舉例如咪唑、2-甲基咪唑、2-乙基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、4-苯基咪唑、1-氰基乙基-2-苯基咪唑、1-(2-氰基乙基)-2-乙基-4-甲基咪唑等之咪唑衍生物;二氰二胺、苄基二甲基胺、4-(二甲基胺基)-N,N-二甲基苄基胺、4-甲氧基-N,N-二甲基苄基胺、4-甲基-N,N-二甲基苄基胺等之胺化合物;己二酸二醯肼、癸二酸二醯肼等之肼化合物;三苯基膦等之磷化合物等。又,亦可使用胍胺、甲基胍胺(acetoguanamine)、苯并胍胺、三聚氰胺、2,4-二胺基-6-甲基丙烯醯氧基乙基-S-三嗪、2-乙烯基-2,4-二胺基-S-三嗪、2-乙烯基-4,6-二胺基-S-三嗪/三聚異氰酸加成物、2,4-二胺基-6-甲基丙烯醯氧基乙基-S-三嗪/三聚異氰酸加
成物等之S-三嗪衍生物。
聚醯亞胺樹脂,可列舉藉由一般所知之芳香族多元羧酸酐或其衍生物與芳香族二胺之合成反應,經由聚醯胺酸(聚醯亞胺前驅物)所得者、與已於有機溶劑中溶解有聚醯胺酸組成物之狀態的作為所謂聚醯亞胺清漆而上市者。
芳香族多元羧酸酐之具體例子,可列舉例如苯均四酸二酐、3,3’,4,4’-二苯甲酮四羧酸二酐、2,2’,3,3’-二苯甲酮四羧酸二酐、3,3’,4,4’-聯苯基四羧酸二酐、2,2’,3,3’-聯苯基四羧酸二酐、2,2-雙(2,3-二羧基苯基)丙烷二酐、雙(3,4-二羧基苯基)醚二酐、雙(3,4-二羧基苯基)碸二酐、1,1-雙(2,3-二羧基苯基)乙烷二酐、雙(2,3-二羧基苯基)甲烷二酐、雙(3,4-二羧基苯基)甲烷二酐、2,2-雙(3,4-二羧基苯基)-1,1,1,3,3,3-六氟丙烷二酐、2,3,6,7-萘四羧酸二酐、1,4,5,8-萘四羧酸二酐、1,2,5,6-萘四羧酸二酐、1,2,3,4-苯四羧酸二酐、3,4,9,10-苝四羧酸二酐、2,3,6,7-蒽四羧酸二酐、1,2,7,8-菲四羧酸二酐等。此等可單獨或混合2種以上使用。此等之中尤特佳為使用苯均四酸二酐作為至少成分之一。
與芳香族多元羧酸酐等之多元羧酸反應的芳香族二胺之具體例子,可列舉例如m-苯二胺、o-苯二胺、p-苯二胺、m-胺基苄基胺、p-胺基苄基胺、4,4’-二胺基二苯基醚、3,3’-二胺基二苯基醚、3,4’-二胺基二苯基醚、雙(3-胺基苯基)硫醚、(3-胺基苯基)(4-胺基苯基)硫
醚、雙(4-胺基苯基)硫醚、雙(3-胺基苯基)硫醚、(3-胺基苯基)(4-胺基苯基)亞碸、雙(3-胺基苯基)碸、(3-胺基苯基)(4-胺基苯基)碸、雙(4-胺基苯基)碸、3,3’-二胺基二苯甲酮、3,4’-二胺基二苯甲酮、4,4’-二胺基二苯甲酮、3,3’-二胺基二苯基甲烷、3,4’-二胺基二苯基甲烷、4,4’-二胺基二苯基甲烷、雙〔4-(3-胺基苯氧基)苯基〕甲烷、雙〔4-(4-胺基苯氧基)苯基〕甲烷、1,1-雙〔4-(3-胺基苯氧基)苯基〕乙烷、1,1-雙〔4-(4-胺基苯氧基)苯基〕-乙烷、1,2-雙〔4-(3-胺基苯氧基)苯基〕乙烷、1,2-雙〔4-(4-胺基苯氧基)苯基〕乙烷、2,2-雙〔4-(3-胺基苯氧基)苯基〕丙烷、2,2-雙〔4-(4-胺基苯氧基)苯基〕丙烷、2,2-雙〔4-(3-胺基苯氧基)苯基〕丁烷、2,2-雙〔3-(3-胺基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、2,2-雙〔4-(4-胺基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、1,3-雙(3-胺基苯氧基)苯、1,3-雙(4-胺基苯氧基)苯、1,4-雙(3-胺基苯氧基)苯、1,4-雙(4-胺基苯氧基)苯、4,4’-雙(3-胺基苯氧基)聯苯基、4,4’-雙(4-胺基苯氧基)聯苯基、雙〔4-(3-胺基苯氧基)苯基〕酮、雙〔4-(4-胺基苯氧基)苯基〕酮、雙〔4-(3-胺基苯氧基)苯基〕硫醚、雙〔4-(4-胺基苯氧基)苯基〕硫醚、雙〔4-(3-胺基苯氧基)苯基〕亞碸、雙〔4-(4-胺基苯氧基)苯基〕亞碸、雙〔4-(3-胺基苯氧基)苯基〕碸、雙〔4-(4-胺基苯氧基)苯基〕碸、雙〔4-(3-胺基苯氧基)苯基〕醚、雙〔4-(4-胺基苯氧基)苯基〕醚、1,4-雙〔4-(3-胺基苯氧基)苯甲醯基〕苯、1,3-雙〔4-(3-胺基苯氧基)苯甲醯基〕
苯、4,4’-雙〔3-(4-胺基苯氧基)苯甲醯基〕二苯基醚、4,4’-雙〔3-(3-胺基苯氧基)苯甲醯基〕二苯基醚、4,4’-雙〔4-(4-胺基-α,α-二甲基苄基)苯氧基〕二苯甲酮、4,4’-雙〔4-(4-胺基-α,α-二甲基苄基)苯氧基〕二苯基碸、雙〔4-{4-(4-胺基苯氧基)苯氧基}苯基〕碸、1,4-雙〔4-(4-胺基苯氧基)苯氧基〕-α,α-二甲基苄基〕苯、1,3-雙〔4-(4-胺基苯氧基)-α,α-二甲基苄基〕苯等。此等係單獨或混合2種以上使用。此等之中,尤特佳為使用4,4’-二胺基二苯基醚作為至少成分之一。
聚醯亞胺清漆可列舉新日本理化(股)製之Rikacoat SN20、Rikacoat PN20、Rikacoat EN20、東麗(股)製之Torayneece、宇部興產(股)製U-Varnish、JSR(股)製之OPTOMER、日產化學(股)製之SE812、住友Bakelite(股)製之CRC8000。
藉由將合成反應所得或上市之聚醯胺酸溶液以加熱等予以處理,來進行由聚醯胺酸環化為聚醯亞胺(醯亞胺化)。聚醯胺酸可藉由僅以加熱進行的法、或化學方法來醯亞胺化。僅以加熱進行的方法時,係藉由將聚醯胺酸例如於200~350℃進行加熱處理來醯亞胺化。又,化學方法係為了迅速進行醯亞胺化,而利用鹼性觸媒,同時將聚醯胺酸加熱處理,以完全地醯亞胺化之方法。上述鹼性觸媒並無特殊限定,可使用以往公知之鹼性觸媒,可列舉例如吡啶、二氮雜雙環十一烯(DBU)、二氮雜雙環壬烯(DBN)、各種3級胺等。此等之鹼性觸媒可單獨使用、亦
可合併使用二種以上。
光硬化性樹脂,只要係藉由活性能量線之照射會硬化而顯示電絕緣性之樹脂即可,特佳為使用分子中具有1個以上之乙烯性不飽和鍵的化合物。具有乙烯性不飽和鍵的化合物,可使用公知慣用之光聚合性寡聚物及光聚合性乙烯基單體等。
光聚合性寡聚物,可列舉不飽和聚酯系寡聚物、(甲基)丙烯酸酯系寡聚物等。(甲基)丙烯酸酯系寡聚物,可列舉酚酚醛清漆(甲基)丙烯酸環氧酯;甲酚酚醛清漆(甲基)丙烯酸環氧酯、雙酚型(甲基)丙烯酸環氧酯等之(甲基)丙烯酸環氧酯;胺基甲酸酯(甲基)丙烯酸酯、環氧基胺基甲酸酯(甲基)丙烯酸酯、聚酯(甲基)丙烯酸酯、聚醚(甲基)丙烯酸酯、聚丁二烯改質(甲基)丙烯酸酯等。再者,本說明書中,(甲基)丙烯酸酯係指總稱丙烯酸酯、甲基丙烯酸酯及該等之混合物的用語,其他類似表述亦相同。
光聚合性乙烯基單體,可列舉公知慣用者,例如苯乙烯、氯苯乙烯、α-甲基苯乙烯等之苯乙烯衍生物;乙酸乙烯酯、丁酸乙烯酯或安息香酸乙烯酯等之乙烯酯類;乙烯基異丁基醚、乙烯基-n-丁基醚、乙烯基-t-丁基醚、乙烯基-n-戊基醚、乙烯基異戊基醚、乙烯基-n-十八烷基醚、乙烯基環己基醚、乙二醇單丁基乙烯基醚、三
乙二醇單甲基乙烯基醚等之乙烯基醚類;丙烯醯胺、甲基丙烯醯胺、N-羥基甲基丙烯醯胺、N-羥基甲基甲基丙烯醯胺、N-甲氧基甲基丙烯醯胺、N-乙氧基甲基丙烯醯胺、N-丁氧基甲基丙烯醯胺等之(甲基)丙烯醯胺類;三烯丙基三聚異氰酸酯、鄰苯二甲酸二烯丙酯、異鄰苯二甲酸二烯丙酯等之烯丙基化合物;(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸四氫呋喃甲酯、(甲基)丙烯酸異莰酯、(甲基)丙烯酸苯酯、(甲基)丙烯酸苯氧基乙酯等之(甲基)丙烯酸之酯類;(甲基)丙烯酸羥基乙酯、(甲基)丙烯酸羥基丙酯、季戊四醇三(甲基)丙烯酸酯等之(甲基)丙烯酸羥基烷酯類;(甲基)丙烯酸甲氧基乙酯、(甲基)丙烯酸乙氧基乙酯等之烷氧基烷二醇單(甲基)丙烯酸酯類;乙二醇二(甲基)丙烯酸酯、丁二醇二(甲基)丙烯酸酯類、新戊二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯等之伸烷基多元醇聚(甲基)丙烯酸酯;二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、乙氧基化三羥甲基丙烷三丙烯酸酯、丙氧基化三羥甲基丙烷三(甲基)丙烯酸酯等之聚氧烷二醇聚(甲基)丙烯酸酯類;羥基三甲基乙酸新戊二醇酯二(甲基)丙烯酸酯等之聚(甲基)丙烯酸酯類;參[(甲基)丙烯醯氧基乙基]三聚異氰酸酯等之三聚異氰酸酯型聚(甲基)丙烯酸酯類等。
光硬化性樹脂,亦可適合使用脂環環氧化合
物、氧雜環丁烷化合物及乙烯基醚化合物等。其中,脂環環氧化合物,可列舉3,4,3’,4’-二環氧基雙環己基、2,2-雙(3,4-環氧基環己基)丙烷、2,2-雙(3,4-環氧基環己基)-1,3-六氟丙烷、雙(3,4-環氧基環己基)甲烷、1-[1,1-雙(3,4-環氧基環己基)]乙基苯、雙(3,4-環氧基環己基)己二酸酯、3,4-環氧基環己基甲基(3,4-環氧基)環己烷羧酸酯、(3,4-環氧基-6-甲基環己基)甲基-3’,4’-環氧基-6-甲基環己烷羧酸酯、伸乙基-1,2-雙(3,4-環氧基環己烷羧酸)酯、環氧環己烷、3,4-環氧基環己基甲基醇、3,4-環氧基環己基乙基三甲氧基矽烷等之具有環氧基的脂環環氧化合物等。
氧雜環丁烷化合物,可列舉雙[(3-甲基-3-氧雜環丁烷基甲氧基)甲基]醚、雙[(3-乙基-3-氧雜環丁烷基甲氧基)甲基]醚、1,4-雙[(3-甲基-3-氧雜環丁烷基甲氧基)甲基]苯、1,4-雙[(3-乙基-3-氧雜環丁烷基甲氧基)甲基]苯、丙烯酸(3-甲基-3-氧雜環丁烷基)甲酯、丙烯酸(3-乙基-3-氧雜環丁烷基)甲酯、甲基丙烯酸(3-甲基-3-氧雜環丁烷基)甲酯、甲基丙烯酸(3-乙基-3-氧雜環丁烷基)甲酯或該等之寡聚物或共聚物等之多官能氧雜環丁烷類,此外可列舉氧雜環丁烷醇與酚醛清漆樹脂、聚(p-羥基苯乙烯)、cardo型雙酚類、杯芳烴類、間苯二酚杯芳烴(calixresorcinarene)類、或倍半矽氧烷等之具有羥基之樹脂的醚化物;具有氧雜環丁烷環之不飽和單體與(甲基)丙烯酸烷酯之共聚物等之氧雜環丁烷化合物。
乙烯基醚化合物,可列舉異葡萄糖醇二乙烯
基醚、氧雜降莰烯二乙烯基醚等之環狀醚型乙烯基醚(環氧乙烷環、氧雜環丁烷環、氧雜環戊烷環等之具有環狀醚基之乙烯基醚);苯基乙烯基醚等之芳基乙烯基醚;n-丁基乙烯基醚、辛基乙烯基醚等之烷基乙烯基醚;環己基乙烯基醚等之環烷基乙烯基醚;氫醌二乙烯基醚、1,4-丁二醇二乙烯基醚、環己烷二乙烯基醚、環己烷二甲醇二乙烯基醚等之多官能乙烯基醚;於α及/或β位具有烷基、烯丙基等之取代基的乙烯基醚化合物等。市售品可列舉例如丸善石油化學(股)製之2-羥基乙基乙烯基醚(HEVE)、二乙二醇單乙烯基醚(DEGV)、2-羥基丁基乙烯基醚(HBVE)、三乙二醇二乙烯基醚等。
使用光硬化性樹脂時,於上述之光硬化性樹脂以外,可使用光聚合起始劑、光酸產生劑、光鹼產生劑等,可使用此等之中1種單獨、或組合2種以上使用。
光聚合起始劑可列舉例如苯偶姻、苯偶姻甲基醚、苯偶姻乙基醚、苯偶姻異丙基醚等之苯偶姻與苯偶姻烷基醚類;苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2,2-二乙氧基-2-苯基苯乙酮、2,2-二乙氧基-2-苯基苯乙酮、1,1-二氯苯乙酮等之苯乙酮類;2-甲基-1-[4-(甲硫基)苯基]-2-嗎啉基丙烷-1-酮、2-苄基-2-二甲基胺基-1-(4-嗎啉基苯基)-丁酮-1、2-(二甲基胺基)-2-[(4-甲基苯基)甲基]-1-[4-(4-嗎啉基)苯基]-1-丁酮等之胺基烷基苯酮類;2-甲基蒽醌、2-乙基蒽醌、2-第三丁基蒽醌、1-氯蒽醌等之蒽醌類;2,4-二甲基噻噸酮、2,4-二乙基噻噸酮、2-氯噻噸
酮、2,4-二異丙基噻噸酮等之噻噸酮類;苯乙酮二甲基縮酮、苄基二甲基縮酮等之縮酮類;二苯甲酮等之二苯甲酮類;或黃嘌呤酮類;(2,6-二甲氧基苯甲醯基)-2,4,4-戊基膦氧化物、雙(2,4,6-三甲基苯甲醯基)-苯基膦氧化物、2,4,6-三甲基苯甲醯基二苯基膦氧化物、乙基-2,4,6-三甲基苯甲醯基苯基次膦酸酯等之膦氧化物類;各種過氧化物類、二茂鈦系起始劑、肟酯系起始劑等。此等亦可與如N,N-二甲基胺基安息香酸乙酯、N,N-二甲基胺基安息香酸異戊酯、安息香酸戊基-4-二甲基胺酯、三乙基胺、三乙醇胺等之三級胺類之光增感劑等合併使用。此等光聚合起始劑可單獨、或組合2種以上使用。
光酸產生劑可列舉例如重氮鎓鹽、錪鹽、溴鎓鹽、氯鎓鹽、鋶鹽、硒鎓(selenonium)鹽、吡喃鎓(pyrylium)鹽、噻喃鎓(thiapyrylium)鹽、吡啶鎓鹽等之鎓鹽;參(三鹵甲基)-s-三嗪(例如2,4,6-參(三氯甲基)-s-三嗪)、2-[2-(5-甲基呋喃-2-基)乙烯基]-4,6-雙(三氯甲基)-s-三嗪、2-[2-(呋喃-2-基)乙烯基]-4,6-雙(三氯甲基)-s-三嗪、2-(4-甲氧基苯基)-4,6-雙(三氯甲基)-s-三嗪、2-甲基-4,6-雙(三氯甲基)-s-三嗪等之鹵化化合物;磺酸之2-硝基苄酯;亞胺基磺酸鹽;1-側氧-2-重氮萘醌-4-磺酸鹽衍生物;N-羥基醯亞胺=磺酸鹽;三(甲烷磺醯氧基)苯衍生物;雙磺醯基重氮甲烷類;磺醯基羰基烷類;磺醯基羰基重氮甲烷類;二碸化合物;鐵芳香烴錯合物等。此等光酸產生劑可單獨、或組合2種以上使用。
光鹼產生劑,為藉由紫外線或可見光等之光照射而分子構造會變化、或分子會開裂,藉此生成可發揮作為聚合反應之觸媒的功能之1種以上的鹼性物質之化合物。鹼性物質可列舉例如2級胺、3級胺。如此之光鹼產生劑,可列舉例如α-胺基苯乙酮化合物、或肟酯化合物、具有醯氧基亞胺基、N-甲醯化芳香族胺基、N-醯基化芳香族胺基、硝基苄基胺基甲酸酯基、烷氧基苄基胺基甲酸酯基等之取代基的化合物等。此等之光鹼產生劑,可單獨、或組合2種以上使用。
有機溶劑可列舉丙酮、甲基乙基酮、環己酮等之酮類;甲苯、二甲苯、四甲基苯等之芳香族烴類;甲基賽璐蘇、乙基賽璐蘇、丁基賽璐蘇、甲基卡必醇、丁基卡必醇、丙二醇單甲基醚、二乙二醇單乙基醚、二丙二醇單乙基醚、三乙二醇單乙基醚等之二醇醚類;乙酸乙酯、乙酸丁酯、賽璐蘇乙酸酯、二乙二醇單乙基醚乙酸酯及上述二醇醚類之酯化物等之酯類;乙醇、丙醇、乙二醇、丙二醇等之醇類;1-甲基-2-吡咯啶酮、1,3-二甲基-2-四氫咪唑酮、2-吡咯啶酮、ε-己內醯胺、甲醯胺、N-甲基甲醯胺、N,N-二甲基甲醯胺、乙醯胺、N-甲基乙醯胺等之醯胺類;四氫呋喃、二噁烷等之醚類;乙腈、苄腈、丙腈等之腈類;氯仿、二氯甲烷、溴苯、二溴苯、氯苯、二氯苯等之鹵素類;N-甲基-2-吡咯啶酮、二甲基苯胺、二丁基苯胺、二異丙基苯胺等之胺類;二甲基亞碸、環丁碸等之含硫類;辛烷、癸烷等之脂肪族烴類;石油醚、石油腦、氫
化石油腦、溶劑石油腦等之石油系溶劑等。此等之中,尤以N-甲基-2-吡咯啶酮或甲基乙基酮,由於操作容易故較佳。
本發明之含有樹脂之薄片中,樹脂3係接觸於固著劑2與纖維素奈米纖維不織布11者。本發明中,樹脂3只要係不阻礙彈性或耐彎曲性之程度即可,亦可被覆纖維素奈米纖維不織布11之外側。樹脂組成物之含浸率,只要係不阻礙含有樹脂之薄片之儲存模數或耐彎曲性的程度,則無特殊限定,以含有樹脂之薄片中之樹脂的濃度計,為10~99體積%、特佳為10~70體積%。藉由使樹脂組成物之含浸率為上述範圍內,可平衡良好地得到良好之耐彎曲性與高強度。
作為形成樹脂3之樹脂組成物,可為含有由熱硬化性樹脂、光硬化性樹脂及熱可塑性樹脂中選出之至少1種者,可依其用途,而1種單獨、或組合2種以上使用。其中就硬化物或成形物之物性的觀點而言,尤以熱硬化性樹脂較佳、更佳為使用環氧樹脂。使用熱硬化性樹脂或光硬化性樹脂作為樹脂組成物時,可適當使用與關於固著劑組成物所列舉者相同之熱硬化性樹脂、光硬化性樹脂、有機溶劑等,但本發明中,就樹脂組成物及固著劑組成物而言,必須使用分別由不同成分所成者。又,熱可塑性樹脂可使用以下所示者。
熱可塑性樹脂可列舉丙烯酸樹脂、改質丙烯酸樹脂、低密度聚乙烯、高密度聚乙烯、乙烯-乙酸乙烯酯共聚物、聚對苯二甲酸乙二酯、聚丙烯、改質聚丙烯、聚苯乙烯、丙烯腈-丁二烯-苯乙烯共聚物、丙烯腈-苯乙烯共聚物、乙酸纖維素、聚乙烯醇、聚氯乙烯、聚偏二氯乙烯、聚乳酸等之通用塑膠類、聚醯胺、熱可塑性聚胺基甲酸酯、聚縮醛、聚碳酸酯、超高分子量聚乙烯、聚對苯二甲酸丁二酯、改質聚苯醚、聚碸(PSF)、聚苯硫醚(PPS)、聚醚碸(PES)、聚醚醚酮、聚芳酯、聚醚醯亞胺、聚醯胺醯亞胺、液晶聚合物、聚醯胺6T、聚醯胺9T、聚四氟乙烯、聚偏二氟乙烯、聚酯醯亞胺、熱可塑性聚醯亞胺等之工程塑膠類、烯烴系、苯乙烯系、聚酯系、胺基甲酸酯系、醯胺系、氯乙烯系、氫化系等之熱可塑性彈性體。本發明中,亦可使用樹脂複合體,例如作為熱硬化性樹脂與熱可塑性樹脂之樹脂複合體,可使用環氧樹脂-PSF、環氧樹脂-PPS、環氧樹脂-PES等。
本發明之固著劑組成物及樹脂組成物中,亦可摻合著色劑作為其他成分。
著色劑,可使用作為著色顏料或染料等而以色指數表示之公知慣用者。可列舉例如Pigment Blue 15、15:1、15:2、15:3、15:4 15:6、16、60、Solvent Blue 35、63、68、70、83、87、94、97、122、136、
67、Pigment Green 7、36、3、5、20、28、Solvent Yellow 163、Pigment Yellow 24、108、193、147、199、202、110、109、139、179、185、93、94、95、128、155、166、180、120、151、154、156、175、181、1、2、3、4、5、6、9、10、12、61、62、62:1、65、73、74、75、97、100、104、105、111、116、167、168、169、182、183、12、13、14、16、17、55、63、81、83、87、126、127、152、170、172、174、176、188、198、Pigment Orange 1、5、13、14、16、17、24、34、36、38、40、43、46、49、51、61、63、64、71、73、Pigment Red 1、2、3、4、5、6、8、9、12、14、15、16、17、21、22、23、31、32、112、114、146、147、151、170、184、187、188、193、210、245、253、258、266、267、268、269、37、38、41、48:1、48:2、48:3、48:4、49:1、49:2、50:1、52:1、52:2、53:1、53:2、57:1、58:4、63:1、63:2、64:1、68、171、175、176、185、208、123、149、166、178、179、190、194、224、254、255、264、270、272、220、144、166、214、220、221、242、168、177、216、122、202、206、207、209、Solvent Red 135、179、149、150、52、207、Pigment Violet 19、23、29、32、36、38、42、Solvent Violet 13、36、Pigment Brown 23、25、Pigment Black 1、7等。
又,本發明之固著劑組成物及樹脂組成物
中,可依需要含有消泡/調平劑、搖變性賦予劑/增黏劑、偶合劑、分散劑、難燃劑等之慣用的添加劑。
消泡劑/調平劑,可使用礦物油、植物油、脂肪族醇、脂肪酸、金屬皂、脂肪酸醯胺、聚氧烷二醇、聚氧烷烷基醚、聚氧烷脂肪酸酯等之化合物等。
搖變性賦予劑/增黏劑,可使用高嶺土、膨潤石、蒙脫土、皂土、滑石、雲母、沸石等之黏土礦物、或不定形無機粒子、聚醯胺系添加劑、改質脲系添加劑、蠟系添加劑等。
作為偶合劑,就烷氧基而言為甲氧基、乙氧基、乙醯基等,就反應性官能基而言為乙烯基、甲基丙烯酸基、丙烯酸基、環氧基、環狀環氧基、巰基、胺基、二胺基、酸酐、脲基、硫醚、異氰酸酯等,例如可使用乙烯基乙氧基矽烷、乙烯基三甲氧基矽烷、乙烯基/參(β-甲氧基乙氧基)矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷等之乙烯基系矽烷化合物;γ-胺基丙基三甲氧基矽烷、N-β-(胺基乙基)γ-胺基丙基三甲氧基矽烷、N-β-(胺基乙基)γ-胺基丙基甲基二甲氧基矽烷、γ-脲基丙基三乙氧基矽烷等之胺基系矽烷化合物、γ-環氧丙氧基丙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、γ-環氧丙氧基丙基甲基二乙氧基矽烷等之環氧基系矽烷化合物;γ-巰基丙基三甲氧基矽烷等之巰基系矽烷化合物;N-苯基-γ-胺基丙基三甲氧基矽烷等之苯基胺基系矽烷化合物等之矽烷偶合劑;異丙基三異硬脂醯化鈦酸酯、四辛基雙(二-十三烷
基亞磷酸酯)鈦酸酯、雙(二辛基焦磷酸酯)氧基乙酸酯鈦酸酯、異丙基三-十二烷基苯磺醯基鈦酸酯、異丙基參(二辛基焦磷酸酯)鈦酸酯、四異丙基雙(二辛基亞磷酸酯)鈦酸酯、四(1,1-二烯丙基氧基甲基-1-丁基)雙-(二-十三烷基)亞磷酸酯鈦酸酯、雙(二辛基焦磷酸酯)伸乙基鈦酸酯、異丙基三辛醯基鈦酸酯、異丙基二甲基丙烯酸基異硬脂醯基鈦酸酯、異丙基三硬脂醯基二丙烯酸基鈦酸酯、異丙基三(二辛基磷酸酯)鈦酸酯、異丙基三異丙苯基苯基鈦酸酯、二異丙苯基苯基氧基乙酸酯鈦酸酯、二異硬脂醯基伸乙基鈦酸酯等之鈦酸酯系偶合劑;含有乙烯性不飽和鋯酸酯之化合物、含有新烷氧基鋯酸酯之化合物、新烷氧基三新癸醯基鋯酸酯、新烷氧基參(十二烷基)苯磺醯基鋯酸酯、新烷氧基參(二辛基)磷酸酯鋯酸酯、新烷氧基參(二辛基)焦磷酸酯鋯酸酯、新烷氧基參(乙二胺基)乙基鋯酸酯、新烷氧基參(m-胺基)苯基鋯酸酯、四(2,2-二烯丙基氧基甲基)丁基,二(二-十三烷基)亞磷酸酯鋯酸酯、新戊基(二烯丙基)氧基,三新癸醯基鋯酸酯、新戊基(二烯丙基)氧基,三(十二烷基)苯-磺醯基鋯酸酯、新戊基(二烯丙基)氧基,三(二辛基)磷酸酯鋯酸酯、新戊基(二烯丙基)氧基,三(二辛基)焦磷酸酯鋯酸酯、新戊基(二烯丙基)氧基,三(N-乙二胺基)乙基鋯酸酯、新戊基(二烯丙基)氧基,三(m-胺基)苯基鋯酸酯、新戊基(二烯丙基)氧基,三甲基丙烯酸基鋯酸酯、新戊基(二烯丙基)氧基,三丙烯酸鋯酸酯、二新戊基(二烯丙基)氧基,二對胺基苯甲醯基鋯酸酯、二新戊基(二烯丙基)氧基,二
(3-巰基)丙酸鋯酸酯、鋯(IV)2,2-雙(2-丙烯醇基甲基)丁醇基,環二[2,2-(雙2-丙烯醇基甲基)丁醇基]焦磷酸酯-O,O等之鋯酸酯系偶合劑;二異丁基(油基)乙醯乙醯基鋁酸酯、烷基乙醯乙酸酯鋁二異丙醇化物等之鋁酸酯系偶合劑等。
分散劑,可使用聚羧酸系、萘磺酸甲醛縮合系、聚乙二醇、聚羧酸部分烷酯系、聚醚系、聚伸烷基多胺系等之高分子型分散劑;烷基磺酸系、四級銨系、高級醇環氧烷系、多元醇酯系、烷基多胺系等之低分子型分散劑等。
難燃劑,可使用氫氧化鋁、氫氧化鎂等之水合金屬系、紅磷、磷酸銨、碳酸銨、硼酸鋅、錫酸鋅、鉬化合物系、溴化合物系、氯化合物系、磷酸酯、含磷多元醇、含磷胺、三聚氰胺三聚氰酸酯、三聚氰胺化合物、三嗪化合物、胍化合物、聚矽氧聚合物等。
本發明之固著劑組成物及樹脂組成物,其他,在不阻礙本發明之目的的範圍內,亦可含有硫酸鋇、二氧化矽、水滑石等之無機填料;耐綸粉末、氟粉末等之有機填料;自由基捕捉劑、紫外線吸收劑、過氧化物分解劑、熱聚合禁止劑、密合促進劑、防鏽劑、表面處理劑、界面活性劑、潤滑劑、抗靜電劑、pH調整劑、抗氧化劑、染料、顏料、螢光劑等。
本發明中,固著劑2之儲存模數,必須高於樹脂3之
儲存模數。此處,固著劑2之儲存模數,意指不含纖維1,而將僅有固著劑組成物之成分的摻合物,於成膜後藉由熱或光硬化而得的硬化膜之儲存模數。同樣地,關於樹脂3之儲存模數,亦同樣,於硬化性樹脂的情況時意指於成膜後藉由熱或光硬化而得的硬化膜之儲存模數,於熱可塑性樹脂的情況時,意指於熔融成膜後去除溶劑而得的塗膜之儲存模數。又,儲存模數,意指試樣的硬度之一指標值,其係一邊施加一定的溫度變化,同時對試樣施以週期性的荷重,進行檢測應變之稱為動態黏彈性測定的評估,由所檢測之應變所算出之值,該值越高,顯示越優良的力學強度。本發明中,只要於任一溫度,固著劑2之儲存模數高於樹脂3之儲存模數即可,其適宜範圍,對於固著劑2之儲存模數而言係30~0.1GPa、更佳為20~0.5GPa,對於樹脂3之儲存模數而言係10~0.001GPa、更佳為5~0.01GPa,較佳為於任一溫度,固著劑2之儲存模數較樹脂3之儲存模數大0.1GPa以上。特佳為於150~250℃的範圍內之任一溫度,固著劑2之儲存模數高於樹脂3之儲存模數、又更佳為於150~250℃之全溫度範圍,固著劑2之儲存模數高於樹脂3之儲存模數。藉此,本發明之含有樹脂之薄片,於150~250℃之高溫區域亦可使用,因此因用途擴大而較佳。
本發明中,固著劑2之玻璃轉移溫度,較佳為高於樹
脂3之玻璃轉移溫度或軟化溫度。此處,固著劑2之玻璃轉移溫度,意指不含纖維1,而將僅有固著劑組成物之成分的摻合物,於成膜後藉由熱或光硬化而得的硬化膜之玻璃轉移溫度。同樣地,關於樹脂3之玻璃轉移溫度或軟化溫度,亦同樣,於硬化性樹脂的情況時,意指於成膜後藉由熱或光硬化而得的硬化膜之玻璃轉移溫度,於熱可塑性樹脂的情況時,意指於熔融成膜後將溶劑去除而得的塗膜之軟化溫度。又,玻璃轉移溫度,意指由前述之動態黏彈性測定所得到之儲存模數(E')與損失彈性率(E")的比(E"/E')所算出之值(損失正切)為最大時的溫度,該溫度越高,顯示越優良的耐熱性。本發明中,玻璃轉移溫度之上限並無特殊限制,其適宜之範圍,對於固著劑2之玻璃轉移溫度而言為130℃以上、更佳為140℃以上,對於樹脂3之玻璃轉移溫度或軟化溫度而言為70℃以上、更佳為80℃以上,固著劑2之玻璃轉移溫度較佳為比樹脂3之玻璃轉移溫度或軟化溫度高5℃以上。
本發明之含有樹脂之薄片,可藉由將纖維素奈米纖維不織布11以固著劑組成物處理,而使纖維1彼此固著後,於經固著之纖維素奈米纖維不織布11中含浸樹脂組成物而得到。例如,亦可藉由在於載體膜等之被塗佈物上配置纖維的狀態下,將固著劑組成物及樹脂組成物依次塗佈、含浸,使固著劑組成物及樹脂組成物中所含之有機溶
劑揮發乾燥,作為乾膜而製造本發明之含有樹脂之薄片,亦可依期望,進一步地,於其上貼合覆蓋膜。此時,樹脂組成物,只要係並非阻礙固著劑組成物對纖維之固著性能者,則樹脂組成物之塗佈過程,可為固著劑之乾燥前,亦可為乾燥後。
此情況時,本發明之固著劑組成物及樹脂組成物,可依需要,將各成分摻合、分散、稀釋,調整為適於塗佈方法之黏度進行塗佈。如上所述,關於固著劑組成物,只要係可滲透於纖維素奈米纖維不織布11使纖維1彼此固著者即可,又,關於樹脂組成物,只要係可將纖維素奈米纖維不織布11之至少一面、特別是兩面,對金屬箔等密合者即可。
被塗佈物較佳為乾膜用之載體膜,但亦可直接塗佈於金屬箔表面或形成有電路之配線板表面。塗佈方法之具體例子,可列舉使用吸量管等之滴下法、浸漬塗佈法、棒塗佈法、旋轉塗佈法、淋幕塗佈法、噴霧塗佈法、輥塗佈法、狹縫塗佈法、刮刀塗佈法、唇口塗佈法、刮刀塗佈(comma coating)法、薄膜塗佈法等之各種塗佈法;或網版印刷、噴霧印刷、噴墨印刷、凸版印刷、凹版印刷、平版印刷等之各種印刷法。
又,載體膜與覆蓋膜,係作為乾膜所用之材料之公知者均可使用,可列舉例如聚乙烯薄膜、聚丙烯薄膜等。載體膜與覆蓋膜,可使用相同之薄膜材料、亦可使用不同的薄膜材料,但關於覆蓋膜,較佳為與樹脂3之接
著性較載體膜小者。
藉由使本發明之含有樹脂之薄片與基板密合,可得到構造體。基板可列舉金屬箔基板、或電路基板(形成有電路之配線板)等。藉由使本發明之含有樹脂之薄片與基板表面熱密合,可形成樹脂絕緣層,亦可藉著重複該過程,使金屬箔層與樹脂絕緣層分別以複數層層合。再者,含有樹脂之薄片,可於在載體膜上製造時,使含有樹脂之薄片彼此層合、亦可於與金屬箔等密合時使含有樹脂之薄片彼此層合。
使用本發明之含有樹脂之薄片來製作構造體時,固著劑組成物及樹脂組成物為熱硬化性樹脂或光硬化性樹脂之組合的情況時,藉由使用僅有加熱硬化之方法、僅有活性能量線照射之方法、於活性能量線照射後加熱硬化之方法、或於加熱硬化後照射活性能量線之方法,可製作構造體。又,使用乾膜的情況時,有覆蓋膜時可剝離覆蓋膜,使含有樹脂之薄片熱密合於基板表面,接著剝離載體膜,藉由上述硬化方法使其硬化,來製造構造體。再者,固著劑組成物及樹脂組成物均使用熱硬化性樹脂時,亦可同時實施纖維彼此之固著及樹脂之含浸的雙方之加熱硬化過程。又,關於進行加熱時的加熱溫度,只要係目標之基材中所含的纖維或固著劑不因高熱而分解的範圍即可,無特別的下限及上限之限制,關於進行活性能量線照射時的曝光量的情況,亦只要並無曝光量過低而產生未硬化部分的情形,則無特別之下限及上限的限制。
又,製作本發明之含有樹脂之薄片時,樹脂組成物為熱可塑性樹脂的情況時,亦可使用將丸粒形狀或薄片形狀之熱可塑性樹脂加熱或加熱、壓接的手法。此處,為了將熱可塑性樹脂,含浸於藉由固著劑所固著之纖維素奈米纖維不織布內,使用裝置加壓雖非必須要件,但藉由進行加壓,熱可塑性樹脂對纖維素奈米纖維不織布內之滲入變得更為容易。進行加壓時,只要不損及目標之含有樹脂之薄片的形狀,則無特別的壓力上限。藉由使該含有樹脂之薄片熱密合於基體表面,可使構造體成形。又,使用乾膜使構造體成形時,可與前述同樣方式地製作。
再者,上述中,乾燥時、加熱硬化時或加熱加壓時所用之裝置,可列舉熱風循環式乾燥爐、IR爐、加熱板、對流烘箱、加熱/加壓輥、壓合機等。又,活性能量線照射之光源,可列舉低壓水銀燈、中壓水銀燈、高壓水銀燈、超高壓水銀燈、氙燈、金屬鹵化物燈等。其他,亦可利用雷射光線等作為活性能量線。
關於本發明之含有樹脂之薄片之構成構件的纖維素奈米纖維不織布、以固著劑使纖維素奈米纖維不織布中之纖維彼此固著者(以下亦稱為「中間體」)、及乾膜之厚度,並無特殊限定,可依目的適當選擇,但特別關於中間體,只要係藉由固著劑使纖維彼此互相固著者即可,因此其厚度,較佳為與纖維素奈米纖維不織布之厚度同等、或不超過纖維素奈米纖維不織布厚度的2倍之程度的膜厚。具體而言,更佳為纖維素奈米纖維不織布厚度的
1~1.5倍之範圍內。中間體之厚度超過纖維素奈米纖維不織布厚度的2倍時,固著劑本身的物性之影響會產生,故不佳。
將本發明之含有樹脂之薄片於基板表面形成,並硬化或成形所得之構造體,可使用作為配線板用之芯材,藉由進行蝕刻處理等,亦可使用作為配線板用之層間絕緣材。又,若將含有樹脂之薄片形成於形成有電路的配線板表面,以僅包覆電路配線的方式進行圖型化處理及硬化或成形而成為構造體,則亦可使用作為配線板之最外層的阻焊劑等。
以上說明之構成的本發明之含有樹脂之薄片,可應用於電子機器用之配線板等,例如可適合應用於配線板用之層間絕緣材或阻焊劑、芯材等,藉此,可得到本發明之所期望的效果。其他,例如藉由將纖維彼此以固著劑組成物固著,使樹脂滲透、乾燥,形成半硬化狀態(B階段)之樹脂絕緣層,且將樹脂絕緣層與金屬箔予以層合壓合,亦可製作多層板。
以下,藉由實施例、比較例以更詳細說明本發明,但本發明不受此等實施例、比較例限制。再者,以下表中之摻合量,均表示質量份。
於經氮取代之附攪拌機的三口燒瓶中,加入脫水N-甲基-2-吡咯啶酮(NMP)溶劑(和光純藥工業(股)製),以1:1莫耳比摻合4,4’-二胺基二苯基醚(ODA)(和光純藥工業(股)製)與1,2,4,5-苯四羧酸二酐(PMDA)(和光純藥工業(股)製),於室溫攪拌16小時以上,得到樹脂固體成分比例為7.5質量%之聚醯胺酸清漆1。
於經氮取代之附攪拌機的三口燒瓶中,加入脫水N-甲基-2-吡咯啶酮(NMP)溶劑(和光純藥工業(股)製),以1:1莫耳比摻合p-苯二胺(PDA)(和光純藥工業(股)製)與3,3’,4,4’-聯苯基四羧酸酐(BPDA)(和光純藥工業(股)製),於室溫攪拌16小時以上,得到樹脂固體成分比例為7.5質量%之聚醯胺酸清漆2。
下述表1中,表示作為固著劑組成物或樹脂組成物所使用之組成物1~4的摻合內容。遵照下述表1中之組成物1~4的記載來配製各組成物。組成物1之複數成分系統的情況時,係將各成分摻合後,使用自轉/公轉混合器攪拌、配製。
將各組成物1~4分別使用塗抹器塗佈於厚18μm之銅
箔上,得到塗膜。
關於組成物1,係以熱風循環式乾燥爐於80℃、30分鐘知大氣條件下乾燥後,於150℃、60分鐘之大氣條件下加熱而得到環氧樹脂硬化物。去除銅箔後,厚度為50μm。使用此硬化物,製作寬5mm、長50mm之儲存模數等評估用試驗片。
關於組成物2,係於塗佈後,以熱風循環式乾燥爐於80℃、30分鐘之大氣條件下乾燥後,於250℃、60分鐘之氮條件下(100ml/min.)加熱而得到醯亞胺化物。去除銅箔後,厚度為50μm。之後,與上述相同方式地製作評估用試驗片。
關於組成物3,除了將加熱操作於300℃、60分鐘之氮條件下進行以外,係與組成物2相同地製作評估用試驗片。
關於組成物4,係將高密度聚乙烯丸粒(比重0.95)適量投入壓合機,於140℃、3MPa、3分鐘加熱加壓後,冷卻至室溫得到成形體後,單片化之後,厚度為50μm。之後,與上述相同地製作評估用試驗片。
下述表2中,表示各實施例及比較例之含有樹脂之薄片或薄片之構成。
將自雙日(股)所獲得的再生纖維素纖維之天絲纖維切絲(3mm長)置入洗淨用網,添加界面活性劑,以洗衣機水洗多次,藉以去除纖維表面之油劑。將所得之精製天絲纖維(切絲)以成為固體成分1.5質量%的方式分散於水中(400L),使用圓盤式精磨機裝置之相川鐵工(股)製SDR14型Labo Refiner(加壓型DISK式),以圓盤間之空隙為1mm,將400L之該水分散體予以20分鐘打漿處理。其後,以將空隙減低至近乎零的等級之條件下繼續打漿處理。經時進行取樣,對取樣漿體評估以JIS P 8121定義之CSF值後,CSF值係經時地減少,一旦接近零後,進一步持續打漿處理時,確認到有增大之傾向。使空隙接近零後,以上述條件繼續打漿處理約14小時,得到CSF值15ml↑之打漿水分散體(固體成分濃度:1.5質量%)。將所得之知打漿水分散體直接使用高壓均質機(Niro Soavi公司(義大利)製NS015H)於操作壓力100MPa下實施1次及5次之微細化處理,分別得到微細纖維素纖維之水分散體M1及M2(固體成分濃度:均為1.5質量%)。
接著,將上述水分散體M2稀釋至固體成分濃度0.1質量%,以摻合機分散後,於設置有PET/耐綸混紡製之平織物(敷島Canvas公司製、NT20,大氣下25℃之水透過量:0.03ml/cm2.s,有以於大氣壓下25℃之過濾而將將微細纖維素纖維99%以上濾離的能力)的批式抄紙機(熊谷理機工業公司製,自動方型薄片機25cm×25cm、80
網目),以單位面積之重量10g/m2的微細纖維素薄片為標準,投入經上述調整之抄紙漿體,之後以對大氣壓之減壓度為4KPa,來實施抄紙(脫水)。
將所得之置於濾布上的由濕潤狀態之濃縮組成物所成的濕紙,由線材上剝離,以1kg/cm2之壓力壓合1分鐘後,以使濕紙面接觸於滾筒面的方式,於濕紙/濾布之2層狀態下,於表面溫度設定為130℃的滾筒乾燥機中仍以濕紙接觸於滾筒面的方式,乾燥約120秒,由所得之經乾燥之2層體,由纖維素之薄片狀構造物上使濾布剝離,得到由白色均勻的纖維素微細纖維所構成之薄片(25cm×25cm)。
進一步地,將所得之微細纖維素薄片,藉由壓延機(由利Roll公司製)實施150℃×1.55t/20cm之熱壓合處理,藉以得到膜厚17μm、對應比表面積之纖維直徑0.442μm、透氣抵抗度11s/100ml、空孔率62%、氯離子含有濃度19ppm之白色纖維素奈米纖維不織布。
關於下述表2中之實施例1,係使用上述纖維素奈米纖維不織布,於其中含浸上述組成物1(黏度0.0005Pa.s)後,以熱風循環式乾燥爐於80℃、30分鐘之大氣條件下乾燥後,於150℃加熱硬化60分鐘,製作由纖維素奈米纖維不織布及固著劑(環氧樹脂組成物之硬化物)所成之中間體。
關於下述表2中之實施例2,係於與實施例1相同之纖維素奈米纖維不織布中,含浸上述組成物2(黏度0.001Pa.s)後,以熱風循環式乾燥爐於80℃、30分鐘之大氣條件下乾燥後,於250℃加熱60分鐘予以醯亞胺化,製作由纖維素奈米纖維不織布及固著劑(聚醯亞胺)所成之中間體。
關於下述表2中之實施例3,係於與實施例1相同之纖維素奈米纖維不織布中,含浸上述組成物3(黏度0.001Pa.s)後,以熱風循環式乾燥爐於80℃、30分鐘之大氣條件下乾燥後,於200℃加熱60分鐘予以醯亞胺化,製作由纖維素奈米纖維不織布及固著劑(聚醯亞胺)所成之中間體。
與實施例1相同地,使用上述組成物1,製作由纖維素奈米纖維不織布及固著劑(環氧樹脂組成物之硬化物)所成之中間體。
實施例1~3及比較例4之各中間體的厚度為33~35μm,由纖維素奈米纖維不織布之厚度所增大的厚度僅有3~5μm。
關於實施例1,係將上述組成物4投入壓合機,於140℃熔融後,含浸於上述中得到之各中間體,於140℃、3MPa、3分鐘加熱加壓後,冷卻至室溫,以製作於經固著劑(環氧樹脂組成物)固著之纖維素奈米纖維不織布中含浸有樹脂(高密度聚乙烯樹脂)的含有樹脂之薄片。
關於實施例2、實施例3,係將上述組成物1,對上述中得到之各中間體,以遍佈纖維全體的方式適量塗佈、含浸,以與上述固著劑或樹脂之評估用試驗片之製作相同的條件加熱硬化,藉此製作於經固著劑(聚醯亞胺)固著之纖維素奈米纖維不織布中含浸有樹脂(環氧樹脂硬化物)的含有樹脂之薄片。
實施例1~3之各含有樹脂之薄片的厚度,係較中間體之厚度厚10~20μm。之後,對於各含有樹脂之薄片,以與上述相同之條件製作評估用試驗片。
關於比較例1,係將上述組成物1,對纖維素奈米纖維不織布,以遍佈纖維全體的方式適量塗佈、含浸,以與上述固著劑或樹脂之評估用試驗片之製作相同的條件加熱硬化,藉此製作於不含固著劑之纖維素奈米纖維不織布中含浸有樹脂(環氧樹脂硬化物)的薄片。
關於比較例2,係於纖維素奈米纖維不織布中,使上述組成物2與比較例1相同地塗佈、含浸後,以熱風循環式乾燥爐於80℃、30分鐘之大氣條件下乾燥
後,於250℃、60分鐘之大氣條件下加熱而醯亞胺化,製作於不含固著劑之纖維素奈米纖維不織布中含浸有樹脂(聚醯亞胺)的薄片。
關於比較例3,係將上述組成物4投入壓合機,於140℃熔融後,含浸於纖維素奈米纖維不織布,於140℃、3MPa、3分鐘加熱加壓後,冷卻至室溫,藉以製作於不含固著劑之纖維素奈米纖維不織布中含浸有樹脂(高密度聚乙烯樹脂)的薄片。
關於比較例4,除了將比較例2中之纖維素奈米纖維不織布變更為具有由上述組成物1所成之固著劑的中間體來使用以外,係與比較例2相同地製作含有樹脂之薄片。
之後,對於各薄片,與上述相同地製作評估用試驗片。
再者,樹脂成分濃度,如下述表2所示,關於實施例1~3及比較例1~4,為相同程度。此處,樹脂成分濃度,係由固著劑量={1-(纖維素奈米纖維不織布之體積/中間體之體積)}×100[體積%]、樹脂量={1-(中間體之體積/含有樹脂之薄片或薄片之體積)}×100[體積%](體積係基於質量及比重來換算)所分別求出。
使用固著劑或樹脂之儲存模數等評估用試驗片,且使用DMA黏彈性測定裝置((股)日立High-Tech Science製
DMA7100)之拉伸模式,以測定頻率1Hz、最小張力及最小壓縮力200mN、應變振幅10μm、昇溫速度5℃/分、大氣下之條件來測定黏彈性,得到於50℃、150℃及250℃之儲存模數,而且得到玻璃轉移溫度或軟化溫度。其結果如下述表1所示。
*1:jER828,三菱化學(股)製
*2:2-乙基-4-甲基咪唑,四國化成(股)製
*3:和光純藥工業(股)製
*4:比重0.95
關於含有樹脂之薄片或薄片評估用試驗片,係除了以薄片中之纖維素奈米纖維不織布或聚芳醯胺不織布的纖維之偏向(斜)方向成為裝置之拉伸方向的方式安裝試驗片,且使最小張力及壓縮力為50mN以外,與上述相同地測定黏彈性,得到於50℃、150℃及250℃之儲存模數。此處,於偏向(斜)方向測定,係為了極力排除纖維素奈米纖維不織布本身之彈性率的影響,調查固著效果所致之彈性率提高的影響之故。關於各實施例,當與未附著有固著劑的比較例之薄片比較時,儲存模數E[GPa]之值較大時為○、較小時為×。
具體說明時,實施例1之含有樹脂之薄片,於50℃、150℃、250℃的所有溫度,儲存模數E[GPa]之值均較未使用固著劑的比較例3之薄片更大,故為「○」。
於實施例2、實施例3之含有樹脂之薄片,亦分別較未使用固著劑之比較例1的薄片之儲存模數E[GPa]之值大,故為「○」。
另一方面,比較例4之含有樹脂之薄片,於50℃、150℃、250℃的所有溫度,儲存模數E[GPa]之值均較未使用固著劑之比較例2的薄片更小,故為「×」。其結果如下述表2所示。
除了將纖維素奈米纖維不織布配置於載體膜上以外,係與上述相同地將固著劑組成物塗佈、含浸,製作各中間體。之後,於乾燥後之固著劑表面,將樹脂組成物成形或塗佈,使其乾燥後,貼合覆蓋膜,得到乾膜。於該乾膜之兩面疊合厚度18μm之表面未處理銅箔(密合時載體膜及覆蓋膜係剝離),以真空壓合機,使加壓條件為1MPa;加熱條件於實施例1為150℃×10分、於實施例2、比較例4為250℃×60分、於實施例3為300℃×60分進行成形,製作樹脂層與銅箔經密合的耐彎曲性評估用試驗片。又,關於比較例1~3,除了未塗佈、含浸固著劑組成物以外,係同樣地製作乾膜、以真空壓合機加壓,以與比較例1~3之薄片製作相同之溫度條件來製作耐彎曲性評估用試驗片。
使用耐彎曲性評估用試驗片,以彎曲半徑0.8mm、彎曲速度175回/分、折彎角度135°、荷重200g、於樹脂層成為內側的方向彎曲,進行彎曲試驗。直到試驗片斷裂為止的折彎次數係100次以上時為○、70~99次為△、69次以下為×。其結果如下述表2所示。評估結果為○時,可稱耐彎曲性優良。
如上述表2所示,實施例1~3之固著劑之儲存模數,相較於樹脂之儲存模數均為較大,另一方面,比較例4中,固著劑之儲存模數較樹脂之儲存模數為小。又,比較例1~3中,僅使用樹脂,未使用固著劑。
如上述表2所示,可知使用固著劑之儲存模數較樹脂之儲存模數更高之固著劑,使纖維素奈米纖維不織布固著,進而含浸樹脂之實施例的含有樹脂之薄片,相較於僅含浸樹脂之比較例的薄片而言,耐彎曲性優良、且儲存模數大。
例如,由實施例1與比較例3的對比明顯可知,將纖維素奈米纖維不織布之纖維彼此藉由固著組成物固著,進而於纖維素奈米纖維不織布含浸樹脂組成物之實施例的含有樹脂之薄片,相較於未藉由固著組成物將纖維素奈米纖維不織布之纖維彼此固著之比較例3而言,於所有的溫度儲存模數均較高,因此可知力學強度高。
特別地,實施例2及實施例3的含有樹脂之薄片,250℃之儲存模數超過1GPa,可知高溫時之力學強度亦優良。另一方面,固著劑之儲存模數較樹脂之儲存模數更低的比較例4中,作為含有樹脂之薄片之儲存模數低。
由以上所述,確認了藉由使用具有使纖維素奈米纖維不織布中之纖維彼此固著的固著劑、與接觸於經固著之纖維的樹脂,且固著劑之儲存模數較樹脂之儲存模數更高的含有樹脂之薄片,可實現優良的力學強度、彈性率及耐彎曲性。該本發明之含有樹脂之薄片,可應用於電子機器用之配線板等,例如可適合應用於配線板用之層間絕緣材或阻焊劑、芯材等。
Claims (6)
- 一種含有樹脂之薄片,其特徵為具有:由包含至少一層的含有70質量%以上之再生纖維素微細纖維的纖維素微細纖維層之單層或3層以下之複數層所構成,且滿足下述(1)~(3)之全部要件的纖維素奈米纖維不織布、使前述纖維素奈米纖維不織布中之纖維彼此固著之固著劑、與鄰接於前述纖維素奈米纖維不織布與固著劑之樹脂,且前述固著劑之儲存模數,高於前述樹脂之儲存模數;(1)構成纖維素微細纖維層之纖維的對應比表面積之纖維直徑為0.20μm以上且1.0μm以下、(2)透氣抵抗度為1s/100ml以上且40s/100ml以下、(3)膜厚為8μm以上且22μm以下。
- 如請求項1之含有樹脂之薄片,其中前述固著劑之玻璃轉移溫度,高於前述樹脂之玻璃轉移溫度或軟化溫度。
- 如請求項1之含有樹脂之薄片,其係藉由固著劑組成物使前述纖維素奈米纖維不織布之纖維彼此固著後,使樹脂組成物含浸於該經固著之纖維素奈米纖維不織布而得到。
- 如請求項3之含有樹脂之薄片,其中前述固著劑組成物之黏度為1Pa.s以下。
- 一種使用含有樹脂之薄片之構造體,其特徵為將如請求項1之含有樹脂之薄片密合於基板而得到。
- 一種配線板,其特徵為具有如請求項5之構造體。
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- 2015-10-28 EP EP15857169.5A patent/EP3216823B1/en active Active
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JP6402005B2 (ja) | 2018-10-10 |
US20170313831A1 (en) | 2017-11-02 |
US10047202B2 (en) | 2018-08-14 |
JP2016089022A (ja) | 2016-05-23 |
CN107075155A (zh) | 2017-08-18 |
EP3216823B1 (en) | 2019-08-14 |
EP3216823A1 (en) | 2017-09-13 |
EP3216823A4 (en) | 2017-11-29 |
CN107075155B (zh) | 2020-05-19 |
WO2016072334A1 (ja) | 2016-05-12 |
TW201630738A (zh) | 2016-09-01 |
KR102380508B1 (ko) | 2022-03-31 |
KR20170082569A (ko) | 2017-07-14 |
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