JP4428521B2 - 透明積層体 - Google Patents
透明積層体 Download PDFInfo
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- JP4428521B2 JP4428521B2 JP2004218963A JP2004218963A JP4428521B2 JP 4428521 B2 JP4428521 B2 JP 4428521B2 JP 2004218963 A JP2004218963 A JP 2004218963A JP 2004218963 A JP2004218963 A JP 2004218963A JP 4428521 B2 JP4428521 B2 JP 4428521B2
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- fiber
- cellulose
- transparent laminate
- sheet
- transparent
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Images
Landscapes
- Laminated Bodies (AREA)
- Non-Insulated Conductors (AREA)
Description
20℃において、サンプルの単位体積当たりの質量を測定して密度を求め、水の密度(1.004g/cm3(20℃))とから、比重を算出した。
<測定装置>
日立ハイテクノロジーズ社製「UV−4100形分光度計」(固体試料測定システム)を使用。
<測定条件>
・6mm×6mmの光源マスク使用
・測定サンプルを積分球開口より22cm離れた位置において測光した。サンプルをこの位置に置くことで、拡散透過光は除去され、積分球内部の受光部に直線透過光のみが届く。
・リファレンスサンプルなし。リファレンス(試料と空気との屈折率差によって生じる反射。フレネル反射が生じる場合は、直線透過率100%ということはあり得ない。)がないため、フレネル反射による透過率のロスが生じている。
・スキャンスピード:300nm/min
・光源:タングステンランプ、重水素ランプ
・光源切り替え:340nm
<試料の作成方法>
バクテリアセルロース:含水バクテリアセルロースを液体窒素で凍結し、減圧乾燥を行
った。
離解バクテリアセルロース:製造例2で作製したグラインダー処理懸濁液を、0.02
重量%懸濁液にして、その懸濁液を液体窒素で凍結し、減
圧乾燥を行った。
<試料の調製及び測定条件>
フリーズドライした各試料に、金蒸着(蒸着膜厚:数nm)を行い、下記条件で電子顕微鏡観察を行った。
測定装置:JEOL 5310(日本電子株式会社製)
加速電圧:10kV
倍率:2000倍
ワーキングディスタンス:20mm
コントラストの調整:AUTO
セイコーインスツルメンツ製「TMA/SS6100」を用い、ASTM D 696に規定された方法に従って下記の測定条件で測定した。
〈測定条件〉
昇温速度:5℃/min
雰囲気:N2中
加熱温度:50〜150℃
荷重:3g
測定回数:3回
試料長:4×15mm
試料厚さ:試料により異なる
モード:引っ張りモード
厚さ約1mmの材料から幅8mm、長さ5mmの試料を作製し、JIS K 7203に規定された方法に従って3点曲げにより測定した。
厚さ約1mmの材料から幅8mm、長さ5mmの試料を作製し、JIS K 7203に規定された方法に従って変形速度5mm/minで測定した。
嵩密度1.2kg/m3で厚さ40μmのBCシートサンプルについてJIS P 8117に規定された方法に従って測定した。
測定機器として三菱化学(株)製ロレスタを用い、4探針プローブ「AS probe MCT−TP03」を使用し、4探針法(JIS R 1637)により抵抗率を測定し、比抵抗に換算した。
まず、凍結乾燥保存状態の酢酸菌の菌株に培養液を加え、1週間静置培養した(25〜30℃)。培養液表面に生成したバクテリアセルロースのうち、厚さが比較的厚いものを選択し、その株の培養液を少量分取して新しい培養液に加えた。そして、この培養液を大型培養器に入れ、25〜30℃で7〜30日間の静地培養を行った。培養液には、グルコース2重量%、バクトイーストエクストラ0.5重量%、バクトペプトン0.5重量%、リン酸水素二ナトリウム0.27重量%、クエン酸0.115重量%、硫酸マグネシウム七水和物0.1重量%とし、塩酸によりpH5.0に調整した水溶液(SH培地)を用いた。
製造例1において、バクテリアセルロースが産生された後、グラインダー処理できる程度まで家庭料理用ミキサーを用いて小さく離解した。そして、このバクテリアセルロース水懸濁液(1重量%濃度)を、ディスク回転速度:1200rpmで30回繰り返しグラインダー処理した。その後、グラインダー処理した懸濁液をガラスフィルターで濾過し、濾過物をホットプレスを用い、圧締圧力2MPa、温度120℃で完全に水を除去し、嵩密度1.2kg/m3、厚さ40μmのBCシートを得た。この離解BCシートについて、透過度を測定したところ、4650sec/100ccであった。
ミクロフィブリル化セルロース:MFC(高圧ホモジナイザー処理で、針葉樹クラフトパルプ(NBKP)をミクロフィブリル化したもの、平均繊維径1μm)を水に十分に撹拌し、1重量%濃度の水懸濁液を7kg調製し、グラインダー(栗田機械作成所製「KM1−10」)にて、この水懸濁液を、ほぼ接触させた状態の1200rpmで回転するディスク間を、中央から外に向かって通過させる操作を30回(30pass)行った。
製造例3において、MFCのグラインダー処理を行わなかったこと以外は、同様にして、繊維含有率約70%、厚さ50μmのMFCシートを得た。
製造例1で得られたBCシートを、表2に示す樹脂に減圧下(0.08MPa)で12時間浸漬処理した後、紫外線硬化タイプの場合には、取り出したシートを8分間紫外線照射して樹脂を硬化させ(照射後、加熱なし。)、また、熱硬化タイプの場合には、取り出したシートを数時間風乾後、150℃、50MPaで10分間加熱プレスして硬化させることにより、それぞれ樹脂複合BCシートを得た。
製造例3で得られたNano MFCシートを、製造例7と同様にしてアクリル樹脂Bに含浸させて紫外線照射により硬化させることによりアクリル樹脂複合Nano MFCシートを得た。
製造例2で得られた離解BCシートを、製造例7と同様にアクリル樹脂Bに含浸させて紫外線照射により硬化させることにより、アクリル樹脂含浸離解BCシートを得た。
製造例4で得られたMFCシートを、製造例7と同様にアクリル樹脂Bに含浸させて紫外線照射により硬化させることにより、アクリル樹脂含浸MFCシートを得た。
下記表3に示すシートをサンプルとして光線透過率を測定し、結果を図3〜5に示すと共に、50μm厚可視光透過率を算出し、結果を表3に示した。
(1)ベースのアクリル樹脂シート材のみ:0.3W/mK(面内)
(2)アクリル樹脂複合BCシート:1W/mK(面内)
であった。
製造例1と同様にして、厚さ約50μmのBCシートを得、このBCシートを無水酢酸へ投入し、120℃、21時間加熱した後、直ちに水中へ投入し、反応を停止させた。次いで、2日間流水洗浄し、その後、温水中70℃で1時間放置した。これを濾紙に挟み、軽くおもりをのせ、乾燥した濾紙を交換し、50℃で減圧乾燥した。このBCシートは、赤外分光法(IRスペクトル法)により、アセチル基がセルロースの水酸基に導入されたアセチル化BCシートであることが確認された。
製造例5,6,11と同様にして得られた樹脂複合BCシート(厚さ60μm)の一方の面に、DCマグネトロンスパッタ法により、下記条件で膜厚110nmのIZO透明導電膜を形成して本発明の透明積層体を得た。この透明積層体について、比抵抗を測定したところ、表5に示す通りであった。
〈成膜条件〉
ターゲット材質:InO3−ZnO(組成比(重量%)約90:10)
反応ガス:Ar/O2
反応圧力:0.3Pa
スパッタリング出力:1.2W/cm2
基板温度:23℃
(1) 20℃〜150℃〜20℃の加熱・冷却試験を約50℃/minで5回繰り返した。
(2) 50μm厚×100mm長×25mm幅のテープ形状試料に500gまでの引張応力を負荷し、その後、弛緩、負荷を5回繰り返した。
厚さ0.7mmのガラス基材に実施例1と同様にしてIZO透明導電膜を形成したもの(比抵抗4.2×104Ω・cm)について、厚さ方向に波長400〜700nmの光を照射した時の全波長域における光線透過率の平均値を調べ、結果を表5に示した。
厚さ100μmのポリカーボネート押出成形フィルムに実施例1と同様にしてIZO透明導電膜を形成したものについて、比抵抗と、温度変化負荷後の比抵抗の変化及び変形の有無と、引張応力負荷後の比抵抗の変化を調べ、結果を表5に示した。
Claims (17)
- 平均繊維径が4〜60nmの繊維とマトリクス材料とを含有し、50μm厚換算における波長400〜700nmの光線透過率が60%以上である繊維強化複合材料であって、該繊維強化複合材料中の該繊維の含有率が10重量%以上である繊維強化複合材料よりなる基材と、該基材の表面に形成された透明導電膜とを有することを特徴とする透明積層体。
- 請求項1において、該繊維がセルロース繊維であることを特徴とする透明積層体。
- 請求項2において、該セルロース繊維が化学修飾及び/又は物理修飾されていることを特徴とする透明積層体。
- 請求項3において、該セルロース繊維がアセチル化されていることを特徴とする透明積層体。
- 請求項2ないし4のいずれか1項において、該セルロース繊維がバクテリアセルロースであることを特徴とする透明積層体。
- 請求項5において、該バクテリアセルロースが離解処理されていないものであることを特徴とする透明積層体。
- 請求項6において、該バクテリアセルロースが三次元交差構造体となっていることを特徴とする透明積層体。
- 請求項5ないし7のいずれか1項において、該バクテリアセルロースが、バクテリアと該バクテリアから産生され該バクテリアに連なっているセルロースとを含む産生物をアルカリ処理してバクテリアを溶解除去したものであることを特徴とする透明積層体。
- 請求項2ないし4のいずれか1項において、該セルロース繊維が植物繊維から分離されたものであることを特徴とする透明積層体。
- 請求項9において、該セルロース繊維がミクロフィブリル化セルロース繊維を更に磨砕処理してなることを特徴とする透明積層体。
- 請求項1ないし10のいずれか1項において、該透明導電膜が、錫ドープ酸化インジウム、アルミニウムドープ酸化亜鉛、及びインジウムドープ酸化亜鉛よりなる群から選ばれる複合金属酸化物薄膜であることを特徴とする透明積層体。
- 請求項1ないし11のいずれか1項において、該透明導電膜の膜厚が0.01〜10μmであることを特徴とする透明積層体。
- 請求項1ないし12のいずれか1項において、該基材の線熱膨張係数が0.05×10−5〜5×10−5k−1であることであることを特徴とする透明積層体。
- 請求項1ないし13のいずれか1項において、該基材の曲げ強度が30MPa以上であることを特徴とする透明積層体。
- 請求項1ないし14のいずれか1項において、該基材の比重が1.0〜2.5であることを特徴とする透明積層体。
- 請求項1ないし15のいずれか1項において、該マトリクス材料が、樹脂材料であることを特徴とする透明積層体。
- 請求項16において、該マトリクス材料が結晶化度10%以下で、ガラス転移温度が110℃以上の合成樹脂であることを特徴とする透明積層体。
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JP5207499B2 (ja) * | 2007-03-30 | 2013-06-12 | スターライト工業株式会社 | フェノール樹脂複合材およびその製造方法 |
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JP5531295B2 (ja) | 2008-07-31 | 2014-06-25 | 国立大学法人京都大学 | 不飽和ポリエステル樹脂とミクロフィブリル化植物繊維を含有する成形材料 |
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JP2013011026A (ja) * | 2011-06-28 | 2013-01-17 | Daicel Corp | セルロースナノファイバーを主成分とする高強度材料及びその製造方法 |
US9862840B2 (en) | 2014-09-17 | 2018-01-09 | National University Corporation Nagoya University | Conducting composition and method for producing the same |
JP6402005B2 (ja) | 2014-11-04 | 2018-10-10 | 太陽ホールディングス株式会社 | 樹脂含有シート、並びに、それを用いた構造体および配線板 |
JP7280035B2 (ja) * | 2018-12-17 | 2023-05-23 | 日東電工株式会社 | 導電性フィルム及び導電性フィルムの製造方法 |
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