JP6443341B2 - 光反射フィルムおよびこれを用いた光反射体 - Google Patents
光反射フィルムおよびこれを用いた光反射体 Download PDFInfo
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- JP6443341B2 JP6443341B2 JP2015553515A JP2015553515A JP6443341B2 JP 6443341 B2 JP6443341 B2 JP 6443341B2 JP 2015553515 A JP2015553515 A JP 2015553515A JP 2015553515 A JP2015553515 A JP 2015553515A JP 6443341 B2 JP6443341 B2 JP 6443341B2
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- IIBYPFWXQQDGFC-UHFFFAOYSA-N trimethyl-[2-(2-methylprop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(C)NC(=O)C(C)=C IIBYPFWXQQDGFC-UHFFFAOYSA-N 0.000 description 1
- LMRVIBGXKPAZLP-UHFFFAOYSA-N trimethyl-[2-methyl-2-(prop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(C)(C)NC(=O)C=C LMRVIBGXKPAZLP-UHFFFAOYSA-N 0.000 description 1
- GHVWODLSARFZKM-UHFFFAOYSA-N trimethyl-[3-methyl-3-(prop-2-enoylamino)butyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCC(C)(C)NC(=O)C=C GHVWODLSARFZKM-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Description
本発明の光反射フィルムは基材を有していてもよい。適用可能な基材としては、フィルム支持体であることが好ましく、フィルム支持体は、透明であっても不透明であってもよく、種々の樹脂フィルムを用いることができる。例えば、ポリオレフィンフィルム(ポリエチレン、ポリプロピレン等)、ポリエステルフィルム(ポリエチレンテレフタレート、ポリエチレンナフタレート等)、ポリ塩化ビニル、3酢酸セルロース等を用いることができ、好ましくはポリエステルフィルムである。ポリエステルフィルム(以降ポリエステルと称す)としては、特に限定されるものではないが、ジカルボン酸成分とジオール成分を主要な構成成分とするフィルム形成性を有するポリエステルであることが好ましい。
本発明において、光反射フィルムは、ポリマーを含む高屈折率層および低屈折率層が積層された積層体(ユニット)を少なくとも1つ以上有する反射層を有する。前記高屈折率層と前記低屈折率層とは、以下のように考える。
本明細書において、「高屈折率層」および「低屈折率層」なる用語は、隣接した2層の屈折率差を比較した場合に、屈折率が高い方の屈折率層を高屈折率層とし、低い方の屈折率層を低屈折率層とすることを意味する。したがって、「高屈折率層」および「低屈折率層」なる用語は、光反射フィルムを構成する各屈折率層において、隣接する2つの屈折率層に着目した場合に、各屈折率層が同じ屈折率を有する形態以外のあらゆる形態を含むものである。
低屈折率層及び高屈折率層は必須にポリマー材料を含む。屈折率層を形成するのがポリマー材料であれば、塗布やスピンコートなどの成膜方法が選択可能となる。これらの方法は簡便であり、基材の耐熱性を問わないので選択肢が広く、特に樹脂基材に対して有効な成膜方法といえる。たとえば塗布型ならばロール・ツー・ロール法などの大量生産方式が採用でき、コスト面でもプロセス時間面でも有利になる。また、ポリマー材料を含む膜はフレキシブル性が高いため、生産時や運搬時に巻き取りを行っても、これらの欠陥が発生しづらく、取扱性に優れているという長所がある。
本発明では、別の形態として前記高屈折率層および前記低屈折率層に含まれるポリマーが、ポリビニルアルコール系樹脂を少なくとも1種含有することが好ましい。
本発明では更に高屈折率層及び/または低屈折率層に金属酸化物粒子を含有することが好ましい。
高屈折率層に用いられる金属酸化物粒子としては、例えば、酸化チタン、酸化亜鉛、酸化アルミニウム(アルミナ)、酸化ジルコニウム、酸化ハフニウム、酸化ニオブ、酸化タンタル、酸化マグネシウム、酸化バリウム、酸化インジウム、酸化錫、酸化鉛、これら酸化物より構成される複酸化物であるニオブ酸リチウム、ニオブ酸カリウム、タンタル酸リチウム、アルミニウム・マグネシウム酸化物(MgAl2O4)等の粒子および複合粒子の中で、屈折率が1.6を満たすものが挙げられる。
本発明において、酸化チタン粒子は、酸化チタンゾルの表面を変性して水または有機溶剤等に分散可能な状態にしたものを用いることが好ましい。水系の酸化チタンゾルの調製方法としては、例えば、特開昭63−17221号公報、特開平7−819号公報、特開平9−165218号公報、特開平11−43327号公報、特開昭63−17221号公報等に記載された事項を参照にすることができる。
一般的に、酸化チタン粒子は、粒子表面の光触媒活性の抑制や、溶媒等への分散性を向上する目的で、表面処理が施された状態で使用されることが多く、例えば、酸化チタン粒子表面をシリカからなる被覆層で覆われたシリカ変性酸化チタン粒子、粒子表面が負電荷を帯びたものや、アルミニウム酸化物からなる被覆層が形成されたpH8〜10で表面が正電荷を帯びたものが知られている。
高屈折率層における金属酸化物粒子の含有量としては、高屈折率層の固形分100質量%に対して、赤外遮蔽の観点および曲面形状のガラスにフィルムを適用した場合の色ムラ低減の観点から、20〜80質量%であることが好ましく、30〜70質量%であることがより好ましく、40〜60質量%であることがさらに好ましい。
主に低屈折率層に用いられる金属酸化物粒子としては、金属酸化物粒子として二酸化ケイ素を用いることが好ましく、コロイダルシリカを用いることが特に好ましい。低屈折率層に含まれる金属酸化物粒子(好ましくは二酸化ケイ素)は、その平均粒径が3〜100nmであることが好ましい。一次粒子の状態で分散された二酸化ケイ素の一次粒子の平均粒径(塗布前の分散液状態での粒径)は、3〜50nmであるのがより好ましく、3〜40nmであるのがさらに好ましく、3〜20nmであるのが特に好ましく、4〜10nmであるのがもっとも好ましい。また、二次粒子の平均粒径としては、30nm以下であることが、ヘイズが少なく可視光透過性に優れる観点で好ましい。低屈折率層中の金属酸化物の平均粒径は、粒子そのものあるいは屈折率層の断面や表面に現れた粒子を電子顕微鏡で観察し、1,000個の任意の粒子の粒径を測定し、その単純平均値(個数平均)として求められる。ここで個々の粒子の粒径は、その投影面積に等しい円を仮定したときの直径で表したものである。
本発明の光反射フィルムは、粘着層を有する。粘着層を構成する粘着剤としては、特に制限されず、例えば、アクリル系粘着剤、シリコン系粘着剤、ウレタン系粘着剤、ポリビニルブチラール系粘着剤、エチレン−酢酸ビニル系粘着剤などを例示することができる。
本発明に係る光反射フィルムは、耐擦過性を高めるための表面保護層として、誘電体多層膜の粘着層が形成される側とは反対側の面にハードコート層(以下、単にHC層とも称する)を有する。
本発明に係る光反射フィルムの前記粘着層の弾性率と前記ハードコート層の弾性率は、下記式(1)を満たす。
前記粘着層の弾性率と前記ハードコート層の弾性率とが、上記式(1)を満たし、前記粘着層とガラスとの貼付け時点の即粘着力が2〜8N/25mmであることを満たすことにより、曲面を持つ被着体への密着性を確保しつつ、貼り直しのためにフィルムを被着体から剥がした際に糊残りがなく、再度貼付けが可能であり、耐久性および遮熱性能に優れた光反射フィルムを提供することができる。曲面をもつ被着体への密着性という観点からは、前記式(1)は、ハードコート層の弾性率[Pa]/粘着層の弾性率[Pa]≧3であることが好ましく、ハードコート層の弾性率[Pa]/粘着層の弾性率[Pa]≧4であることがより好ましい。上限は特に規定はないが、曲げガラスへの貼る際の効率を維持でき、また貼った後の剥がれ防止を効果的に維持するためにもハードコート層の弾性率[Pa]/粘着層の弾性率[Pa]≦20、好ましくはハードコート層の弾性率[Pa]/粘着層の弾性率[Pa]≦10である。
また、熱線遮蔽効果の点から、光反射フィルムに熱線遮蔽吸収能を有する熱線遮蔽性微粒子を含有することが好ましい。前記熱線遮蔽性微粒子は、平均粒径が0.2μm以下であることが好ましい。これは熱線遮蔽性微粒子による散乱および吸収により可視光の反射が目立たなくなるためである。前記熱線遮蔽性微粒子としては、Sn、Ti、Si、Zn、Zr、Fe、Al、Cr、Co、Ce、In、Ni、Ag、Cu、Pt、Mn、Ta、W、V、Moの金属、酸化物、窒化物、硫化物あるいはSbやFのドープ物の各単独物もしくはこれらの中から少なくとも2種以上を選択してなる複合物が挙げられ、熱線遮蔽効果の点からはアンチモンドープ酸化スズ(ATO)または酸化インジウムスズ(ITO)であることが好ましい。
本発明の光反射フィルムの製造方法について特に制限はなく、高屈折率層および低屈折率層が交互に積層された積層体を少なくとも1つ形成することができるのであれば、いかなる方法でも用いられうる。
本発明により提供される光反射フィルムは、幅広い分野に応用することができる。例えば、建物の屋外の窓や自動車窓等長期間太陽光に晒らされる設備に貼り合せ、赤外遮蔽効果を付与する赤外遮蔽フィルム等の窓貼用フィルムとして用いることができる。
[光反射フィルム(赤外遮蔽フィルム)の製造]
<反射層1の形成>
米国特許第6049419号に記載の溶融押し出し方法に従い、ポリエチレンナフタレート(PEN)TN8065S(帝人化成社製)とポリメチルメタクリレート(PMMA)樹脂アクリペットVH(三菱レイヨン社製)とを、300℃に溶融し、押出しにより積層し、(PMMA(152nm)/PEN(137nm))64/(PMMA(164nm)/PEN(148nm))64/(PMMA(177nm)/PEN(160nm))64/(PMMA(191m)/PEN(173nm))64となるように縦横約3倍に延伸した後、熱固定、冷却を行って、計256層交互積層した反射層1を得た。ここで、上記層構成において、「(PMMA(152nm)/PEN(137nm))64」とは、膜厚152nmのPMMA、膜厚137nmのPENをこの順に積層したユニットを64個積層させたという意味である。
下記の処方で粘着層塗布液を作製した。
BASF製UV吸収剤 Tinuvin477(固形分80%) 2.1部
イソシアネート系硬化剤 日本ポリウレタン工業製 コロネートL55E(固形分55%) 5部
上記粘着層塗布液をセパレーターSP−PET(銘柄:PET−O2−BU)(三井化学東セロ株式会社製)のシリコン面に対して、コンマコーターにて乾燥膜厚が10μmになるように塗工し、80℃、1分間乾燥し、第2給紙から反射層を形成したフィルムを給紙し、反射層とラミネートして、反射層上に粘着層を形成した。
紫外線硬化性樹脂として、ビームセット577(荒川化学工業株式会社製)を用い、溶媒としてメチルエチルケトンを添加した。さらに、フッ素系界面活性剤(商品名:フタージェント(登録商標)650A、株式会社ネオス製)を0.08質量%添加し、全固形分が40質量部となるように調製して、ハードコート層用塗布液Aを作製した。
実施例1からハードコート層用塗布液を下記塗布液Bに変更した以外は同様にして光反射フィルムを作成した。
赤外線吸収剤としてATO(商品名:SR35M、ANP社製)を用い、紫外線硬化性樹脂として、ビームセット577(荒川化学工業株式会社製)を用い、溶媒としてメチルエチルケトンを添加した。さらに、フッ素系界面活性剤(商品名:フタージェント(登録商標)650A、株式会社ネオス製)を0.08質量%添加し、全固形分が40質量部、およびATOの添加量が全固形分に対して55質量%となるように調製して、ハードコート層用塗布液Bを作製した。
基材としてフィルム支持体を用い、高屈折率層および低屈折率層を以下の構成に変更した以外は実施例2と同様にして光反射フィルムを作成した。
基材2として、ポリエチレンテレフタレートフィルム(A4300、両面易接着層、厚さ:50μm、長さ200m×幅210mm、東洋紡績株式会社製)を準備した。
《低屈折率層用塗布液》
はじめに低屈折率層用塗布液を調製した。具体的には、430部のコロイダルシリカ(10質量%)(スノーテックスOXS;日産化学工業株式会社製)、150部のホウ酸水溶液(3質量%)、85部の水、300部のポリビニルアルコール(4質量%)(JP−45;重合度:4500;ケン化度:88mol%;日本酢ビ・ポバール株式会社製)、3部の界面活性剤(5質量%)(ソフタゾリンLSB−R;川研ファインケミカル株式会社製)、を45℃でこの順に添加した。そして、純水で1000部に仕上げ、低屈折率層用塗布液を調製した。
次に、高屈折率層用塗布液を調製した。具体的には、あらかじめシリカ変性酸化チタン粒子の分散液を調製し、これに溶媒等を添加した。
20層重層塗布可能なスライドホッパー塗布装置を用い、低屈折率層用塗布液および高屈折率層用塗布液を45℃に保温しながら、45℃に加温した基材2上に、21層重層塗布を行った。この際、最下層および最上層は低屈折率層とし、それ以外は低屈折率層および高屈折率層がそれぞれ交互に積層されるように設定した。塗布量については、乾燥時の膜厚が低屈折率層は各層150nm、高屈折率層は各層130nmになるように調節した。なお、前記膜厚は、製造した光反射フィルムを切断し、その切断面を電子顕微鏡により観察することで確認した。この際、2つの層間の界面を明確に観測することができない場合には、XPS表面分析装置により得た層中に含まれるTiO2の厚さ方向のXPSプロファイルにより界面を決定した。
実施例3からハードコート層の照射量を3J/cm2に変更し、粘着層塗布液の硬化剤を5部から7部に変更した以外は同様にして光反射フィルムを作成した。
実施例3から粘着層を以下の記載の通り変更した以外は同様にして光反射フィルムを作成した。
BASF製UV吸収剤 Tinuvin477(固形分80%) 2.1部
信越化学工業製 シランカップリング剤 KBM−403(固形分100%) 0.09部
イソシアネート系硬化剤 日本ポリウレタン工業製 コロネートL55E(固形分55%) 0.5部
(実施例6)
実施例3から粘着層を以下の記載の通り変更した以外は同様にして作成した。
BASF製UV吸収剤 Tinuvin477(固形分80%) 2.1部
イソシアネート系硬化剤 日本ポリウレタン工業製 コロネートL55E(固形分55%) 0.5部
(比較例1)
実施例1から粘着層を以下の記載の通り変更した以外は同様にして光反射フィルムを作成した。
酢酸エチル 121.6部
T−477(トリアジン系UV吸収剤) 3.15部(濃度80%)
KBM403(シランカップリング剤) 0.90部(濃度10%)
コロネートL55E(トリレンジイソシアネート) 5部(濃度55%)
(比較例2)
実施例3から粘着層を比較例1の記載の通り変更した以外は同様にして光反射フィルムを作成した。
特開2007−232931の実施例1に記載の近赤外線吸収層をPET上に設け反対側に、実施例1の粘着層を作製し、光反射フィルムを作製した。
ガラス基材上に、ハードコート層塗布液、粘着層塗布液、をそれぞれ単独で塗布して乾燥時膜厚2μmの各々のサンプルを作製し、ナノインデンテーション法(セイコーインスツルメンツ社製、走査型プローブ顕微鏡 SPI3800Nに、HYSITRON社製、TriboScopeを装着した装置、圧子は90°Cube corner tip、最大荷重を20μN)で測定した。測定数n=3とし、弾性率の単位はPaとして、測定値の平均値を求めた。結果を下記の表1に示す。
粘着力の測定はJIS A5759 6.8.1に基づき測定を行った。水洗いし、アルコールで脱脂したフロート板ガラスに、短冊状(幅25mm×長さ30cm)の光反射フィルムを設置し、圧着ローラを用いて毎分約300mmの早さで1往復させて圧着した。引っ張り試験機(東洋精機株式会社製)を用いて当該サンプルを180度引きはがし試験により、粘着力(即粘着力)を求めた。結果を下記の表1に示す。
<赤外透過率>
分光光度計(積分球使用、日立製作所社製、U−4000型)を用い、各赤外遮蔽フィルム試料の300nm〜2000nmの領域における赤外透過率(800〜1300nm)を測定した。結果を下記の表1に示す。
作成した光反射フィルムを曲面ガラス(曲率半径3m以下)に水貼りし、目視により外観を以下の評価基準に従って評価した。結果を下記の表1に示す。
○:問題なく綺麗に貼れた
△:端部の一部にしわがみられた
×:しわが数か所見られた。
作成した光反射フィルムを曲面ガラス(曲率半径3m以下)に水貼りし、25℃、50%RHの条件で3ヶ月放置後、23℃、50%RHの条件で以下の評価基準に従って3カ月後の密着性及び外観を評価した。結果を下記の表1に示す。
○:問題なし
△:端部が一部浮きあがっている
×:端部に剥がれがみられた。
作成した光反射フィルムを曲面ガラス(曲率半径3m以下)に水貼りし、25℃、50%RHの条件で7日間放置後、23℃、50%RHの条件で引っ張り試験機(東洋精機株式会社製)を用いて引っ張り試験を行い、以下の評価基準に従って粘着力を評価した。結果を下記の表1に示す。
○:粘着力が2N以上、糊残りなし
△:粘着力が2N以上、糊が僅かに残る
×:粘着力が2N未満で糊が全面に残る。
JISB7753に規定するサンシャインウェザーメーター(スガ試験機(製)S80)を用いてブラックパネル温度計63℃、相対湿度50%、1サイクル2時間、1サイクル中18分間降雨という条件下で3000時間後の密着性を、以下の評価基準に従って評価した。
○:問題なし
△:端部が一部浮きあがっている
×:端部に剥がれがみられた。
11 基材、
12 下引層、
13 反射層、
14 低屈折率層、
15 高屈折率層、
16 ハードコート層、
17 透明接着層、
18 基体、
L 太陽光。
Claims (8)
- ポリマーを含む高屈折率層とポリマーを含む低屈折率層とが積層されてなる積層体を少なくとも1つ以上有する反射層と、
一方の最外層に配置される粘着層と、
他方の最外層に配置されるハードコート層と、を含む光反射フィルムにおいて、
前記粘着層の弾性率と前記ハードコート層の弾性率とが下記式(1)を満たし、
前記粘着層とガラスとの貼付け時点の即粘着力が2〜8N/25mmであることを特徴とする、光反射フィルム。
式(1)ハードコート層の弾性率[Pa]/粘着層の弾性率[Pa]≧3 - 貼付け時点の前記粘着層とガラスとの即粘着力が4〜8N/25mmであり、
貼付け状態のまま、30℃、湿度60%RHの条件で1週間放置した時点の前記粘着層とガラスとの経時粘着力が7〜15N/25mmであることを特徴とする、請求項1に記載の光反射フィルム。 - 前記経時粘着力が10〜15N/25mmであることを特徴とする請求項2に記載の光反射フィルム。
- 前記高屈折率層および前記低屈折率層に含まれるポリマーが、ポリエステル、ポリカーボネートおよびポリ(メタ)アクリレートからなる群から選択される少なくとも1種を含むことを特徴とする請求項1〜3のいずれか1項に記載の光反射フィルム。
- 前記高屈折率層および前記低屈折率層に含まれるポリマーが、ポリビニルアルコール系樹脂を少なくとも1種含有することを特徴とする請求項1〜4のいずれか1項に記載の光反射フィルム。
- 前記ハードコート層が熱線遮蔽性微粒子を含有することを特徴とする請求項1〜5のいずれか1項に記載の光反射フィルム。
- 請求項1〜6のいずれか1項に記載の光反射フィルムを光透過性基体に貼り付けた光反射体。
- 前記光透過性基体が曲面を有する、請求項7に記載の光反射体。
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