JP4960601B2 - Light diffusion plate film - Google Patents

Light diffusion plate film Download PDF

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JP4960601B2
JP4960601B2 JP2005110115A JP2005110115A JP4960601B2 JP 4960601 B2 JP4960601 B2 JP 4960601B2 JP 2005110115 A JP2005110115 A JP 2005110115A JP 2005110115 A JP2005110115 A JP 2005110115A JP 4960601 B2 JP4960601 B2 JP 4960601B2
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film
biaxially oriented
oriented polyester
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temperature
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JP2006292838A (en
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誉之 渡部
淳 小山松
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Teijin DuPont Films Japan Ltd
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本発明は、液晶表示装置に用いる光拡散板用フィルムに関する。   The present invention relates to a light diffusion plate film used in a liquid crystal display device.

近年TV受像機として液晶ディスプレイが多く流通するようになってきた。液晶ディスプレイは、ディスプレイ内に液晶素子の背後に設置された光源からの光を反射するための光拡散板を備える。液晶ディスプレイを高輝度化するためには、光量を増加させる必要があり、通常は光源から発生する熱を受けて光拡散板にたわみが発生する。このたわみが原因で、液晶ディスプレイの画面全体に輝度斑が生じる。
この問題について従来から解決が期待されており、大画面化による輝度斑問題を改善する手段の一つとして、例えば熱膨張係数の低いフィルムを用いることが提案されている。
In recent years, many liquid crystal displays have been distributed as TV receivers. The liquid crystal display includes a light diffusing plate for reflecting light from a light source installed behind the liquid crystal element in the display. In order to increase the brightness of the liquid crystal display, it is necessary to increase the amount of light. Usually, the light diffusing plate bends due to heat generated from the light source. Due to this deflection, luminance spots appear on the entire screen of the liquid crystal display.
Conventionally, a solution to this problem has been expected, and as one of means for improving the luminance unevenness problem due to the enlargement of the screen, for example, the use of a film having a low coefficient of thermal expansion has been proposed.

特開2001−220432号公報JP 2001-220432 A 特開2001−247696号公報JP 2001-247696 A 特開2002−019064号公報JP 2002-019064 A 特開2002−350617号公報JP 2002-350617 A 特開2003−266622号公報JP 2003-266622 A 特開2004−067853号公報JP 2004-067853 A 特開2004−133021号公報JP 2004-133021 A

しかし、上記の従来の技術のみでは、光拡散板のたわみを抑制するためには未だに不十分であり、フィルムのMD方向とTD方向とでの熱収縮率と屈折率のバランスが悪く、熱膨張係数が十分に低くても比較的湿度の高い条件で使用するとたわみが発生してしまう。   However, the above conventional technology alone is still insufficient to suppress the deflection of the light diffusion plate, the balance between the thermal shrinkage rate and the refractive index in the MD direction and the TD direction of the film is poor, and the thermal expansion Even if the coefficient is sufficiently low, deflection occurs when used under relatively high humidity conditions.

本発明の目的は、湿熱による耐たわみ特性に優れ、液晶表示装置の高輝度化が可能な、液晶表示装置に用いる光拡散板用のフィルムを提供することにある。   An object of the present invention is to provide a film for a light diffusing plate used in a liquid crystal display device, which has excellent deflection resistance due to wet heat and can increase the brightness of the liquid crystal display device.

すなわち本発明は、熱固定後の二軸配向ポリエステルフィルムに対して、該二軸配向ポリエステルフィルムを構成するポリエステルのガラス転移温度(Tg)−40℃からTgの範囲の温度で30分間〜72時間の間40〜90%RHの湿度でオフアニール処理を行って得られる、湿熱たわみ率が20%未満の二軸配向ポリエステルフィルムからなる光拡散板用フィルムである。なお、湿熱たわみ率は、本明細書の実施例の欄に定義される方法を用いて測定される数値である。 That is, in the present invention, the glass transition temperature (Tg) of the polyester constituting the biaxially oriented polyester film is 30 minutes to 72 hours at a temperature in the range of −40 ° C. to Tg with respect to the biaxially oriented polyester film after heat setting. It is a film for a light diffusion plate made of a biaxially oriented polyester film having a wet heat deflection rate of less than 20% , which is obtained by performing an off-annealing treatment at a humidity of 40 to 90% RH . The wet heat deflection rate is a numerical value measured using the method defined in the example column of this specification.

本発明によれば、湿熱による耐たわみ特性に優れ、液晶表示装置の高輝度化が可能な光拡散板として有用なポリエステルフィルムを提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the polyester film useful as a light-diffusion board which is excellent in the bending-proof characteristic by wet heat and can raise the brightness | luminance of a liquid crystal display device can be provided.

以下、本発明を詳細に説明する。
本発明において二軸配向ポリエステルの湿熱たわみ率は20%未満であることが肝要である。たわみ率20%未満である光拡散板用ポリエステルフィルムは従来知られていないものであるが、このたわみ率はポリエステルフィルムを二軸延伸により製膜した後に、後述の条件にてオフアニールすることによって得ることができる。
Hereinafter, the present invention will be described in detail.
In the present invention, it is important that the wet heat deflection rate of the biaxially oriented polyester is less than 20%. A polyester film for a light diffusing plate having a deflection rate of less than 20% is not conventionally known, but this deflection rate is obtained by forming a polyester film by biaxial stretching and then performing off-annealing under the conditions described later. Obtainable.

[ポリエステル]
本発明において、二軸配向フィルムを構成するポリエステルとしては、ポリエチレンテレフタレートを用いる。このポリエチレンテレフタレートは、ホモポリマーであってもよく、共重合成分を含むコポリマーでもよいが、ホモポリマーが好ましい。
[polyester]
In the present invention, polyethylene terephthalate is used as the polyester constituting the biaxially oriented film. The polyethylene terephthalate may be a homopolymer or a copolymer containing a copolymer component, but a homopolymer is preferred.

コポリマーである場合、エチレンテレフタレートの繰返し単位が、全繰返し単位の好ましくは90モル%以上、さらに好ましくは95モル%以上を占めるポリマーを用いる。共重合成分の割合が10モル%を超えると、フィルムの光線透過率が低下し、また熱安定性や寸法安定性が低下して好ましくない。   In the case of a copolymer, a polymer in which the repeating unit of ethylene terephthalate accounts for preferably 90 mol% or more, more preferably 95 mol% or more of all repeating units is used. When the proportion of the copolymer component exceeds 10 mol%, the light transmittance of the film is lowered, and thermal stability and dimensional stability are lowered, which is not preferable.

ポリエチレンテレフタレートの固有粘度(オルソクロロフェノール中35℃での測定値から算出)は、好ましくは0.4以上、さらに好ましくは0.5〜1.2、特に好ましくは0.55〜0.85である。0.4未満であるとフィルムの機械的強度が低下して好ましくない。固有粘度が1.2を超えると押出し機の負担が増大し、樹脂が発熱して重合度が低下するので好ましくない。   The intrinsic viscosity of polyethylene terephthalate (calculated from the measured value in orthochlorophenol at 35 ° C.) is preferably 0.4 or more, more preferably 0.5 to 1.2, and particularly preferably 0.55 to 0.85. is there. If it is less than 0.4, the mechanical strength of the film is lowered, which is not preferable. An intrinsic viscosity exceeding 1.2 is not preferable because the burden on the extruder increases, the resin generates heat, and the degree of polymerization decreases.

ポリエチレンテレフタレートは、例えばテレフタル酸とエチレングリコールとを重縮合反応させる方法、テレフタル酸の低級アルキルエステルとエチレングリコールとをエステル交換反応させた後重縮合反応させる方法、テレフタル酸のビスグリコールエステルを重縮合させる方法等の方法によって製造することができる。重縮合反応に使用する触媒としては、アンチモン化合物(Sb化合物)、チタン化合物(Ti化合物)、ゲルマニウム化合物(Ge化合物)などが挙げられる。   Polyethylene terephthalate, for example, polycondensation reaction of terephthalic acid and ethylene glycol, polycondensation reaction after transesterification of lower alkyl ester of terephthalic acid and ethylene glycol, polycondensation of bisglycol ester of terephthalic acid It can manufacture by methods, such as the method of making it. Examples of the catalyst used for the polycondensation reaction include an antimony compound (Sb compound), a titanium compound (Ti compound), a germanium compound (Ge compound), and the like.

[滑剤]
本発明における二軸配向ポリエステルフィルムは、その生産性を確保するために、表面に多数の微細突起を有していることが好ましい。微細突起をフィルムに付与するためには、ポリエステルフィルム中に滑剤として不活性粒子を分散含有させるか、ポリステルフィルムのうえに不活性粒子を含有する易滑層を設ければよい。微細突起を有することにより優れた易滑性を得ることができる。
[Lubricant]
The biaxially oriented polyester film in the present invention preferably has a large number of fine protrusions on the surface in order to ensure the productivity. In order to impart fine protrusions to the film, inert particles may be dispersed and contained as a lubricant in the polyester film, or an easy-sliding layer containing inert particles may be provided on the polyester film. Excellent slipperiness can be obtained by having fine protrusions.

不活性粒子としては、炭酸カルシウム、炭酸マグネシウム、酸化カルシウム、酸化亜鉛、酸化マグネシウム、酸化ケイ素、ケイ酸ソーダ、水酸化アルミニウム、酸化鉄、酸化ジルコニウム、硫酸バリウム、酸化チタン、酸化錫、三酸化アンチモン、カーボンブラック、二硫化モリブデン等の無機微粒子、アクリル系架橋重合体、スチレン系架橋重合体、架橋シリコーン樹脂、フッ素樹脂、ベンゾグアナミン樹脂、フェノール樹脂、ナイロン樹脂等の有機微粒子を例示することができる。   Inactive particles include calcium carbonate, magnesium carbonate, calcium oxide, zinc oxide, magnesium oxide, silicon oxide, sodium silicate, aluminum hydroxide, iron oxide, zirconium oxide, barium sulfate, titanium oxide, tin oxide, and antimony trioxide. Examples thereof include inorganic fine particles such as carbon black and molybdenum disulfide, and organic fine particles such as acrylic cross-linked polymers, styrene cross-linked polymers, cross-linked silicone resins, fluororesins, benzoguanamine resins, phenol resins, and nylon resins.

不活性粒子の平均粒径は好ましくは50〜150nmである。50nm未満であると易滑性が発現せず、150nmを超えると抜け落ちが発生して好ましくない。不活性粒子の比重は好ましくは3以下である。3を超えると水分散液中で沈降して生産工程上不都合であり好ましくない。   The average particle size of the inert particles is preferably 50 to 150 nm. If the thickness is less than 50 nm, the slipperiness does not appear, and if it exceeds 150 nm, the slipping off occurs, which is not preferable. The specific gravity of the inert particles is preferably 3 or less. If it exceeds 3, it precipitates in the aqueous dispersion, which is inconvenient in the production process and is not preferred.

不活性粒子の配合量は、フィルム中に含有させる場合には、ポリエステル100重量部あたり例えば0.0025〜0.036重量部、好ましくは0.0025〜0.012重量部である。易滑層を設けて易滑層中に含有させる場合には、易滑層を構成する組成物100重量部あたり好ましくは5〜30重量%である。なお、平均粒径が100〜150nmの不活性粒子を用いるときには5〜10重量%の範囲で、平均粒径が50〜90nmの不活性粒子を用いるときには8〜30重量%の範囲で用いるとよい。この平均粒径は、一次粒子の平均粒径であり、透過電子顕微鏡による10万倍の拡大写真で観察できる一次粒子の像をトレース又は投影して画像解析装置により面積円相当直径として求めた平均粒径である。   When the inert particles are incorporated in the film, the amount is, for example, 0.0025 to 0.036 parts by weight, preferably 0.0025 to 0.012 parts by weight per 100 parts by weight of the polyester. When providing a slippery layer and making it contain in a slippery layer, Preferably it is 5 to 30 weight% per 100 weight part of compositions which comprise a slippery layer. In addition, when using an inert particle with an average particle diameter of 100-150 nm, it is good to use in the range of 5-10 weight%, and when using an inert particle with an average particle diameter of 50-90 nm, it is good to use in the range of 8-30 weight%. . This average particle diameter is an average particle diameter of primary particles, and is an average obtained by tracing or projecting an image of primary particles that can be observed with a magnified photograph at a magnification of 100,000 by a transmission electron microscope to obtain an area equivalent circle diameter by an image analyzer. The particle size.

[湿熱たわみ率]
本発明において二軸配向ポリエステルフィルムは、湿熱たわみ率が20%未満、好ましくは15%以下である。湿熱たわみ率が20%以上であると、液晶ディスプレイにて光拡散板として長時間使用するとバックライトからの熱によりたわみが発生する。また、湿熱たわみ率が20%以上であると輝度斑の原因となり液晶ディスプレイの品位が損なわれる。なお、湿熱たわみ率は実施例のたわみ率の項に記載のとおり定義される。
[Heat heat deflection rate]
In the present invention, the biaxially oriented polyester film has a wet heat deflection rate of less than 20%, preferably 15% or less. When the wet heat deflection rate is 20% or more, when used as a light diffusing plate in a liquid crystal display for a long time, deflection occurs due to heat from the backlight. Further, if the wet heat deflection rate is 20% or more, it causes brightness spots and the quality of the liquid crystal display is impaired. The wet heat deflection rate is defined as described in the section of the deflection rate in the examples.

[屈折率]
二軸配向ポリエステルフィルムのMD方向の屈折率とTD方向の屈折率の差の絶対値は、好ましくは0.01以下、さらに好ましくは0.008以下、特に好ましくは0.006以下である。差の絶対値が0.01を超えると温度がかかったときのMDとTDの挙動に著しい差が生じるためバランスが崩れたわみが生じやすくなる。たわみが発生すると液晶画面に輝度斑が発生し品位が著しく損なわれるため好ましくない。
なお、MDはフィルムの縦方向であり、TDはMDと直交する方向である。
[Refractive index]
The absolute value of the difference between the refractive index in the MD direction and the refractive index in the TD direction of the biaxially oriented polyester film is preferably 0.01 or less, more preferably 0.008 or less, and particularly preferably 0.006 or less. If the absolute value of the difference exceeds 0.01, a remarkable difference is caused in the behavior of MD and TD when the temperature is applied, so that the balance is easily lost. Deflection is not preferable because luminance spots appear on the liquid crystal screen and the quality is significantly impaired.
MD is the longitudinal direction of the film, and TD is the direction orthogonal to the MD.

[熱収縮率]
二軸配向ポリエステルフィルムは、150℃30分間の条件でのMD方向の熱収縮率とTD方向の熱収縮率の差の絶対値が、好ましくは0.5以下、さらに好ましくは0.4以下、特に好ましくは0.3以下である。差の絶対値が0.5を超えると、温度がかかったときにフィルムのバランスが崩れたわみが生じやすくなる。たわみが発生すると液晶画面に輝度斑が発生し品位が著しく損なわれるため好ましくない。
[Heat shrinkage]
In the biaxially oriented polyester film, the absolute value of the difference between the thermal shrinkage rate in the MD direction and the thermal shrinkage rate in the TD direction at 150 ° C. for 30 minutes is preferably 0.5 or less, more preferably 0.4 or less, Especially preferably, it is 0.3 or less. If the absolute value of the difference exceeds 0.5, the film tends to be out of balance when the temperature is applied. Deflection is not preferable because luminance spots appear on the liquid crystal screen and the quality is significantly impaired.

[厚み]
二軸配向ポリエステルフィルムの厚みは、好ましくは20〜300μm、さらに好ましくは20〜250μm、特に好ましくは25〜200μmである。厚みが20μm未満であると腰が弱く加工時に平面性が失われたり、傷が生じたりし易く好ましくない。厚みが300μmを超えると腰が強すぎて加工作業性が悪く、透明性が低下して好ましくない。
[Thickness]
The thickness of the biaxially oriented polyester film is preferably 20 to 300 μm, more preferably 20 to 250 μm, and particularly preferably 25 to 200 μm. If the thickness is less than 20 μm, the waist is weak and flatness is lost during processing, and scratches are liable to occur. If the thickness exceeds 300 μm, the waist is too strong, the workability is poor, and the transparency is lowered, which is not preferable.

[ヘイズ]
二軸配向ポリエステルフィルムのヘイズ値は、好ましくは3%以下、さらに好ましくは2%以下、特に好ましくは1.5%以下である。ヘイズ値が3%を超えると、光拡散板に要求される輝度が得られず好ましくない。
[Haze]
The haze value of the biaxially oriented polyester film is preferably 3% or less, more preferably 2% or less, and particularly preferably 1.5% or less. If the haze value exceeds 3%, the luminance required for the light diffusion plate cannot be obtained, which is not preferable.

[色相]
二軸配向ポリエスエルフィルムは、L*a*b*表色系におけるb*値が、好ましくは−1以上1.5以下、さらに好ましくは−0.5以上1.5以下、特に好ましくは−0.5以上1.3以下である。b*値が−1未満であると青みを帯び、1を超えると黄みを帯びていずれも液晶モニターには好ましくない。
[Hue]
In the biaxially oriented polyester film, the b * value in the L * a * b * color system is preferably −1 or more and 1.5 or less, more preferably −0.5 or more and 1.5 or less, and particularly preferably − 0.5 or more and 1.3 or less. When the b * value is less than −1, the color is bluish, and when it exceeds 1, the color is yellowish.

[製造方法]
本発明における二軸配向ポリエステルフィルムの上述の物性は、ポリエステルフィルムを二軸延伸法にて製膜の後、オフアニール処理することにより達成することができる。
[Production method]
The above-mentioned physical properties of the biaxially oriented polyester film in the present invention can be achieved by subjecting the polyester film to a biaxial stretching method and then an off-annealing treatment.

オフアニールに供する二軸配向ポリエステルフィルム自体は、従来より公知の二軸配向フィルムの製造方法により製造することができる。例えば、逐次二軸延伸法、同時二軸延伸法、インフレーション法によって製造することができる。これらのうち逐次二軸延伸法が好ましい。   The biaxially oriented polyester film itself subjected to off-annealing can be produced by a conventionally known method for producing a biaxially oriented film. For example, it can be produced by a sequential biaxial stretching method, a simultaneous biaxial stretching method, and an inflation method. Of these, the sequential biaxial stretching method is preferred.

逐次二軸延伸法により二軸配向ポリエステルフィルムを製造するためには、例えば次のようにすればよい。先ず、必要に応じて不活性粒子を配合したポリエステルを、ダイを通して溶融押出し、予め20〜40℃程度に設定されたキャスティングドラム上にて急冷固化させて未延伸フィルムを得る。未延伸フィルムは、その後、延伸温度90〜140℃にて、フィルム走行方向(縦方向)に3.0〜4.5倍、これと直角方向(横方向)に3.0〜4.5倍、面積倍率で9〜20倍に延伸する。   In order to produce a biaxially oriented polyester film by the sequential biaxial stretching method, for example, the following may be performed. First, polyester blended with inert particles as necessary is melt-extruded through a die and rapidly cooled and solidified on a casting drum set to about 20 to 40 ° C. to obtain an unstretched film. The unstretched film is then stretched at 90 to 140 ° C., 3.0 to 4.5 times in the film running direction (longitudinal direction), and 3.0 to 4.5 times in the direction perpendicular to the film (lateral direction) The film is stretched 9 to 20 times in area magnification.

本発明においては、二軸延伸後、フィルムを熱固定することが好ましい。熱固定温度は、好ましくは180〜235℃、さらに好ましくは180〜225℃、特に好ましくは180〜220℃である。熱固定温度が235℃を超えると、ポリエステルが結晶化しすぎて全光線透過率が低下することがあり好ましくない。180℃未満では熱収縮率のMD・TDのバランスが崩れ、たわみが抑制できないことがあり好ましくない。   In the present invention, the film is preferably heat-set after biaxial stretching. The heat setting temperature is preferably 180 to 235 ° C, more preferably 180 to 225 ° C, and particularly preferably 180 to 220 ° C. When the heat setting temperature exceeds 235 ° C., the polyester is excessively crystallized, and the total light transmittance may be lowered. If it is less than 180 degreeC, the balance of MD * TD of a thermal contraction rate will collapse | crumble and a deflection may not be suppressed and it is unpreferable.

ヘイズ値は、主としてポリエステルフィルム中の不活性粒子の種類、平均粒径、含有量、粒子周辺に生じるボイドの程度や、易接着層に含有される不活性粒子の種類、平均粒径、含有量によって変わるので、これらを調整することで所望のヘイズ値を満たすようにすればよい。   The haze value is mainly the type of inert particles in the polyester film, the average particle size, the content, the degree of voids generated around the particles, the type of inert particles contained in the easy adhesion layer, the average particle size, the content. Therefore, it is only necessary to adjust these so as to satisfy a desired haze value.

本発明の物性を備える二軸配向ポリエステルフィルムを得るためには、熱固定後の二軸配向ポリエステルフィルムに対して、さらにオフアニール処理を行なう。すなわち、上記の方法で製膜して得た二軸配向ポリエステルフィルムに対して、フィルムのポリエステルのガラス転移温度(Tg)−40℃からTgの範囲の温度で30分間〜72時間の間40〜90%Rの湿度で熱処理する。これを本明細書ではオフアニール処理という。このときフィルムのTg以上の温度で熱処理するとフィルムが熱で変形してしまい光拡散板に必要な平面性が失われてしまう。熱処理する温度がTg−40℃より低いとフィルム内の残存応力を緩和することができず、オフアニール処理の効果が得られない。 In order to obtain a biaxially oriented polyester film having the physical properties of the present invention, an off-annealing treatment is further performed on the biaxially oriented polyester film after heat setting. That is, with respect to the biaxially oriented polyester film obtained by film formation by the above method, the glass transition temperature (Tg) of the polyester of the film is from 40 ° C. to Tg for 30 minutes to 72 hours for 40 to 40 hours. treated at a humidity of 90% R H. This is referred to as off-annealing in this specification. At this time, if the heat treatment is performed at a temperature equal to or higher than the Tg of the film, the film is deformed by heat and the flatness necessary for the light diffusion plate is lost. If the heat treatment temperature is lower than Tg−40 ° C., the residual stress in the film cannot be relaxed, and the effect of off-annealing treatment cannot be obtained.

以下、実施例を挙げて本発明をさらに詳細に説明する。
なお、「部」は重量部を意味する。また、各特性値の測定方法は下記の通りである。
Hereinafter, the present invention will be described in more detail with reference to examples.
“Parts” means parts by weight. Moreover, the measuring method of each characteristic value is as follows.

(1)フィルムの厚み
外付マイクロメータで100点測定し、この平均値を求めてフィルムの厚みとした。
(1) Film thickness 100 points were measured with an external micrometer, and the average value was obtained as the film thickness.

(2)屈折率
製膜したフィルムを、アッベ屈折率計(D線589nm)で測定した。MD方向の屈折率をnMD、TD方向の屈折率をnTDとした。
(2) Refractive index The film formed was measured with an Abbe refractometer (D line 589 nm). The refractive index in the MD direction was n MD , and the refractive index in the TD direction was n TD .

(3)熱収縮率
フィルムのサンプルを150℃の温度に30分間おいたときの熱収縮率を、JIS−Z1709に従い測定して、各々N=3の平均値をとった。なお、MD方向はフィルムの縦方向、TDはMDと直交する方向である。
(3) Heat Shrinkage The heat shrinkage when a film sample was placed at a temperature of 150 ° C. for 30 minutes was measured according to JIS-Z1709, and each average value of N = 3 was taken. The MD direction is the longitudinal direction of the film, and TD is the direction orthogonal to the MD.

(4)ヘイズ
日本電色工業社製のへイズ測定器(NDH−2000)を使用してJISK−7136に基づきフィルムのへイズを測定した。
(4) Haze The haze of the film was measured based on JISK-7136 using the Nippon Denshoku Industries Co., Ltd. haze measuring device (NDH-2000).

(5)易接着性塗膜の厚み
サンプルをオスミウム酸にて染色し、エポキシ樹脂に包埋し、ミクロトームにてフィルム端面がきれいに見えるように100nm厚でスライスしたサンプルを透過電子顕微鏡(日本電子製JEM−1200EX)を用いて、易接着層をクローズアッププするように5〜10万倍の倍率で観察し、任意の個所100個所について測定し、算術平均した厚みを採用した。
(5) Thickness of easy-adhesive coating film Samples were dyed with osmic acid, embedded in epoxy resin, and sliced with a thickness of 100 nm so that the film end face could be seen with a microtome. Transmission electron microscope (manufactured by JEOL Ltd.) JEM-1200EX) was used, observed at a magnification of 5 to 100,000 times so as to close up the easy-adhesion layer, measured at 100 arbitrary positions, and an arithmetically averaged thickness was adopted.

(6)湿熱たわみ率
湿熱たわみ率は以下の方法にて求めた。フィルムからサンプルを24×24cmの大きさに切り出し、図1のように2cm間隔で格子状に線を引いた。このサンプルの4辺を、ガラス板に両面粘着テープで固定した。ガラス板としては、ガラス面とフィルムの貼り付き防止のために、表面がサンドマット処理してあるものを使用した。粘着テープで固定される位置は、フィルムの端でその幅は各辺1cmとした。固定の様子を図1に示す。この状態で、サンプルを温度60℃、相対湿度90%RHの恒温恒湿オーブンに1時間放置した。その後、オーブンから取り出して室温にて1時間放置し、フィルムの状態が安定したところで、フィルムのたわみ具合を目視で観察し、下記の基準で湿熱たわみ率を求めた。
(6) Moisture heat deflection rate The moisture heat deflection rate was determined by the following method. Samples were cut out from the film into a size of 24 × 24 cm, and lines were drawn in a lattice pattern at intervals of 2 cm as shown in FIG. Four sides of this sample were fixed to a glass plate with a double-sided adhesive tape. As the glass plate, a glass plate having a surface subjected to sand mat treatment was used in order to prevent the glass surface and the film from sticking to each other. The position fixed with the adhesive tape was the edge of the film, and the width was 1 cm on each side. The fixed state is shown in FIG. In this state, the sample was left in a constant temperature and humidity oven at a temperature of 60 ° C. and a relative humidity of 90% RH for 1 hour. Thereafter, the film was taken out from the oven and allowed to stand at room temperature for 1 hour. When the state of the film was stabilized, the degree of deflection of the film was visually observed, and the wet heat deflection rate was determined according to the following criteria.

[湿熱たわみ率の求め方]
ガラス板に固定したサンプルに蛍光灯の照明を反射させ、以下の規則にしたがって、たわんでいる20mm×20mmのますの個数を数えた。
1)反射した蛍光灯の光が、フィルムのたわみで歪んでいて、かつガラス板からフィルムが浮いている20mm×20mmのます → ×
2)ガラス板からフィルムは浮いていないが、反射した蛍光灯の光がフィルムのたわみで歪んでみえる20mm×20mmのます → ×
3)反射した蛍光灯が歪んではいないものの、ガラス板から浮き上がっている20mm×20mmのます → △
4)反射した蛍光灯の光が歪まず、ガラス板から浮き上がってもいない20mm×20mmのます → ○
それぞれ×は1個、△は0.5個とカウントした。たわんでいる20mm×20mmのますの合計数を、ます全部の個数100(端は粘着テープで固定しているため除く)で割ってたわみ率を求めた。
たわみ率 = たわんだます(個)/100(個)×100(%)
○:20%未満(良好)
×:20%以上(不良)
この実験をn=5実施し、その算術平均を結果とした。
[How to determine the heat-heat deflection rate]
The sample fixed to the glass plate was reflected by the fluorescent light, and the number of bent 20 mm × 20 mm was counted according to the following rules.
1) The reflected fluorescent light is distorted by the deflection of the film, and the film floats from the glass plate.
2) Although the film is not lifted from the glass plate, the reflected fluorescent lamp light appears to be distorted by the deflection of the film.
3) Although the reflected fluorescent lamp is not distorted, it is 20 mm x 20 mm raised from the glass plate → △
4) The light of the reflected fluorescent light is not distorted and is not lifted off the glass plate.
Each x was counted as 1 and Δ was counted as 0.5. The total number of flexures of 20 mm × 20 mm bent was divided by the total number of 100 (excluding because the ends were fixed with adhesive tape) to obtain the deflection rate.
Deflection rate = Deflection (pieces) / 100 (pieces) x 100 (%)
○: Less than 20% (good)
×: 20% or more (defect)
This experiment was performed with n = 5, and the arithmetic average was taken as the result.

[実施例1]
ジメチルテレフタレート96部、エチレングリコール58部及び酢酸マンガン0.038部を夫々反応器に仕込み、攪拌下内温が240℃になるまでメタノールを留出せしめながらエステル交換反応を行い、該エステル交換反応が終了したのちトリメチルホスフェート0.097部及び三酸化アンチモン0.041部を添加した。引き続いて反応生成物を昇温し、最終的に高真空下280℃の条件で重縮合を行って固有粘度([η])0.64のポリエステルチップを得た。
[Example 1]
96 parts of dimethyl terephthalate, 58 parts of ethylene glycol and 0.038 part of manganese acetate were charged into the reactor, respectively, and the ester exchange reaction was conducted while distilling methanol until the internal temperature reached 240 ° C. with stirring. After completion, 0.097 parts of trimethyl phosphate and 0.041 parts of antimony trioxide were added. Subsequently, the temperature of the reaction product was raised, and finally, polycondensation was performed under a high vacuum condition at 280 ° C. to obtain a polyester chip having an intrinsic viscosity ([η]) of 0.64.

上記ポリエステルチップを160℃で3時間乾燥したのち、280℃で溶融押出し、20℃に保持した冷却ドラム上で急冷固化せしめ未延伸フィルムを得た。この未延伸フィルムを95℃で縦方向に3.6倍に延伸し、次いで下面、さらに上面に下記の塗剤P(塗布液)を乾燥後の厚みが0.06μmになるように塗布し、120℃で横方向に3.6倍に延伸したのち、熱固定温度220℃で熱処理し、厚みが100μmの二軸配向フィルムを得た。   The polyester chip was dried at 160 ° C. for 3 hours, melt-extruded at 280 ° C., and rapidly cooled and solidified on a cooling drum maintained at 20 ° C. to obtain an unstretched film. This unstretched film was stretched 3.6 times in the longitudinal direction at 95 ° C., and then the following coating agent P (coating liquid) was applied on the lower surface and further on the upper surface so that the thickness after drying was 0.06 μm, The film was stretched 3.6 times in the transverse direction at 120 ° C. and then heat-treated at a heat setting temperature of 220 ° C. to obtain a biaxially oriented film having a thickness of 100 μm.

得られた二軸配向フィルムを、240mm×240mmの大きさに裁断した。このフィルムを各フィルム同士の貼り付きを防止するためにテフロン(登録商標)シートに包んでつるした。この状態で75℃、50%R、1時間の条件でオフアニール処理した。得られたフィルムの物性を表1および2に示す。 The obtained biaxially oriented film was cut into a size of 240 mm × 240 mm. This film was hung by being wrapped in a Teflon (registered trademark) sheet in order to prevent sticking between the films. In this state, off-annealing treatment was performed under conditions of 75 ° C., 50% R H , and 1 hour. The physical properties of the obtained film are shown in Tables 1 and 2.

[塗剤P]
(P成分1)共重合ポリエステル樹脂(Tg:68℃) 60重量%。
酸成分:テレフタル酸(90mol%)、イソフタル酸(6mol%)、5―スルホイソフタル酸カリウム(4mol%)。
グリコール成分:エチレングリコール(95mol%)、ネオペンチレングリコール(5mol%)。
(P成分2)N,N’―エチレンビスカプリル酸アミド 5重量%。
(P成分3)アクリル共重合体(数平均分子量:248,000)20重量%。
組成:メチルアクリレート(65mol%)、エチルアクリレート(28mol%)、2―ヒドロキシエチルメタクリレート(2mol%)、N―メチロールメタクリルアミド(5mol%)。
(P成分4)アクリル系樹脂微粒子(平均粒径0.03μm) 10重量%。
(P成分5)ポリオキシエチレンノニルフェニルエーテル 5重量%。
[Coating agent P]
(P component 1) Copolyester resin (Tg: 68 ° C.) 60% by weight.
Acid component: terephthalic acid (90 mol%), isophthalic acid (6 mol%), potassium 5-sulfoisophthalate (4 mol%).
Glycol component: ethylene glycol (95 mol%), neopentylene glycol (5 mol%).
(P component 2) N, N′-ethylenebiscaprylic acid amide 5% by weight.
(P component 3) Acrylic copolymer (number average molecular weight: 248,000) 20% by weight.
Composition: methyl acrylate (65 mol%), ethyl acrylate (28 mol%), 2-hydroxyethyl methacrylate (2 mol%), N-methylol methacrylamide (5 mol%).
(P component 4) Acrylic resin fine particles (average particle size 0.03 μm) 10% by weight.
(P component 5) 5% by weight of polyoxyethylene nonylphenyl ether.

Figure 0004960601
Figure 0004960601

[実施例2]
実施例1と同様に製膜後、オフアニール条件を60℃、50%R、3時間とした以外は実施例1と同様に実施した。得られたフィルムの物性を表1および2に示す。
[Example 2]
After the film formation in the same manner as in Example 1, the same process as in Example 1 was performed except that the off-annealing conditions were 60 ° C., 50% RH , and 3 hours. The physical properties of the obtained film are shown in Tables 1 and 2.

[比較例1]
オフアニールをしなかった以外は、実施例1と同様にして厚み100μmの二軸配向フィルムを得た。得られたフィルムの物性を表1および2に示す。
[Comparative Example 1]
A biaxially oriented film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that off-annealing was not performed. The physical properties of the obtained film are shown in Tables 1 and 2.

[比較例2]
延伸倍率を、縦方向を3.2倍、横方向を4.2倍に変更した以外は実施例1と同様にして厚み100μmの二軸配向フィルムを得た。オフアニールをしても、製膜条件が適切でないためたわみが発生した。得られたフィルムの物性を表1および2に示す。
[Comparative Example 2]
A biaxially oriented film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the stretching ratio was changed to 3.2 times in the longitudinal direction and 4.2 times in the transverse direction. Even when off-annealing was performed, the film formation conditions were not appropriate, so that deflection occurred. The physical properties of the obtained film are shown in Tables 1 and 2.

[比較例3]
オフアニールの温度を120℃、50%R、1時間に変更した以外は実施例1と同様にして厚み100μmの二軸配向フィルムを得た。オフアニールの条件が適切でないため、オフアニール後のフィルムの平面性が失われていた。得られたフィルムの物性を表1および2に示す。
[Comparative Example 3]
A biaxially oriented film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the off-annealing temperature was changed to 120 ° C., 50% R H and 1 hour. Since the conditions for off-annealing were not appropriate, the flatness of the film after off-annealing was lost. The physical properties of the obtained film are shown in Tables 1 and 2.

[参考例1]
熱固定温度を238℃に変更した以外は実施例1と同様にして厚み100μmの二軸配向フィルムを得た。たわみは良いが、光学特性が悪化したため、光拡散板用フィルムとして不適切だった。
[Reference Example 1]
A biaxially oriented film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the heat setting temperature was changed to 238 ° C. Although the deflection was good, the optical characteristics deteriorated, so it was inappropriate as a film for a light diffusion plate.

本発明によれば、湿熱耐性が高く、たわみの少ない液晶表示装置に用いる光拡散板用の基板として好適なフィルムを提供することができる。   According to the present invention, it is possible to provide a film suitable as a substrate for a light diffusing plate that is used in a liquid crystal display device that has high resistance to moist heat and has little deflection.

湿熱たわみ率の評価におけるサンプルの格子の様子である。It is a mode of a lattice of a sample in evaluation of a wet heat deflection rate.

Claims (6)

熱固定後の二軸配向ポリエステルフィルムに対して、該二軸配向ポリエステルフィルムを構成するポリエステルのガラス転移温度(Tg)−40℃からTgの範囲の温度で30分間〜72時間の間40〜90%RHの湿度でオフアニール処理を行って得られる、湿熱たわみ率が20%未満の二軸配向ポリエステルフィルムからなる光拡散板用フィルム。
(ただし、上記湿熱たわみ率は、フィルムからサンプルを24cm×24cmの大きさに切り出し2cm間隔で格子状に線を引きますを作成し、該サンプルの4辺を、表面がサンドマット処理してあるガラス板に固定した状態で、温度60℃、相対湿度90%RHの恒温恒湿オーブンに1時間放置後、室温にて1時間放置したところで、たわみが認められるますの割合として求めた値である。)
With respect to the biaxially oriented polyester film after heat setting, the glass transition temperature (Tg) of the polyester constituting the biaxially oriented polyester film is 40 to 90 hours at a temperature in the range of −40 ° C. to Tg for 30 minutes to 72 hours. A film for a light diffusing plate comprising a biaxially oriented polyester film having a wet heat deflection rate of less than 20%, which is obtained by performing an off-annealing treatment at a humidity of% RH.
(However, the wet heat deflection rate is obtained by cutting a sample from a film into a size of 24 cm × 24 cm and drawing lines in a lattice pattern at intervals of 2 cm, and the surface of the sample is sand-matted on the four sides. It is a value obtained as a ratio of the amount of bending that is observed when left in a constant temperature and humidity oven with a temperature of 60 ° C. and a relative humidity of 90% RH for 1 hour and then at room temperature for 1 hour. .)
前記湿熱たわみ率が20%未満の二軸配向ポリエステルフィルムのMD方向の屈折率とTD方向の屈折率の差の絶対値が0.01以下である、請求項1記載の光拡散板用フィルム。 The film for light diffusing plates according to claim 1, wherein an absolute value of a difference between a refractive index in the MD direction and a refractive index in the TD direction of the biaxially oriented polyester film having a wet heat deflection rate of less than 20% is 0.01 or less. 前記湿熱たわみ率が20%未満の二軸配向ポリエステルフィルムの150℃30分間の条件でのMD方向の熱収縮率とTD方向の熱収縮率との差の絶対値が0.5以下である、請求項1または2に記載の光拡散板用フィルム。 The absolute value of the difference between the thermal shrinkage rate in the MD direction and the thermal shrinkage rate in the TD direction under the condition of 150 ° C. for 30 minutes of the biaxially oriented polyester film having a wet heat deflection rate of less than 20% is 0.5 or less. The film for light diffusing plates according to claim 1 or 2. 請求項1〜3のいずれか1項に記載の光拡散板用フィルムからなる液晶表示装置用の光拡散板。   The light diffusing plate for liquid crystal display devices which consists of a film for light diffusing plates of any one of Claims 1-3. 請求項4記載の光拡散板を備える液晶表示装置。   A liquid crystal display device comprising the light diffusing plate according to claim 4. 湿熱たわみ率が20%未満の二軸配向ポリエステルフィルムからなる光拡散板用フィルムを製造するに際して、熱固定後の二軸配向ポリエステルフィルムに対して、該二軸配向ポリエステルフィルムを構成するポリエステルのガラス転移温度(Tg)−40℃からTgの範囲の温度で30分間〜72時間の間40〜90%RHの湿度でオフアニール処理を行う、光拡散板用フィルムの製造方法。
(ただし、上記湿熱たわみ率は、フィルムからサンプルを24cm×24cmの大きさに切り出し2cm間隔で格子状に線を引きますを作成し、該サンプルの4辺を、表面がサンドマット処理してあるガラス板に固定した状態で、温度60℃、相対湿度90%RHの恒温恒湿オーブンに1時間放置後、室温にて1時間放置したところで、たわみが認められるますの割合として求めた値である。)
When manufacturing a film for a light diffusing plate comprising a biaxially oriented polyester film having a wet heat deflection rate of less than 20%, the polyester glass constituting the biaxially oriented polyester film with respect to the biaxially oriented polyester film after heat setting Transition temperature (Tg) A method for producing a film for a light diffusion plate, wherein an off-annealing treatment is performed at a temperature in the range of −40 ° C. to Tg for 30 minutes to 72 hours at a humidity of 40 to 90% RH.
(However, the wet heat deflection rate is obtained by cutting a sample from a film into a size of 24 cm × 24 cm and drawing lines in a lattice pattern at intervals of 2 cm, and the surface of the sample is sand-matted on the four sides. It is a value obtained as a ratio of the amount of bending that is observed when left in a constant temperature and humidity oven with a temperature of 60 ° C. and a relative humidity of 90% RH for 1 hour and then at room temperature for 1 hour. .)
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JP4052021B2 (en) * 2002-06-04 2008-02-27 帝人デュポンフィルム株式会社 Oriented polyester film and laminated film using the same
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JP2004335517A (en) * 2003-04-30 2004-11-25 Teijin Dupont Films Japan Ltd Base film for solar battery

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