JP6694407B2 - Method for producing retardation film - Google Patents
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- JP6694407B2 JP6694407B2 JP2017066164A JP2017066164A JP6694407B2 JP 6694407 B2 JP6694407 B2 JP 6694407B2 JP 2017066164 A JP2017066164 A JP 2017066164A JP 2017066164 A JP2017066164 A JP 2017066164A JP 6694407 B2 JP6694407 B2 JP 6694407B2
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
- B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mathematical Physics (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Polarising Elements (AREA)
- Liquid Crystal (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
本発明は、位相差フィルムの製造方法に関するものである。 The present invention relates to a method for producing a retardation film.
液晶ディスプレイ等に用いられる位相差フィルムや視野角補償フィルムとして、支持体上に配向層および液晶層が設けられたものが知られている。配向層は、液晶層の液晶化合物を一定方向に並べるための膜であり、配向素子を含む塗膜に配向処理を行って配向規制力が与えられる。 As a retardation film or a viewing angle compensation film used for a liquid crystal display or the like, one having an alignment layer and a liquid crystal layer on a support is known. The alignment layer is a film for arranging the liquid crystal compounds of the liquid crystal layer in a certain direction, and an alignment regulating force is given to the coating film including the alignment element by performing alignment treatment.
配向処理としては、これまで、ナイロンなどの布を巻いたローラを一定圧力で基板に押し込みながら回転させるラビング方式が広く用いられていた。しかし、基板の摩擦によって微細な粉塵や静電気が生じてしまうという問題があり、近年、偏光を照射して配向規制力を与える光配向方式が用いられるようになっている。配向層上に形成された液晶層中の液晶化合物は、配向層の配向に従って規則正しく配列した状態になる。液晶化合物を均一に配向させることは、液晶ディスプレイの視野角向上、生産性向上のために重要である。そこで、液晶化合物の配向を均一なものとするために種々の検討がなされている。 As an orientation treatment, a rubbing method in which a roller wound with a cloth such as nylon is rotated while being pressed against a substrate with a constant pressure has been widely used. However, there is a problem that fine dust and static electricity are generated due to the friction of the substrate, and in recent years, an optical alignment method has been used in which polarized light is applied to provide an alignment regulating force. The liquid crystal compound in the liquid crystal layer formed on the alignment layer is in a state of being regularly arranged according to the alignment of the alignment layer. Aligning the liquid crystal compound uniformly is important for improving the viewing angle and productivity of the liquid crystal display. Therefore, various studies have been made to make the alignment of the liquid crystal compound uniform.
特許文献１には、光配向工程の前もしくは後、または両方で配向層を加熱処理する方法が記載されている。これにより配向層と液晶層との接着性が改善され、液晶ディスプレイのコントラスト比を向上させることができることが記載されている。 Patent Document 1 describes a method of heat-treating an alignment layer before or after a photo-alignment step, or both. It is described that this improves the adhesion between the alignment layer and the liquid crystal layer and can improve the contrast ratio of the liquid crystal display.
また、特許文献２には、均一に配列された液晶材料を含む位相差層を得るため、透明基板と配向層との間に透明無機物質からなる遮蔽層を設けた位相差フィルムが開示されている。 Further, Patent Document 2 discloses a retardation film in which a shielding layer made of a transparent inorganic substance is provided between a transparent substrate and an alignment layer in order to obtain a retardation layer containing a liquid crystal material uniformly arranged. There is.
ロールツーロール方式で層が形成される場合、液晶層まで作製された位相差フィルムの両側に透過光を遮断（クロスニコル配置）するように二枚の偏光板を配置させて光学顕微鏡で観察すると、微小な光る点、いわゆる「輝点」が見られる。輝点は、液晶化合物が均一に配向していない箇所、つまり配向欠陥を示すものである。配向欠陥が存在する箇所では、位相差フィルムを所望の複屈折率にすることが困難であり、液晶ディスプレイの品質を低下させることになる。 When the layer is formed by the roll-to-roll method, two polarizing plates are arranged on both sides of the retardation film made up to the liquid crystal layer so as to block transmitted light (crossed Nicols arrangement) and observed with an optical microscope. , A minute shining point, so-called "bright spot" can be seen. The bright spots indicate locations where the liquid crystal compound is not uniformly aligned, that is, alignment defects. It is difficult to make the retardation film have a desired birefringence at a location where an alignment defect is present, which deteriorates the quality of the liquid crystal display.
本発明は上記事情に鑑みてなされたものであり、輝点の発生が抑制される位相差フィルムの製造方法を提供することを目的とする。 The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for producing a retardation film in which the generation of bright spots is suppressed.
従来の配向層の製造には、例えば、図７に示すように、連続フィルム支持体が送出しロール５１から搬送されて、ダイコーター５２により配向層形成用材料が塗布され、温調板５３とオーブン５４によって乾燥した後、硬化前に一旦金属ロール５５に巻き取られる工程が存在する。
本発明者らの鋭意検討の結果、液晶層を形成後に発生する輝点は、巻き取り工程での金属ロール５５あるいは搬送中のタッチロールと塗膜とが接して生じる凹凸に起因することを見出し、本発明をなすに至った。
In the conventional production of an alignment layer, for example, as shown in FIG. 7, a continuous film support is delivered and conveyed from a roll 51, a die coater 52 applies an alignment layer forming material, and a temperature control plate 53 is provided. After being dried by the oven 54, there is a step of being temporarily wound around a metal roll 55 before being cured.
As a result of intensive studies by the present inventors, it was found that the bright spots generated after the liquid crystal layer is formed are caused by the unevenness caused by the contact between the metal roll 55 in the winding step or the touch roll being transported and the coating film. The present invention has been completed.
すなわち、本発明の位相差フィルムの製造方法は、
搬送される連続フィルム支持体上に、液晶化合物に対する配向規制力を備える配向層を形成するための配向層形成用材料を塗布および乾燥して第１の塗膜を形成する工程、
第１の塗膜に偏光を照射することにより配向規制力を付与して配向層を形成する工程、および
配向層上に液晶化合物を含む液晶層形成用材料を塗布および乾燥して第２の塗膜を形成する工程と、
第２の塗膜中の液晶化合物を配向させ、配向を固定して液晶層を形成する工程と、
を備える位相差フィルムの製造方法であって、
第１の塗膜を形成する工程の後、配向層を形成する工程の前に、第１の塗膜に押圧力を作用させた状態で、第１の塗膜をヒートロール上で加熱する工程を有するものである。
That is, the method for producing the retardation film of the present invention,
A step of forming a first coating film by coating and drying an alignment layer forming material for forming an alignment layer having an alignment regulating force on a liquid crystal compound, on a transported continuous film support,
A step of applying an alignment regulating force by irradiating the first coating film with polarized light to form an alignment layer, and applying and drying a liquid crystal layer-forming material containing a liquid crystal compound on the alignment layer to form a second coating film. A step of forming a film,
Aligning the liquid crystal compound in the second coating film and fixing the alignment to form a liquid crystal layer;
A method of manufacturing a retardation film comprising:
After the step of forming the first coating film, and before the step of forming the alignment layer, a step of heating the first coating film on a heat roll in a state in which a pressing force is applied to the first coating film. Is to have.
加熱する工程において、第１の塗膜が形成された連続フィルム支持体は、第１の塗膜とヒートロールとが接した状態で搬送されることが好ましい。 In the heating step, the continuous film support on which the first coating film is formed is preferably conveyed in a state where the first coating film and the heat roll are in contact with each other.
本発明の位相差フィルムの製造方法においては、第１の塗膜が形成された連続フィルム支持体をヒートロールに巻きかけることによって、第１の塗膜に押圧力を作用させてもよい。 In the method for producing a retardation film of the present invention, a pressing force may be applied to the first coating film by winding the continuous film support on which the first coating film is formed around a heat roll.
本発明の位相差フィルムの製造方法においては、第１の塗膜が形成された連続フィルム支持体を、ヒートロールとニップロールとで挟むことによって、第１の塗膜に押圧力を作用させてもよい。 In the method for producing a retardation film of the present invention, even if a pressing force is applied to the first coating film by sandwiching the continuous film support on which the first coating film is formed with a heat roll and a nip roll. Good.
加熱する工程において、第１の塗膜が形成された連続フィルム支持体は、連続フィルム支持体とヒートロールとが接し、かつ、第１の塗膜が形成された連続フィルム支持体をヒートロールとニップロールとで挟むことにより第１の塗膜に押圧力を作用させてもよい。 In the heating step, the continuous film support on which the first coating film is formed is in contact with the continuous film support and a heat roll, and the continuous film support on which the first coating film is formed is a heat roll. A pressing force may be applied to the first coating film by sandwiching it with a nip roll.
加熱する工程において、第１の塗膜が形成された連続フィルム支持体は、第１の塗膜とヒートロールとが接した状態で搬送される場合、ヒートロールの表面粗さＲｚ（ｈ）は０．８以下であることが好ましい。 In the heating step, when the continuous film support on which the first coating film is formed is conveyed in a state where the first coating film and the heat roll are in contact, the surface roughness Rz (h) of the heat roll is It is preferably 0.8 or less.
第１の塗膜が形成された連続フィルム支持体が、連続フィルム支持体とヒートロールとが接した状態で搬送される場合、ニップロールの表面粗さＲｚ（ｎ）は２．０以下であることが好ましい。 When the continuous film support on which the first coating film is formed is conveyed in a state where the continuous film support and the heat roll are in contact with each other, the surface roughness Rz (n) of the nip roll is 2.0 or less. Is preferred.
ここで、表面粗さＲｚは、粗さ曲線からその平均線の方向に基準長さだけを抜き取り、この抜き取り部分の山頂線と谷底線との間隔を粗さ曲線の縦倍率の方向に測定し、この値をマイクロメートル（μｍ）で表したものをいう。 Here, the surface roughness Rz is obtained by extracting only the reference length in the direction of the average line from the roughness curve, and measuring the distance between the peak line and the valley bottom line of this extracted portion in the direction of the longitudinal magnification of the roughness curve. , This value is expressed in micrometers (μm).
本発明の位相差フィルムの製造方法において、加熱する工程は、偏光を塗膜に照射する直前に行うことが好ましい。 In the method for producing a retardation film of the present invention, the heating step is preferably performed immediately before irradiating the coating film with polarized light.
押圧力は、線圧で５Ｎ／ｃｍ以上であることが好ましい。 The pressing force is preferably 5 N / cm or more in linear pressure.
本発明の位相差フィルムの製造方法によれば、第１の塗膜を形成する工程の後、配向層を形成する工程の前に、第１の塗膜に押圧力を作用させた状態で、第１の塗膜をヒートロール上で加熱する工程を有するものとすることにより、配向層の凹凸を小さくすることができる、輝点を低減することができる。 According to the method for producing a retardation film of the present invention, after the step of forming the first coating film and before the step of forming the alignment layer, a pressing force is applied to the first coating film, By providing the step of heating the first coating film on the heat roll, the unevenness of the alignment layer can be reduced, and the bright spots can be reduced.
以下、本発明の位相差フィルムの製造方法について図面を参照しながら説明する。 Hereinafter, the method for producing the retardation film of the present invention will be described with reference to the drawings.
本発明の位相差フィルムの製造方法は、図１に示すように、
搬送される連続フィルム支持体上に、液晶化合物に対する配向規制力を備える配向層を形成するための配向層形成用材料を塗布および乾燥して第１の塗膜を形成する工程（ＳＴ１）
第１の塗膜に偏光を照射することにより配向規制力を付与して配向層を形成する工程（ＳＴ３）、および
配向層上に液晶化合物を含む液晶層形成用材料を塗布および乾燥して第２の塗膜を形成する工程（ＳＴ４）と、
第２の塗膜中の液晶化合物を配向させ、配向を固定して液晶層を形成する工程（ＳＴ５）と、
を備える位相差フィルムの製造方法であって、
第１の塗膜を形成する工程（ＳＴ１）の後、配向層を形成する工程（ＳＴ３）の前に、第１の塗膜に押圧力を作用させた状態で、第１の塗膜をヒートロール上で加熱する工程（ＳＴ２）を有するものである。
The method for producing the retardation film of the present invention, as shown in FIG.
A step of forming a first coating film by coating and drying an alignment layer forming material for forming an alignment layer having an alignment controlling force on a liquid crystal compound on a conveyed continuous film support (ST1)
A step (ST3) of forming an alignment layer by irradiating the first coating film with polarized light to give an alignment regulating force, and applying and drying a liquid crystal layer forming material containing a liquid crystal compound on the alignment layer The step (ST4) of forming the second coating film,
A step of orienting the liquid crystal compound in the second coating film and fixing the orientation to form a liquid crystal layer (ST5),
A method of manufacturing a retardation film comprising:
After the step (ST1) of forming the first coating film, and before the step (ST3) of forming the alignment layer, the first coating film is heated while a pressing force is applied to the first coating film. It has a step (ST2) of heating on a roll.
（ＳＴ２：第１の塗膜に押圧力を作用させた状態で、第１の塗膜をヒートロール上で加熱する工程）
まず、本発明の特徴的な工程である、第１の塗膜に押圧力を作用させた状態で、第１の塗膜をヒートロール上で加熱する工程（以下、「ＳＴ２工程」という）について図を参照しながら説明する。
(ST2: a step of heating the first coating film on a heat roll in a state where a pressing force is applied to the first coating film)
First, the step of heating the first coating film on a heat roll in the state where pressing force is applied to the first coating film, which is a characteristic step of the present invention (hereinafter referred to as “ST2 step”) Description will be made with reference to the drawings.
ＳＴ２工程としては、例えば、図２に示すように、第１の塗膜１２が形成された連続フィルム支持体１１（以下、フィルム１０と記載する）を、第１の塗膜１２とヒートロール２０とが接した状態で、ヒートロール２０に巻きかけて搬送し、加熱する形態が挙げられる。フィルム１０には搬送張力がかかっているため、ラップ角θを付与した状態で巻きかけることにより、第１の塗膜１２に押圧力を作用させた状態とすることができる。 As the ST2 step, for example, as shown in FIG. 2, a continuous film support 11 (hereinafter referred to as a film 10) on which a first coating film 12 is formed, a first coating film 12 and a heat roll 20. In the state where the and are in contact with each other, there may be mentioned a mode in which they are wound around the heat roll 20 and conveyed and heated. Since the transport tension is applied to the film 10, the film 10 can be put in a state in which a pressing force is applied to the first coating film 12 by winding the film 10 with the wrap angle θ applied.
第１の塗膜１２に押圧力を作用させた状態で加熱することにより、第１の塗膜１２の凹凸を良好に低減することができ、均一な配向状態にすることができる。したがって、配向層の上に形成される液晶層の配列も均一な状態にすることができ、輝点を低減することができる。 By heating the first coating film 12 while applying a pressing force, the irregularities of the first coating film 12 can be satisfactorily reduced and a uniform alignment state can be obtained. Therefore, the alignment of the liquid crystal layer formed on the alignment layer can be made uniform, and the bright spots can be reduced.
ヒートロール２０は、温度が５０℃〜１２０℃に維持されるように、温度制御手段２１によって制御される。温度は、６０℃〜１２０℃がさらに好ましい。６０℃以上であることによって、第１の塗膜１２の凹凸をさらに小さくすることができる。 The heat roll 20 is controlled by the temperature control means 21 so that the temperature is maintained at 50 ° C. to 120 ° C. The temperature is more preferably 60 ° C to 120 ° C. When the temperature is 60 ° C. or higher, the unevenness of the first coating film 12 can be further reduced.
また、ラップ角θは、３０°以上１８０°以下が好ましい、９０°以上１８０°以下がより好ましい。３０°以上であることにより、第１の塗膜１２の凹凸を低減するのに充分な押圧力を作用させることができる。 The wrap angle θ is preferably 30 ° or more and 180 ° or less, more preferably 90 ° or more and 180 ° or less. When the angle is 30 ° or more, a pressing force sufficient to reduce the unevenness of the first coating film 12 can be applied.
搬送速度は、１０ｍ／ｍｉｎ以上５０ｍ／ｍｉｎ以下であることが好ましく１０ｍ／ｍｉｎ以上３０ｍ／ｍｉｎ以下であることが好ましい。１０ｍ／ｍｉｎ以上であることにより、生産性を維持することができる。５０ｍ／ｍｉｎ以下であることにより、ヒートロール上の滞在時間を長く確保することができる。滞在時間を長くすることで、より有効に加熱されるとともに、確実に処理を行うことができる。 The transport speed is preferably 10 m / min or more and 50 m / min or less, and more preferably 10 m / min or more and 30 m / min or less. When it is 10 m / min or more, productivity can be maintained. When it is 50 m / min or less, the staying time on the heat roll can be secured for a long time. By lengthening the staying time, the heating can be performed more effectively and the treatment can be performed reliably.
なお、ＳＴ２工程は、特に制限はないが、第１の塗膜を形成する工程（ＳＴ１）の後、配向層を形成する工程（ＳＴ３）の前に実施すればよく、偏光を第１の塗膜に照射する直前に行うことがより好ましい。 The step ST2 is not particularly limited, but it may be performed after the step (ST1) of forming the first coating film and before the step (ST3) of forming the alignment layer. More preferably, it is performed immediately before irradiating the film.
第１の塗膜１２がヒートロール２０に接する場合は、ヒートロール２０の表面粗さＲｚ（ｈ）は２．０以下であることが好ましく、より好ましくは、０．８μｍ以下である。２．０μｍ以下であることにより、輝点を良好に低減することができる。
ヒートロール２０の表面にごみ等による凹凸があると輝点の原因となるため、ヒートロール２０の搬送上流側に、ヒートロール２０の表面を清掃するための装置を備えてもよい。
When the first coating film 12 contacts the heat roll 20, the surface roughness Rz (h) of the heat roll 20 is preferably 2.0 or less, and more preferably 0.8 μm or less. When it is 2.0 μm or less, bright spots can be favorably reduced.
Since unevenness due to dust or the like on the surface of the heat roll 20 causes bright spots, a device for cleaning the surface of the heat roll 20 may be provided on the upstream side of the conveyance of the heat roll 20.
また、他の例として、図３に示すように、第１の塗膜１２が形成された連続フィルム支持体１１を、第１の塗膜１２とヒートロール２０とが接した状態で、かつ、ヒートロール２０とニップロール３０でフィルム１０を挟んで搬送し、加熱してもよい。フィルム１０をヒートロール２０に巻きかけ、さらにニップロール３０で挟むことにより、第１の塗膜１２をより平坦にすることができ、凹凸による輝点の発生を低減することができる。 Further, as another example, as shown in FIG. 3, the continuous film support 11 on which the first coating film 12 is formed is in a state where the first coating film 12 and the heat roll 20 are in contact with each other, and The film 10 may be sandwiched between the heat roll 20 and the nip roll 30 to be conveyed and heated. By winding the film 10 around the heat roll 20 and further sandwiching it with the nip roll 30, the first coating film 12 can be made more flat, and the occurrence of bright spots due to unevenness can be reduced.
押圧力は、ニップロールで挟まれている場合、線圧で５Ｎ／ｃｍ以上であることが好ましく、１０Ｎ／ｃｍ以上がより好ましい。５Ｎ／ｃｍ以上であることにより、ヒートロール２０上で第１の塗膜の表面を充分に平滑にすることができる。線圧は、ニップロールの変形が過度にならないようにするために、５０Ｎ／ｃｍ以下が好ましい。 When the pressing force is sandwiched by nip rolls, the linear pressure is preferably 5 N / cm or more, more preferably 10 N / cm or more. By being 5 N / cm or more, the surface of the first coating film can be sufficiently smoothed on the heat roll 20. The linear pressure is preferably 50 N / cm or less in order to prevent excessive deformation of the nip roll.
上記一例では、ヒートロール２０に巻きかけて第１の塗膜１２に押圧力を作用させた状態としたが、さらに他の例として、図４に示すように、フィルム１０をヒートロールに巻きかけず、ニップロール３０で挟んで、第１の塗膜１２に押圧力が作用した状態にしてもよい。 In the above example, the first coating film 12 is wound around the heat roll 20 to exert the pressing force, but as another example, as shown in FIG. 4, the film 10 is wrapped around the heat roll. Instead, it may be sandwiched by the nip rolls 30 so that the pressing force acts on the first coating film 12.
上記では、第１の塗膜１２がヒートロール２０に接する形態について説明したが、連続フィルム支持体１１がヒートロール２０に接してもよい。例えば、図５に示すように、フィルム１０を、連続フィルム支持体１１とヒートロール２０とが接するようにヒートロール２０に巻きかけ、かつ、フィルム１０をヒートロール２０とニップロール３０とで挟むことにより、第１の塗膜１２に押圧力を作用させてもよい。
あるいは、フィルム１０をヒートロール２０にまきかけないでヒートロール２０とニップロール３０とで挟むことにより第１の塗膜１２に押圧力を作用させてもよい。
Although the first coating film 12 is in contact with the heat roll 20 in the above description, the continuous film support 11 may be in contact with the heat roll 20. For example, as shown in FIG. 5, by winding the film 10 around the heat roll 20 so that the continuous film support 11 and the heat roll 20 are in contact with each other, and sandwiching the film 10 between the heat roll 20 and the nip roll 30. The pressing force may be applied to the first coating film 12.
Alternatively, the pressing force may be applied to the first coating film 12 by sandwiching the film 10 between the heat roll 20 and the nip roll 30 without sprinkling the film 10 on the heat roll 20.
連続フィルム支持体１１とヒートロール２０とが接する場合、第１の塗膜１２はニップロール３０と接触するため、ニップロール３０の表面粗さＲｚ（ｎ）は２．０以下であることが好ましく、０．８μｍ以下がより好ましい。２．０以下であることにより、配向層の凹凸を低減することができ、輝点を良好に低減することができる。
また、ヒートロールの加熱手段は蒸気式、ガス式、熱媒循環式、低周波誘導加熱方式など方式は問わない。また、支持体温度を高い状態に保ちつつ押圧すればよいことから、加熱された処理室内で押圧してもよい。さらにヒートロールに加えて、予熱ヒーターと保温ロールとの組み合わせなどを用いてもよい。
When the continuous film support 11 and the heat roll 20 are in contact with each other, the first coating film 12 is in contact with the nip roll 30. Therefore, the surface roughness Rz (n) of the nip roll 30 is preferably 2.0 or less, and 0 It is more preferably 0.8 μm or less. When it is 2.0 or less, the unevenness of the alignment layer can be reduced, and the bright spots can be favorably reduced.
The heating means of the heat roll may be a steam type, a gas type, a heat medium circulating type, a low frequency induction heating type, or the like. Further, since the pressing may be performed while keeping the support temperature high, the pressing may be performed in the heated processing chamber. Further, in addition to the heat roll, a combination of a preheating heater and a heat retention roll may be used.
以下、加熱する工程（ＳＴ２）以外の工程について工程順に説明する。 Hereinafter, steps other than the heating step (ST2) will be described in the order of steps.
（ＳＴ１：第１の塗膜を形成する工程）
搬送方向に搬送される連続フィルム支持体上に、液晶化合物に対する配向規制力を備える配向層を形成するための配向層形成用材料を塗布および乾燥する。
以下、各構成要素の詳細を説明する。
(ST1: Step of forming first coating film)
An alignment layer-forming material for forming an alignment layer having an alignment regulating force for a liquid crystal compound is applied and dried on a continuous film support that is transported in the transport direction.
The details of each component will be described below.
−連続フィルム支持体−
連続フィルム支持体としては、バックアップロールに巻きかけることが可能なポリマーフィルムを用いることが好ましい。支持体として用いられるポリマーフィルムの材料の例には、セルロースアシレートフィルム（例えば、セルローストリアセテートフィルム（屈折率１．４８）、セルロースジアセテートフィルム、セルロースアセテートブチレートフィルム、セルロースアセテートプロピオネートフィルム）、ポリエチレン、ポリプロピレン等のポリオレフィン、ポリエチレンテレフタレートやポリエチレンナフタレート等のポリエステル系樹脂フィルム、ポリエーテルスルホンフィルム、ポリメチルメタクリレート等のポリアクリル系樹脂フィルム、ポリウレタン系樹脂フィルム、ポリカーボネートフィルム、ポリスルホンフィルム、ポリエーテルフィルム、ポリメチルペンテンフィルム、ポリエーテルケトンフィルム、（メタ）アクリルニトリルフィルム、ポリオレフィン、脂環式構造を有するポリマー（ノルボルネン系樹脂（商品名「アートン（登録商標）」、ＪＳＲ社製、非晶質ポリオレフィン（商品名「ゼオネックス（登録商標）」、日本ゼオン社製））、などが挙げられる。このうちトリアセチルセルロース、ポリエチレンテレフタレート（ＰＥＴ）、脂環式構造を有するポリマーが好ましく、特にトリアセチルセルロースが好ましい。
-Continuous film support-
As the continuous film support, it is preferable to use a polymer film that can be wound around a backup roll. Examples of the material of the polymer film used as the support include a cellulose acylate film (eg, cellulose triacetate film (refractive index 1.48), cellulose diacetate film, cellulose acetate butyrate film, cellulose acetate propionate film). Polyolefin such as polyethylene, polypropylene, polyester resin film such as polyethylene terephthalate and polyethylene naphthalate, polyethersulfone film, polyacrylic resin film such as polymethylmethacrylate, polyurethane resin film, polycarbonate film, polysulfone film, polyether Film, polymethylpentene film, polyetherketone film, (meth) acrylonitrile film Polyolefin, polymer having alicyclic structure (norbornene-based resin (trade name "Arton (registered trademark)", manufactured by JSR, amorphous polyolefin (trade name "Zeonex (registered trademark)", manufactured by Zeon Corporation)), Among these, triacetyl cellulose, polyethylene terephthalate (PET) and a polymer having an alicyclic structure are preferable, and triacetyl cellulose is particularly preferable.
支持体の膜厚としては、５μｍ〜１０００μｍ程度であればよく、好ましくは１０μｍ〜２５０μｍであり、より好ましくは１５μｍ〜９０μｍである。 The thickness of the support may be about 5 μm to 1000 μm, preferably 10 μm to 250 μm, and more preferably 15 μm to 90 μm.
−配向層形成用材料−
光配向に用いられる配向層形成用材料としては、例えば、特開２００６−２８５１９７号公報、特開２００７−７６８３９号公報、特開２００７−１３８１３８号公報、特開２００７−９４０７１号公報、特開２００７−１２１７２１号公報、特開２００７−１４０４６５号公報、特開２００７−１５６４３９号公報、特開２００７−１３３１８４号公報、特開２００９−１０９８３１号公報、特許第３８８３８４８号、特許第４１５１７４６号に記載のアゾ化合物、特開２００２−２２９０３９号公報に記載の芳香族エステル化合物、特開２００２−２６５５４１号公報、特開２００２−３１７０１３号公報に記載の光配向性単位を有するマレイミドおよび／またはアルケニル置換ナジイミド化合物、特許第４２０５１９５号、特許第４２０５１９８号に記載の光架橋性シラン誘導体、特表２００３−５２０８７８号公報、特表２００４−５２９２２０号公報、特許第４１６２８５０号に記載の光架橋性ポリイミド、ポリアミド、またはエステル、特開平９−１１８７１７号公報、特表平１０−５０６４２０号公報、特表２００３−５０５５６１号公報、ＷＯ２０１０/１５０７４８号、特開２０１３−１７７５６１号公報、特開２０１４−１２８２３号公報に記載の光二量化可能な化合物、特にシンナメート化合物、カルコン化合物、クマリン化合物が挙げられる。特に好ましい例としては、アゾ化合物、光架橋性ポリイミド、ポリアミド、エステル、シンナメート化合物、カルコン化合物が挙げられる。
-Material for forming alignment layer-
Examples of the alignment layer forming material used for optical alignment include, for example, JP 2006-285197 A, JP 2007-76839 A, JP 2007-138138 A, JP 2007-94071 A and JP 2007 A. -121721, JP-A-2007-140465, JP-A-2007-156439, JP-A-2007-133184, JP-A-2009-109831, JP-A-38384848, and JP-A-4151746. Compound, aromatic ester compound described in JP-A-2002-229039, maleimide and / or alkenyl-substituted nadimide compound having a photoalignment unit described in JP-A-2002-265541 and JP-A-2002-317013, Patent No. 4205195, Patent No. 42 Photo-crosslinkable silane derivative described in No. 5198, Japanese Patent Publication No. 2003-520878, No. 2004-529220, and Japanese Patent No. 4162850, the photocrosslinkable polyimide, polyamide, or ester, JP-A-9-118717. Japanese Patent Publication No. 10-506420, Japanese Patent Publication No. 2003-505561, Japanese Patent Publication No. 2010/150748, Japanese Patent Laid-Open No. 2013-177561, Japanese Patent Laid-Open No. 2014-12823, and dimerizable compounds, particularly cinnamate. Examples thereof include compounds, chalcone compounds, and coumarin compounds. Particularly preferred examples include azo compounds, photocrosslinkable polyimides, polyamides, esters, cinnamate compounds and chalcone compounds.
−塗布方法−
配向層形成用材料を塗布する際の方法としてはカーテンコーティング法、ディップコーティング法、スピンコーティング法、印刷コーティング法、スプレーコーティング法、スロットコーティング法、ロールコーティング法、スライドコーティング法、ブレードコーティング法、グラビアコーティング法、ワイヤーバー法等の公知の方法が挙げられる。
-Coating method-
The method for applying the alignment layer forming material includes a curtain coating method, a dip coating method, a spin coating method, a printing coating method, a spray coating method, a slot coating method, a roll coating method, a slide coating method, a blade coating method and a gravure method. Known methods such as a coating method and a wire bar method can be used.
−乾燥工程−
乾燥は、オーブン、温風、ＩＲヒーター等によって、３０℃〜１４０℃で、１０秒〜１０分間程度行うことが好ましい。また、温風乾燥においては支持体側から温風をあてる構成でもよく、温風が塗膜を流動させないように拡散板を設置した構成としてもよい。
-Drying process-
Drying is preferably performed at 30 ° C. to 140 ° C. for about 10 seconds to 10 minutes using an oven, warm air, an IR heater or the like. Further, in warm air drying, warm air may be applied from the support side, or a diffusion plate may be installed so that the warm air does not flow the coating film.
（ＳＴ３：配向層を形成する工程）
偏光を照射して配向層を形成する工程（ＳＴ３）について説明する。
第１の塗膜に偏光を照射することにより配向規制力を付与して配向層を形成する工程である。配向規制力を付与する工程とは、配向層形成用材料に光反応を生じせしめるための操作である。
偏光を照射して配向層を形成する工程として、例えば、図６に示すように、連続フィルム支持体１１上に第１の塗膜１２が形成されたフィルム１０をＹ方向に搬送しながら、フィルム１０上に、光配向装置からの偏光を照射する形態が挙げられる。光配向装置は、棒状光源４０と棒状光源からの光をフィルム１０方向へ反射する凹面反射鏡４１と、棒状光源４０の長手方向（図中Ｘ方向）に配列された複数の平行板４２からなるルーバー４３と、ルーバー４３によって平行光化された光を直線偏光するワイヤーグリッド偏光子４４とから構成される。そして、ワイヤーグリッド偏光子４４から発せられる偏光が第１の塗膜１２に照射される。
(ST3: Step of forming alignment layer)
The step (ST3) of irradiating polarized light to form the alignment layer will be described.
This is a step of forming an alignment layer by irradiating the first coating film with polarized light to impart an alignment regulating force. The step of imparting the alignment regulating force is an operation for causing a photoreaction in the alignment layer forming material.
As the step of irradiating polarized light to form the alignment layer, for example, as shown in FIG. 6, while transporting the film 10 having the first coating film 12 formed on the continuous film support 11 in the Y direction, On top of this, a form in which polarized light from the photo-alignment device is irradiated onto The optical alignment device includes a rod-shaped light source 40, a concave reflecting mirror 41 that reflects light from the rod-shaped light source toward the film 10, and a plurality of parallel plates 42 arranged in the longitudinal direction of the rod-shaped light source 40 (X direction in the drawing). The louver 43 and the wire grid polarizer 44 that linearly polarizes the light collimated by the louver 43. Then, the polarized light emitted from the wire grid polarizer 44 is applied to the first coating film 12.
棒状光源４０として、通常使われる光源、例えばタングステンランプ、ハロゲンランプ、キセノンランプ、キセノンフラッシュランプ、水銀ランプ、水銀キセノンランプ、カーボンアークランプ等のランプ、各種のレーザー（例、半導体レーザー、ヘリウムネオンレーザー、アルゴンイオンレーザー、ヘリウムカドミウムレーザー、ＹＡＧ（Yttrium Aluminum Garnet）レーザー）、発光ダイオード、陰極線管などを挙げることができる。偏光のピーク波長は、２００ｎｍ〜４００ｎｍが好ましい。 As the rod-shaped light source 40, a light source normally used, for example, a tungsten lamp, a halogen lamp, a xenon lamp, a xenon flash lamp, a mercury lamp, a mercury xenon lamp, a carbon arc lamp or the like, various lasers (eg, semiconductor laser, helium neon laser) , An argon ion laser, a helium cadmium laser, a YAG (Yttrium Aluminum Garnet) laser), a light emitting diode, a cathode ray tube and the like. The peak wavelength of polarized light is preferably 200 nm to 400 nm.
光配向では、上記のような非接触の光照射によって光配向材料を配向させるため、ラビングのような不均一な物理的凹凸形状が発生しにくい。そのため、光配向によって配向規制力を付与された配向層を利用して作製した光学フィルムを用いた液晶表示装置では光漏れが低減され、高コントラストが実現できる。 In the photo-alignment, since the photo-alignment material is aligned by the non-contact light irradiation as described above, nonuniform physical uneven shape such as rubbing is unlikely to occur. Therefore, in a liquid crystal display device using an optical film produced by using an alignment layer having an alignment regulating force provided by optical alignment, light leakage is reduced and high contrast can be realized.
（ＳＴ４：第２の塗膜を形成する工程）
配向層上に液晶化合物を含む液晶層形成用材料を塗布および乾燥して第２の塗膜を形成する。液晶層形成用材料の塗布および乾燥は、上記配向層形成用材料の塗布および乾燥と同様の方法を用いることができ、その詳細な説明は省略する。
(ST4: Step of forming second coating film)
A liquid crystal layer-forming material containing a liquid crystal compound is applied onto the alignment layer and dried to form a second coating film. The application and drying of the liquid crystal layer forming material can be performed by the same method as the above-mentioned application and drying of the alignment layer forming material, and detailed description thereof will be omitted.
−液晶層形成用材料−
液晶層形成用材料は、棒状液晶化合物もしくは円盤状液晶化合物および少なくともキラル剤を含有し、さらに、配向制御剤、重合開始剤および配向助剤などのその他の成分を含有していてもよい。
-Material for forming liquid crystal layer-
The material for forming a liquid crystal layer contains a rod-shaped liquid crystal compound or a discotic liquid crystal compound and at least a chiral agent, and may further contain other components such as an orientation control agent, a polymerization initiator and an orientation aid.
−−棒状液晶化合物−−
棒状液晶化合物としては、アゾメチン類、アゾキシ類、シアノビフェニル類、シアノフェニルエステル類、安息香酸エステル類、シクロヘキサンカルボン酸フェニルエステル類、シアノフェニルシクロヘキサン類、シアノ置換フェニルピリミジン類、アルコキシ置換フェニルピリミジン類、フェニルジオキサン類、トラン類およびアルケニルシクロヘキシルベンゾニトリル類が好ましく用いられる。以上のような低分子液晶性分子だけではなく、高分子液晶性分子も用いることができる。
--- Rod-shaped liquid crystal compound ---
As the rod-shaped liquid crystal compound, azomethines, azoxys, cyanobiphenyls, cyanophenyl esters, benzoic acid esters, cyclohexanecarboxylic acid phenyl esters, cyanophenylcyclohexanes, cyano-substituted phenylpyrimidines, alkoxy-substituted phenylpyrimidines, Phenyldioxane, tolan and alkenylcyclohexylbenzonitrile are preferably used. In addition to the above low-molecular liquid crystal molecules, high-molecular liquid crystal molecules can be used.
棒状液晶化合物を重合によって配向を固定することがより好ましく、重合性棒状液晶化合物としては、Ｍａｋｒｏｍｏｌ． Ｃｈｅｍ．， １９０巻、２２５５頁（１９８９年）、Ａｄｖａｎｃｅｄ Ｍａｔｅｒｉａｌｓ ５巻、１０７頁（１９９３年）、米国特許４６８３３２７号公報、同５６２２６４８号公報、同５７７０１０７号公報、ＷＯ９５／２２５８６号公報、同９５／２４４５５号公報、同９７／００６００号公報、同９８／２３５８０号公報、同９８／５２９０５号公報、特開平１−２７２５５１号公報、同６−１６６１６号公報、同７−１１０４６９号公報、同１１−８００８１号公報、および特願２００１−６４６２７号公報などに記載の化合物を用いることができる。さらに棒状液晶化合物としては、例えば、特表平１１−５１３０１９号公報や特開２００７−２７９６８８号公報に記載のものも好ましく用いることができる。 It is more preferable to fix the orientation of the rod-shaped liquid crystal compound by polymerization. As the polymerizable rod-shaped liquid crystal compound, Makromol. Chem. , 190, 2255 (1989), Advanced Materials, 5 (107) (1993), U.S. Pat. Nos. 4,683,327, 5,622,648, 5,770,107, WO95 / 22586, 95/24455. JP, 97/00600, 98/23580, 98/52905, JP-A 1-272551, 6-16616, 7-110469, 11-80081. The compounds described in the gazette and Japanese Patent Application No. 2001-64627 can be used. Further, as the rod-shaped liquid crystal compound, for example, those described in JP-A-11-513019 and JP-A-2007-279688 can be preferably used.
−−円盤状液晶化合物−−
円盤状液晶化合物としては、例えば、特開２００７−１０８７３２号公報や特開２０１０−２４４０３８号公報に記載のものを好ましく用いることができる。
−− Discotic liquid crystal compound−−
As the discotic liquid crystal compound, for example, those described in JP2007-108732A and JP2010-244038A can be preferably used.
（ＳＴ５：液晶層の形成）
第２の塗膜中の液晶化合物を配向させ、配向を固定して液晶層を形成する。
(ST5: Formation of liquid crystal layer)
The liquid crystal compound in the second coating film is oriented and the orientation is fixed to form a liquid crystal layer.
−液晶化合物の配向−
液晶層形成用材料の配向固定（硬化）の前には、第２の塗膜の液晶化合物の配向処理を行う。配向処理は、室温等により乾燥させる、または加熱することにより行うことができる。配向処理で形成される液晶層は、サーモトロピック性液晶化合物の場合、一般に温度または圧力の変化により転移させることができる。リオトロピック性をもつ液晶化合物の場合には、溶媒量等の組成比によっても転移させることができる。
-Alignment of liquid crystal compound-
Before fixing (curing) the alignment of the liquid crystal layer forming material, the alignment treatment of the liquid crystal compound of the second coating film is performed. The orientation treatment can be performed by drying at room temperature or by heating. In the case of a thermotropic liquid crystal compound, the liquid crystal layer formed by the alignment treatment can be generally transformed by a change in temperature or pressure. In the case of a liquid crystal compound having a lyotropic property, the transition can be performed also by the composition ratio such as the amount of solvent.
棒状液晶化合物がスメクチック相を発現する場合、ネマチック相を発現する温度領域の方が、棒状液晶化合物がスメクチック相を発現する温度領域よりも高いことが普通である。従って、棒状液晶化合物がネマチック相を発現する温度領域まで棒状液晶化合物を加熱し、次に、加熱温度を棒状液晶化合物がスメクチック相を発現する温度領域まで低下させることにより、棒状液晶化合物をネマチック相からスメクチック相に転移させることができる。このような方法をスメクチック相とすることで、液晶化合物が高秩序度で配向した液晶層を提供することができる。 When the rod-shaped liquid crystal compound develops a smectic phase, the temperature range in which the nematic phase is developed is usually higher than the temperature range in which the rod-shaped liquid crystal compound develops the smectic phase. Therefore, by heating the rod-shaped liquid crystal compound to a temperature range where the rod-shaped liquid crystal compound develops a nematic phase, and then lowering the heating temperature to a temperature region where the rod-shaped liquid crystal compound develops a smectic phase, the rod-shaped liquid crystal compound is changed to a nematic phase. To a smectic phase. By using such a method as a smectic phase, a liquid crystal layer in which a liquid crystal compound is aligned with high order can be provided.
棒状液晶化合物がネマチック相を発現する温度領域では、棒状液晶化合物がモノドメインを形成するまで一定時間加熱する必要がある。加熱時間は、１０秒間〜５分間が好ましく、1０秒間〜３分間がさらに好ましく、1０秒間〜２分間が最も好ましい。
棒状液晶化合物がスメクチック相を発現する温度領域では、棒状液晶化合物がスメクチック相を発現するまで一定時間加熱する必要がある。加熱時間は、１０秒間〜５分間が好ましく、１０秒間〜３分間がさらに好ましく、１０秒間〜２分間が最も好ましい。
In the temperature range where the rod-shaped liquid crystal compound develops a nematic phase, it is necessary to heat for a certain period of time until the rod-shaped liquid crystal compound forms a monodomain. The heating time is preferably 10 seconds to 5 minutes, more preferably 10 seconds to 3 minutes, and most preferably 10 seconds to 2 minutes.
In the temperature range where the rod-shaped liquid crystal compound develops a smectic phase, it is necessary to heat for a certain period of time until the rod-shaped liquid crystal compound develops a smectic phase. The heating time is preferably 10 seconds to 5 minutes, more preferably 10 seconds to 3 minutes, and most preferably 10 seconds to 2 minutes.
−配向の固定−
第２の塗膜中の液晶化合物の配向を固定して液晶層を形成する。
配向の固定は、熱重合や活性エネルギー線による重合で行うことができ、その重合に適した重合性基や重合開始剤を適宜選択することで行うことができる。製造適性等を考慮すると紫外線照射による重合反応を好ましく用いることができる。紫外線の照射量が少ないと、未重合の重合性棒状液晶が残存し、光学特性の温度変化や、経時劣化の起きる原因となる。
そのため、残存する重合性棒状液晶の割合が５%以下になる様に照射条件を決めることが好ましく、その照射条件は重合性組成物の処方や第２の塗膜の厚さにもよるが目安として紫外線照射量は、５０〜１０００ｍＪ／ｃｍ２が好ましく、１００〜５００ｍＪ／ｃｍ２がより好ましい。
-Fixation of orientation-
The orientation of the liquid crystal compound in the second coating film is fixed to form a liquid crystal layer.
The orientation can be fixed by thermal polymerization or polymerization with an active energy ray, and can be performed by appropriately selecting a polymerizable group and a polymerization initiator suitable for the polymerization. Considering production suitability and the like, a polymerization reaction by irradiation with ultraviolet rays can be preferably used. When the irradiation amount of ultraviolet rays is small, unpolymerized polymerizable rod-shaped liquid crystal remains, which may cause temperature change of optical characteristics and deterioration with time.
Therefore, it is preferable to determine the irradiation condition so that the ratio of the remaining polymerizable rod-shaped liquid crystal is 5% or less. The irradiation condition depends on the composition of the polymerizable composition and the thickness of the second coating film, but is a guideline. UV irradiation dose as is preferably 50~1000mJ / cm 2, and more preferably 100 to 500 mJ / cm 2.
光照射に用いる光源は、通常使われる光源、例えばタングステンランプ、ハロゲンランプ、キセノンランプ、キセノンフラッシュランプ、水銀ランプ、水銀キセノンランプ、カーボンアークランプ等のランプ、各種のレーザー（例、半導体レーザー、ヘリウムネオンレーザー、アルゴンイオンレーザー、ヘリウムカドミウムレーザー、ＹＡＧ（Yttrium Aluminum Garnet）レーザー）、発光ダイオード、陰極線管などを挙げることができる。
その他、液晶層の詳細は、特開２００８−２２５２８１号公報や特開２００８−０２６７３０号公報の記載を参酌できる。
The light source used for light irradiation is a commonly used light source, such as a tungsten lamp, a halogen lamp, a xenon lamp, a xenon flash lamp, a mercury lamp, a mercury xenon lamp, a carbon arc lamp, and various lasers (eg, semiconductor laser, helium). Examples thereof include a neon laser, an argon ion laser, a helium cadmium laser, a YAG (Yttrium Aluminum Garnet) laser), a light emitting diode, and a cathode ray tube.
In addition, for details of the liquid crystal layer, the descriptions in JP-A-2008-225281 and JP-A-2008-026730 can be referred to.
以下に、実施例を挙げて本発明をさらに具体的に説明する。以下の実施例に示す材料、使用量、割合、処理内容、処理手順等は、本発明の趣旨を逸脱しない限り、適宜、変更することができる。従って、本発明の範囲は以下に示す具体例に限定されるものではない。 Hereinafter, the present invention will be described more specifically with reference to examples. The materials, usage amounts, ratios, processing contents, processing procedures, and the like shown in the following examples can be appropriately changed without departing from the spirit of the present invention. Therefore, the scope of the present invention is not limited to the specific examples shown below.
［実施例１］
（ＳＴ１：第１の塗膜の形成）
セルローストリアセテートフィルムＴＤ８０ＵＬ（富士フイルム製）の支持体表面をアルカリ鹸化処理した。具体的には、５５℃の１．５規定の水酸化ナトリウム水溶液に支持体を２分間浸漬した後、室温の水洗浴槽中で洗浄し、３０℃の０．１規定の硫酸を用いて中和した。中和した後、室温の水洗浴槽中で洗浄し、更に１００℃の温風で乾燥した。
次に、支持体表面に、下記の組成の配向層形成材料をワイヤーバーで塗布した。６０℃の温風で６０秒、さらに１００℃の温風で１２０秒乾燥し、第１の塗膜を形成した。
[Example 1]
(ST1: formation of first coating film)
The support surface of the cellulose triacetate film TD80UL (manufactured by Fuji Film) was subjected to alkali saponification treatment. Specifically, the support is immersed for 2 minutes in a 1.5N aqueous sodium hydroxide solution at 55 ° C, washed in a water washing bath at room temperature, and neutralized with 0.1N sulfuric acid at 30 ° C. did. After neutralization, the product was washed in a water-washing bath at room temperature and dried with warm air at 100 ° C.
Next, an alignment layer forming material having the following composition was applied to the surface of the support with a wire bar. It was dried with hot air at 60 ° C. for 60 seconds and further with hot air at 100 ° C. for 120 seconds to form a first coating film.
−配向層形成用材料の調製−
光配向用素材Ｐ−１ １．０質量部
ブトキシエタノール ３３質量部
プロピレングリコールモノメチルエーテル ３３質量部
水 ３３質量部
-Preparation of alignment layer forming material-
Material for photo-alignment P-1 1.0 part by mass Butoxyethanol 33 parts by mass Propylene glycol monomethyl ether 33 parts by mass Water 33 parts by mass
（ＳＴ２：加熱する工程）
図３に示すように、第１の塗膜１２が形成された連続フィルム支持体１１（フィルム１０）をヒートロール２０に巻きかけ、第１の塗膜１２とヒートロール２０とが接するように、ヒートロール２０とニップロール３０で挟んで搬送し、第１の塗膜を加熱した。ヒートロール２０は、温度制御手段２１によって温度が６０℃に維持されていた。ヒートロール、ニップロール、および搬送条件の詳細を以下に示す。
ヒートロール：直径：２００ｍｍ、材質ＳＵＳ、表面粗さＲｚ：０．８
ニップロール：直径：１００ｍｍ、材質合成ゴム、表面粗さＲｚ：２．０
ラップ角：９０°
搬送速度：３０ｍ／ｍｉｎ
ラップ時間：０．３１sec
線圧：１０Ｎ／ｃｍ
(ST2: heating step)
As shown in FIG. 3, the continuous film support 11 (film 10) on which the first coating film 12 is formed is wound around the heat roll 20 so that the first coating film 12 and the heat roll 20 are in contact with each other. The first coating film was heated by being sandwiched between the heat roll 20 and the nip roll 30 and conveyed. The temperature of the heat roll 20 was maintained at 60 ° C. by the temperature control means 21. Details of the heat roll, the nip roll, and the transport conditions are shown below.
Heat roll: Diameter: 200 mm, material SUS, surface roughness Rz: 0.8
Nip roll: Diameter: 100 mm, material synthetic rubber, surface roughness Rz: 2.0
Lap angle: 90 °
Transport speed: 30m / min
Lap time: 0.31sec
Linear pressure: 10N / cm
（ＳＴ３：配向層を形成する工程）
次に、第１の塗膜上に直線偏光を照射して、光配向処理を行った。
このとき、ワイヤーグリッド偏光子(Moxtek社製, ProFlux PPL02)を第１の塗膜の面と平行に、かつ、ワイヤーグリッド偏光子の透過軸と配向層の吸収軸が平行になるようにセットして露光し、光配向処理を行った。この際用いる紫外線の照度はＵＶ（ultra-violet）−Ａ領域（波長３８０ｎｍ〜３２０ｎｍの積算）において１００ｍＷ／ｃｍ２、照射量はＵＶ−Ａ領域において１０００ｍＪ／ｃｍ２とした。
(ST3: Step of forming alignment layer)
Next, the first coating film was irradiated with linearly polarized light to perform a photo-alignment treatment.
At this time, set the wire grid polarizer (Moxtek, ProFlux PPL02) parallel to the surface of the first coating film, and also set the transmission axis of the wire grid polarizer and the absorption axis of the alignment layer to be parallel. Exposure, and photo-alignment treatment was performed. The illuminance of ultraviolet rays used at this time was 100 mW / cm 2 in the UV (ultra-violet) -A region (integration of wavelengths of 380 nm to 320 nm), and the irradiation amount was 1000 mJ / cm 2 in the UV-A region.
（ＳＴ４，ＳＴ５：第２の塗膜の形成，液晶層の形成）
続いて、下記の液晶層形成用材料を調製した。
(ST4, ST5: formation of second coating film, formation of liquid crystal layer)
Then, the following liquid crystal layer forming material was prepared.
−液晶層形成用材料の調製−
逆波長分散液晶性化合物 Ｒ−３ １００質量部
光重合開始剤 ３．０質量部
（イルガキュア８１９、ＢＡＳＦ（株）製）
含フッ素化合物Ａ ０．８質量部
架橋性ポリマー Ｏ−２ ０．３質量部
クロロホルム ５８８質量部
-Preparation of liquid crystal layer forming material-
Reverse wavelength dispersion liquid crystalline compound R-3 100 parts by mass Photopolymerization initiator 3.0 parts by mass (Irgacure 819, manufactured by BASF Ltd.)
Fluorine-containing compound A 0.8 part by mass Crosslinkable polymer O-2 0.3 part by mass Chloroform 588 parts by mass
配向層上に液晶層形成用材料を、バーコーターを用いて塗布した。膜面温度１００℃で６０秒間加熱熟成し、７０℃まで冷却した後に、空気下にて空冷メタルハライドランプ（アイグラフィックス（株）製）を用いて１０００ｍJ／ｃｍ２の紫外線を照射して、その配向状態を固定化することにより液晶層を形成した。形成された液晶層は、偏光照射方向に対し遅相軸方向が直交（すなわち、偏光板の吸収軸とも直交）であった（逆波長分散液晶性化合物が偏光照射方向に対して直交に配向していた）。自動複屈折率計（ＫＯＢＲＡ−２１ＡＤＨ、王子計測機器（株）社製）を用いて、Ｒｅの光入射角度依存性および光軸のチルト角を測定したところ、波長５５０ｎｍにおいてＲｅが１３０ｎｍ、Ｒｔｈが６５ｎｍ、Ｒｅ（４５０）／Ｒｅ（５５０）が０．８３、Ｒｅ（６５０）／Ｒｅ（５５０）が１．０５、光軸のチルト角は０°で、逆波長分散液晶性化合物はホモジニアス配向であった。 The liquid crystal layer forming material was applied onto the alignment layer using a bar coater. After heat aging at a film surface temperature of 100 ° C. for 60 seconds and cooling to 70 ° C., it was irradiated with 1000 mJ / cm 2 of ultraviolet rays using an air-cooled metal halide lamp (manufactured by Eye Graphics Co., Ltd.) under air, A liquid crystal layer was formed by fixing the alignment state. In the formed liquid crystal layer, the slow axis direction was orthogonal to the polarized light irradiation direction (that is, also orthogonal to the absorption axis of the polarizing plate) (the reverse wavelength dispersion liquid crystalline compound was aligned perpendicular to the polarized light irradiation direction). Was). When the light incident angle dependency of Re and the tilt angle of the optical axis were measured using an automatic birefringence meter (KOBRA-21ADH, manufactured by Oji Scientific Instruments Co., Ltd.), Re was 130 nm and Rth was 550 nm. 65 nm, Re (450) / Re (550) is 0.83, Re (650) / Re (550) is 1.05, the tilt angle of the optical axis is 0 °, and the reverse wavelength dispersion liquid crystal compound is in a homogeneous alignment. there were.
［実施例２］
ニップロールを使用しなかった以外は、実施例１と同様に位相差フィルムを作製した。
[Example 2]
A retardation film was produced in the same manner as in Example 1 except that the nip roll was not used.
［実施例３］
連続フィルム支持体１１がヒートロール２０に接するようにし、第１の塗膜が接するニップロールの表面粗さＲｚを２にした以外は、実施例１と同様に位相差フィルムを作製した。
[Example 3]
A retardation film was produced in the same manner as in Example 1 except that the continuous film support 11 was in contact with the heat roll 20 and the surface roughness Rz of the nip roll with which the first coating film was in contact was 2.
［実施例４］
ヒートロール２０の温度を５０℃にした以外は、実施例１と同様に位相差フィルムを作製した。
[Example 4]
A retardation film was produced in the same manner as in Example 1 except that the temperature of the heat roll 20 was set to 50 ° C.
［実施例５］
搬送速度を５０ｍ／ｍｉｎにし、ラップ時間を０．１９secにした以外は、実施例１と同様に位相差フィルムを作製した。
[Example 5]
A retardation film was produced in the same manner as in Example 1 except that the transport speed was 50 m / min and the wrap time was 0.19 sec.
［実施例６］
ニップロールを用いなかった以外は、実施例５と同様に位相差フィルムを作製した。
[Example 6]
A retardation film was produced in the same manner as in Example 5 except that the nip roll was not used.
［実施例７］
搬送速度を３０ｍ／ｍｉｎにし、ラップ時間を０．１０secにした以外は、実施例６と同様に位相差フィルムを作製した。
[Example 7]
A retardation film was produced in the same manner as in Example 6 except that the transport speed was 30 m / min and the wrap time was 0.10 sec.
［実施例８］
線圧を５Ｎ／ｃｍにした以外は、実施例１と同様に位相差フィルムを作製した。
[Example 8]
A retardation film was produced in the same manner as in Example 1 except that the linear pressure was 5 N / cm.
［比較例１］
連続フィルム支持体１１側をヒートロール２０に接するようにし、第１の塗膜が接するニップロールを使用しなかった以外には、実施例１と同様に位相差フィルムを作製した。
[Comparative Example 1]
A retardation film was produced in the same manner as in Example 1 except that the continuous film support 11 side was in contact with the heat roll 20 and no nip roll in contact with the first coating film was used.
［比較例２］
搬送速度３０ｍ／ｍｉｎとし、ヒートロール２０に巻き掛けず、加熱も行わなかった。
[Comparative example 2]
The conveyance speed was 30 m / min, the heating roller 20 was not wound, and heating was not performed.
［輝点評価方法］
作製した位相差フィルムの両側に透過光を遮断（クロスニコル配置）するように２枚の偏光板を配置した後、片側から光を照射し、反対側から光学顕微鏡（100倍）で観察して輝点の数を測定した。
[Bright spot evaluation method]
After arranging two polarizing plates on both sides of the produced retardation film so as to block transmitted light (crossed Nicols arrangement), irradiate light from one side and observe with an optical microscope (100x) from the other side. The number of bright spots was measured.
（評価基準）
Ａ：５個／ｍｍ２以下
Ｂ：５個／ｍｍ２より多く４０個／ｍｍ２以下
Ｃ：４０個／ｍｍ２より多く６０個／ｍｍ２以下
Ｄ：６１個／ｍｍ２以上
(Evaluation criteria)
A: 5 pieces / mm 2 or less B: 5 pieces / mm 2 or more and 40 pieces / mm 2 or less C: 40 pieces / mm 2 or more and 60 pieces / mm 2 or less D: 61 pieces / mm 2 or more
表１に示すように、本発明の位相差フィルムは、第１の塗膜１２に押圧力が作用していない比較例１および加熱しない比較例２に比べ、良好に輝点が低減されている。
第１の塗膜１２とヒートロール２０が接し、かつニップロールでフィルム１０を挟んだ実施例１、搬送張力のみで押圧力を作用させて加熱をした実施例２、および第１の塗膜１２がニップロール３０側にして加熱した実施例３から、第１の塗膜１２がヒートロール２０側に配置され、かつ、ニップロール３０で挟まれた方がより好ましいことがわかる。
また、実施例１および実施例４から、ヒートロール２０はより高い温度が好ましいことがわかる。
また、実施例５、実施例６、および実施例７からラップ時間はより長い方が好ましいことがわかる。
また、実施例１および実施例８から、線圧は高い方が好ましいことがわかる。
As shown in Table 1, in the retardation film of the present invention, the bright spots are satisfactorily reduced as compared with Comparative Example 1 in which the pressing force does not act on the first coating film 12 and Comparative Example 2 in which the first coating film 12 is not heated. ..
Example 1 in which the first coating film 12 and the heat roll 20 were in contact with each other and the film 10 was sandwiched by the nip rolls, Example 2 in which the pressing force was applied only by the conveying tension to heat the film 10, and the first coating film 12 were From Example 3 in which heating is performed on the nip roll 30 side, it is more preferable that the first coating film 12 is disposed on the heat roll 20 side and sandwiched by the nip roll 30.
Further, it can be seen from Examples 1 and 4 that the heat roll 20 preferably has a higher temperature.
Further, it is understood from Examples 5, 6, and 7 that a longer lap time is preferable.
Further, it can be seen from Examples 1 and 8 that a higher linear pressure is preferable.
１０ フィルム
１１ 連続フィルム支持体
１２ 第１の塗膜
２０ ヒートロール
２１ 温度制御手段
３０ ニップロール
４０ 棒状光源
４１ 凹面反射鏡
４２ 平行板
４３ ルーバー
４４ ワイヤーグリッド偏光子
５１ 送出しロール
５２ ダイコーター
５３ 温調板
５４ 乾燥機
５５ 巻き取りロール
θ ラップ角
10 film 11 continuous film support 12 first coating film 20 heat roll 21 temperature control means 30 nip roll 40 rod-shaped light source 41 concave mirror 42 parallel plate 43 louver 44 wire grid polarizer 51 delivery roll 52 die coater 53 temperature control plate 54 Dryer 55 Take-up roll θ Wrap angle
Claims (9)
前記第１の塗膜に偏光を照射することにより前記配向規制力を付与して前記配向層を形成する工程、および
前記配向層上に前記液晶化合物を含む液晶層形成用材料を塗布および乾燥して第２の塗膜を形成する工程と、
前記第２の塗膜中の前記液晶化合物を配向させ、該配向を固定して液晶層を形成する工程と、
を備える位相差フィルムの製造方法であって、
前記第１の塗膜を形成する工程の後、前記配向層を形成する工程の前に、前記第１の塗膜に押圧力を作用させた状態で、前記第１の塗膜をヒートロール上で加熱する工程を有する位相差フィルムの製造方法。 A step of forming a first coating film by coating and drying an alignment layer forming material for forming an alignment layer having an alignment regulating force on a liquid crystal compound, on a transported continuous film support,
A step of applying the alignment regulating force by irradiating the first coating film with polarized light to form the alignment layer, and applying and drying a liquid crystal layer forming material containing the liquid crystal compound on the alignment layer. Forming a second coating film,
Aligning the liquid crystal compound in the second coating film and fixing the alignment to form a liquid crystal layer;
A method of manufacturing a retardation film comprising:
After the step of forming the first coating film and before the step of forming the alignment layer, the first coating film is placed on a heat roll while a pressing force is applied to the first coating film. The manufacturing method of the retardation film which has the process of heating by.
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| PCT/JP2018/005493 WO2018179973A1 (en) | 2017-03-29 | 2018-02-16 | Method for manufacturing phase difference film |
| KR1020197021245A KR20190094459A (en) | 2017-03-29 | 2018-02-16 | Manufacturing method of retardation film |
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