CN114341685A - Optical film and method for producing optical film - Google Patents
Optical film and method for producing optical film Download PDFInfo
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- CN114341685A CN114341685A CN202080062840.4A CN202080062840A CN114341685A CN 114341685 A CN114341685 A CN 114341685A CN 202080062840 A CN202080062840 A CN 202080062840A CN 114341685 A CN114341685 A CN 114341685A
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- liquid crystal
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- optical film
- cholesteric
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- 238000001308 synthesis method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides an optical film and a method for manufacturing the optical film, the optical film comprises a support and a cholesteric liquid crystal layer arranged on the support, the cholesteric liquid crystal layer comprises an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from the surface of the cholesteric liquid crystal layer opposite to the surface opposite to the support to face the thickness direction.
Description
Technical Field
The present invention relates to an optical film and a method for manufacturing the optical film.
Background
In a coating process using a roll-to-roll coating apparatus, periodic film thickness variations are likely to occur on the surface of a coating film due to disturbances occurring in the process, such as vibration, pulsation of liquid feed, and uneven conveyance of a support. In cholesteric liquid crystal films used for decorative films, optical elements, and the like, color unevenness due to film thickness variation is easily observed, and suppression of color unevenness is required.
The reason why color unevenness was observed was as follows: since the film thickness periodically varies in the direction of application, the orientation of the director loss of the liquid crystal molecules present on the surface of the applied film periodically changes, and the surface reflectance periodically changes. When the film thickness variation is suppressed, color unevenness is suppressed. However, it is difficult to completely suppress the interference generated in the process. Therefore, conventionally, in order to improve the coating liquid, a treatment for reducing the viscosity of the coating liquid by reducing the solid content concentration of the coating liquid has been performed. However, the degree of suppressing color unevenness is insufficient.
For example, as a method for producing an optically uniform film, japanese patent application laid-open No. 2006-78617 discloses a method for producing an optical film comprising: the production method comprises a step of applying a polymerizable composition comprising a polymerizable nematic liquid crystal compound, a polymerizable chiral agent and a polymerization initiator to a base material together with a solvent; and a step of irradiating the substrate coated with the polymerizable composition with radiation, wherein the amount of the polymerizable chiral agent is 15 to 18 (weight ratio) relative to 100 total solid content of the polymerizable composition, and the optical film has a phase separation structure of at least 2 layers including a layer having a spirally curved molecular structure and a layer having an isotropic molecular structure.
Disclosure of Invention
Technical problem to be solved by the invention
In the method for producing an optical film disclosed in jp 2006-78617 a, an optical film in which a layer having a molecular structure that curves in a spiral, a layer having an isotropic molecular structure, and a layer having a molecular structure that curves in a spiral are sequentially stacked on a substrate can be obtained. That is, since the outermost layer is a layer having a molecular structure that is spirally curved, color unevenness cannot be suppressed.
The present invention has been made in view of such circumstances, and according to one embodiment of the present invention, an optical film and a method for manufacturing an optical film can be provided, which can exhibit optical characteristics of cholesteric liquid crystal and suppress color unevenness.
Means for solving the technical problem
The present invention includes the following modes.
< 1> the present invention provides an optical film comprising a support and a cholesteric liquid crystal layer provided on the support, wherein the cholesteric liquid crystal layer comprises an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from the surface of the cholesteric liquid crystal layer on the side opposite to the surface facing the support in the thickness direction.
< 2> the optical film according to < 1>, wherein,
there are at least 1 intermediate layer between the support and the cholesteric liquid crystal layer.
< 3> the optical film according to < 2>, wherein,
the at least 1 intermediate layer is at least one layer selected from the group consisting of other cholesteric liquid crystal layers, nematic liquid crystal layers and smectic liquid crystal layers, and alignment layers.
< 4> the optical film according to any one of < 1> to < 3>, wherein,
the thickness of the isotropic phase region is greater than 0% and 27% or less with respect to the thickness of the cholesteric liquid crystal layer.
< 5 > a method for producing an optical film, which comprises applying a polymerizable liquid crystal composition comprising a polymerizable liquid crystal compound and a chiral compound on a support, to produce the optical film of any one of < 1> to < 4 >; a step of irradiating the coated side of the support, on which the polymerizable liquid crystal composition is coated, with infrared light at an incident angle of 40 ° or more with respect to the normal direction of the support, and cooling the non-coated side of the polymerizable liquid crystal composition, on which the support is not coated; and irradiating the support with ultraviolet light while maintaining a temperature higher than the liquid crystal-isotropic phase transition temperature on the coated side and a temperature lower than the liquid crystal-isotropic phase transition temperature on the non-coated side.
< 6 > the method for producing an optical film according to < 5 >, wherein,
the content of the chiral compound is 3 to 12 parts by mass per 100 parts by mass of the polymerizable liquid crystal compound.
< 7 > the method for producing an optical film according to < 5 > or < 6 >, wherein,
the difference between the temperature of the coating side and the temperature of the non-coating side is 20 to 80 ℃.
Effects of the invention
According to one embodiment of the present invention, an optical film and a method for manufacturing an optical film can be provided, which can exhibit optical characteristics of cholesteric liquid crystals and can suppress color unevenness.
Detailed Description
The optical film and the method for producing the optical film of the present invention will be described in detail below.
In the present specification, the numerical range expressed by the term "to" means a range in which the numerical values before and after the term "to" are included as the minimum value and the maximum value, respectively.
In the numerical ranges recited in the present specification, an upper limit or a lower limit recited in a certain numerical range may be replaced with an upper limit or a lower limit recited in another numerical range recited in a stepwise manner. In addition, in the numerical ranges described in the present specification, the upper limit value or the lower limit value described in a certain numerical range may be replaced with the values shown in the examples.
In the present specification, the amount of each component in the composition refers to the total amount of a plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
In the present specification, a combination of two or more preferred embodiments is a more preferred embodiment.
In the present specification, the term "step" includes not only an independent step but also a step that can achieve the intended purpose of the step even when the step is not clearly distinguished from other steps.
[ optical film ]
The optical film of the present invention includes a support and a cholesteric liquid crystal layer provided on the support, wherein the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from a surface of the cholesteric liquid crystal layer opposite to a surface facing the support in a thickness direction.
As a method for producing an optical film having optical uniformity, for example, japanese patent application laid-open No. 2006-78617 discloses a method for producing an optical film comprising: the production method comprises a step of applying a polymerizable composition comprising a polymerizable nematic liquid crystal compound, a polymerizable chiral agent and a polymerization initiator to a base material together with a solvent; and a step of irradiating the substrate coated with the polymerizable composition with radiation, wherein the amount of the polymerizable chiral agent is 15 to 18 (weight ratio) relative to 100 total solid content of the polymerizable composition. According to this production method, an optical film can be obtained in which a layer having a molecular structure that is spirally curved, a layer having an isotropic molecular structure, and a layer having a molecular structure that is spirally curved are sequentially stacked on a base. That is, the outermost layer is a layer having a molecular structure that is spirally bent (cholesteric liquid crystal layer fixed in a cholesteric phase).
In a coating process using a roll-to-roll coating apparatus, periodic film thickness variations are likely to occur on the surface of a coating film due to disturbances occurring in the process, such as vibration, pulsation of liquid feed, and uneven conveyance of a support. Since the film thickness periodically varies in the direction of application, the orientation of the director loss of the liquid crystal molecules present on the surface of the applied film periodically changes. As a result, the surface reflectance was periodically changed in the coating direction, and color unevenness was observed. In the optical film obtained by the production method disclosed in jp 2006-78617 a, color unevenness occurs because the outermost layer is a cholesteric liquid crystal layer fixed in a cholesteric phase.
In contrast, an optical film according to an embodiment of the present invention includes a support and a cholesteric liquid crystal layer provided on the support, the cholesteric liquid crystal layer including an isotropic phase region and a cholesteric phase region, the isotropic phase region being formed from a surface of the cholesteric liquid crystal layer opposite to a surface facing the support in a thickness direction. Since the orientation of the director loss of the liquid crystal molecules is random on the surface of the cholesteric liquid crystal layer, the occurrence of color unevenness can be suppressed, and the optical characteristics of the cholesteric liquid crystal can be exhibited by having a cholesteric phase region.
Hereinafter, each structure of the optical film of the present invention will be described in detail.
(support)
The optical film of the present invention has a support. The kind of the support is not particularly limited, and examples thereof include a glass plate, a quartz plate, and a polymer film is preferable. Examples of the polymer film include transparent films such as polyester films (for example, films of polyethylene terephthalate, polyethylene naphthalate, and the like), cellulose films (for example, films of cellulose acetate butyrate, triacetyl cellulose (TAC), and the like), polycarbonate films, poly (meth) acrylic films (films of polymethyl methacrylate, and the like), polystyrene films (films of polystyrene, acrylonitrile styrene copolymer, and the like), polyolefin films (for example, films of polyethylene, polypropylene, cyclic or norbornene-structured polyolefin, ethylene-propylene copolymer, and the like), polyamide films (for example, films of nylon, aromatic polyamide, and the like), polyimide films, polysulfone films, polyether sulfone films, polyether ether ketone films, polyphenylene sulfide films, polyvinyl alcohol films, polyvinylidene chloride films, polyvinyl butyral films, polyoxymethylene films, epoxy resin films, and films formed of mixed polymers of the above-mentioned polymer materials.
The support in the optical film according to the embodiment of the present invention may be a support used in film formation, or may be another support in which a support used in film formation is used as a temporary support and the temporary support is peeled off and then bonded.
The thickness of the support is not particularly limited, but is preferably 5 μm to 100 μm, and more preferably 10 μm to 50 μm, in consideration of manufacturing applicability, manufacturing cost, application of the optical film, and the like.
The support may also be a support subjected to a rubbing treatment. The rubbing treatment can be performed, for example, by pressing a roll wound with a rubbing cloth against a support body with a predetermined pressure and rotating the support body. Examples of the rubbing cloth include paper, gauze, felt, rubber, nylon, rayon, and polyester fibers.
(cholesteric liquid Crystal layer)
The optical film of the present invention has a cholesteric liquid crystal layer provided on a support. In the optical film of the present invention, the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from a surface of the cholesteric liquid crystal layer opposite to a surface facing the support in a thickness direction. In the optical film according to an embodiment of the present invention, the cholesteric liquid crystal layer including the isotropic phase region and the cholesteric liquid crystal region is preferably the outermost layer.
In the present invention, a layer including at least a cholesteric phase region is referred to as a cholesteric liquid crystal layer. The cholesteric phase region is a region formed of a cholesteric phase in which rod-shaped liquid crystal molecules or discotic liquid crystal molecules are arranged in a spiral shape. Whether or not the layer includes a cholesteric phase region can be determined by using a Scanning Electron Microscope (SEM) by the following method, for example.
A film piece having a width of 5 mm. times.length of 2mm was cut out from the optical film using a roller cutter. The film pieces were embedded in an epoxy resin, and cut in the thickness direction using a microtome (product name "RM 2265", manufactured by Leica Biosystems). The SEM image of the cross section was observed using a scanning electron microscope (model "S-4800", manufactured by Hitachi High-Technologies Corporation, observation magnification: 10000 times, acceleration voltage: 2.0kV), and it was confirmed whether or not there was a thick and thin stripe pattern resulting from a change in the refractive index of the cholesteric phase. When the stripe pattern was confirmed, it was determined that the cholesteric liquid crystal layer included cholesteric phase regions.
The isotropic phase region is a region in which the liquid crystal molecules are randomly aligned. Whether or not the layer includes the isotropic phase region can be determined by the following method, for example.
The SEM image of the cross section was observed in the same manner as the determination of whether or not the layer included the cholesteric phase region. It was confirmed whether or not there was a light and dark stripe pattern resulting from a change in the refractive index of the cholesteric phase. When no color shade is present and no stripe pattern is observed, it is determined that the layer includes the isotropic phase region.
In the present invention, the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from a surface (i.e., an air interface) of the cholesteric liquid crystal layer on a side opposite to a surface facing the support in a thickness direction. That is, in the monolayer, an isotropic phase region and a cholesteric phase region are present at least in the thickness direction. The presence or absence of the isotropic phase region and the cholesteric phase region in the single layer, and the presence or absence of the isotropic phase region formed in the thickness direction from the air interface, can be determined, for example, by the following method.
Similarly to the determination of whether or not the layer includes a cholesteric phase region, the SEM image of the cross section was observed to confirm whether or not there was a light and dark stripe pattern resulting from a change in refractive index of the cholesteric phase. When a stripe pattern is observed, indicating that the difference in shade of the stripe pattern decreases from the interface on the side opposite to the air interface toward the air interface, and finally the difference in shade is not observed, it is determined that an isotropic phase region and a cholesteric phase region are present at least in the thickness direction in the single layer, and an isotropic phase region is formed from the air interface toward the thickness direction.
In addition, in the case of a 2-layer laminated structure, which is a laminated body in which an isotropic layer formed only of an isotropic phase region and a cholesteric liquid crystal layer formed only of a cholesteric phase region are sequentially laminated, it was confirmed that the difference in shade, which indicates a stripe pattern, was constant in the cholesteric liquid crystal layer when a SEM image of a cross section was observed. Therefore, the laminate and the single layer including the isotropic phase region and the cholesteric phase region can be discriminated.
In the present invention, the thickness of the isotropic phase region is preferably more than 0% and 27% or less, more preferably more than 0% and 20% or less, and still more preferably more than 0% and 15% or less, with respect to the thickness of the cholesteric liquid crystal layer. If the thickness of the isotropic phase region is more than 0%, color unevenness can be suppressed. On the other hand, it is preferable that the thickness of the isotropic phase region is 27% or less because the optical characteristics of the cholesteric liquid crystal can be more exhibited. The thickness of the isotropic phase region can be measured, for example, by the following method.
Similarly to the determination of whether or not the layer includes a cholesteric phase region, the SEM image of the cross section was observed to confirm whether or not there was a light and dark stripe pattern resulting from a change in refractive index of the cholesteric phase. As the thickness of the isotropic phase region, the distance from the following position to the air interface was measured: the observation of the stripe pattern showed that the difference in shade of the stripe pattern decreased from the interface on the opposite side of the air interface toward the air interface, and finally, the difference in shade was not confirmed.
When the thickness of the cholesteric liquid crystal layer is measured, the interface between the cholesteric liquid crystal layer and another layer can be determined by the following method, for example.
In the optical film according to one embodiment of the present invention, when a cholesteric liquid crystal layer including an isotropic phase region and a cholesteric liquid crystal region is formed on a surface of a support, an interface between the support and the cholesteric liquid crystal layer can be identified by observing an SEM image of a cross section. In the case where an intermediate layer is provided between the cholesteric liquid crystal layer and the support as described later, if the intermediate layer in contact with the cholesteric liquid crystal layer is a layer other than the cholesteric liquid crystal layer, the interface between the cholesteric liquid crystal layer and the intermediate layer can be identified by observing an SEM image of the cross section.
When the intermediate layer in contact with the cholesteric liquid crystal layer is a cholesteric liquid crystal layer formed only of a cholesteric phase region, the interface can be determined by, for example, the following method. A cholesteric liquid crystal layer including an isotropic phase region and a cholesteric phase region will be described as a specific cholesteric liquid crystal layer, and a cholesteric liquid crystal layer as an intermediate layer will be described as an intermediate cholesteric liquid crystal layer.
In the case of a cholesteric liquid crystal layer, if SEM images of the cross section are observed, a light and dark stripe pattern resulting from a change in refractive index of the cholesteric phase can be confirmed. The 1-period component of the darker and lighter regions of the fringe pattern corresponds to 180 degrees of the bend of the liquid crystal. Therefore, the 2-period component of the darker region, the lighter region, the darker region, and the lighter region of the fringe pattern corresponds to 360 degrees of the bend of the liquid crystal. That is, the width of the 2-period component indicating the shade of the stripe pattern corresponds to the length of the pitch of the helical structure in the cholesteric phase. In the case of a laminate in which the intermediate cholesteric liquid crystal layer is in contact with the specific cholesteric liquid crystal layer, it can be determined that the position at which the length of the pitch of the helical structure in the cholesteric phase changes in the thickness direction is the interface between the specific cholesteric liquid crystal layer and the intermediate cholesteric liquid crystal layer.
In addition, even if the pitch of the helical structure in the cholesteric phase is the same in the specific cholesteric liquid crystal layer and the intermediate cholesteric liquid crystal layer, the interface between the specific cholesteric liquid crystal layer and the intermediate cholesteric liquid crystal layer can be specified. In the specific cholesteric liquid crystal layer, the difference in shade indicating the stripe pattern becomes smaller from the interface on the side opposite to the air interface toward the air interface, whereas in the intermediate cholesteric liquid crystal layer, the difference in shade indicating the stripe pattern is constant. Therefore, by observing the difference in shade, it is possible to specify that the position where the difference in shade begins to decrease is the interface between the specific cholesteric liquid crystal layer and the intermediate cholesteric liquid crystal layer.
The thickness of the cholesteric liquid crystal layer including the isotropic phase region and the cholesteric phase region is not particularly limited, but is preferably 1 μm to 20 μm, and more preferably 2 μm to 10 μm.
(intermediate layer)
In the optical film according to an embodiment of the present invention, at least 1 intermediate layer may be provided between the support and the cholesteric liquid crystal layer. The kind of the intermediate layer is not particularly limited, but is preferably at least one layer selected from the group consisting of other cholesteric liquid crystal layers, nematic liquid crystal layers and smectic liquid crystal layers, and alignment layers. The number of intermediate layers may be 1 or 2 or more.
The cholesteric liquid crystal layer is a layer having a cholesteric phase in which rod-like liquid crystal compounds or discotic liquid crystal compounds are spirally arranged. The cholesteric liquid crystal layer can be formed by: for example, after a polymerizable liquid crystal composition containing a polymerizable liquid crystal compound and a chiral compound is applied, the composition is dried at a temperature lower than the liquid crystal-isotropic phase transition temperature, and irradiated with ultraviolet rays. The pitch of the helical structure in the cholesteric phase can be adjusted by changing the type of the polymerizable liquid crystal compound, the type of the chiral compound, or the content of the chiral compound relative to the polymerizable liquid crystal compound. The selective reflection wavelength will change if the pitch of the helical structure in the cholesteric phase changes.
The nematic liquid crystal layer is a layer having a nematic phase in which rod-like liquid crystal compounds are one-dimensionally aligned. The nematic liquid crystal layer can be formed by the following method: for example, after a polymerizable liquid crystal composition containing a polymerizable nematic liquid crystal compound is applied, the composition is dried at a temperature lower than the liquid crystal-isotropic phase transition temperature, and irradiated with ultraviolet rays.
The smectic liquid crystal layer is a layer having a smectic phase formed by one-dimensionally aligning a rod-like liquid crystal compound and having a layered structure. The smectic liquid crystal layer can be formed by the following method: for example, after a polymerizable liquid crystal composition containing a polymerizable smectic liquid crystal compound is applied, the composition is dried at a temperature lower than the liquid crystal-isotropic phase transition temperature, and irradiated with ultraviolet rays.
The alignment layer is a layer having an alignment regulating force for the liquid crystal compound. Examples of the alignment layer include a rubbing-treated alignment layer and a photo-alignment layer.
The thickness of the intermediate layer is not particularly limited, and is, for example, 0.5 to 5.0. mu.m.
(method for producing optical film)
The method for manufacturing the optical film of the present invention includes: a step of applying a polymerizable liquid crystal composition containing a polymerizable liquid crystal compound and a chiral compound onto a support (hereinafter referred to as "application step"); a step of irradiating the coated side of the support, on which the polymerizable liquid crystal composition is coated, with infrared light at an incident angle of 40 ° or more with respect to the normal direction of the support, and cooling the non-coated side of the polymerizable liquid crystal composition, on which the support is not coated (hereinafter referred to as "infrared irradiation and cooling step"); and a step of irradiating the support with ultraviolet light while maintaining a temperature higher than the liquid crystal-isotropic phase transition temperature on the coating side and a temperature lower than the liquid crystal-isotropic phase transition temperature on the non-coating side (hereinafter referred to as "ultraviolet irradiation step").
< coating Process >
The method for producing an optical film of the present invention includes a step of applying a polymerizable liquid crystal composition containing a polymerizable liquid crystal compound and a chiral compound on a support. The support is not described here because it is as described above.
[ polymerizable liquid Crystal Compound ]
The polymerizable liquid crystal composition contains a polymerizable liquid crystal compound. The polymerizable liquid crystal compound is a liquid crystal compound having a polymerizable group. The liquid crystal compound may be a rod-like liquid crystal compound or a discotic liquid crystal compound, but is preferably a rod-like liquid crystal compound.
Examples of the rod-like liquid crystal compound include a rod-like nematic liquid crystal compound. As the rod-like nematic liquid crystal compound, preferably used are an azomethine-based compound, an azoxy-based compound, a cyanobiphenyl-based compound, a cyanophenyl ester-based compound, a benzoate-based compound, a cyclohexanecarboxylic acid phenyl ester-based compound, a cyanophenylcyclohexane-based compound, a cyano-substituted phenylpyrimidine-based compound, an alkoxy-substituted phenylpyrimidine-based compound, a phenyldioxane-based compound, a tolan-based compound, or an alkenylcyclohexylbenzonitrile-based compound. The polymerizable liquid crystal compound may be a low molecular liquid crystal compound or a high molecular liquid crystal compound.
The polymerizable liquid crystal compound is obtained by introducing a polymerizable group into a liquid crystal compound. Examples of the polymerizable group include a polymerizable unsaturated group, an epoxy group, and an aziridine group. Among these, the polymerizable group is preferably a polymerizable unsaturated group, and particularly preferably an ethylenically unsaturated group. The number of the polymerizable groups of the polymerizable liquid crystal compound is preferably 1 to 6, and more preferably 1 to 3. From the viewpoint of durability of the optical film, the polymerizable liquid crystal compound further preferably has 2 polymerizable groups in the molecule.
Examples of the polymerizable liquid crystal compound include compounds described in Makromol. chem., 190, 2255 (1989), Advanced Materials 5, 107 (1993), U.S. Pat. No. 4683327, U.S. Pat. No. 5622648, U.S. Pat. No. 5770107, International publication No. 95/22586, International publication No. 95/24455, International publication No. 97/00600, International publication No. 98/23580, International publication No. 98/52905, Japanese patent laid-open No. 1-272551, Japanese patent laid-open No. 6-16616, Japanese patent laid-open No. 7-110469, Japanese patent laid-open No. 11-80081, and Japanese patent laid-open No. 2001-328973.
As the polymerizable liquid crystal compound, for example, a compound represented by the following general formula (1) is preferably used.
[ chemical formula 1]
(1)Q1-L1-A1-L3-M-L4-A2-L2-Q2
In the general formula (1), Q1And Q2Each independently is a polymerizable group, L1、L2、L3And L4Each independently represents a single bond or a 2-valent linking group, A1And A2Each independently represents a 2-valent hydrocarbon group having 2 to 20 carbon atoms, and M represents a mesogenic group.
As Q1And Q2Examples of the polymerizable group include the polymerizable groups of the polymerizable liquid crystal compounds described above, and preferred examples are the same.
As L1、L2、L3And L4The linking group is preferably a divalent linking group selected from the group consisting of-O-, -S-, -CO-, -NR-, -CO-O-, -O-CO-O-, -CO-NR-, -NR-CO-, -O-CO-NR-, -NR-CO-O-, and NR-CO-NR-. Wherein R is an alkyl group having 1 to 7 carbon atoms or a hydrogen atom.
In the general formula (1), Q1-L1-and Q2-L2-is preferably CH2＝CH-CO-O-、CH2＝C(CH3) -CO-O-and CH2Most preferred is CH (c) (cl) -CO-O —2＝CH-CO-O-。
A1And A2The 2-valent hydrocarbon group having 2 to 20 carbon atoms is preferably an alkylene group, alkenylene group or alkynylene group having 2 to 12 carbon atoms, and particularly preferablyIs an alkylene group having 2 to 12 carbon atoms. The 2-valent hydrocarbon group is preferably a chain, and may contain non-adjacent oxygen atoms or sulfur atoms. The 2-valent hydrocarbon group may have a substituent, and examples of the substituent include a halogen atom (e.g., fluorine, chlorine, and bromine), a cyano group, a methyl group, and an ethyl group.
The mesogenic group represented by M is a group representing a main skeleton of a liquid crystal molecule contributing to formation of a liquid crystal.
The mesogenic group represented by M is not particularly limited, and for example, "FlusseKristalle in Tabellen II" (VEB Deutsche Verlag fur Grundstoff Industrie, Leipzig, 1984), particularly, the descriptions on pages 7 to 16, the editorial Committee for liquid crystal display, the liquid crystal display (Bolus, 2000), and particularly, the description on Chapter 3 can be referred to.
More specifically, examples of the mesogenic group represented by M include the structures described in paragraph 0086 of Japanese patent application laid-open No. 2007-279688.
The mesogenic group is preferably a group containing at least one cyclic structure selected from the group consisting of an aromatic hydrocarbon group, a heterocyclic group, and an alicyclic group, for example. Among them, the mesogenic group is preferably a group containing an aromatic hydrocarbon group, more preferably a group containing 2 to 5 aromatic hydrocarbon groups, and further preferably a group containing 3 to 5 aromatic hydrocarbon groups.
The mesogenic group is further preferably the following group: a group comprising 3 to 5 phenylene groups and having the phenylene groups attached as-CO-O-.
The cyclic structure contained in the mesogenic group may further have an alkyl group having 1 to 10 carbon atoms such as a methyl group as a substituent.
Specific examples of the compound represented by the following general formula (1) are shown below, but the compound is not limited thereto.
[ chemical formula 2]
The polymerizable liquid crystal compound contained in the polymerizable liquid crystal composition may be 1 type, or 2 or more types.
The content of the polymerizable liquid crystal compound is preferably 70 to 99% by mass, more preferably 80 to 98% by mass, and particularly preferably 85 to 95% by mass, based on the total solid content of the polymerizable liquid crystal composition.
[ chiral compound ]
The polymerizable liquid crystal composition contains a chiral compound. The chiral compound has an effect of inducing a helical structure of the polymerizable liquid crystal compound. The direction of bending or the pitch of the induced helix varies depending on the kind of the chiral compound.
The kind of chiral compound is not particularly limited, and may be a known chiral compound (for example, as described in the handbook of liquid crystal devices, chapter 3, items 4 to 3, chiral agents for TN and STN, page 199, edited by 142 th committee of Japan society for academic interest, 1989). Examples of the chiral compound include isosorbide derivatives and isomannide derivatives.
The chiral compound usually contains an asymmetric carbon atom, but may be a compound containing no asymmetric carbon atom as long as it has chirality. Examples of the compound not containing an asymmetric carbon atom include axially asymmetric compounds having a binaphthyl structure, spirally asymmetric compounds having a spiroalkene structure, and plane asymmetric compounds having a cyclic-aromatic structure.
The chiral compound may have a polymerizable group. When the chiral compound has a polymerizable group, a polymer having a structural unit derived from the polymerizable liquid crystal compound and a structural unit derived from the chiral compound can be formed by a polymerization reaction of the chiral compound and the polymerizable liquid crystal compound. When the chiral compound has a polymerizable group, the polymerizable group is preferably the same kind of group as the polymerizable group of the polymerizable liquid crystal compound. Therefore, the polymerizable group of the chiral compound is preferably a polymerizable unsaturated group, an epoxy group or an aziridine group, more preferably a polymerizable unsaturated group, and particularly preferably an ethylenically unsaturated group. Also, the chiral compound itself may be a liquid crystal compound.
In the polymerizable liquid crystal composition, the content of the chiral compound is preferably 2 to 12 parts by mass, more preferably 3 to 10 parts by mass, and still more preferably 4 to 8 parts by mass, based on 100 parts by mass of the content of the polymerizable liquid crystal compound.
The polymerizable liquid crystal composition may contain, in addition to the polymerizable liquid crystal compound and the chiral compound, other components such as a polymerization initiator, an alignment control agent, a crosslinking assistant, an infrared absorber, and a solvent, as required.
[ polymerization initiator ]
The polymerizable liquid crystal composition preferably contains a polymerization initiator. The polymerization initiator is preferably a photopolymerization initiator. The photopolymerization initiator is preferably a compound having an action of generating a radical as a polymerization active species by irradiation of ultraviolet rays.
Examples of the photopolymerization initiator include an alkylphenone-based photopolymerization initiator, an acylphosphine oxide-based photopolymerization initiator, an intramolecular hydrogen abstraction-type photopolymerization initiator, an oxime ester-based photopolymerization initiator, and a cationic photopolymerization initiator. Among them, the photopolymerization initiator is preferably an acylphosphine oxide-based photopolymerization initiator, and specifically, is preferably (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide or bis (2,4, 6-trimethylbenzoyl) phenylphosphine oxide.
The polymerizable liquid crystal composition may contain 1 or 2 or more kinds of polymerization initiators.
In the polymerizable liquid crystal composition, the content of the polymerization initiator is preferably 1 to 15 parts by mass, more preferably 2 to 8 parts by mass, and still more preferably 3 to 5 parts by mass, based on 100 parts by mass of the content of the polymerizable liquid crystal compound.
[ orientation controlling agent ]
The polymerizable liquid crystal composition preferably contains an alignment controlling agent. The alignment control agent is preferably a horizontal alignment agent capable of reducing or substantially leveling the tilt angle of the molecules of the rod-like liquid crystal compound in the air interface.
Examples of the horizontal aligning agent include compounds described in the paragraphs [0012] to [0030] of Japanese patent laid-open No. 2012-211306, compounds described in the paragraphs [0037] to [0044] of Japanese patent laid-open No. 2012-101999, fluorine-containing (meth) acrylate polymers described in the paragraphs [0018] to [0043] of Japanese patent laid-open No. 2007-272185, and compounds described in detail in Japanese patent laid-open No. 2005-099248 together with the synthesis method. The horizontal aligning agent may be a polymer containing polymerized units of a fluoroaliphatic group-containing monomer in an amount of more than 50% by mass based on the total polymerized units, as described in Japanese patent application laid-open No. 2004-331812.
Examples of the other alignment control agent include a vertical alignment agent. By blending the vertical alignment agent, the vertical alignment of the liquid crystal compound can be controlled. Examples of the vertical alignment agent include boric acid compounds and/or onium salts described in Japanese patent laid-open publication No. 2015-38598.
The content of the alignment control agent in the polymerizable liquid crystal composition is preferably 0.01 to 1.0 part by mass, more preferably 0.03 to 0.5 part by mass, and still more preferably 0.05 to 0.2 part by mass, based on 100 parts by mass of the content of the polymerizable liquid crystal compound.
[ crosslinking assistant ]
The polymerizable liquid crystal composition preferably contains a crosslinking assistant. The crosslinking assistant is polymerized with the polymerizable liquid crystal compound to increase the crosslinking density, thereby improving the strength of the optical film. The crosslinking assistant is preferably a polyfunctional polymerizable monomer which is polymerizable with the polymerizable liquid crystal compound and has 2 or more polymerizable groups in 1 molecule. The crosslinking assistant is more preferably a polyfunctional ethylenically unsaturated monomer, and still more preferably a polyfunctional (meth) acrylate having 3 or more (meth) acryloyl groups in 1 molecule.
Examples of the polyfunctional (meth) acrylate having 3 or more (meth) acryloyl groups in 1 molecule include trimethylolpropane tri (meth) acrylate, trimethylolethane tri (meth) acrylate, 1,2, 4-cyclohexane tetra (meth) acrylate, pentaglycerol triacrylate, pentaerythritol tetra (meth) acrylate, pentaerythritol tri (meth) acrylate, (di) pentaerythritol triacrylate, (di) pentaerythritol pentaacrylate, (di) pentaerythritol tetra (meth) acrylate, (di) pentaerythritol hexa (meth) acrylate, tripentaerythritol triacrylate, and tripentaerythritol hexatriacrylate.
The crosslinking assistant contained in the polymerizable liquid crystal composition may be 1 kind or 2 or more kinds.
In the polymerizable liquid crystal composition, the content of the crosslinking assistant is preferably 0.01 to 5.0 parts by mass, more preferably 0.1 to 3.0 parts by mass, and still more preferably 0.5 to 2.0 parts by mass, based on 100 parts by mass of the content of the polymerizable liquid crystal compound.
[ Infrared absorber ]
The polymerizable liquid crystal composition may contain an infrared absorber. Examples of the infrared absorber include known spectral sensitizing dyes, dyes or pigments which absorb light and interact with a polymerization initiator.
The content of the infrared absorber in the polymerizable liquid crystal composition is preferably 15 parts by mass or less, more preferably 0.1 to 10 parts by mass, and still more preferably 1 to 5 parts by mass, based on 100 parts by mass of the content of the polymerizable liquid crystal compound.
[ solvent ]
The polymerizable liquid crystal composition preferably contains a solvent. The solvent is preferably an organic solvent.
Specific examples of the organic solvent include an amide solvent (e.g., N, N-dimethylformamide), a sulfoxide solvent (e.g., dimethylsulfoxide), a heterocyclic compound (e.g., pyridine), a hydrocarbon solvent (e.g., benzene, hexane, etc.), a halogenated alkyl solvent (e.g., chloroform, dichloromethane), an ester solvent (e.g., methyl acetate, butyl acetate, etc.), a ketone solvent (e.g., acetone, methyl ethyl ketone, cyclohexanone, 2-butanone, etc.), and an ether solvent (e.g., tetrahydrofuran, 1, 2-dimethoxyethane, etc.). Among them, the organic solvent is preferably a ketone solvent.
The polymerizable liquid crystal composition may contain 1 or 2 or more kinds of organic solvents.
The content of the solvent in the polymerizable liquid crystal composition is preferably 30 to 90% by mass, more preferably 40 to 80% by mass, and still more preferably 50 to 70% by mass, based on the total mass of the polymerizable liquid crystal composition.
The coating mechanism for coating the polymerizable liquid crystal composition on the support may be a known coating mechanism.
Examples of the coating mechanism include mechanisms utilizing an extrusion die coating method, a curtain coating method, a dip coating method, a spin coating method, a printing coating method, a spray coating method, a slit coating method, a roll coating method, a slide coating method, a blade coating method, a gravure coating method, a wire bar method, and the like.
Before the polymerizable liquid crystal composition is applied to the support, the support may be subjected to rubbing treatment. The rubbing treatment can be performed, for example, by pressing a roll wound with a rubbing cloth against a support body with a predetermined pressure and rotating the support body. Examples of the rubbing cloth include paper, gauze, felt, rubber, nylon, rayon, and polyester fibers.
< Infrared irradiation and Cooling Process >
The method for producing an optical film of the present invention comprises the steps of: after the coating step, the coated side of the support, on which the polymerizable liquid crystal composition is coated, is irradiated with infrared rays at an incident angle of 40 ° or more with respect to the normal direction of the support, and the non-coated side of the support, on which the polymerizable liquid crystal composition is not coated, is cooled. Hereinafter, the coated side of the support coated with the polymerizable liquid crystal composition is simply referred to as "coated side", and the non-coated side of the support not coated with the polymerizable liquid crystal composition is simply referred to as "non-coated side".
The infrared irradiation mechanism is not particularly limited, and for example, a far infrared heater, a mid infrared heater, a near infrared heater, or the like can be used.
The wavelength range of the irradiated infrared ray is preferably 800nm to 25000nm (25 μm).
In order to efficiently heat the coated side, it is preferable to irradiate the coated side with parallel infrared rays. That is, the infrared ray is preferably irradiated using a parallel irradiation type infrared ray irradiation device.
The preferred exposure surface illuminance of infrared rays is 30KW/m2～500KW/m2More preferably 100KW/m2～400KW/m2。
The irradiation time of the infrared ray is not particularly limited, and is, for example, 1 minute to 5 minutes. Preferably, the surface temperature of the coated surface on which the polymerizable liquid crystal composition is coated is measured by contacting the coated surface with a thermocouple, and the surface temperature is irradiated with infrared rays until the surface temperature becomes higher than the liquid crystal-isotropic phase transition temperature. More preferably, the irradiation with infrared light is carried out until the surface temperature becomes a temperature higher by 10 ℃ or more than the liquid crystal-isotropic phase transition temperature. From the viewpoint of easy handling, the liquid crystal-isotropic phase transition temperature of the polymerizable liquid crystal composition is preferably 60 to 180 ℃, more preferably 100 to 150 ℃. The liquid crystal-isotropic phase transition temperature can be measured by observing the phase transition caused by the temperature rise of the polymerizable liquid crystal composition using a polarizing microscope. The measurement method is, for example, as follows.
First, a polymerizable liquid crystal composition is coated on glass. The glass coated with the polymerizable liquid crystal composition was set on a heating apparatus (high temperature stage: product name "FP 82 HT", central processing unit: product name "FP 90", manufactured by Mettler TOLEDO Co.). The polymerizable liquid crystal composition was heated while being observed with a polarizing microscope (product name "Eclipse E600 WPOL", manufactured by Nikon Solutions co., ltd.). After confirming that the polymerizable liquid crystal composition became an isotropic phase during the heating, the temperature was lowered at 1 ℃/min, and the temperature at which the composition was converted into a cholesteric liquid crystal phase was measured.
The incident angle with respect to the normal direction of the support when infrared rays are irradiated is preferably 40 ° or more, more preferably 70 ° or more, and further preferably 80 ° or more. If the incident angle is 40 ° or more, the proportion of isotropic phase region in the cholesteric liquid crystal layer decreases, and the proportion of cholesteric phase region increases. Therefore, the reflectance at the selective reflection wavelength from the cholesteric phase region is increased, and the color rendering property is excellent. The upper limit of the incident angle may be less than 90 °.
The cooling mechanism is not particularly limited, and examples thereof include a mechanism using a cold air blower, a cooling roller, and the like.
The cooling time is not particularly limited, and is, for example, 1 minute to 5 minutes. The surface temperature of the non-coated surface of the non-coated polymerizable liquid crystal composition is preferably measured by bringing the non-coated surface into contact with a thermocouple, and the surface is cooled until the surface temperature becomes lower than the liquid crystal-isotropic phase transition temperature. Further, it is more preferable to cool the liquid crystal until the surface temperature becomes 20 ℃ or more lower than the liquid crystal-isotropic phase transition temperature.
In this step, the temperature of the coated side is preferably higher than the liquid crystal-isotropic phase transition temperature (preferably higher than the liquid crystal-isotropic phase transition temperature by 10 ℃ or more), and the temperature of the non-coated side is preferably lower than the liquid crystal-isotropic phase transition temperature (preferably lower than the liquid crystal-isotropic phase transition temperature by 20 ℃ or more). The difference between the temperature of the coating side and the temperature of the non-coating side is preferably 20 to 80 ℃, and more preferably 30 to 65 ℃. The temperature of the coated side can use the surface temperature of the coated side, while the temperature of the non-coated side can use the surface temperature of the non-coated side. When the temperature difference is 20 ℃ to 80 ℃, an isotropic phase region is easily formed on the air interface side, and a cholesteric phase region is easily formed on the support side.
The start time and the end time of the infrared irradiation step and the cooling step may be the same or different. For example, the infrared irradiation and cooling may be started at the same time, the cooling may be started after the infrared irradiation is started, or the infrared irradiation may be started after the cooling is started. Further, the irradiation of infrared rays and the cooling may be stopped at the same time, the cooling may be stopped after the irradiation of infrared rays is stopped, or the irradiation of infrared rays may be stopped after the cooling is stopped.
< ultraviolet irradiation Process >
The method for producing an optical film of the present invention comprises the steps of: after the infrared irradiation and cooling step, the support is irradiated with ultraviolet rays while maintaining a temperature higher than the liquid crystal-isotropic phase transition temperature on the coated side and a temperature lower than the liquid crystal-isotropic phase transition temperature on the non-coated side.
The ultraviolet irradiation means is not particularly limited, and a mercury lamp, a metal halide lamp, an ultraviolet fluorescent lamp, a UV-LED (light emitting diode), or a UV-LD (laser diode) can be used.
The peak wavelength of the ultraviolet ray is preferably 200nm to 405nm, more preferably 220nm to 390nm, and still more preferably 220nm to 380 nm.
The illuminance of the exposed surface of the ultraviolet ray is preferably 30mW/cm2～800mW/cm2More preferably 100mW/cm2～500mW/cm2。
The irradiation time of the ultraviolet ray is not particularly limited, and is, for example, 1 second to 10 seconds.
When ultraviolet light is irradiated, a temperature higher than the liquid crystal-isotropic phase transition temperature may be maintained on the coated side, and a temperature lower than the liquid crystal-isotropic phase transition temperature may be maintained on the non-coated side. Therefore, only the ultraviolet ray can be irradiated in a state where the coating side is irradiated with the infrared ray and the non-coating side is cooled, and then the irradiation with the infrared ray and the cooling are stopped. Further, the ultraviolet ray irradiation may be performed while one of the infrared ray irradiation and the cooling is continued and the other is stopped. Further, the coating side may be irradiated with ultraviolet rays while the non-coating side is cooled while the coating side is irradiated with infrared rays.
The ultraviolet irradiation may be performed from the coating side or from the non-coating side.
Examples
The present invention will be described more specifically with reference to the following examples, but the present invention is not limited to the following examples as long as the gist of the present invention is not exceeded.
[ preparation of coating solutions 1 to 3 for Forming liquid Crystal layer ]
Coating liquids 1 to 3 for forming liquid crystal layers were prepared by mixing the components shown in Table 1 in the amounts shown in Table 1 (unit: parts by mass).
[ Table 1]
| Coating liquid 1 | Coating liquid 2 | Coating liquid 3 | |
| Polymerizable liquid crystal compound | 100 | 100 | 100 |
| Chiral compounds | 5.5 | 6.7 | - |
| Polymerization initiator | 4 | 4 | 4 |
| Orientation control agent | 0.1 | 0.1 | 0.1 |
| Crosslinking aid | 1 | 1 | 1 |
| Solvent(s) | 170 | 170 | 170 |
Details of the polymerizable liquid crystal compound, the chiral compound, the polymerization initiator, the alignment controller, the crosslinking assistant, and the solvent in table 1 are as follows.
Polymerizable liquid crystal compound: a rod-like liquid crystal compound represented by the following structural formula
[ chemical formula 3]
A chiral compound: product name "Paliocolor LC 756", manufactured by BASF Corp
Polymerization initiator: bis (2,4, 6-trimethylbenzoyl) phenylphosphine oxide (product name "Omnirad 819", manufactured by IGM Resins B.V. Inc.)
Orientation control agent: a compound represented by the following structural formula (produced by the method described in Japanese patent laid-open No. 2005-99248)
[ chemical formula 4]
Wherein R is O (CH)2)2O(CH2)2(CF2)6F。
Crosslinking coagents: pentaerythritol tetraacrylate (product name "A-TMMT", Shin-Nakamura Chemical Co., Ltd.; manufactured by Ltd.)
Solvent: 2-butanone (manufactured by FUJIFILM Wako Pure Chemical Corporation)
The selective reflection wavelength of coating liquid 1 was 540 nm. The selective reflection wavelength of coating liquid 2 was 450 nm.
< example 1>
As the support, a 130mm × 100mm × 25 μm polyethylene terephthalate (PET) film (product name "Cosmoshine A4100", Toyobo Co., Ltd.) was used, with respect to the main surfaceRubbing treatment was carried out (rubbing cloth: rayon, pressure: 0.98N, rotation speed: 1000rpm, (recycling) conveyance speed: 10m/min, number of times: 1 round trip). On the surface subjected to the rubbing treatment, coating solution 1 was applied using a wire bar under a condition that the moving speed of the wire bar was 10 m/min. At this time, a vibration exciter was used so that the bar coating apparatus was accelerated at a frequency of 25Hz and an acceleration of 0.2Gal (2 mm/s)2) The mode of vibration is adjusted. The support on which the coating solution 1 was applied was fixed by being attached to a frame.
Subsequently, the coated surface of the support on which the coating liquid 1 was applied was irradiated with infrared rays from a near-infrared heater (product name "HEAT-BEAM (registered trademark)", manufactured by Hybec Corporation, parallel irradiation type) at an incident angle of 80 ° with respect to the normal direction of the support, and the non-coated surface of the support was dried by blowing cold air at 23 ℃ for 2 minutes at an air speed of 3 m/s. Thermocouples were brought into contact with the coated side and the non-coated side, respectively. The surface temperature was measured, and it was confirmed that the coated surface was 130 ℃ and the non-coated surface was 70 ℃. The temperature state was maintained, and an illuminance of 60mW/cm was applied from the non-coating surface side of the support body using a UV-LED irradiation device (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, an optical film having a cholesteric liquid crystal layer with a thickness of 3 μm formed on a support was obtained. In the coating liquid 1, the "liquid crystal-isotropic phase transition temperature" was measured using a heating device (high temperature stage: product name "FP 82 HT", central processing device: product name "FP 90", manufactured by Mettler TOLEDO corporation) and a polarizing microscope (product name "Eclipse E600 WPOL", manufactured by Nikon Solutions co., ltd.) and was 117 ℃.
< example 2>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Subsequently, the support coated with coating solution 1 was dried at 100 ℃ for 2 minutes in a hot air oven. In the coldAfter cooling to room temperature, the substrate was irradiated with UV-LED (product name "high output UV-LED irradiator", manufactured by CCS Inc.) at an illuminance of 60mW/cm from the non-coating surface side of the substrate2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, a 1 st cholesteric liquid crystal layer having a thickness of 3.0 μm was formed on the support.
Further, coating liquid 2 was applied to the cholesteric liquid crystal layer in the same manner as in example 1. The coated surface of the support on which the coating liquid 2 was applied was irradiated with infrared rays from a near-infrared heater (product name "HEAT-BEAM (registered trademark)", manufactured by Hybec Corporation, parallel irradiation type) at an incident angle of 80 ° with respect to the normal direction of the support, and the non-coated surface of the support was dried by blowing cold air at 23 ℃ for 2 minutes at an air speed of 3 m/s. Thermocouples were brought into contact with the coated side and the non-coated side, respectively. The surface temperature was measured, and it was confirmed that the coated surface was 130 ℃ and the non-coated surface was 70 ℃. The temperature state was maintained, and an illuminance of 60mW/cm was applied from the non-coating surface side of the support body using a UV-LED irradiation device (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, an optical film having a 2 nd cholesteric liquid crystal layer having a thickness of 3.5 μm formed on the 1 st cholesteric liquid crystal layer was obtained. That is, in the optical film of example 2, the 1 st cholesteric liquid crystal layer from the coating liquid 1 and the 2 nd cholesteric liquid crystal layer from the coating liquid 2 were formed in this order on the support. In the coating liquid 2, the "liquid crystal-isotropic phase transition temperature" was measured using a heating device (high temperature stage: product name "FP 82 HT", central processing device: product name "FP 90", manufactured by Mettler TOLEDO corporation) and a polarizing microscope (product name "Eclipse E600 WPOL", manufactured by Nikon Solutions co., ltd.) and was 117 ℃.
< example 3>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 3 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Subsequently, the support coated with coating liquid 3 was dried at 100 ℃ for 2 minutes in a hot air oven. After cooling to room temperature, the substrate was irradiated with an illuminance of 60mW/cm from the non-coating surface side of the support using a UV-LED irradiation apparatus (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, a nematic liquid crystal layer having a thickness of 1.0 μm was formed on the support.
Further, coating solution 1 was applied to the nematic liquid crystal layer in the same manner as in example 1. The support coated with the coating solution 1 was dried and irradiated with ultraviolet rays (peak wavelength: 365nm) in the same manner as the method of drying the support coated with the coating solution 3 and the method of irradiating with ultraviolet rays. Thus, a 1 st cholesteric liquid crystal layer having a thickness of 3.0 μm was formed on the nematic liquid crystal layer.
Further, coating liquid 2 was applied to the cholesteric liquid crystal layer 1 in the same manner as in example 1. The coated surface of the support on which the coating liquid 2 was applied was irradiated with infrared rays from a near-infrared heater (product name "HEAT-BEAM (registered trademark)", manufactured by Hybec Corporation, parallel irradiation type) at an incident angle of 80 ° with respect to the normal direction of the support, and the non-coated surface of the support was dried by blowing cold air at 23 ℃ for 2 minutes at an air speed of 3 m/s. Thermocouples were brought into contact with the coated side and the non-coated side, respectively. The surface temperature was measured, and it was confirmed that the coated surface was 130 ℃ and the non-coated surface was 70 ℃. The temperature state was maintained, and an illuminance of 60mW/cm was applied from the non-coating surface side of the support body using a UV-LED irradiation device (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, an optical film having a 2 nd cholesteric liquid crystal layer having a thickness of 3.5 μm formed on the 1 st cholesteric liquid crystal layer was obtained. That is, in the optical film of example 3, the nematic liquid crystal layer from coating liquid 3, the 1 st cholesteric liquid crystal layer from coating liquid 1, and the 2 nd cholesteric liquid crystal layer from coating liquid 2 were formed in this order on the support.
< example 4>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Next, the coating surface of the support coated with the coating solution 1 was irradiated with infrared light and dried in the same manner as in example 1, except that the incident angle with respect to the normal direction of the support was changed from 80 ° to 70 °. The surface temperature was measured, and it was confirmed that the coated surface was 135 ℃ and the non-coated surface was 90 ℃, and ultraviolet rays were irradiated in the same manner as in example 1. Thus, a cholesteric liquid crystal layer having a thickness of 3 μm was formed on the support.
< example 5 >
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Next, the coating surface of the support coated with the coating solution 1 was irradiated with infrared light and dried in the same manner as in example 1, except that the incident angle with respect to the normal direction of the support was changed from 80 ° to 45 °. The surface temperature was measured, and it was confirmed that the coated surface was 141 ℃ and the non-coated surface was 108 ℃, and ultraviolet rays were irradiated in the same manner as in example 1. Thus, a cholesteric liquid crystal layer having a thickness of 3 μm was formed on the support.
< comparative example 1>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Subsequently, the support coated with coating solution 1 was dried at 100 ℃ for 2 minutes in a hot air oven. After cooling to normal temperature (25 ℃), the substrate was irradiated with 60mW/cm of illumination light from the non-coated surface of the substrate using a UV-LED irradiation apparatus (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Irradiated with ultraviolet rays for 6 seconds (peak wavelength: 3)65 nm). Thus, a 1 st cholesteric liquid crystal layer having a thickness of 3.0 μm was formed on the support.
Further, coating liquid 2 was applied to the cholesteric liquid crystal layer 1 in the same manner as in example 1. The support coated with coating solution 2 was dried and irradiated with ultraviolet rays (peak wavelength: 365nm) in the same manner as the method for drying the support coated with coating solution 1 and the method for irradiating with ultraviolet rays. Thus, an optical film having a 2 nd cholesteric liquid crystal layer having a thickness of 3.5 μm formed on the 1 st cholesteric liquid crystal layer was obtained. That is, in the optical film of comparative example 1, the 1 st cholesteric liquid crystal layer from coating liquid 1 and the 2 nd cholesteric liquid crystal layer from coating liquid 2 were formed in this order on the support.
< comparative example 2>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Subsequently, the support coated with coating solution 1 was dried at 100 ℃ for 2 minutes in a hot air oven. After cooling to room temperature, the substrate was irradiated with an illuminance of 60mW/cm from the non-coating surface side of the support using a UV-LED irradiation apparatus (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, a cholesteric liquid crystal layer having a thickness of 3.0 μm was formed on the support.
Further, coating liquid 2 was applied to the cholesteric liquid crystal layer in the same manner as in example 1. The support coated with coating solution 2 was dried at 130 ℃ for 2 minutes in a hot air oven. After cooling to room temperature, the substrate was irradiated with an illuminance of 60mW/cm from the non-coating surface side of the support using a UV-LED irradiation apparatus (product name "high output UV-LED irradiator", manufactured by CCS Inc.)2Ultraviolet light (peak wavelength: 365nm) was irradiated for 6 seconds. Thus, an optical film having an isotropic layer with a thickness of 3.5 μm formed on a support was obtained. That is, in the optical film of comparative example 2, the cholesteric form from coating solution 1 was formed on the support in this orderLiquid crystal layer and isotropic layer from coating liquid 2.
< comparative example 3>
The support was subjected to rubbing treatment in the same manner as in example 1. Coating solution 1 was applied in the same manner as in example 1, and the support coated with the coating solution was fixed to a frame.
Next, the coated surface of the support on which the coating solution 1 was applied was irradiated with infrared rays and dried in the same manner as in example 1, except that the incident angle with respect to the normal direction of the support was changed from 80 ° to 0 °, and cold air was not blown to the non-coated surface of the support. The surface temperature was measured, and it was confirmed that the coated surface was 160 ℃ and the non-coated surface was 157 ℃, and ultraviolet rays were irradiated in the same manner as in example 1. Thus, an optical film was obtained in which an isotropic layer having a thickness of 3 μm was formed on a support.
The phase state of the outermost layer was analyzed for the optical films obtained in examples and comparative examples. The film thickness variation cycle, film thickness difference, and reflectance of the optical film were measured. Further, the presence or absence of color unevenness in the outermost layer was evaluated. The analysis method, measurement method and evaluation method are as follows. The results are shown in Table 2. Table 2 shows the layer structure of the obtained optical film. For example, when an optical film having a layer derived from coating liquid 1 and a layer derived from coating liquid 2 formed in this order on a support is described as "coating liquid 2/coating liquid 1". Table 2 shows the incident angle of infrared rays when infrared rays are irradiated when the outermost layer is formed. When infrared rays are not irradiated, the description is "-".
(analysis of phase State)
From the optical film thus produced, a film piece having a width of 5mm × a length of 2mm was cut out using a roller cutter. The film pieces were embedded with epoxy resin, and cut off using a microtome (product name "RM 2265", manufactured by Leica Biosystems). An SEM image of a cross section of the outermost layer was observed using a scanning electron microscope (model "S-4800", manufactured by Hitachi High-Technologies Corporation, observation magnification: 10000 times, acceleration voltage: 2.0kV), and it was confirmed whether or not there was a dark and light stripe pattern resulting from a change in the refractive index of the cholesteric phase. That is, when the stripe pattern is observed in the outermost layer, it can be determined that the outermost layer is a cholesteric liquid crystal layer including cholesteric phase regions. Specifically, when a stripe pattern was observed in the entire outermost layer, it was determined that the outermost layer was a cholesteric liquid crystal layer formed only of cholesteric phase regions. When the stripe pattern is present in the outermost layer, but the difference in shade of the stripe pattern is small from the interface on the support side of the outermost layer toward the air interface side, and finally no difference in shade is observed, it is determined that the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region, and the isotropic phase region is formed from the air interface side of the cholesteric liquid crystal layer toward the thickness direction. When the stripe pattern was not confirmed at all in the outermost layer, it was determined that the entire outermost layer was an isotropic layer.
When the outermost layer was a cholesteric liquid crystal layer and included an isotropic phase region and a cholesteric phase region, the thickness of the isotropic phase region was measured, and the ratio of the thickness of the isotropic phase region to the thickness of the outermost layer was calculated. Specifically, the distance from the following position to the air interface is taken as the thickness of the isotropic phase region: the difference in shade of the stripe pattern decreases from the interface on the support side of the outermost layer toward the air interface side, and finally the difference in shade is not observed. In table 2, the ratio of the thickness of the isotropic phase region to the thickness of the outermost layer is described as "the ratio of the isotropic phase region". In the case where the outermost layer is an isotropic layer, the proportion of isotropic phase region is described as 100% in table 2. In the case where the outermost layer is a cholesteric liquid crystal layer formed only of cholesteric phase regions, the proportion of isotropic phase regions is described as 0% in table 2.
(measurement of film thickness fluctuation period)
The 2 polarizing plates were arranged on the observation window so that the transmission axes were orthogonal to each other. The fabricated optical film was sandwiched between 2 polarizing plates. When the optical film was observed from the upper side of the polarizing plate disposed on the upper side, it was confirmed that the color tone was periodically changed toward the coating direction of the coating liquid at the end (edge) of the optical film. That is, a stripe pattern in which lines having a darker color and lines having a lighter color are alternately arranged was confirmed. As described later, no stripe pattern was observed in the central portions of the optical films produced in examples 1 to 5 and comparative examples 2 to 3. The total width of the continuous darker line and the lighter line was defined as 1 cycle, and the length of the 10-cycle component was measured. The measured length was divided by 10 to calculate a value as a film thickness variation cycle.
(measurement of film thickness Difference)
The 2 polarizing plates were arranged on the observation window so that the transmission axes were orthogonal to each other. The fabricated optical film was sandwiched between 2 polarizing plates. When the optical film was observed from the upper side of the polarizing plate disposed on the upper side, it was confirmed that the color tone was periodically changed toward the coating direction of the coating liquid at the end (edge) of the optical film. That is, a stripe pattern in which lines having a darker color and lines having a lighter color are alternately arranged was confirmed. The produced optical film was cut with a roller cutter, and 3 pieces of the film including the darker colored lines and 3 pieces of the film including the lighter colored lines were obtained. A film piece including a thick color line was embedded with an epoxy resin, and cut in the thickness direction using a microtome (product name "RM 2265", manufactured by Leica Biosystems) to obtain a cross section. Similarly, a film piece including a light-colored wire was embedded in an epoxy resin, and cut in the thickness direction using a microtome (product name "RM 2265", manufactured by Leica Biosystems) to obtain a cross section. Each cross section was observed with a scanning electron microscope (model "S-4800", manufactured by Hitachi High-Technologies Corporation, observation magnification: 5000 times, acceleration voltage: 2.0kV) and the film thickness was measured. The difference between the average value of the film thicknesses measured using the small film pieces including the darker lines and the average value of the film thicknesses measured using the small film pieces including the lighter lines was defined as the film thickness difference.
(measurement of reflectance)
The reflectance of the reflection peaks at 540nm and 450nm was measured using a spectrophotometer (product name "V-670", manufactured by JASCO Corporation) at an incident angle of 5 deg. The case where the reflectance was 30% or more was judged as "pass". In addition, the reflectance of the reflection peak at 540nm was measured in the case of using coating liquid 1, and the reflectance of the reflection peak at 450nm was measured in the case of using coating liquid 2. In the case where coating liquid 2 was not used, "-" was shown in table 2 as the reflectance of the reflection peak at 450 nm.
(presence/absence of color unevenness)
The 2 polarizing plates were arranged on the observation window so that the transmission axes were orthogonal to each other. The fabricated optical film was sandwiched between 2 polarizing plates. The center of the optical film was visually observed from the upper side of the polarizing plate disposed on the upper side, and the presence or absence of color unevenness on the surface of the outermost layer was evaluated. The evaluation criteria are as follows.
A: no color unevenness was confirmed.
B: color unevenness was confirmed.
[ Table 2]
As shown in table 2, in examples 1 to 5, the optical film had a support and a cholesteric liquid crystal layer provided on the support, and the cholesteric liquid crystal layer included an isotropic phase region and a cholesteric phase region, and the isotropic phase region was formed from the surface of the cholesteric liquid crystal layer opposite to the surface facing the support in the thickness direction, and it was confirmed that even if the film thickness was periodically varied, the optical characteristics of the cholesteric liquid crystal were exhibited and color unevenness was suppressed. In particular, in examples 1 to 4, it was confirmed that the thickness of the isotropic phase region was 27% or less with respect to the thickness of the outermost layer, and the reflectance at the selective reflection wavelength was high.
On the other hand, in comparative example 1, since the outermost layer was a cholesteric liquid crystal layer formed only of cholesteric liquid crystal phase regions, color unevenness was observed.
In comparative example 2, the outermost layer was an isotropic layer formed only of isotropic phase regions, and thus the optical properties of cholesteric liquid crystals were not exhibited.
In comparative example 3, the outermost layer was an isotropic layer formed only of isotropic phase regions, and thus the optical properties of cholesteric liquid crystals were not exhibited.
As described above, the optical film according to one embodiment of the present invention includes a support and a cholesteric liquid crystal layer provided on the support, the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region, the isotropic phase region is formed from a surface of the cholesteric liquid crystal layer opposite to a surface facing the support in a thickness direction, and even if a film thickness periodically fluctuates, the optical characteristics of the cholesteric liquid crystal layer are exhibited and color unevenness is suppressed.
In addition, all disclosures of japanese patent application No. 2019-179605, filed on 30/9/2019, are incorporated in the present specification by reference. All documents, patent applications, and technical standards described in the present specification are incorporated by reference into the present specification to the same extent as if each document, patent application, and technical standard was specifically and individually indicated to be incorporated by reference.
Claims (7)
1. An optical film comprising a support and a cholesteric liquid crystal layer provided on the support,
the cholesteric liquid crystal layer includes an isotropic phase region and a cholesteric phase region,
the isotropic phase region is formed from a surface of the cholesteric liquid crystal layer opposite to a surface facing the support in a thickness direction.
2. The optical film according to claim 1,
there are at least 1 intermediate layer between the support and the cholesteric liquid crystal layer.
3. The optical film according to claim 2,
the at least 1 intermediate layer is at least one layer selected from the group consisting of other cholesteric liquid crystal layers, nematic liquid crystal layers and smectic liquid crystal layers, and alignment layers.
4. The optical film according to any one of claims 1 to 3,
the thickness of the isotropic phase region is greater than 0% and 27% or less with respect to the thickness of the cholesteric liquid crystal layer.
5. A method for manufacturing an optical film according to any one of claims 1 to 4, comprising the steps of:
a step of applying a polymerizable liquid crystal composition containing a polymerizable liquid crystal compound and a chiral compound onto a support;
a step of irradiating the coated side of the support, on which the polymerizable liquid crystal composition is coated, with infrared light at an incident angle of 40 ° or more with respect to the normal direction of the support, and cooling the non-coated side of the support, on which the polymerizable liquid crystal composition is not coated; and
and irradiating the support with ultraviolet rays while maintaining the coating side at a temperature higher than the liquid crystal-isotropic phase transition temperature and the non-coating side at a temperature lower than the liquid crystal-isotropic phase transition temperature.
6. The method for manufacturing an optical film according to claim 5,
the content of the chiral compound is 3 to 12 parts by mass per 100 parts by mass of the polymerizable liquid crystal compound.
7. The method for manufacturing an optical film according to claim 5 or 6,
the difference between the temperature of the coating side and the temperature of the non-coating side is 20-80 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2019179605 | 2019-09-30 | ||
| JP2019-179605 | 2019-09-30 | ||
| PCT/JP2020/023363 WO2021065088A1 (en) | 2019-09-30 | 2020-06-15 | Optical film and method for manufacturing optical film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114341685A true CN114341685A (en) | 2022-04-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202080062840.4A Pending CN114341685A (en) | 2019-09-30 | 2020-06-15 | Optical film and method for producing optical film |
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| Country | Link |
|---|---|
| JP (1) | JPWO2021065088A1 (en) |
| CN (1) | CN114341685A (en) |
| WO (1) | WO2021065088A1 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2355315B (en) * | 1999-09-17 | 2003-10-08 | Merck Patent Gmbh | Circular polarizer with optically anisotropic and isotropic layers |
| JP2006039164A (en) * | 2004-07-27 | 2006-02-09 | Nitto Denko Corp | Method for manufacturing optical film, optical film, polarizing plate, liquid crystal panel and liquid crystal display |
| JP2006078617A (en) * | 2004-09-08 | 2006-03-23 | Nitto Denko Corp | Manufacturing method of optical film, optical film, polarizing plate, liquid crystal panel, and liquid crystal display |
| JP2009003400A (en) * | 2007-05-18 | 2009-01-08 | Tokyo Institute Of Technology | Light reflecting film and laser oscillating element using it |
| WO2018123832A1 (en) * | 2016-12-27 | 2018-07-05 | 富士フイルム株式会社 | Optical film and manufacturing method therefor |
-
2020
- 2020-06-15 CN CN202080062840.4A patent/CN114341685A/en active Pending
- 2020-06-15 WO PCT/JP2020/023363 patent/WO2021065088A1/en active Application Filing
- 2020-06-15 JP JP2021551137A patent/JPWO2021065088A1/ja active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2355315B (en) * | 1999-09-17 | 2003-10-08 | Merck Patent Gmbh | Circular polarizer with optically anisotropic and isotropic layers |
| JP2006039164A (en) * | 2004-07-27 | 2006-02-09 | Nitto Denko Corp | Method for manufacturing optical film, optical film, polarizing plate, liquid crystal panel and liquid crystal display |
| JP2006078617A (en) * | 2004-09-08 | 2006-03-23 | Nitto Denko Corp | Manufacturing method of optical film, optical film, polarizing plate, liquid crystal panel, and liquid crystal display |
| JP2009003400A (en) * | 2007-05-18 | 2009-01-08 | Tokyo Institute Of Technology | Light reflecting film and laser oscillating element using it |
| WO2018123832A1 (en) * | 2016-12-27 | 2018-07-05 | 富士フイルム株式会社 | Optical film and manufacturing method therefor |
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| Publication number | Publication date |
|---|---|
| JPWO2021065088A1 (en) | 2021-04-08 |
| WO2021065088A1 (en) | 2021-04-08 |
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