WO2010143683A1 - 赤外光反射板、及び赤外光反射性合わせガラス - Google Patents
赤外光反射板、及び赤外光反射性合わせガラス Download PDFInfo
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- WO2010143683A1 WO2010143683A1 PCT/JP2010/059830 JP2010059830W WO2010143683A1 WO 2010143683 A1 WO2010143683 A1 WO 2010143683A1 JP 2010059830 W JP2010059830 W JP 2010059830W WO 2010143683 A1 WO2010143683 A1 WO 2010143683A1
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- light
- light reflecting
- liquid crystal
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Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10165—Functional features of the laminated safety glass or glazing
- B32B17/10431—Specific parts for the modulation of light incorporated into the laminated safety glass or glazing
- B32B17/1044—Invariable transmission
- B32B17/10458—Polarization selective transmission
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10678—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer comprising UV absorbers or stabilizers, e.g. antioxidants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3016—Polarising elements involving passive liquid crystal elements
Definitions
- the present invention relates to an infrared light reflection plate having a plurality of light reflection layers formed by fixing a cholesteric liquid crystal phase, and mainly relates to an infrared light reflection plate used for heat insulation of windows of buildings and vehicles.
- the present invention also relates to an infrared light reflective laminated glass using the infrared light reflection plate.
- the special metal film can be manufactured by laminating a plurality of layers by, for example, the vacuum film forming method disclosed in Patent Document 1. Although these special metal film coatings produced by vacuum film formation have excellent reflection performance, the vacuum process has low productivity and high production cost.
- Patent Document 2 proposes a heat ray reflective transparent substrate having a layer containing metal fine particles.
- Patent Document 3 discloses a heat ray blocking sheet having a layer containing an infrared absorbing dye. When an infrared absorbing dye is used, the solar transmittance can be lowered, but there is a problem that the heat shielding performance is lowered due to an increase in film surface temperature due to the absorption of solar radiation and the re-release of the heat.
- Patent Document 4 discloses a laminated optical film having a retardation film having a predetermined characteristic and a reflective circularly polarizing plate and having reflectivity for infrared rays, and a cholesteric liquid crystal phase is used as the retardation film.
- An example is disclosed.
- Patent Document 5 discloses an infrared light reflective article including a visible light transmissive substrate and an infrared light reflective cholesteric liquid crystal layer.
- Patent Document 6 discloses a polarizing element having a plurality of cholesteric liquid crystal layers, but such a laminate formed by laminating cholesteric liquid crystal layers mainly includes light in the visible light region. Is used for the purpose of efficiently reflecting light.
- JP-A-6-263486 Japanese Patent Laid-Open No. 2002-131553 JP-A-6-194517 Japanese Patent No. 4109914 Special table 2009-514022 Japanese Patent No. 3500127
- the ⁇ / 2 plate is a special retardation plate, and its production is difficult and the production cost increases. Further, the material is limited to a special one, and as a result, the application may be limited. Further, the ⁇ / 2 plate usually acts as a ⁇ / 2 plate for light incident from the normal direction with respect to the layer surface, but strictly speaking, for light incident obliquely, ⁇ / Does not function as two plates. For this reason, the configuration in which the ⁇ / 2 plates are combined has a problem that light incident from an oblique direction cannot be completely reflected.
- an object of the present invention is to improve the reflection characteristics of an infrared light reflection plate having a plurality of light reflection layers formed by fixing a cholesteric liquid crystal phase without requiring the use of a ⁇ / 2 plate. More specifically, the present invention provides a selective reflection characteristic for broadband light, which is a combination of an inexpensive substrate with in-plane retardation variation and a plurality of light reflecting layers in which a cholesteric liquid crystal phase is fixed. It is an object to provide an excellent infrared light reflecting plate and infrared light reflecting laminated glass.
- the present inventors diligently studied. As a result, the cholesteric liquid crystal phase having selective reflection characteristics with respect to light in the same wavelength region and having opposite optical rotation (ie right or left optical rotation) is fixed. It was found that if the light reflecting layer is arranged on the substrate adjacent to each other, it is possible to reflect both the left circularly polarized light and the right circularly polarized light in the wavelength range without being affected by the optical characteristics of the substrate. By further forming a pair of light reflecting layers having selective reflection characteristics for light in other wavelength ranges and fixing cholesteric liquid crystal phases having opposite optical rotations (that is, right or left optical rotation). It was also found that the characteristics could be broadened.
- the reflection center wavelengths of the light reflection layers X1 and X2 are ⁇ X1 (nm), which are equal to each other and reflect circularly polarized light in opposite directions,
- the reflection center wavelengths of the light reflection layers Y1 and Y2 are ⁇ Y1 (nm), which are equal to each other and reflect circularly polarized light in opposite directions, ⁇ X1 and ⁇ Y1 are not equal, and the refractive index anisotropy ⁇ n X1 and ⁇ n X2 of the light reflecting layers X1 and X2 satisfy ⁇ n X2 ⁇ n X1 , respectively, and the refractive index of each of the light reflecting layers Y1 and Y2 Anisotropy ⁇ n Y1 and ⁇ n
- An infrared light reflector that reflects infrared rays having a wavelength of 700 nm or more.
- the reflection center wavelength ⁇ X1 (nm) of the light reflection layers X1 and X2 is in the range of 900 to 1050 nm
- the reflection center wavelength ⁇ Y1 (nm) of the light reflection layers Y1 and Y2 is in the range of 1050 to 1300 nm.
- the light reflecting layers X2 and Y2 are layers formed by fixing the cholesteric liquid crystal phase using the liquid crystal composition applied to the respective surfaces of the light reflecting layers X1 and Y1 as the cholesteric liquid crystal phase.
- the infrared light reflector according to any one of [1] to [3].
- Two light reflection layers X3 and X4 each having a cholesteric liquid crystal phase fixed on the light reflection layer X2, and two light beams having a cholesteric liquid crystal phase fixed on the light reflection layer Y2.
- the reflection center wavelengths of the light reflection layers X3 and X4 are ⁇ X3 (nm), which are equal to each other and reflect circularly polarized light in opposite directions, Mutually equal a light reflective layer Y3 and Y4 each reflection center wavelength is the wavelength lambda Y3 (nm), and reflects the different direction of the circularly polarized light from each other, and, ⁇ X3 and ⁇ Y3 are not equal to each other and ⁇ X1 and ⁇ Y1 are not equal to each other,
- the infrared light reflector according to any one of [1] to [5].
- An infrared light reflective laminated glass having two glass plates and an infrared light reflection plate of any one of [1] to [9] between them.
- the reflection characteristics can be improved without requiring the use of a ⁇ / 2 plate.
- a reflection characteristic for broadband light comprising a combination of an inexpensive substrate with in-plane retardation variation and a plurality of light reflecting layers in which a cholesteric liquid crystal phase is fixed. It is possible to provide an infrared light reflector and an infrared light reflective laminated glass using the same.
- the refractive index anisotropy ⁇ n of a layer formed by fixing a cholesteric liquid crystal phase is defined as follows.
- the refractive index anisotropy ⁇ n of a layer formed by fixing a cholesteric liquid crystal phase means ⁇ n at a wavelength exhibiting selective reflection characteristics (specifically, near a wavelength of 1000 nm).
- a layer on which a cholesteric liquid crystal phase in which the helical axis is uniformly oriented with respect to the film surface is fixed is formed on a substrate (glass, film) subjected to orientation treatment or provided with an orientation film.
- the selective reflection of the layer is measured, and the peak width Hw is obtained.
- the spiral pitch p of the sample is separately measured.
- the helical pitch can be measured by observing a cross-section TEM.
- the reflection center wavelengths are equal to each other of each layer, it is a matter of course that an error generally allowed in the technical field to which the present invention belongs is also considered. In general, the reflection center wavelength will be regarded as the same even if there is a difference of about ⁇ 30 nm.
- the infrared light reflector shown in FIG. 1 has light reflecting layers 14a and 14b formed by fixing a cholesteric liquid crystal phase on one surface of a substrate 12, and the cholesteric liquid crystal phase is fixed on the other surface of the substrate 12.
- the light reflecting layers 16a and 16b are formed.
- the substrate 12 is, for example, a polymer film, and there is no particular limitation on the optical characteristics thereof.
- a member having a variation in the in-plane retardation Re is used as a substrate.
- ⁇ / 2 is used as a substrate, and its optical characteristics are improved in light reflection characteristics. It is distinguished from the prior art that is actively used. However, as a matter of course, it does not preclude the use of a retardation plate whose phase difference is accurately adjusted, such as a ⁇ / 2 plate, as the substrate 12.
- the optical characteristics of the substrate 12 are not particularly limited, and may be a phase difference plate showing a phase difference or an optically isotropic substrate. That is, the substrate 12 does not have to be a retardation plate such as a ⁇ / 2 plate whose optical characteristics are strictly adjusted.
- the in-plane retardation Re (1000) at a wavelength of 1000 nm of the substrate 12 may be made of a polymer film or the like having a variation of 20 nm or more. Furthermore, it may be made of a polymer film or the like having a variation of Re (1000) of 100 nm or more.
- the in-plane retardation of the substrate is not particularly limited. For example, a retardation plate having an in-plane retardation Re (1000) of a wavelength of 1000 nm of 800 to 13000 nm can be used. Examples of polymer films that can be used as the substrate will be described later.
- the light reflecting layers 14a, 14b, 16a, and 16b are layers formed by fixing the cholesteric liquid crystal phase
- the light reflecting layers 14a, 14b, 16a, and 16b exhibit light selective reflectivity that reflects light of a specific wavelength based on the helical pitch of the cholesteric liquid crystal phase.
- the adjacent light reflective layer 14a and 14b, together with the spiral directions of the respective cholesteric liquid crystal phase are opposite to each other, the reflection center wavelength lambda 14 is the same.
- the adjacent light reflective layer 16a and 16b, together with the spiral directions of the respective cholesteric liquid crystal phase are opposite to each other, the reflection center wavelength lambda 16 is the same.
- the light reflecting layers 14a and 14b selectively reflect the left circularly polarized light and the right circularly polarized light having the predetermined wavelength ⁇ 14 , and the light reflecting layers 16a and 16b The left circularly polarized light and the right circularly polarized light having the wavelength ⁇ 16 are selectively reflected.
- the infrared light reflection 10 shown in FIG. 1 is an infrared light reflection plate that reflects infrared light having a wavelength of 700 nm or more, that is, the center wavelength ⁇ 14 of selective reflection by the light reflection layers 14a and 14b, and the light reflection layer 16a. It is preferable that the center wavelength ⁇ 16 of selective reflection by 16b is also 700 nm or more. In one example, one of the reflection center wavelengths ⁇ 14 and ⁇ 16 is in the range of 900 to 1050 nm (preferably 800 to 1000 nm, more preferably 850 to 950 nm), and the other is 1050 to 1300 nm (preferably 1000 to 1200 nm, more preferably 1050 to 1150 nm).
- the helical pitch of the cholesteric liquid crystal phase exhibiting the reflection center wavelength is generally about 500 to 1350 nm (preferably about 500 to 900 nm, more preferably about 550 to 800 nm).
- the thickness of each light reflecting layer is about 1 ⁇ m to 8 ⁇ m (preferably about 3 to 8 ⁇ m). However, it is not limited to these ranges.
- a light reflecting layer having a desired helical pitch can be formed by adjusting the type and concentration of materials (mainly liquid crystal material and chiral agent) used for forming the layer. Moreover, the thickness of a layer can be made into a desired range by adjusting the application quantity.
- the adjacent light reflecting layers 14a and 14b have the spiral directions of the respective cholesteric liquid crystal phases opposite to each other, and similarly, the adjacent light reflecting layers 16a and 16b have the spiral directions of the respective cholesteric liquid crystal phases.
- the opposite is true.
- it is possible to reflect both the left circularly polarized light and the right circularly polarized light having the same wavelength by arranging adjacent light reflecting layers made of cholesteric liquid crystal phases in the opposite directions and having the same selective reflection center wavelength. it can. This action is irrelevant to the optical characteristics of the substrate 12 and is obtained without being affected by the optical characteristics of the substrate 12.
- a method comprising forming a layer composed of a desired cholesteric liquid crystal phase on separate temporary supports, and laminating and laminating these layers; or a cholesteric suitable as each light reflecting layer in a liquid crystal composition
- a material capable of forming a liquid crystal phase is mixed, and the composition is applied to the surface of a support to form a film, followed by phase separation during drying and thermal alignment to form a two-layer cholesteric liquid crystal layer
- the method of doing; etc. are known.
- the former method using the lamination process is expensive, and the latter method using the phase separation increases the film thickness as a whole, deteriorates the orientation state, and causes fluctuations in the interface of the phase separation.
- the orientation state deteriorates as well.
- a laminated structure of the light reflecting layer is obtained by repeating the coating, it is preferable because a costly process such as laminating is unnecessary and a process that is difficult to control such as phase separation is not necessary.
- the refractive index anisotropy [Delta] n 14a of the light reflecting layer 14a, and the refractive index anisotropy [Delta] n 14b of the light reflecting layer 14b is to satisfy the [Delta] n 14b ⁇ [Delta] n 14a, and refraction of the light reflecting layer 16a
- the index anisotropy ⁇ n 16a and the refractive index anisotropy ⁇ n 16b of the light reflecting layer 16b satisfy ⁇ n 16b ⁇ n 16a .
- a liquid crystal composition is applied to the surface of each of the light reflecting layers 14a and 16a to form a cholesteric liquid crystal phase, and the state is fixed to form the light reflecting layers 14b and 16b, respectively.
- the alignment state of the light reflecting layers 14b and 16b is good and exhibits desired light reflecting characteristics.
- the value is close to ⁇ n indicated by the rod-shaped liquid crystal. Therefore, if a light reflecting layer is formed using a liquid crystal composition containing a rod-like liquid crystal having a higher ⁇ n as a main raw material, ⁇ n of the light reflecting layer is naturally increased. On the other hand, when the concentration of the chiral agent added to obtain a desired helical pitch is high, the compounding ratio of the rod-like liquid crystal is relatively lowered, so that ⁇ n as a composition becomes small. Therefore, if a lower light reflection layer is formed using a liquid crystal composition that originally contains a rod-like liquid crystal having a high ⁇ n and a small amount of additive such as a chiral agent, ⁇ n of the lower light reflection layer is increased. .
- a liquid crystal with a high ⁇ n is in the desired cholesteric liquid crystal phase state even without the addition of an additive such as a chiral agent, so there is no disorder of the interface or disorder due to the presence of the additive, etc., and a lower layer is formed. it can.
- the liquid crystal composition for the upper layer can be applied to the surface of the lower layer in which the alignment state is good and is not disturbed, the desired cholesteric liquid crystal phase can be formed more stably, and the upper layer satisfying the desired characteristics can be formed. This is presumably due to the ability to form a light reflecting layer.
- the light reflection layer 14a is made of a liquid crystal composition containing a right-turning chiral agent, that is, selectively reflects right-circularly polarized light
- the light reflection layer 14b contains a left-turning chiral agent.
- the left circularly polarized light is selectively reflected
- the light reflecting layer 16a is formed of a liquid crystal composition containing a right-turning chiral agent, that is, the right circularly polarized light is selectively reflected, and the light reflecting layer.
- 16b is made of a liquid crystal composition containing a left-turning chiral agent, that is, selectively reflects left circularly polarized light.
- FIG. 2 sectional drawing of the infrared-light reflecting plate of other embodiment of this invention is shown.
- the infrared light reflecting plate 10 ′ shown in FIG. 2 is the same as the infrared light reflecting plate 10 in FIG. 1, the light reflecting layers 14a and 14b on one surface of the substrate 12, and the light reflecting layer on the other surface. 16a and 16b. These characteristics and the relationship between them are the same as those of the infrared light reflection plate 10.
- the infrared light reflection plate 10 ′ further includes light reflection layers 18a and 18b on the surface of the light reflection layer 14b, and light reflection layers 20a and 20b on the surface of the light reflection layer 16b.
- the light reflecting layers 18a and 18b and the light reflecting layers 20a and 20b have the cholesteric liquid crystal phases in the spiral directions opposite to each other, and The reflection center wavelength is the same.
- the reflection center wavelength lambda 18 of the light reflecting layer 18a and 18b, reflection center wavelength lambda 20 of the light reflecting layers 20a and 20b, together are different from each other, they are reflected in the light reflection layer 14a and 14b the central wavelength lambda 14 and the reflection center wavelength ⁇ 16 of the light reflecting layers 16a and 16b are not equal.
- the infrared light reflection plate 10 ′ like the infrared light reflection plate 10, has selective reflection characteristics for the left circularly polarized light and the right circularly polarized light having the reflection center wavelength ⁇ 14 by the light reflective layers 14a and 14b, and the light reflective layer together show selective reflection characteristics with respect to left circularly polarized light and right circularly polarized light of the reflected center wavelength lambda 16 by 16a and 16b, the selective reflection characteristics with respect to left circularly polarized light and right circularly polarized light reflected by the light reflecting layer 18a and 18b center wavelength lambda 18,
- selective reflection characteristics for the left circularly polarized light and the right circularly polarized light having the reflection center wavelength ⁇ 20 by the light reflection layers 20a and 20b are shown, and the wavelength band of selective reflection is made wider.
- any of the reflection center wavelengths ⁇ 14 , ⁇ 16 , ⁇ 18, and ⁇ 20 is in the range of 800 to 1000 nm (more preferably, 850 to 950 nm), and any of 900 to 1100 nm (more preferably, 950). Is in the range of 1000 to 1200 nm (more preferably, 1050 to 1150 nm), and one is in the range of 1100 to 1300 nm (preferably, 1150 to 1250 nm). However, it is not limited to this example.
- the group of the light reflecting layers 14a and 14b arranged on the same surface is compared with the group of the light reflecting layers 18a and 18b, the group of the light reflecting layers closer to the substrate, that is, the light reflecting layer 14a and The reflection center wavelength ⁇ 14 of the set 14b is preferably shorter than the reflection center wavelength ⁇ 18 of the set of the light reflection layers 18a and 18b, and similarly, the light reflection layer 16a disposed on the same surface. 16b and the set of the light reflecting layers 20a and 20b are compared, the reflection center wavelength ⁇ 16 of the set of the light reflecting layers closer to the substrate, that is, the set of the light reflecting layers 16a and 16b is the light reflecting layer 20a.
- the reflection characteristics for the short wavelength light are improved.
- the effect as a structural member will be kept good. That is, ⁇ 14 , ⁇ 16 , ⁇ 18 and ⁇ 20 are not equal to each other, and it is preferable that ⁇ 14 ⁇ 18 and ⁇ 16 ⁇ 20 are satisfied.
- the formation method of the light reflection layers 18a, 18b, 20a, and 20b there is no restriction
- a simpler method as described above, there is a method in which a liquid crystal composition is applied to the surface of the lower layer to form a cholesteric liquid crystal phase, and then the alignment state is fixed.
- the surface properties and orientation state of the lower layer affect the orientation state and the like of the layer formed thereon. Therefore, in the case of manufacturing by this method, the refractive index of the light reflecting layer 18a is different.
- the refractive index anisotropy [Delta] n 18b of the light reflecting layer 18b is to satisfy the [Delta] n 18b ⁇ [Delta] n 18a, and the refractive index anisotropy [Delta] n 20a of the light reflecting layer 20a, and refraction of the light reflecting layer 20b
- the rate anisotropy ⁇ n 20b preferably satisfies ⁇ n 20b ⁇ n 20a .
- the mode of the infrared light reflector of the present invention is not limited to the mode shown in FIGS. It is also possible to have a configuration in which light reflecting layers are laminated such as 3 sets (total 6 layers), 4 sets (total 8 layers) or more on both surfaces of the substrate. Further, the number of light reflecting layers may be different on one surface of the substrate and the other surface. Moreover, the aspect which has 2 or more sets of light reflection layers which show the same reflection center wavelength may be sufficient.
- the infrared light reflector of the present invention may of course be used in combination with other infrared light reflectors for the purpose of broadening the reflection wavelength. Moreover, you may have the light reflection layer which reflects the light of a predetermined wavelength by principles other than the selective reflection characteristic of a cholesteric liquid crystal phase. Examples of members that can be combined include the composite film described in JP-A-4-504555 and the layers constituting the composite film, and the multilayer laminate described in JP-A-2008-545556.
- the infrared light reflection plate of the present invention may have an easy-adhesion layer as the outermost layer in order to make it easy to adhere to other members.
- the easy adhesion layer contains polyvinyl butyral resin as a main component
- the thermal adhesiveness with the interlayer film of the laminated glass is improved, and the infrared light reflector of the present invention can be easily sandwiched in the laminated glass. it can.
- the adhesion between the easy-adhesion layer and the intermediate film is high, the light resistance is excellent, and even when exposed to natural light for a long time, there is no deterioration due to generation of bubbles and the like, which is preferable.
- It is preferable to add an ultraviolet absorber to the easy-adhesion layer because the light resistance is further improved and yellowing of the light reflecting layer due to long-term natural light irradiation can be suppressed.
- the infrared light reflecting plate of the present invention it is preferable to use a curable liquid crystal composition for forming each light reflecting layer.
- the liquid crystal composition contains at least a rod-like liquid crystal compound, an optically active compound (chiral agent), and a polymerization initiator. Two or more of each component may be included.
- a polymerizable liquid crystal compound and a non-polymerizable liquid crystal compound can be used in combination. Also, a combination of a low-molecular liquid crystal compound and a high-molecular liquid crystal compound is possible.
- it contains at least one selected from various additives such as a horizontal alignment agent, a non-uniformity inhibitor, a repellency inhibitor, and a polymerizable monomer. May be.
- a polymerization inhibitor, an antioxidant, an ultraviolet absorber, a light stabilizer, and the like can be further added to the liquid crystal composition as necessary so long as the optical performance is not deteriorated.
- Rod-like liquid crystal compound An example of the rod-like liquid crystal compound that can be used in the present invention is a rod-like nematic liquid crystal compound.
- the rod-like nematic liquid crystal compound include azomethines, azoxys, cyanobiphenyls, cyanophenyl esters, benzoic acid esters, cyclohexanecarboxylic acid phenyl esters, cyanophenylcyclohexanes, cyano-substituted phenylpyrimidines, alkoxy-substituted Phenylpyrimidines, phenyldioxanes, tolanes and alkenylcyclohexylbenzonitriles are preferably used. Not only low-molecular liquid crystal compounds but also high-molecular liquid crystal compounds can be used.
- the rod-like liquid crystal compound used in the present invention may be polymerizable or non-polymerizable.
- the rod-like liquid crystal compound having no polymerizable group is described in various documents (for example, Y. Goto et.al., Mol. Cryst. Liq. Cryst. 1995, Vol. 260, pp. 23-28).
- the polymerizable rod-like liquid crystal compound can be obtained by introducing a polymerizable group into the rod-like liquid crystal compound.
- the polymerizable group include an unsaturated polymerizable group, an epoxy group, and an aziridinyl group, preferably an unsaturated polymerizable group, and particularly preferably an ethylenically unsaturated polymerizable group.
- the polymerizable group can be introduced into the molecule of the rod-like liquid crystal compound by various methods.
- the number of polymerizable groups possessed by the polymerizable rod-like liquid crystal compound is preferably 1 to 6, more preferably 1 to 3.
- Examples of the polymerizable rod-like liquid crystal compound are described in Makromol. Chem. 190, 2255 (1989), Advanced Materials 5, 107 (1993), US Pat. Nos. 4,683,327, 5,622,648, and 5,770,107, International Publication WO95 / 22586. No. 95/24455, No. 97/00600, No. 98/23580, No. 98/52905, JP-A-1-272551, JP-A-6-16616, and JP-A-7-110469.
- Two or more kinds of polymerizable rod-like liquid crystal compounds may be used in combination.
- the alignment temperature can be lowered.
- the liquid crystal composition exhibits a cholesteric liquid crystal phase, and for that purpose, it preferably contains an optically active compound.
- the rod-like liquid crystal compound is a molecule having an illegitimate carbon atom
- a cholesteric liquid crystal phase may be stably formed without adding an optically active compound.
- the optically active compound includes various known chiral agents (for example, Liquid Crystal Device Handbook, Chapter 3-4-3, TN, chiral agent for STN, 199 pages, edited by Japan Society for the Promotion of Science, 142nd Committee, 1989). ) Can be selected.
- the optically active compound generally contains an asymmetric carbon atom, but an axially asymmetric compound or a planar asymmetric compound that does not contain an asymmetric carbon atom can also be used as a chiral agent.
- the axial asymmetric compound or the planar asymmetric compound include binaphthyl, helicene, paracyclophane, and derivatives thereof.
- the optically active compound (chiral agent) may have a polymerizable group.
- the optically active compound has a polymerizable group and the rod-like liquid crystal compound used in combination also has a polymerizable group, it is derived from the rod-like liquid crystal compound by a polymerization reaction of the polymerizable optically active compound and the polymerizable rod-like liquid crystal compound.
- a polymer having a repeating unit and a repeating unit derived from an optically active compound can be formed.
- the polymerizable group possessed by the polymerizable optically active compound is preferably the same group as the polymerizable group possessed by the polymerizable rod-like liquid crystal compound.
- the polymerizable group of the optically active compound is also preferably an unsaturated polymerizable group, an epoxy group or an aziridinyl group, more preferably an unsaturated polymerizable group, and an ethylenically unsaturated polymerizable group.
- the optically active compound may be a liquid crystal compound.
- the optically active compound in the liquid crystal composition is preferably 1 to 30 mol% with respect to the liquid crystal compound used in combination. A smaller amount of the optically active compound is preferred because it often does not affect liquid crystallinity. Therefore, the optically active compound used as the chiral agent is preferably a compound having a strong twisting power so that a twisted orientation with a desired helical pitch can be achieved even with a small amount. Examples of such a chiral agent exhibiting a strong twisting force include those described in JP-A-2003-287623, which can be preferably used in the present invention.
- the infrared light reflecting plate of the present invention has a structure in which light reflecting layers whose spiral directions of cholesteric liquid crystal phases are opposite to each other are adjacent to each other.
- the pair of adjacent light reflecting layers is characterized in that the refractive index anisotropy of the lower light reflecting layer is larger than the refractive index anisotropy of the upper light reflecting layer.
- the refractive index anisotropy of the layer is affected by the refractive index anisotropy of the liquid crystal material used as the main raw material, the amount of added chiral agent, and the like.
- a right-turning chiral agent a strong twisting power is provided to the market more than a left-turning chiral agent.
- the amount of right-turning chiral agent added can be made smaller than the amount of left-turning chiral agent added.
- the refractive index anisotropy ⁇ n can be lowered. Therefore, as the liquid crystal composition for forming the lower light reflecting layer, a composition containing a right-turning chiral agent is used, and as the liquid crystal composition for forming the information light reflecting layer, the left-turning property is used.
- An embodiment using a composition containing a chiral agent is preferable because of a wide selection of materials.
- the liquid crystal composition used for forming the light reflecting layer is preferably a polymerizable liquid crystal composition, and for that purpose, it preferably contains a polymerization initiator.
- the polymerization initiator to be used is preferably a photopolymerization initiator capable of starting the polymerization reaction by irradiation with ultraviolet rays.
- photopolymerization initiators include ⁇ -carbonyl compounds (described in US Pat. Nos. 2,367,661 and 2,367,670), acyloin ether (described in US Pat. No. 2,448,828), ⁇ -hydrocarbon substituted aromatics.
- the amount of the photopolymerization initiator used is preferably 0.1 to 20% by mass, more preferably 1 to 8% by mass of the liquid crystal composition (solid content in the case of a coating liquid).
- Alignment control agent An alignment control agent that contributes to stable or rapid cholesteric liquid crystal phase may be added to the liquid crystal composition.
- the alignment control agent include fluorine-containing (meth) acrylate-based polymers and compounds represented by the following general formulas (X1) to (X3). You may contain 2 or more types selected from these. These compounds can reduce the tilt angle of the molecules of the liquid crystal compound or can be substantially horizontally aligned at the air interface of the layer.
- horizontal alignment means that the major axis of the liquid crystal molecule is parallel to the film surface, but it is not required to be strictly parallel. An orientation with an inclination angle of less than 20 degrees is meant.
- R 1 , R 2 and R 3 each independently represent a hydrogen atom or a substituent
- X 1 , X 2 and X 3 each represent a single bond or a divalent linking group.
- the substituents represented by R 1 to R 3 are each preferably a substituted or unsubstituted alkyl group (more preferably an unsubstituted alkyl group or a fluorine-substituted alkyl group), an aryl group (particularly a fluorine-substituted alkyl group).
- An aryl group having a group is preferred), a substituted or unsubstituted amino group, an alkoxy group, an alkylthio group, and a halogen atom.
- the divalent linking groups represented by X 1 , X 2 and X 3 are each an alkylene group, an alkenylene group, a divalent aromatic group, a divalent heterocyclic residue, —CO—, —NRa— (Ra Is a divalent linking group selected from the group consisting of —O—, —S—, —SO—, —SO 2 —, and combinations thereof. Is preferred.
- the divalent linking group is selected from the group consisting of an alkylene group, a phenylene group, —CO—, —NRa—, —O—, —S— and —SO 2 — or selected from the group. It is more preferably a divalent linking group in which at least two groups are combined.
- the number of carbon atoms of the alkylene group is preferably 1-12.
- the alkenylene group preferably has 2 to 12 carbon atoms.
- the number of carbon atoms of the divalent aromatic group is preferably 6-10.
- R represents a substituent
- m represents an integer of 0 to 5.
- Preferred substituents for R are the same as those mentioned as preferred ranges for the substituents represented by R 1 , R 2 , and R 3 .
- m preferably represents an integer of 1 to 3, particularly preferably 2 or 3.
- R 4 , R 5 , R 6 , R 7 , R 8 and R 9 each independently represent a hydrogen atom or a substituent.
- the substituents represented by R 4 , R 5 , R 6 , R 7 , R 8 and R 9 are preferably the substituents represented by R 1 , R 2 and R 3 in the general formula (XI). It is the same as that mentioned as a thing.
- Examples of the compounds represented by the formulas (X1) to (X3) that can be used as the alignment control agent in the present invention include compounds described in JP-A-2005-99248.
- the alignment control agent one type of the compounds represented by the general formulas (X1) to (X3) may be used alone, or two or more types may be used in combination.
- the amount of the compound represented by any one of the general formulas (X1) to (X3) in the liquid crystal composition is preferably 0.01 to 10% by mass, and 0.01 to 5% by mass of the liquid crystal compound. % Is more preferable, and 0.02 to 1% by mass is particularly preferable.
- the infrared light reflection plate of the present invention has a substrate, but the substrate is self-supporting, and there is no limitation on the material and optical characteristics as long as it supports the light reflection layer. Depending on the application, high transparency to ultraviolet light will be required. It is not necessary to use a retardation plate such as a ⁇ / 2 plate manufactured by managing the production process so as to satisfy a predetermined optical characteristic. Can be used. If this is expressed by the variation of the in-plane retardation Re (1000) at a wavelength of 1000 nm, the variation of Re (1000) may be 20 nm or more, or may be 100 nm or more.
- the in-plane retardation of the substrate is not particularly limited. For example, a retardation plate having an in-plane retardation Re (1000) of a wavelength of 1000 nm of 800 to 13000 nm can be used.
- polymer films having high transparency to visible light examples include polymer films for various optical films used as members of display devices such as liquid crystal display devices.
- the substrate examples include polyester films such as polyethylene terephthalate (PET), polybutylene terephthalate, and polyethylene naphthalate (PEN); polycarbonate (PC) films and polymethyl methacrylate films; polyolefin films such as polyethylene and polypropylene; polyimide films, An acetyl cellulose (TAC) film etc. are mentioned.
- the infrared light reflecting plate of the present invention is preferably produced by a coating method.
- An example of a manufacturing method is (1) Applying a curable liquid crystal composition to the surface of a substrate or the like to make a cholesteric liquid crystal phase; (2) irradiating the curable liquid crystal composition with ultraviolet rays to advance a curing reaction, fixing a cholesteric liquid crystal phase, and forming a light reflection layer; Is a production method comprising at least By repeating the steps of (1) and (2) twice on one surface of the substrate and twice on the other surface of the substrate; or by simultaneously repeating twice on both surfaces of the substrate, An infrared light reflector having the same configuration as that shown in FIG. 1 can be manufactured. Also, repeat steps (1) and (2) 4 times on one surface of the substrate and 4 times on the other surface of the substrate; or 4 times simultaneously on both surfaces of the substrate. Thus, an infrared light reflector having the same configuration as that shown in FIG. 2 can be produced.
- the curable liquid crystal composition is applied to the surface of the substrate or the lower light reflection layer.
- the curable liquid crystal composition is preferably prepared as a coating solution in which a material is dissolved and / or dispersed in a solvent.
- the coating liquid can be applied by various methods such as a wire bar coating method, an extrusion coating method, a direct gravure coating method, a reverse gravure coating method, and a die coating method.
- a liquid crystal composition can be discharged from a nozzle using an ink jet apparatus to form a coating film.
- the curable liquid crystal composition applied to the surface to become a coating film is brought into a cholesteric liquid crystal phase.
- the coating film may be dried and the solvent may be removed to obtain a cholesteric liquid crystal phase.
- the cholesteric liquid crystal phase can be stably formed by heating to the temperature of the isotropic phase and then cooling to the cholesteric liquid crystal phase transition temperature.
- the liquid crystal phase transition temperature of the curable liquid crystal composition is preferably in the range of 10 to 250 ° C., more preferably in the range of 10 to 150 ° C. from the viewpoint of production suitability and the like.
- a cooling step or the like may be required to lower the temperature to a temperature range exhibiting a liquid crystal phase.
- a high temperature is required to make the isotropic liquid state higher than the temperature range once exhibiting the liquid crystal phase, which is disadvantageous from waste of thermal energy, deformation of the substrate, and alteration.
- the coating film in the cholesteric liquid crystal phase is irradiated with ultraviolet rays to advance the curing reaction.
- a light source such as an ultraviolet lamp is used.
- the curing reaction of the liquid crystal composition proceeds, the cholesteric liquid crystal phase is fixed, and a light reflecting layer is formed.
- the amount of irradiation energy of ultraviolet rays is not particularly limited, but is generally preferably about 100 mJ / cm 2 to 800 mJ / cm 2 .
- ultraviolet irradiation may be performed under heating conditions. Moreover, it is preferable to maintain the temperature at the time of ultraviolet irradiation in the temperature range which exhibits a cholesteric liquid crystal phase so that a cholesteric liquid crystal phase may not be disturbed. Also, since the oxygen concentration in the atmosphere is related to the degree of polymerization, if the desired degree of polymerization is not reached in the air and the film strength is insufficient, the oxygen concentration in the atmosphere is reduced by a method such as nitrogen substitution. It is preferable. A preferable oxygen concentration is preferably 10% or less, more preferably 7% or less, and most preferably 3% or less.
- the reaction rate of the curing reaction (for example, polymerization reaction) that proceeds by irradiation with ultraviolet rays is 70% or more from the viewpoint of maintaining the mechanical strength of the layer and suppressing unreacted substances from flowing out of the layer. Preferably, it is 80% or more, more preferably 90% or more.
- a method of increasing the irradiation amount of ultraviolet rays to be irradiated and polymerization under a nitrogen atmosphere or heating conditions are effective.
- a method of further promoting the reaction by a thermal polymerization reaction by maintaining the polymer at a temperature higher than the polymerization temperature, or a method of irradiating ultraviolet rays again (however, irradiation is performed under conditions satisfying the conditions of the present invention).
- the reaction rate can be measured by comparing the absorption intensity of the infrared vibration spectrum of a reactive group (for example, a polymerizable group) before and after the reaction proceeds.
- the cholesteric liquid crystal phase is fixed and the light reflecting layer is formed.
- the state in which the liquid crystal phase is “fixed” is the most typical and preferred mode in which the orientation of the liquid crystal compound in the cholesteric liquid crystal phase is maintained.
- the layer has no fluidity and is oriented by an external field or external force. It shall mean a state in which the fixed orientation form can be kept stable without causing a change in form.
- the alignment state of the cholesteric liquid crystal phase is fixed by a curing reaction that proceeds by ultraviolet irradiation.
- the liquid crystal composition may have a high molecular weight due to a curing reaction and may no longer have liquid crystallinity.
- the infrared light reflection plate of the present invention may have an easy-adhesion layer containing a polyvinyl butyral resin as at least one outermost layer.
- Laminated glass is generally produced by thermally bonding an intermediate film formed on the inner surfaces of two glass plates.
- the surface of the light reflecting layer is thermally bonded to the intermediate film.
- these adhesion forces are insufficient, when exposed to natural light for a long time and the temperature rises, bubbles are generated between the light reflecting layer and the intermediate film, and the transparency is lowered.
- the surface of the easy-adhesion layer only needs to be thermally bonded to the intermediate film when sandwiched in the glass plate, thereby improving adhesion. As a result, the light resistance is improved.
- the polyvinyl butyral resin is a kind of polyvinyl acetal produced by reacting polyvinyl alcohol and butyraldehyde with an acid catalyst, and is a resin having a repeating unit having the following structure.
- the easy adhesion layer is formed by coating.
- it may be formed by coating on the surface of a light reflecting layer formed by fixing a cholesteric liquid crystal phase. More specifically, one type of polyvinyl butyral resin is dissolved in an organic solvent to prepare a coating solution, the coating solution is applied to the surface of a light reflection layer, etc., and heated and dried as desired.
- An adhesive layer can be formed.
- a solvent used for preparing the coating solution for example, methoxypropyl acetate (PGMEA), methyl ethyl ketone (MEK), isopropanol (IPA) and the like can be used.
- a solvent used for preparing the coating solution for example, methoxypropyl acetate (PGMEA), methyl ethyl ketone (MEK), isopropanol (IPA) and the like can be used.
- Various conventionally known methods can be used as the coating method.
- the preferred temperature for drying varies depending on the material used for the preparation
- an ultraviolet absorber to the easy-adhesion layer.
- usable ultraviolet absorbers include benzotriazole-based, benzodithiol-based, coumarin-based, benzophenone-based, salicylic acid ester-based, and cyanoacrylate-based ultraviolet absorbers; titanium oxide, zinc oxide, and the like.
- particularly preferable ultraviolet absorbers include Tinuvin 326, 328, 479 (all manufactured by Ciba Japan).
- the type and blending amount of the ultraviolet absorber are not particularly limited and may be appropriately selected depending on the intended purpose.
- the easy-adhesion layer makes the transmittance of ultraviolet rays having a wavelength of 380 nm or less 0.1% or less. An action is preferable because yellowing due to ultraviolet rays can be remarkably reduced. Therefore, it is preferable to determine the type and blending amount of the ultraviolet absorber so as to satisfy this characteristic.
- the present invention relates to an infrared light reflective laminated glass using the infrared light reflection plate of the present invention, specifically, an infrared light having two glass plates and the infrared light reflection plate of the present invention in between. It relates to light reflective glass. It is preferable to use the infrared light reflector of the present invention having an easy-adhesion film as the outermost layer.
- the two glass plates used for the production of laminated glass are each a glass plate for laminated glass having an intermediate film on the surface, and general ones can be used.
- the intermediate film generally contains a polyvinyl butyral resin (PVB) or an ethylene / vinyl acetate copolymer (EVA) as a main raw material.
- PVB polyvinyl butyral resin
- EVA ethylene / vinyl acetate copolymer
- the easy-adhesion layer has good adhesion to an intermediate film made of any material as a main raw material. In particular, it is excellent in thermal adhesiveness with an intermediate film made mainly of polyvinyl butyral resin.
- a preferable range changes according to a use. For example, it is generally preferable to use a glass plate having a thickness of 2.0 to 2.3 mm in the application of a windshield (window shield) of a transportation vehicle.
- the thickness of the intermediate film is generally about 380 to 760 ⁇ m.
- infrared light reflecting plate and infrared light reflecting laminated glass are selected to have a reflection peak at a wavelength of 700 nm or more (more preferably from 800 to 1300 nm). Reflective properties are shown.
- the reflection plate having such characteristics is attached to a building such as a house, an office building, or a window of a vehicle such as an automobile as a member for heat insulation of solar radiation.
- the infrared-light reflecting plate of this invention can be used for the use as a member for heat insulation of solar radiation itself (for example, glass for heat insulation, a film for heat insulation).
- the infrared light reflecting plate and infrared light reflecting laminated glass of the present invention can reflect a maximum reflectance of 90% or more at a wavelength of 800 to 1300 nm, and of course, a maximum reflectance of 100% is most preferable.
- Other important performances as an infrared light reflecting plate and an infrared light reflecting laminated glass are transmittance of visible light and haze. By adjusting the selection of materials and manufacturing conditions, etc., an infrared light reflecting plate exhibiting preferable visible light transmittance and haze can be provided according to applications.
- an infrared light reflecting plate and an infrared light reflecting property in which the visible light transmittance is 90% or more and the infrared reflectance satisfies the above range Laminated glass can be used.
- each of the prepared coating solutions was applied at room temperature on a PET film manufactured by Fuji Film Co., Ltd. using a wire bar so that the dry film thickness after drying was 6 ⁇ m.
- the variation in Re (1000) of this PET film is shown in the table below.
- Infrared light reflectors shown in the following table were prepared by the above method. Each of the produced reflectors was evaluated by measuring the maximum reflectance of solar radiation at 800 to 1300 nm using a spectrophotometer.
- the PET film used as the substrate had a Re of about 4000 to 5000 nm.
- the PET film used in Comparative Example 3 had a Re of 4050 nm.
- Re variation of the substrate means variation of in-plane retardation Re (1000) having a wavelength of 1000 nm.
- the measurement of Re of a film having a large Re is obtained by the following method because it is difficult to obtain an accurate value with a general phase difference measuring apparatus. The measurement is performed using a polarizing microscope and a spectrum meter attached thereto.
- an interference filter with a known transmission center wavelength ⁇ is inserted into the optical path of a polarizing microscope, and the order (Re / ⁇ ) of the front Re of the sample at the wavelength ⁇ is grasped by observing the conoscopic image of the sample.
- Front Re means Re measured by making incident light incident on the sample film from the normal direction.
- the film is biaxial, an image with an order of 0 is seen, and the order of Re is determined from the number of interference fringes from that point to the vertical incidence position of the image. If the film is uniaxial or the orientation of order 0 is not visible, Re is a known retardation film and its slow axis is the sample until the vertical incident position of the image is near the 0th order interference color.
- the order of Re is determined by overlapping the sample so as to be orthogonal to the slow axis.
- the polarization microscope of the sample is measured at a diagonal position with the polarizing microscope in an orthoscope state.
- the transmittance gives a minimum value when the order is an integer including 0, and gives a maximum value when (2n + 1) / 2 (n is an integer including 0). Therefore, the transmission filter transmission center obtained by the above method is used.
- Re can be determined at the wavelength with the maximum and minimum transmittance. This is approximated to a quartic curve with respect to the wavelength and extrapolated to obtain Re at 1000 nm.
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Abstract
Description
特許文献2には、金属微粒子を含有する層を有する熱線反射性透明基材が提案されている。金属微粒子を含有する膜は、可視光の透過性能に優れるものの、遮熱に大きく関与する波長700~1200nmの範囲の光に対する反射率が低く、遮熱性能を高くできないという問題がある。
また、特許文献3には、赤外線吸収色素を含む層を有する熱線遮断シートが開示されている。赤外線吸収色素を利用すると、日射透過率を下げることができるものの、日射の吸収による膜面温度上昇と、その熱の再放出によって遮熱性能が低下するという問題がある。
また、特許文献5には、可視光透過性サブストレートと赤外光反射性コレステリック液晶層とを備えた赤外光反射性物品が開示されている。
また、特許文献6には、複数のコレステリック液晶層を備えた偏光素子が開示されているが、この様な、コレステリック液晶層を積層してなる積層体は、主には、可視光領域の光を効率的に反射させる用途に供せられるものである。
[1] 波長1000nmにおける面内レターデーションRe(1000)のバラツキが20nm以上である基板、
基板の一方の表面上に、コレステリック液晶相を固定してなる少なくとも2つの光反射層X1及びX2(但し、光反射層X1及びX2は、基板側からこの順で配置されているものとする)、並びに
基板の他方の表面上に、コレステリック液晶相を固定してなる少なくとも2つの光反射層Y1及びY2(但し、光反射層Y1及びY2は、基板側からこの順で配置されているものとする)、を少なくとも有し、
光反射層X1及びX2それぞれの反射中心波長がλX1(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
光反射層Y1及びY2のそれぞれの反射中心波長がλY1(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
λX1及びλY1が等しくなく、並びに
光反射層X1及びX2それぞれの屈折率異方性ΔnX1及びΔnX2が、ΔnX2<ΔnX1を満足し、且つ光反射層Y1及びY2それぞれの屈折率異方性ΔnY1及びΔnY2が、ΔnY2<ΔnY1を満足する、
波長700nm以上の赤外線を反射する赤外光反射板。
[2] 基板のRe(1000)のバラツキが100nm以上である[1]の赤外光反射板。
[3] 光反射層X1及びX2の反射中心波長λX1(nm)が、900~1050nmの範囲にあり、光反射層Y1及びY2の反射中心波長λY1(nm)が、1050~1300nmの範囲にある[1]又は[2]の赤外光反射板。
[4] 光反射層X2及びY2がそれぞれ、光反射層X1及びY1のそれぞれの表面に塗布された液晶組成物をコレステリック液晶相とし、該コレステリック液晶相を固定することで形成された層である[1]~[3]のいずれかの赤外光反射板。
[5] 波長1000nmの面内レターデーションRe(1000)が、800~13000nmである[1]~[4]のいずれかの赤外光反射板。
[6] 光反射層X2の上に、コレステリック液晶相を固定してなる2つの光反射層X3及びX4を有するとともに、光反射層Y2の上に、コレステリック液晶相を固定してなる2つの光反射層Y3及びY4を有し、
光反射層X3及びX4のそれぞれの反射中心波長がλX3(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
光反射層Y3及びY4それぞれの反射中心波長が波長λY3(nm)であり互いに等しく、且つ互いに異なる方向の円偏光を反射し、並びに、
λX3及びλY3が互いに等しくなく且つλX1及びλY1のいずれとも等しくない、
[1]~[5]のいずれかの赤外光反射板。
[7] 少なくとも1つの最外層として、易接着層を有する[1]~[6]のいずれかの赤外光反射板。
[8] 前記易接着層が、ポリビニルブチラール樹脂を含有する[7]の赤外光反射板。
[9] 前記易接着層が、少なくとも1種の紫外線吸収剤を含有する[7]又は[8]の赤外光反射板。
[10] 2枚のガラス板と、その間に[1]~[9]のいずれかの赤外光反射板とを有する赤外光反射性合わせガラス。
また、本明細書において、コレステリック液晶相を固定してなる層の屈折率異方性Δnは、以下の通り定義される。
本明細書においては、コレステリック液晶相を固定して形成される層の屈折率異方性Δnは、選択反射特性を示す波長(具体的には、波長1000nm近傍)でのΔnを意味する。具体的には、まず、サンプルとして、螺旋軸を膜面に対して均一に配向させたコレステリック液晶相を固定した層を配向処理した、若しくは配向膜を付与した基板(ガラス、フィルム)上に形成する。当該層の選択反射を測定し、そのピーク幅Hwを求める。また、サンプルの螺旋ピッチpを別途測定する。螺旋ピッチは、断面TEM観察することによって測定可能である。これらの値を以下の式に代入することで、サンプルの屈折率異方性Δnを求めることができる。
Δn=Hw/p
図1に示す赤外光反射板は、基板12の一方の表面に、コレステリック液晶相を固定してなる光反射層14a及び14bを有し、基板12の他方の表面に、コレステリック液晶相を固定してなる光反射層16a及び16bを有する。基板12は、例えば、ポリマーフィルムであり、その光学特性については特に制限はない。本発明では、特に、面内レターデーションReについてばらつきのある部材を基板として用いることが1つの特徴であり、この点で、基板としてλ/2を用い、その光学特性を光反射特性の改善に積極的に利用している従来技術とは区別される。但し、勿論、基板12としてλ/2板等の正確に位相差が調整されている位相差板を利用することを妨げるものではない。
なお、同一の面上に配置されている光反射層14a及び14bの組と、光反射層18aと18bの組とを比較すると、より基板に近い光反射層の組、即ち光反射層14a及び14bの組の反射中心波長λ14が、光反射層18aと18bの組の反射中心波長λ18より短波長であるのが好ましく、同様に、同一の面上に配置されている光反射層16a及び16bの組と、光反射層20aと20bの組とを比較すると、より基板に近い光反射層の組、即ち光反射層16a及び16bの組の反射中心波長λ16が、光反射層20aと20bの組の反射中心波長λ20より短波長であるのが好ましい。上層になるほど、光反射層を形成する過程で、安定なコレステリック液晶相が得られ難くなり、その結果、所望の選択反射特性が得られ難くなるという傾向がある。よって、エネルギーの高い(熱上昇効果の高い)短波長の光に対する反射特性を示す光反射層の組を基板側に形成すれば、当該短波長の光に対する反射特性は良好となるので、遮熱用部材としての効果が良好に保たれるであろう。即ち、λ14、λ16、λ18及びλ20はいずれも互いに等しくなく、λ14<λ18且つλ16<λ20を満足しているのが好ましい。
1.光反射層形成用材料
本発明の赤外光反射板では、各光反射層の形成に、硬化性の液晶組成物を用いるのが好ましい。前記液晶組成物の一例は、棒状液晶化合物、光学活性化合物(キラル剤)、及び重合開始剤を少なくとも含有する。各成分を2種以上含んでいてもよい。例えば、重合性の液晶化合物と非重合性の液晶化合物との併用が可能である。また、低分子液晶化合物と高分子液晶化合物との併用も可能である。更に、配向の均一性や塗布適性、膜強度を向上させるために、水平配向剤、ムラ防止剤、ハジキ防止剤、及び重合性モノマー等の種々の添加剤から選ばれる少なくとも1種を含有していてもよい。また、前記液晶組成物中には、必要に応じて、さらに重合禁止剤、酸化防止剤、紫外線吸収剤、光安定化剤等を光学的性能を低下させない範囲で添加することができる。
本発明に使用可能な棒状液晶化合物の例は、棒状ネマチック液晶化合物である。前記棒状ネマチック液晶化合物の例には、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、トラン類及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。低分子液晶化合物だけではなく、高分子液晶化合物も用いることができる。
重合性棒状液晶化合物は、重合性基を棒状液晶化合物に導入することで得られる。重合性基の例には、不飽和重合性基、エポキシ基、及びアジリジニル基が含まれ、不飽和重合性基が好ましく、エチレン性不飽和重合性基が特に好ましい。重合性基は種々の方法で、棒状液晶化合物の分子中に導入できる。重合性棒状液晶化合物が有する重合性基の個数は、好ましくは1~6個、より好ましくは1~3個である。重合性棒状液晶化合物の例は、Makromol.Chem.,190巻、2255頁(1989年)、Advanced Materials 5巻、107頁(1993年)、米国特許第4683327号明細書、同5622648号明細書、同5770107号明細書、国際公開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、及び特開2001-328973号公報などに記載の化合物が含まれる。2種類以上の重合性棒状液晶化合物を併用してもよい。2種類以上の重合性棒状液晶化合物を併用すると、配向温度を低下させることができる。
前記液晶組成物は、コレステリック液晶相を示すものであり、そのためには、光学活性化合物を含有しているのが好ましい。但し、上記棒状液晶化合物が不正炭素原子を有する分子である場合には、光学活性化合物を添加しなくても、コレステリック液晶相を安定的に形成可能である場合もある。前記光学活性化合物は、公知の種々のキラル剤(例えば、液晶デバイスハンドブック、第3章4-3項、TN、STN用カイラル剤、199頁、日本学術振興会第142委員会編、1989に記載)から選択することができる。光学活性化合物は、一般に不斉炭素原子を含むが、不斉炭素原子を含まない軸性不斉化合物あるいは面性不斉化合物もカイラル剤として用いることができる。軸性不斉化合物または面性不斉化合物の例には、ビナフチル、ヘリセン、パラシクロファンおよびこれらの誘導体が含まれる。光学活性化合物(キラル剤)は、重合性基を有していてもよい。光学活性化合物が重合性基を有するとともに、併用する棒状液晶化合物も重合性基を有する場合は、重合性光学活性化合物と重合性棒状液晶合物との重合反応により、棒状液晶化合物から誘導される繰り返し単位と、光学活性化合物から誘導される繰り返し単位とを有するポリマーを形成することができる。この態様では、重合性光学活性化合物が有する重合性基は、重合性棒状液晶化合物が有する重合性基と、同種の基であることが好ましい。従って、光学活性化合物の重合性基も、不飽和重合性基、エポキシ基又はアジリジニル基であることが好ましく、不飽和重合性基であることがさらに好ましく、エチレン性不飽和重合性基であることが特に好ましい。
また、光学活性化合物は、液晶化合物であってもよい。
前記光反射層の形成に用いる液晶組成物は、重合性液晶組成物であるのが好ましく、そのためには、重合開始剤を含有しているのが好ましい。本発明では、紫外線照射により硬化反応を進行させるので、使用する重合開始剤は、紫外線照射によって重合反応を開始可能な光重合開始剤であるのが好ましい。光重合開始剤の例には、α-カルボニル化合物(米国特許第2367661号、同2367670号の各明細書記載)、アシロインエーテル(米国特許第2448828号明細書記載)、α-炭化水素置換芳香族アシロイン化合物(米国特許第2722512号明細書記載)、多核キノン化合物(米国特許第3046127号、同2951758号の各明細書記載)、トリアリールイミダゾールダイマーとp-アミノフェニルケトンとの組み合わせ(米国特許第3549367号明細書記載)、アクリジン及びフェナジン化合物(特開昭60-105667号公報、米国特許第4239850号明細書記載)及びオキサジアゾール化合物(米国特許第4212970号明細書記載)等が挙げられる。
前記液晶組成物中に、安定的に又は迅速にコレステリック液晶相となるのに寄与する配向制御剤を添加してもよい。配向制御剤の例には、含フッ素(メタ)アクリレート系ポリマー、及び下記一般式(X1)~(X3)で表される化合物が含まれる。これらから選択される2種以上を含有していてもよい。これらの化合物は、層の空気界面において、液晶化合物の分子のチルト角を低減若しくは実質的に水平配向させることができる。尚、本明細書で「水平配向」とは、液晶分子長軸と膜面が平行であることをいうが、厳密に平行であることを要求するものではなく、本明細書では、水平面とのなす傾斜角が20度未満の配向を意味するものとする。液晶化合物が空気界面付近で水平配向する場合、配向欠陥が生じ難いため、可視光領域での透明性が高くなり、また赤外領域での反射率が増大する。一方、液晶化合物の分子が大きなチルト角で配向すると、コレステリック液晶相の螺旋軸が膜面法線からずれるため、反射率が低下したり、フィンガープリントパターンが発生し、ヘイズの増大や回折性を示すため好ましくない。
配向制御剤として利用可能な前記含フッ素(メタ)アクリレート系ポリマーの例は、特開2007-272185号公報の[0018]~[0043]等に記載がある。
なお、本発明では、配向制御剤として、前記一般式(X1)~(X3)で表される化合物の一種を単独で用いてもよいし、二種以上を併用してもよい。
本発明の赤外光反射板は、基板を有するが、当該基板は自己支持性があり、上記光反射層を支持するものであれば、材料及び光学的特性についてなんら限定はない。用途によっては、紫外光に対する高い透明性が要求されるであろう。所定の光学特性を満足するように、生産工程を管理して製造される、λ/2板等の位相差板でなくてもよく、市場に供給されているいずれのガラス板やポリマーフィルム等を用いることができる。このことを、波長1000nmの面内レターデーションRe(1000)のバラツキで表現すれば、Re(1000)のバラツキが20nm以上あってもよく、また100nm以上あってもよい。また基板の面内レターデーションについても特に制限はなく、例えば、波長1000nmの面内レターデーションRe(1000)が、800~13000nmである位相差板等を用いることができる。
本発明の赤外光反射板は、塗布方法によって作製されるのが好ましい。製造方法の一例は、
(1) 基板等の表面に、硬化性の液晶組成物を塗布して、コレステリック液晶相の状態にすること、
(2) 前記硬化性の液晶組成物に紫外線を照射して硬化反応を進行させ、コレステリック液晶相を固定して光反射層を形成すること、
を少なくとも含む製造方法である。
(1)及び(2)の工程を、基板の一方の表面上で2回繰り返し、基板の他方の表面上で2回繰り返すことで;又は基板の双方の表面上で同時に2回繰り返すことで、図1に示す構成と同様の構成の赤外光反射板を作製することができる。また、(1)及び(2)の工程を、基板の一方の表面上で4回繰り返し、基板の他方の表面上で4回繰り返すことで;又は基板の双方の表面上で同時に4回繰り返すことで、図2に示す構成と同様の構成の赤外光反射板を作製することができる。
紫外線の照射エネルギー量については特に制限はないが、一般的には、100mJ/cm2~800mJ/cm2程度が好ましい。また、前記塗膜に紫外線を照射する時間については特に制限はないが、硬化膜の充分な強度及び生産性の双方の観点から決定されるであろう。
なお、本発明においては、コレステリック液晶相の光学的性質が層中において保持されていれば十分であり、最終的に光反射層中の液晶組成物がもはや液晶性を示す必要はない。例えば、液晶組成物が、硬化反応により高分子量化して、もはや液晶性を失っていてもよい。
上記した通り、本発明の赤外光反射板は、少なくとも1つの最外層として、ポリビニルブチラール樹脂を含有する易接着層を有していてもよい。合わせガラスは、一般的には、2枚のガラス板の内面に形成された中間膜を熱接着して作製される。この合わせガラスの内部に、1層又は2層以上のコレステリック液晶相を固定して形成された光反射層を有する積層体を挟み込む場合には、該光反射層の表面を中間膜と熱接着させることになるが、これらの密着力が不十分であるため、長時間自然光に曝され、温度が上昇すると、光反射層と中間膜との間に気泡が発生して、透明性が低下する。本発明の赤外光反射板の最外層に易接着層を形成することで、ガラス板中に挟み込む際に、当該易接着層の表面を中間膜と熱接着させればよく、密着力が改善され、ひいては耐光性が改善される。
合わせガラスの作製に用いる2枚のガラス板は、それぞれ、表面に中間膜を有する合わせガラス用のガラス板であり、一般的なものを使用することができる。中間膜は、一般的には、ポリビニルブチラール樹脂(PVB)又はエチレン・酢酸ビニル共重合体(EVA)を主原料として含有する。前記易接着層は、いずれの材料を主原料とする中間膜に対しても接着性が良好である。特に、ポリビニルブチラール樹脂を主原料とする中間膜との熱接着性に優れる。
本発明の赤外光反射板及び赤外光反射性合わせガラスは、波長700nm以上(より好ましくは800~1300nm)に反射ピークのある選択反射特性を示す。この様な特性の反射板は、住宅、オフィスビル等の建造物、又は自動車等の車両の窓に、日射の遮熱用の部材として貼付される。又は、本発明の赤外光反射板は、日射の遮熱用の部材そのもの(たとえば、遮熱用ガラス、遮熱用フィルム)として、その用途に供することができる。
赤外光反射板及び赤外光反射性合わせガラスとしてその他の重要な性能は、可視光の透過率とヘイズである。材料の選択及び製造条件等を調整して、用途に応じて、好ましい可視光の透過率及びヘイズを示す赤外光反射板を提供できる。例えば可視光の透過率が高い用途に用いられる態様では、可視光の透過率が90%以上であり、且つ赤外の反射率が上記範囲を満足する赤外光反射板及び赤外光反射性合わせガラスとすることができる。
(2) 室温にて30秒間乾燥させてコレステリック液晶相とした後、125℃の雰囲気で2分間加熱し、その後95℃でフュージョン製Dバルブ(ランプ90mW/cm)にて、出力60%で6~12秒間UV照射し、コレステリック液晶相を固定して、膜(光反射層)を作製した。
(3)室温まで冷却した後、PETフィルムの他方の表面に対して、上記工程(1)及び(2)を繰り返した。
作製した各反射板について、分光光度計を用いて800~1300nmでの日射の最大反射率を測定して評価した。
なお、基板として使用したPETフィルムはいずれもReが4000~5000nm程度であった。また比較例3で使用したPETフィルムは、Reが4050nmであった。
また、下記表中、基板のReバラツキとは、波長1000nmの面内レターデーションRe(1000)のバラツキを意味する。Reが大きなフィルムのReの測定は、一般的な位相差測定装置では正確な値を得ることが困難であるため、以下のような方法によって求める。測定は偏光顕微鏡とそれに取り付けたスペクトルメータを用いて行なう。まず、透過中心波長λが機知の干渉フィルターを偏光顕微鏡の光路に挿入し、試料のコノスコープ像を観察することによって波長λでの試料の正面Reの次数(Re/λ)を把握する。なお「正面Re」とは、入射光を試料フィルムのフィルムに対して法線方向から入射させて測定されるReを意味する。フィルムが二軸性の場合は、次数が0の像が見えるので、そこを基点として像の垂直入射位置までの干渉縞の本数からReの次数を決定する。また、フィルムが一軸性もしくは、次数が0の方位が見えない場合は、像の垂直入射位置が0次の干渉色近傍になるまで、Reが機知の位相差膜をその遅相軸が試料の遅相軸と直交するように試料に重ねることで、Reの次数を決定する。次に偏光顕微鏡をオルソスコープの状態にして、且つ対角位で試料の偏光顕微スペクトル測定を行う。 透過率は次数が0を含めた整数の場合に極小値を与え、(2n+1)/2の場合(nは0を含む整数)に極大値をあたえるので、上記の方法によって求めた干渉フィルター透過中心波長λでの次数を用いて、透過率極大極小の波長でのReを決定することができる。これを波長に対する4次曲線近似して外挿することによって、1000nmでのReを求める。
12 基板
14a 光反射層(光反射層X1)
14b 光反射層(光反射層X2)
16a 光反射層(光反射層Y1)
16b 光反射層(光反射層Y2)
18a 光反射層(光反射層X3)
18b 光反射層(光反射層X4)
20a 光反射層(光反射層Y3)
20b 光反射層(光反射層Y4)
Claims (10)
- 波長1000nmにおける面内レターデーションRe(1000)のバラツキが20nm以上である基板、
基板の一方の表面上に、コレステリック液晶相を固定してなる少なくとも2つの光反射層X1及びX2(但し、光反射層X1及びX2は、基板側からこの順で配置されているものとする)、並びに
基板の他方の表面上に、コレステリック液晶相を固定してなる少なくとも2つの光反射層Y1及びY2(但し、光反射層Y1及びY2は、基板側からこの順で配置されているものとする)、を少なくとも有し、
光反射層X1及びX2それぞれの反射中心波長がλX1(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
光反射層Y1及びY2のそれぞれの反射中心波長がλY1(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
λX1及びλY1が等しくなく、並びに
光反射層X1及びX2それぞれの屈折率異方性ΔnX1及びΔnX2が、ΔnX2<ΔnX1を満足し、且つ光反射層Y1及びY2それぞれの屈折率異方性ΔnY1及びΔnY2が、ΔnY2<ΔnY1を満足する、
波長700nm以上の赤外線を反射する赤外光反射板。 - 基板のRe(1000)のバラツキが100nm以上である請求項1に記載の赤外光反射板。
- 光反射層X1及びX2の反射中心波長λX1(nm)が、900~1050nmの範囲にあり、光反射層Y1及びY2の反射中心波長λY1(nm)が、1050~1300nmの範囲にある請求項1又は2に記載の赤外光反射板。
- 光反射層X2及びY2がそれぞれ、光反射層X1及びY1のそれぞれの表面に塗布された液晶組成物をコレステリック液晶相とし、該コレステリック液晶相を固定することで形成された層である請求項1~3のいずれか1項に記載の赤外光反射板。
- 波長1000nmの面内レターデーションRe(1000)が、800~13000nmである請求項1~4のいずれか1項に記載の赤外光反射板。
- 光反射層X2の上に、コレステリック液晶相を固定してなる2つの光反射層X3及びX4を有するとともに、光反射層Y2の上に、コレステリック液晶相を固定してなる2つの光反射層Y3及びY4を有し、
光反射層X3及びX4のそれぞれの反射中心波長がλX3(nm)であり互いに等しく、且つ互いに逆方向の円偏光を反射し、
光反射層Y3及びY4それぞれの反射中心波長が波長λY3(nm)であり互いに等しく、且つ互いに異なる方向の円偏光を反射し、並びに、
λX3及びλY3が互いに等しくなく且つλX1及びλY1のいずれとも等しくない、
請求項1~5のいずれか1項に記載の赤外光反射板。 - 少なくとも1つの最外層として、易接着層を有する請求項1~6のいずれか1項に記載の赤外光反射板。
- 前記易接着層が、ポリビニルブチラール樹脂を含有する請求項7に記載の赤外光反射板。
- 前記易接着層が、少なくとも1種の紫外線吸収剤を含有する請求項7又は8に記載の赤外光反射板。
- 2枚のガラス板と、その間に請求項1~9のいずれか1項に記載の赤外光反射板とを有する赤外光反射性合わせガラス。
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Also Published As
Publication number | Publication date |
---|---|
EP2442161A4 (en) | 2012-11-07 |
EP2442161A1 (en) | 2012-04-18 |
JP2010286643A (ja) | 2010-12-24 |
US20120086904A1 (en) | 2012-04-12 |
JP5020289B2 (ja) | 2012-09-05 |
CN102804003A (zh) | 2012-11-28 |
CN102804003B (zh) | 2015-11-25 |
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