WO2014119577A1 - 表示装置及び積層光学フィルム - Google Patents
表示装置及び積層光学フィルム Download PDFInfo
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- WO2014119577A1 WO2014119577A1 PCT/JP2014/051850 JP2014051850W WO2014119577A1 WO 2014119577 A1 WO2014119577 A1 WO 2014119577A1 JP 2014051850 W JP2014051850 W JP 2014051850W WO 2014119577 A1 WO2014119577 A1 WO 2014119577A1
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- Prior art keywords
- piezoelectric layer
- polymer piezoelectric
- polymer
- display device
- layer
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- Y10T428/31565—Next to polyester [polyethylene terephthalate, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31786—Of polyester [e.g., alkyd, etc.]
Definitions
- the present invention relates to a display device and a laminated optical film.
- polymer piezoelectric materials using helical chiral polymers having optical activity have been reported.
- a polymer piezoelectric material is disclosed that exhibits a piezoelectric constant of about 10 pC / N at room temperature by stretching a molded product of polylactic acid (see, for example, Japanese Patent Laid-Open No. Hei 5-152638).
- high piezoelectricity of about 18 pC / N is produced by a special orientation method called forging (see, for example, JP-A-2005-213376). .
- a touch panel using a molecular oriented polylactic acid film and a touch input device using this touch panel are also known (see, for example, International Publication No. 2010/143528 pamphlet).
- a linear polarizer may be used in a display device such as a liquid crystal display device or an organic electroluminescence display device (for example, Japanese Patent Application Laid-Open Nos. 2006-268018, 2009-192611, and 2009-). No. 21408).
- an object of the present invention is to provide a display device in which a decrease in contrast of a display image is suppressed, and to provide a laminated optical film that can suppress a decrease in contrast of a display image when used in a display device. .
- the crystalline polymer piezoelectric layer has a crystallinity of 20% to 80% and a product of the normalized molecular orientation and the crystallinity of 25 to 700.
- ⁇ 3> The display device according to ⁇ 1> or ⁇ 2>, wherein a linear polarizer does not exist between the crystalline polymer piezoelectric layer and the optical compensation layer.
- ⁇ 4> The display device according to any one of ⁇ 1> to ⁇ 3>, further including a liquid crystal cell or an organic electroluminescence element.
- ⁇ 5> comprising a pair of linear polarizers, and a liquid crystal cell, the crystalline polymer piezoelectric layer, and the optical compensation layer disposed between the pair of linear polarizers, ⁇ 1> to ⁇ 4
- the display device according to any one of the above.
- ⁇ 6> A pair of linear polarizers, a liquid crystal cell disposed between the pair of linear polarizers, and the crystalline polymer piezoelectric layer and the optical disposed on the viewer side of the pair of linear polarizers
- a decrease in contrast of the display image when the display image is observed through a polarizer such as sunglasses is suppressed.
- an organic electroluminescence element is provided, and the crystalline polymer piezoelectric layer and the optical compensation layer are disposed between the linear polarizer and the organic electroluminescence element. 4>.
- the organic electroluminescence element is further provided, and the crystalline polymer piezoelectric layer and the optical compensation layer are arranged on the viewing side with respect to the linear polarizer, and any one of ⁇ 1> to ⁇ 4>
- the display device according to Item 1 According to the display device according to ⁇ 8>, in particular, a decrease in contrast of the display image when the display image is observed through a polarizer such as sunglasses is suppressed.
- the stabilizer (B) is contained in an amount of 0.01 to 10 parts by weight per 100 parts by weight of the helical chiral polymer (A). It is a display apparatus as described in above.
- the stabilizer (B) includes a stabilizer (B3) having one functional group in one molecule selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group.
- the 50% or less internal haze to visible light of the crystalline polymer piezoelectric layer, and is the piezoelectric constant d 14 measured by a displacement method at 25 ° C. is 1 Pm/V more, ⁇ 1> to ⁇ 12>.
- a laminated optical system comprising: a crystalline polymer piezoelectric layer containing a helical chiral polymer (A) having an optical activity having a weight average molecular weight of 50,000 to 1,000,000; and an optical compensation layer satisfying the following formula 1. It is a film.
- the crystalline polymer piezoelectric layer has a crystallinity of 20% to 80%, and a product of the normalized molecular orientation and the crystallinity of 25 to 700.
- the stabilizer (B) includes a stabilizer (B3) having one functional group in one molecule selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group. It is a laminated optical film of description. ⁇ 19> 50% or less internal haze to visible light of the crystalline polymer piezoelectric layer, and is the piezoelectric constant d 14 measured by a displacement method at 25 ° C. is 1 Pm/V more, ⁇ 15> - ⁇ 18>.
- the laminated optical film according to any one of 18>.
- helical chiral polymer (A) is a polylactic acid polymer having a main chain containing a repeating unit represented by the following formula (1): The laminated optical film described in 1.
- the present invention it is possible to provide a display device in which a decrease in contrast of a display image is suppressed, and to provide a laminated optical film that can suppress a decrease in contrast of a display image when used in a display device.
- FIG. 1 is an exploded side view conceptually showing a liquid crystal display device which is an example of a display device of a first embodiment. It is a disassembled side view which shows notionally the liquid crystal display device which is an example of the display apparatus of 2nd Embodiment. It is an exploded side view which shows notionally an organic EL display which is an example of a display of a 3rd embodiment. It is an exploded side view which shows notionally an organic EL display which is an example of a display of a 4th embodiment.
- the display device of the present invention includes a crystalline polymer piezoelectric layer containing an optically active helical chiral polymer (A) having a weight average molecular weight of 50,000 to 1,000,000, an optical compensation layer satisfying the following formula 1, and a linear And a polarizer.
- the laminated optical film of the present invention includes the polymer piezoelectric layer and the optical compensation layer.
- the term “polymer piezoelectric layer” simply means a crystalline polymer piezoelectric layer.
- the crystalline polymer piezoelectric layer described above is used as a member of a display device having a linear polarizer, the contrast of a display image may be lowered.
- the reason for the decrease in contrast of the display image is presumed as follows. That is, in the above-described polymer piezoelectric layer, the piezoelectric performance tends to improve as the product of Xc and MORc increases (for example, as the molecular orientation of the helical chiral polymer (A) increases).
- the polymer piezoelectric layer has a relatively dense structure with a portion having relatively high crystallinity and a portion having a low crystallinity, and the influence on the refractive index of light passing through the polymer piezoelectric layer tends to increase. .
- the above-described polymer piezoelectric layer is used as a member of a display device including a linear polarizer, light leakage may occur from the linear polarizer due to the crystal structure of the polymer piezoelectric layer. Yes, this light leakage is thought to cause a decrease in contrast of the display image.
- the present inventor has found that a reduction in contrast of a display image is suppressed by combining the above crystalline polymer piezoelectric layer and the optical compensation layer satisfying the above formula 1, and thus completed the present invention. It was.
- the display device of the present invention there is no particular limitation on the arrangement of the polymer piezoelectric layer (that is, the crystalline polymer piezoelectric layer; the same shall apply hereinafter), the optical compensation layer, and the linear polarizer.
- the polymer piezoelectric layer and the optical compensation layer are present on the side opposite to the viewing side of the linear polarizer (the side opposite to the viewing side; the same shall apply hereinafter) (that is, the linear polarizer).
- the embodiment in which is the viewer side; for example, a first embodiment and a third embodiment to be described later a decrease in contrast of the display image due to light leakage from the linear polarizer is suppressed.
- the optical compensation layer is removed from the display device of this mode, light that should be blocked by the linear polarizer leaks, and the contrast of the display image is lowered.
- sunglasses are used in the display device of the present invention.
- the optical compensation layer is removed from the display device of this embodiment, when the display image is observed through a polarizer such as sunglasses, the polarization state of the light that has passed through the linear polarizer of the display device is a polymer piezoelectric layer. The contrast of the displayed image is lowered.
- ” on the left side is an absolute value of “0.06 ⁇ Xc ⁇ MORc ⁇ d + Rth” and is 500 or less as shown in equation 1.
- the left side is preferably 400 or less, more preferably 300 or less, and particularly preferably 250 or less. Note that the fact that the left side is 250 or less means that the following Expression 2 is satisfied.
- the configuration of a known display device can be appropriately selected.
- the polymer piezoelectric layer is added to a known display device, if there is a member satisfying the above formula 1 among the constituent members of the display device, the member can be used as an optical compensation layer. (In other words, it is not necessary to provide an optical compensation layer separately from this member).
- the display device of the present invention preferably further includes a display unit (image display unit) in addition to the polymer piezoelectric layer, the optical compensation layer, and the linear polarizer.
- a display unit image display unit
- Examples of the display unit include a liquid crystal cell and an organic electroluminescence (hereinafter also referred to as “organic EL”) element.
- the arrangement of the polymer piezoelectric layer, the optical compensation layer, and the linear polarizer is not particularly limited, but there is no linear polarizer between the polymer piezoelectric layer and the optical compensation layer. It is preferable. Thereby, the phenomenon in which the light before compensation is incident on the linear polarizer is suppressed, and as a result, the contrast reduction of the display image can be further suppressed.
- the absorption axis of the linear polarizer and the crystal axis of the polymer piezoelectric layer are substantially parallel or substantially perpendicular from the viewpoint of further suppressing a decrease in contrast of the display image.
- substantially parallel means that when an angle formed by two axes is expressed in a range of 0 ° to 90 °, this angle is 0 ° to 3 ° (preferably 0 ° to 1 °). Refers to that.
- the term “substantially perpendicular” means that when the angle between the two axes is expressed in the range of 0 ° to 90 °, this angle is 87 ° to 90 ° (preferably 89 ° to 90 °).
- the crystal axis of the polymer piezoelectric layer refers to an axis parallel to the main orientation direction of the molecular chain of the helical chiral polymer (A).
- the main orientation direction of the molecular chain of the helical chiral polymer (A) is specifically the direction in which the highest anisotropy appears when the normalized molecular orientation MORc is measured.
- the direction of the crystal axis of the polymer piezoelectric layer is substantially equal to the main stretching direction in this stretching.
- the crystal axis of the polymer piezoelectric layer is substantially equal to the direction of this uniaxial stretching.
- the display device includes a pair of linear polarizers, and a liquid crystal cell, the polymer piezoelectric layer, and the optical compensation layer disposed between the pair of linear polarizers.
- a display device that is, a liquid crystal display device.
- the polymer piezoelectric layer and the optical compensation layer are disposed inside a liquid crystal panel including a pair of linear polarizers and a liquid crystal cell disposed between the pair of linear polarizers. It is a form.
- FIG. 1 is an exploded side view conceptually showing a liquid crystal display device 100 as an example of the display device of the first embodiment.
- the liquid crystal display device 100 includes a polarizing plate 14A that is a linear polarizer, an optical compensation layer 20 that is an example of an optical compensation layer in the present invention, and a polymer piezoelectric layer in the present invention.
- a liquid crystal panel 30 in which a polymer piezoelectric layer 18 as an example, a liquid crystal cell 16, and a polarizing plate 14B as a linear polarizer are sequentially arranged.
- the liquid crystal display device 100 includes a light source 12 (for example, a backlight) on the non-viewing side (opposite the viewing side X) when viewed from the liquid crystal panel 30.
- the viewing-side polarizing plate 14A may be referred to as an “upper polarizing plate”
- the anti-viewing side (light source side) polarizing plate 14B may be referred to as a “lower polarizing plate”.
- a known liquid crystal molecule is disposed between a pair of substrates (for example, between a substrate with a thin film transistor (TFT) and a counter substrate such as a color filter substrate or a monochrome filter substrate). It can be configured.
- TFT thin film transistor
- the liquid crystal display mode includes a TN (Twisted Nematic) mode, an STN (Super Twisted Nematic) mode, an IPS (In-Plane Switching) mode, a VA (Vertical Alignment) mode, an OCB (Optically Compensated Bend) mode, and the like. It is done. Details of the polymer piezoelectric layer 18 and the optical compensation layer 20 will be described later.
- the liquid crystal display device 100 includes the optical compensation layer 20, when the display image of the liquid crystal panel 30 is observed from the viewing side X, the display image is considered to be caused by the crystal structure of the polymer piezoelectric layer 18. Contrast reduction is suppressed. That is, when the optical compensation layer 20 is removed from the liquid crystal display device 100, when the display image of the liquid crystal panel 30 is observed from the viewing side X (especially during black display or halftone display), the polarizing plate 14A is originally used. The light to be blocked leaks and the contrast of the display image is lowered.
- liquid crystal display device 100 at least two of the constituent members may be bonded with an adhesive or the like. Moreover, when manufacturing the liquid crystal display device 100, a laminated optical film including the polymer piezoelectric layer 18 and the optical compensation layer 20 may be prepared in advance, and the liquid crystal display device 100 may be manufactured using the prepared laminated optical film. .
- Adhesives for bonding each member include, for example, acrylic resin, urethane resin, cellulose, vinyl acetate resin, ethylene-vinyl acetate resin, epoxy resin, nylon-epoxy, vinyl chloride resin, chloroprene rubber, cyanoacrylate , Silicone, modified silicone, aqueous polymer-isocyanate, styrene-butadiene rubber, nitrile rubber, acetal resin, phenol resin, polyamide resin, polyimide resin, melamine resin, urea resin, bromine resin, starch, polyester Resin, polyolefin resin or the like is used.
- the liquid crystal display device 100 may include a constituent member of a known liquid crystal display device.
- the configuration of the liquid crystal display device 100 is the same as that of a known liquid crystal display device.
- the positions of the optical compensation layer 20 and the polymer piezoelectric layer 18 are arranged between the polarizing plate 14 ⁇ / b> A on the viewing side X and the liquid crystal cell 16, and the polarizing plate 14 ⁇ / b> B on the liquid crystal cell 16 and light source 12 side.
- the example which changed during is given.
- an example in which the arrangement of the optical compensation layer 20 and the polymer piezoelectric layer 18 is exchanged is also given.
- liquid crystal display device 100 an example in which the light source 12 is omitted and a reflective electrode is provided in the liquid crystal cell 16 (and the polarizing plate 14B is also omitted in some cases) is a reflective liquid crystal display device. Can be mentioned. These modifications can be combined as appropriate.
- the display device includes a pair of linear polarizers, a liquid crystal cell disposed between the pair of linear polarizers, and the polymer disposed on the viewing side of the pair of linear polarizers.
- a display device having a piezoelectric layer and the optical compensation layer that is, a liquid crystal display device.
- the liquid crystal panel including a pair of linear polarizers and a liquid crystal cell arranged between the pair of linear polarizers does not include the polymer piezoelectric layer and the optical compensation layer. These are the forms arranged outside the liquid crystal panel (viewing side).
- FIG. 2 is an exploded side view conceptually showing the liquid crystal display device 110 as an example of the display device of the second embodiment.
- the configuration of the liquid crystal display device 110 is the same as that of the liquid crystal display device 100 (FIG. 1), in which the optical compensation layer 20 and the polymer piezoelectric layer 18 are not included in the liquid crystal panel.
- the liquid crystal display device 100 is the same as the above-described liquid crystal display device 100 except that the liquid crystal display device 100 is disposed in the same manner (preferred embodiments and modified examples are also the same).
- the liquid crystal display device 110 when the display image of the liquid crystal panel 40 is observed from the viewing side X through a polarizer such as sunglasses, a decrease in contrast of the display image is suppressed. That is, when the optical compensation layer 20 is removed from the liquid crystal display device 110, when the display image of the liquid crystal panel 40 is observed from the viewing side X through a polarizer such as sunglasses (particularly during black display or halftone display). The polarization state of the light that has passed through the linear polarizer of the display device is changed by the polymer piezoelectric layer 18, and the contrast of the display image is lowered.
- the principle of the contrast reduction suppression by the liquid crystal display device 110 is the same as the principle of the contrast reduction suppression by the liquid crystal display device 100 described above. That is, the polarizing plate 14 ⁇ / b> A in the liquid crystal display device 100 corresponds to a polarizer such as sunglasses in the liquid crystal display device 110.
- a display device includes an organic EL element, and the polymer piezoelectric layer and the optical compensation layer are arranged between the linear polarizer and the organic EL element ( That is, an organic EL display device).
- an organic EL display device According to the display device according to the third embodiment, a decrease in contrast of the display image due to the crystal structure of the polymer piezoelectric layer is suppressed by the same principle as that of the display device according to the first embodiment.
- the configuration other than the above configuration is a configuration of a known organic EL display device (for example, an organic EL display device described in JP2009-21408A). Can be referred to as appropriate.
- FIG. 3 is an exploded side view conceptually showing the organic EL display device 120 as an example of the display device of the third embodiment.
- the organic EL display device 120 includes a polarizing plate 54 that is a linear polarizer, a quarter-wave plate 55, an optical compensation layer 20 that is an example of an optical compensation layer in the present invention, and a polymer piezoelectric film in the present invention.
- the polymer piezoelectric layer 18, which is an example of the layer, the upper ITO transparent electrode 52, the organic EL element layer 56, and the metal reflective electrode 58 are arranged.
- the laminated body of the polarizing plate 54 and the quarter wavelength plate 55 functions as a circularly polarizing plate, and suppresses external light reflection.
- a decrease in contrast of the display image due to the crystal structure of the polymer piezoelectric layer 18 is suppressed by providing the optical compensation layer 20.
- a display device includes an organic EL element, and the display device (that is, organic EL) in which the polymer piezoelectric layer and the optical compensation layer are arranged on the viewing side with respect to the linear polarizer.
- Display device the display device (organic EL display device) according to the fourth embodiment, when a display image is observed from a viewing side through a polarizer such as sunglasses, based on the same principle as that of the display device according to the second embodiment. A decrease in contrast of the display image due to the crystal structure of the molecular piezoelectric layer is suppressed.
- the configuration other than the above configuration is a configuration of a known organic EL display device (for example, an organic EL display device described in JP2009-21408A). Can be referred to as appropriate.
- FIG. 4 is an exploded side view conceptually showing the organic EL display device 130 which is an example of the display device of the fourth embodiment.
- the configuration of the organic EL display device 130 is such that the positions of the optical compensation layer 20 and the polymer piezoelectric layer 18 are more visible than the polarizing plate 54 in the organic EL display device 120 (FIG. 3).
- the organic EL display device 120 is the same as the above-described organic EL display device 120 except that the organic EL display device 120 is arranged in the above.
- the laminated body of the polarizing plate 54 and the quarter wavelength plate 55 functions as a circularly polarizing plate, and suppresses external light reflection.
- the contrast of the display image due to the crystal structure of the polymer piezoelectric layer 18 is reduced in the optical compensation layer 20. It is suppressed by providing.
- electrodes having optical transparency may be provided on both surfaces (main surfaces on both sides) of the polymer piezoelectric layer. That is, the configuration of each display device may be a configuration including a piezoelectric device (for example, a touch panel) in which electrodes having light permeability are provided on both surfaces of the polymer piezoelectric layer.
- the “main surface” refers to the surface having the largest area among the surfaces of the polymer piezoelectric layer.
- an electrode having optical transparency is preferable. For example, ITO, ZnO, IZO (registered trademark), a conductive polymer, or the like is used.
- the electrode is preferably an electrode having an internal haze of 50% or less (total light transmittance of 50% or more).
- an electrode exists between the polymer piezoelectric layer and the optical compensation layer. Contrast reduction is suppressed by providing the optical compensation layer.
- the electrode provided in the said piezoelectric device for example, touch panel
- it is formed in the 1st main surface and 2nd main surface of the polylactic acid film described in the international publication 2010/143528 pamphlet, for example.
- the structure of the electrode can be referred to as appropriate.
- a laminated piezoelectric device in which a polymer piezoelectric layer and electrodes are repeatedly stacked may be used instead of the polymer piezoelectric layer.
- at least one of the plurality of polymer piezoelectric layers is the polymer piezoelectric layer in the present invention. Even in this form, the contrast reduction of the display image is suppressed by providing the optical compensation layer.
- An example of such a laminated piezoelectric device is one in which units of electrodes and polymer piezoelectric layers are repeatedly stacked, and finally the main surface of the polymer piezoelectric layer not covered with electrodes is covered with electrodes.
- the unit having two repetitions is a laminated piezoelectric element in which an electrode, a polymer piezoelectric layer, an electrode, a polymer piezoelectric layer, and an electrode are stacked in this order.
- the polymer piezoelectric layers used in the laminated piezoelectric element one of the polymer piezoelectric layers may be the polymer piezoelectric layer of the present invention, and the other layers may not be the polymer piezoelectric layer of the present invention.
- the multilayer piezoelectric device includes a plurality of polymer piezoelectric layers according to the present invention
- the optical activity of the optically active polymer included in the polymer piezoelectric layer according to the present invention is L
- the optically active polymer contained in the polymer piezoelectric layer may be L-form or D-form.
- the arrangement of the polymer piezoelectric layer can be appropriately adjusted according to the use of the piezoelectric element. For example, a first layer of a polymer piezoelectric layer containing an L-type optically active polymer as a main component is laminated with a second polymer piezoelectric layer containing an L-type optically active polymer as a main component via an electrode.
- the uniaxial stretching direction (main stretching direction) of the first polymer piezoelectric layer intersects, preferably orthogonally intersects with the uniaxial stretching direction (main stretching direction) of the second polymer piezoelectric layer. This is preferable because the direction of displacement between the polymer piezoelectric layer and the second polymer piezoelectric layer can be made uniform, and the piezoelectricity of the entire laminated piezoelectric element is enhanced.
- the first layer of the polymer piezoelectric layer containing the L-type optically active polymer as the main component is laminated with the second polymer piezoelectric layer containing the D-type optically active polymer as the main component via the electrode.
- the first polymer piezoelectric layer is arranged so that the uniaxial stretching direction (main stretching direction) of the first polymer piezoelectric layer is substantially parallel to the uniaxial stretching direction (main stretching direction) of the second polymer piezoelectric layer, the first This is preferable because the directions of displacement of the polymer piezoelectric layer and the second polymer piezoelectric layer can be made uniform, and the piezoelectricity of the entire laminated piezoelectric element is enhanced.
- the “optically active polymer” refers to a helical chiral polymer (A) having an optical activity having a weight average molecular weight of 50,000 to 1,000,000 (the same applies hereinafter).
- the form of the display device of the present invention may be a form in which the first embodiment and the second embodiment are combined, or a form in which the third embodiment and the fourth embodiment are combined. It may be.
- the polymer piezoelectric layer for example, the polymer piezoelectric layer 18
- the optical compensation layer for example, the optical compensation layer 20
- the linear polarizer for example, the polarizing plates 14A, 14B, 54
- the display device and the laminated optical film of the present invention have a polymer piezoelectric layer containing a helical chiral polymer (A) having an optical activity having a weight average molecular weight of 50,000 to 1,000,000 (for example, the aforementioned polymer piezoelectric layer 18). At least one layer.
- Polymeric piezoelectric layer of the structure is excellent in piezoelectric properties (i.e., greater piezoelectric constant d 14 is), excellent transparency.
- the piezoelectric constant is one of the tensors of the piezoelectric constant, and is a constant obtained from the degree of polarization generated in the direction of the shear stress when a shear stress is applied in the direction of the stretching axis of the stretched material.
- the piezoelectric constant is as described in paragraphs 0013 to 0014 of Japanese Patent No. 4934235.
- Polymeric piezoelectric layer in the present invention are preferably piezoelectric constant d 14 measured by a displacement method at 25 ° C. is 1 Pm/V more.
- Polymeric piezoelectric layer in the present invention more preferably, not more than 50% internal haze to visible light, and the piezoelectric constant d 14 measured by a displacement method at 25 ° C. is 1 Pm/V more.
- the “piezoelectric constant (displacement method)] means 10 Hz, 300 Vpp between a pair of conductive layers of a piezoelectric constant measurement sample in which a conductive layer is formed on both surfaces of a 32 mm ⁇ 5 mm polymer piezoelectric layer.
- a sine wave AC voltage is applied, and the difference distance between the maximum and minimum displacements at this time is measured as a displacement (mp-p), and the measured displacement (mp-p) is measured at a reference length of 30 mm.
- a value obtained by dividing the value obtained by dividing the value obtained by dividing the value obtained by dividing the value by the electric field strength ((applied voltage (V)) / (film thickness)) applied to the film by 2 is indicated.
- This “piezoelectric constant d 14 measured by the displacement method” can be measured by the method described in paragraphs 0058 to 0059 of Japanese Patent No. 4934235, for example.
- the upper limit of the piezoelectric constant is not particularly limited, but from the viewpoint of balance such as transparency described later, the piezoelectric material using the helical chiral polymer is preferably 50 pm / V or less, and more preferably 30 pm / V or less. From the viewpoint of the balance with similarly transparency is preferably a piezoelectric constant d 14 measured by a resonance method is not more than 15pC / N.
- the optically active polymer is oriented.
- an index representing this orientation there is a “molecular orientation degree MOR”.
- the molecular orientation MOR Molecular Orientation Ratio
- the microwave measurement method That is, the sample surface (film surface) is placed in the microwave resonance waveguide of a known microwave molecular orientation degree measuring apparatus (also referred to as a microwave transmission type molecular orientation meter) in the microwave traveling direction. ) To be vertical.
- the sample is rotated by 0 to 360 ° in a plane perpendicular to the traveling direction of the microwave, and the microwave transmitted through the sample is transmitted.
- the degree of molecular orientation MOR is determined by measuring the strength.
- the normalized molecular orientation MORc can be measured with a known molecular orientation meter, for example, a microwave molecular orientation meter MOA-2012A or MOA-6000 manufactured by Oji Scientific Instruments Co., Ltd. at a resonance frequency near 4 GHz or 12 GHz.
- the normalized molecular orientation MORc can be controlled by crystallization conditions (for example, heating temperature and heating time) and stretching conditions (for example, stretching temperature and stretching speed) when the polymer piezoelectric layer is manufactured.
- the normalized molecular orientation MORc has a correlation with the birefringence ⁇ n obtained by dividing the retardation (retardation) by the thickness of the polymer piezoelectric layer. Specifically, retardation can be measured using RETS100 manufactured by Otsuka Electronics Co., Ltd. MORc and ⁇ n are approximately in a linear proportional relationship, and when ⁇ n is 0, MORc is 1.
- the crystallinity (Xc) of the polymer piezoelectric layer is determined by DSC (Differential scanning calorimetry) method, and the crystallinity of the polymer piezoelectric layer in the present invention is preferably 20% to 80%, More preferably, it is 30% to 70%.
- the crystallinity is within the above range, the piezoelectricity and transparency of the polymer piezoelectric layer are well balanced, and when the polymer piezoelectric layer is stretched, whitening and breakage are unlikely to occur and it is easy to manufacture.
- the crystallinity is 20% or more, the piezoelectricity tends to be improved.
- the crystallinity is 80% or less, the transparency tends to increase.
- the crystallinity of the polymer piezoelectric layer can be adjusted in the range of 20% to 80% by adjusting the crystallization and stretching conditions when the polymer piezoelectric layer is manufactured.
- the transparency of the polymer piezoelectric layer can be evaluated by, for example, visual observation or haze measurement.
- the polymer piezoelectric layer preferably has an internal haze with respect to visible light of 50% or less.
- the internal haze is applied to a polymer piezoelectric layer having a thickness of 0.03 mm to 0.07 mm in accordance with JIS-K7105 using a haze measuring machine [TC Density Co., Ltd., TC-HIII DPK]. It is a value when it is used and measured at 25 ° C., and details of the measuring method will be described in detail in Examples.
- the internal haze of the polymer piezoelectric layer is more preferably 20% or less, further preferably 5% or less, further preferably 3.0% or less, further preferably 2.0% or less, and particularly preferably 1.0% or less. . Further, the lower the internal haze of the polymer piezoelectric layer, the better. However, from the viewpoint of balance with the piezoelectric constant and the like, it is preferably 0.0% to 50%, preferably 0.01% to 20%. Is more preferable, 0.01% to 5% is more preferable, 0.01% to 3.0% is further preferable, 0.01% to 2.0% is further preferable, and 0.01% to 1%. 0.0% is particularly preferable.
- internal haze refers to the internal haze of the polymer piezoelectric layer in the present invention.
- the internal haze is a haze excluding haze due to the shape of the outer surface of the polymer piezoelectric layer, as will be described later in Examples.
- the polymer piezoelectric layer in the present invention preferably has a normalized molecular orientation MORc of 1.0 to 15.0, more preferably 4.0 to 10.0.
- the product of the crystallinity of the polymer piezoelectric layer and the normalized molecular orientation MORc is preferably 25 to 700. By adjusting to this range, high piezoelectricity and high transparency are maintained.
- the product of the crystallinity of the polymer piezoelectric layer and the normalized molecular orientation MORc is 25 or more, the piezoelectricity tends to increase.
- the product of the crystallinity of the polymer piezoelectric layer and the normalized molecular orientation MORc is 700 or less, the transparency tends to increase.
- the product of the crystallinity and MORc is more preferably 40 to 700, still more preferably 75 to 680, still more preferably 90 to 660, still more preferably 125 to 650, and still more preferably 180 to 350.
- the product of the crystallinity and MORc is in the range of 40 to 700, the balance between piezoelectricity and transparency is better, and the dimensional stability is better.
- the product of the crystallinity of the polymer piezoelectric layer and the normalized molecular orientation MORc can be adjusted by adjusting the crystallization and stretching conditions when the polymer piezoelectric layer is produced. .
- the polymer piezoelectric layer according to the present invention preferably has a crystallinity of 20% to 80% and a product of the crystallinity and the normalized molecular orientation MORc of 25 to 700. Further preferred ranges of crystallinity and MORc are as described above.
- the thickness (d) of the polymer piezoelectric layer is not particularly limited, but can be, for example, 10 ⁇ m to 100 ⁇ m, preferably 20 ⁇ m to 90 ⁇ m, and more preferably 30 ⁇ m to 80 ⁇ m.
- the polymer piezoelectric layer preferably has a low dimensional change rate at a temperature under heating, particularly in an environment in which it is incorporated and used in a piezoelectric device such as a touch panel or equipment. This is because if the dimension of the polymer piezoelectric layer changes under the usage environment of the piezoelectric device or the like, the position of the wiring connected to the piezoelectric device may be moved to cause a malfunction.
- the dimensional stability of the polymer piezoelectric layer is evaluated by the dimensional change rate before and after being treated for 10 minutes at 150 ° C., which is a temperature slightly higher than the usage environment of the piezoelectric device or the like.
- the dimensional change rate is preferably 10% or less, and more preferably 5% or less.
- the polymer piezoelectric layer in the present invention contains at least one helical chiral polymer (A) having optical activity having a weight average molecular weight of 50,000 to 1,000,000.
- the helical chiral polymer having optical activity refers to a polymer having molecular optical activity whose molecular structure is a helical structure.
- the helical chiral polymer (A) having an optical activity having a weight average molecular weight of 50,000 to 1,000,000 is also referred to as “optically active polymer (A)” or simply “optically active polymer”.
- optically active polymer examples include polypeptides, cellulose, cellulose derivatives, polylactic acid polymers, polypropylene oxide, poly ( ⁇ -hydroxybutyric acid), and the like.
- polypeptide examples include poly (glutarate ⁇ -benzyl), poly (glutarate ⁇ -methyl) and the like.
- cellulose derivative examples include cellulose acetate and cyanoethyl cellulose.
- the optically active polymer preferably has an optical purity of 95.00% ee or more, more preferably 99.00% ee or more, from the viewpoint of improving the piezoelectricity of the polymer piezoelectric layer. More preferably, it is% ee or more. Desirably, it is 100.00% ee.
- the optical purity of the optically active polymer is a value calculated by the following formula.
- Optical purity (% ee) 100 ⁇
- Optical purity (% ee) 100 ⁇
- the value obtained by the method using a high performance liquid chromatography is used for the quantity [mass%] of the L form of an optically active polymer and the quantity [mass%] of the D form of an optically active polymer. Details of the specific measurement will be described later.
- a compound having a main chain containing a repeating unit represented by the following formula (1) is preferable from the viewpoint of increasing optical purity and improving piezoelectricity.
- Examples of the compound having a repeating unit represented by the formula (1) as a main chain include polylactic acid polymers. Among them, polylactic acid is preferable, and L-lactic acid homopolymer (PLLA) or D-lactic acid homopolymer (PDLA) is most preferable.
- polylactic acid is preferable, and L-lactic acid homopolymer (PLLA) or D-lactic acid homopolymer (PDLA) is most preferable.
- PLLA L-lactic acid homopolymer
- PDLA D-lactic acid homopolymer
- the polylactic acid polymer refers to “polylactic acid”, “a copolymer of L-lactic acid or D-lactic acid and a copolymerizable polyfunctional compound”, or a mixture of both.
- the above-mentioned “polylactic acid” is a polymer in which lactic acid is polymerized by an ester bond and is connected for a long time, a lactide method via lactide, and a direct polymerization method in which lactic acid is heated in a solvent under reduced pressure and polymerized while removing water. It is known that it can be manufactured by, for example.
- polylactic acid examples include a homopolymer of L-lactic acid, a homopolymer of D-lactic acid, a block copolymer containing at least one polymer of L-lactic acid and D-lactic acid, and L-lactic acid and D-lactic acid.
- Examples of the “copolymerizable polyfunctional compound” include glycolic acid, dimethyl glycolic acid, 3-hydroxybutyric acid, 4-hydroxybutyric acid, 2-hydroxypropanoic acid, 3-hydroxypropanoic acid, 2-hydroxyvaleric acid, 3 -Hydroxyvaleric acid, 4-hydroxyvaleric acid, 5-hydroxyvaleric acid, 2-hydroxycaproic acid, 3-hydroxycaproic acid, 4-hydroxycaproic acid, 5-hydroxycaproic acid, 6-hydroxycaproic acid, 6-hydroxy Hydroxycarboxylic acids such as methylcaproic acid and mandelic acid, glycolides, cyclic esters such as ⁇ -methyl- ⁇ -valerolactone, ⁇ -valerolactone and ⁇ -caprolactone, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid , Pimelic acid, azelaic acid, sebacic acid, undecanedioic acid, Polyvalent carboxylic acids such as decaned
- the “copolymer of L-lactic acid or D-lactic acid and a copolymerizable polyfunctional compound” includes a block copolymer or a graft copolymer having a polylactic acid sequence capable of forming a helical crystal.
- the concentration of the structure derived from the copolymer component in the optically active polymer is preferably 20 mol% or less.
- the optically active polymer is a polylactic acid polymer
- the copolymer component is preferably 20 mol% or less based on the total.
- the optically active polymer (for example, polylactic acid polymer) is obtained by, for example, a method of directly dehydrating and condensing lactic acid described in JP-A-59-096123 and JP-A-7-033861. US Pat. Nos. 2,668,182 and 4,057,357 can be used for the production by ring-opening polymerization using lactide, which is a cyclic dimer of lactic acid. Furthermore, the optically active polymer (for example, polylactic acid-based polymer) obtained by each of the above production methods has, for example, a case where polylactic acid is produced by the lactide method so that the optical purity is 95.00% ee or more. It is preferable to polymerize lactide having an optical purity of 95.00% ee or higher by crystallization operation.
- the optically active polymer in the present invention has a weight average molecular weight (Mw) of 50,000 to 1,000,000. If the lower limit of the weight average molecular weight of the optically active polymer is less than 50,000, the mechanical strength when the optically active polymer is molded is insufficient.
- the lower limit of the weight average molecular weight of the optically active polymer is preferably 100,000 or more, and more preferably 150,000 or more.
- the upper limit of the weight average molecular weight of the optically active polymer exceeds 1,000,000, it becomes difficult to mold the optically active polymer (for example, to form a film shape by extrusion molding or the like).
- the upper limit of the weight average molecular weight is preferably 800,000 or less, and more preferably 300,000 or less.
- the molecular weight distribution (Mw / Mn) of the optically active polymer is preferably 1.1 to 5, more preferably 1.2 to 4, from the viewpoint of the strength of the polymer piezoelectric layer. Further, it is preferably 1.4 to 3.
- the weight average molecular weight Mw and molecular weight distribution (Mw / Mn) of the polylactic acid polymer are measured by gel permeation chromatography (GPC) by the following GPC measurement method.
- -GPC measuring device Waters GPC-100 -column- Made by Showa Denko KK, Shodex LF-804 -Sample preparation-
- a polylactic acid polymer is dissolved in a solvent (for example, chloroform) at 40 ° C. to prepare a sample solution having a concentration of 1 mg / mL.
- a solvent for example, chloroform
- -Measurement condition 0.1 mL of the sample solution is introduced into the column at a solvent [chloroform], a temperature of 40 ° C., and a flow rate of 1 mL / min.
- polylactic acid polymer commercially available polylactic acid may be used.
- examples of commercially available polylactic acid include PURASORB (PD, PL) manufactured by PURAC, LACEA (H-100, H-400) manufactured by Mitsui Chemicals, Ingeo 4032D, 4043D manufactured by NatureWorks, and the like.
- the optically active polymer is produced by the lactide method or the direct polymerization method in order to increase the weight average molecular weight (Mw) of the polylactic acid polymer to 50,000 or more. It is preferable to do.
- the polymer piezoelectric layer in the present invention may contain only one kind of the optically active polymer described above, or may contain two or more kinds.
- the content of the optically active polymer (the total content in the case of two or more types; the same shall apply hereinafter) is not particularly limited, but relative to the total mass of the polymer piezoelectric layer. It is preferably 80% by mass or more. When the content is 80% by mass or more, the piezoelectric constant tends to be larger.
- the polymeric piezoelectric layer in the present invention comprises at least one stabilizer (B) having a weight average molecular weight of 200 to 60,000 having at least one functional group selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group. It is preferable to include. Thereby, the hydrolyzability of the optically active polymer is further suppressed, and the wet heat resistance of the polymer piezoelectric layer is further improved.
- a method for reducing unreacted monomers and impurities, low molecular weight compounds such as chain and cyclic oligomers in a polymer such as polyester for example, JP-A-9-12688
- a method of adding an aromatic carbodiimide for example, JP-T-2001-525473
- a method of adding an oxazoline compound for example, JP-A-2007-77193
- a method of improving the reliability of a polymer piezoelectric layer containing a helical chiral polymer having optical activity by suppressing the hydrolyzability of the optically active polymer without significantly impairing its piezoelectric properties and transparency was not known.
- the inventors have added a specific amount of a stabilizer (B) having a specific functional group to a helical chiral polymer having optical characteristics without greatly reducing piezoelectricity and transparency.
- the present inventors have found that the hydrolyzability of aliphatic polyester can be suppressed, and the heat and moisture resistance and reliability of the polymer piezoelectric layer can be improved.
- the effect of adding a specific amount of the stabilizer (B) is not clear, but is considered as follows.
- the hydrolysis of the optically active polymer is presumed to proceed according to the following scheme. Therefore, in order to suppress hydrolysis, a method of suppressing contact with moisture by a laminate or the like, or forming a crosslinked structure in a hydrolyzed portion in the system, or blocking a free carboxy group is considered. It is done. Therefore, a stabilizer having a functional group that easily forms an interaction with both functional groups of a hydroxyl group and a carboxy group, more preferably a stabilizer having a functional group that easily forms an interaction with a plurality of hydroxyl groups and carboxy groups. It is considered that the hydrolysis can be suppressed by using.
- the optically active polymer is crystallized.
- the part where the stabilizer is likely to be crystallized specifically, the region where the molecular chain is not broken
- the part where the stabilizer is difficult to be crystallized the region where the molecular chain is partially broken and a hydroxyl group or a carboxy group is generated
- the stabilizer is present in a portion having a low crystallinity, which has lower heat and heat resistance than a portion having high crystallinity, and is present uniformly without inhibiting the crystallization of the portion that tends to be crystallized. It is considered that the moisture and heat resistance can be improved efficiently.
- a compound having an oxazoline group known as a stabilizer for optically active polymers is used, the oxazoline group reacts with a carboxy group, but hardly reacts with a hydroxyl group.
- oxazoline is also present in the portion that is likely to be crystallized, making it difficult to crystallize, and depending on the structure of the compound used, it becomes a nucleus of crystal growth and is locally large. Crystals can be formed. Therefore, there is a concern that the transparency of the polymer piezoelectric layer is lowered. Further, since oxazoline hardly moves to a portion having lower crystallinity, it is considered that it is difficult to sufficiently obtain a moist heat resistance improving effect.
- the specific functional group capable of interacting with both the hydroxyl group and the carboxy group is selected from the group consisting of a carbodiimide group, an isocyanate group, and an epoxy group having the following structure:
- the functional group include at least one functional group. Among them, a carbodiimide group is preferable from the viewpoint of effects.
- the weight average molecular weight of the stabilizer (B) is preferably 200 to 60000, more preferably 200 to 30000, and still more preferably 300 to 18000. If the molecular weight is within the above range, it is presumed that the stabilizer (B) can be easily transferred as described above, and the effect of improving the heat and moisture resistance can be sufficiently obtained.
- the carbodiimide compound having a carbodiimide group used as the stabilizer (B) has one or more carbodiimide groups in the molecule.
- the carbodiimide compound including the polycarbodiimide compound
- those synthesized by a generally well-known method can be used.
- an organophosphorus compound or organometallic compound is used as a catalyst, and various isocyanates can be synthesized by subjecting them to a decarboxylation condensation reaction in a solvent-free or inert solvent at a temperature of about 70 ° C. or higher. Can be mentioned.
- Examples of the monocarbodiimide compound contained in the carbodiimide compound include dicyclohexylcarbodiimide, dimethylcarbodiimide, diisobutylcarbodiimide, dioctylcarbodiimide, t-butylisopropylcarbodiimide, diphenylcarbodiimide, di-t-butylcarbodiimide, di- ⁇ -naphthylcarbodiimide and the like.
- dicyclohexylcarbodiimide or bis-2,6-diisopropylphenylcarbodiimide is preferable from the viewpoint of easy industrial availability.
- polycarbodiimide compound contained in the carbodiimide compound those produced by various methods can be used.
- Conventional methods for producing polycarbodiimides see, for example, US Pat. No. 2,941,956, Japanese Patent Publication No. 47-33279, J.0rg.Chem.28, 2069-2075 (1963), Chemical Review 1981, Vol. 4, p619-621) can be used.
- a carbodiimide compound described in Japanese Patent No. 4084953 can also be used.
- polycarbodiimide compound examples include poly (4,4′-dicyclohexylmethanecarbodiimide), poly (tetramethylxylylenecarbodiimide), poly (N, N-dimethylphenylcarbodiimide), and poly (N, N′-di-2,6).
- -Diisopropylphenylcarbodiimide and the like, and any carbodiimide compound having one or more carbodiimide groups in the molecule having such a function is not particularly limited.
- the carbodiimide compound a commercially available product may be used.
- B2756 (trade name) manufactured by Tokyo Chemical Industry Co., Ltd., Carbodilite LA-1, manufactured by Nisshinbo Chemical Co., Ltd., Stabaxol P, Stabaxol P400, and Stabaxol I Product name).
- Examples of the compound having an isocyanate group (isocyanate compound) used as the stabilizer (B) include hexyl isocyanate, cyclohexyl isocyanate, benzyl isocyanate, phenethyl isocyanate, butyl isocyanatoacetate, dodecyl isocyanate, octadecyl isocyanate, and isocyanate 3- ( Triethoxysilyl) propyl, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, m-phenylene diisocyanate, p-phenylene diisocyanate, 4,4'-diphenylmethane diisocyanate, 2,4'-diphenylmethane diisocyanate, 2, 2'-diphenylmethane diisocyanate, 3,3'-dimethyl-4,4'-biphenylene diisocyanate, 3,3
- Examples of the compound having an epoxy group (epoxy compound) used as the stabilizer (B) include N-glycidylphthalimide, orthophenylphenyl glycidyl ether, phenyl glycidyl ether, pt-butylphenyl glycidyl ether, hydroquinone diglycidyl.
- Ether resorcin diglycidyl ether, 1,6-hexanediol diglycidyl ether, diethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, trimethylolpropane triglycidyl ether, bisphenol A-diglycidyl ether, hydrogenated bisphenol A-diglycidyl ether , Phenol novolac type epoxy resin, cresol novolac type epoxy resin, epoxidized polybutadiene, etc.
- a preferred embodiment of the stabilizer (B) is a stabilizer having one or more functional groups selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group, and having a number average molecular weight of 200 to 900.
- the weight average molecular weight of the stabilizer (B1) having a number average molecular weight of 200 to 900 is about 200 to 900, and the number average molecular weight and the weight average molecular weight of the stabilizer (B1) are almost the same value. .
- the stabilizer (B1) specifically, dicyclohexylcarbodiimide, bis-2,6-diisopropylphenylcarbodiimide, hexyl isocyanate, octadecyl isocyanate, 3- (triethoxysilyl) propyl isocyanate, N-glycidyl
- examples thereof include phthalimide, orthophenylphenyl glycidyl ether, phenyl glycidyl ether, pt-butylphenyl glycidyl ether, and the like.
- the stabilizer (B2) include poly (4,4′-dicyclohexylmethanecarbodiimide), poly (tetramethylxylylene carbodiimide), poly (N, N-dimethylphenylcarbodiimide), poly ( N, N'-di-2,6-diisopropylphenylcarbodiimide), diphenylmethane diisocyanate polyisocyanate, 1,6-hexamethylene diisocyanate polyisocyanate, xylylene diisocyanate polyisocyanate, isophorone diisocyanate polyisocyanate, phenol novolac epoxy Examples thereof include resins, cresol novolac type epoxy resins, and epoxidized polybutadiene.
- the moisture and heat resistance is particularly improved by including a stabilizer (B1) having a relatively low molecular weight and a stabilizer (B2) having a multifunctional and relatively high molecular weight.
- a stabilizer (B1) having a relatively low molecular weight and a stabilizer (B2) having a multifunctional and relatively high molecular weight.
- the stabilizer (B2) is preferably in the range of 10 parts by weight to 150 parts by weight from the viewpoint of achieving both transparency and wet heat resistance, and more preferably in the range of 50 parts by weight to 100 parts by weight. .
- the stabilizer (B) includes a stabilizer (B3) having one functional group in one molecule selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group, and improves dimensional stability. From this point of view, this is a preferred embodiment. Since the stabilizer (B3) has only one functional group selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group in one molecule, it has an optical activity having a hydroxyl group or a carboxyl group generated by hydrolysis. The part of the polymer (A) is not easily cross-linked with the stabilizer (B3) interposed therebetween.
- the weight average molecular weight of the compound having one functional group selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group in one molecule is preferably 200 to 2000, more preferably 200 to 1500, and more preferably 300 to 900. Further preferred.
- the compound having one functional group selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group in one molecule include dicyclohexylcarbodiimide, bis-2,6-diisopropylphenylcarbodiimide, hexyl isocyanate, and octadecyl isocyanate.
- 3- (triethoxysilyl) propyl isocyanate N-glycidylphthalimide, orthophenylphenyl glycidyl ether, phenyl glycidyl ether, and pt-butylphenyl glycidyl ether.
- dicyclohexylcarbodiimide and bis-2,6-diisopropylphenylcarbodiimide are preferable, and bis-2,6-diisopropylphenylcarbodiimide is more preferable.
- the stabilizer (B3) and the stabilizer (B4) having two or more functional groups selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group in one molecule for example, the aforementioned stabilizer (B2 ) May be used in combination.
- the stabilizer (B4) having two or more functional groups selected from the group consisting of a carbodiimide group, an epoxy group, and an isocyanate group in one molecule with respect to 100 parts by weight of the stabilizer (B3)
- the range of 200 parts by weight is preferable from the viewpoint of the balance of transparency, heat-and-moisture resistance, and dimensional stability, and the range of 10 to 100 parts by weight is more preferable.
- the number average molecular weight (Mn) and the weight average molecular weight (Mw) of the stabilizer (B) are both measured using a gel permeation chromatograph (GPC) described in the section of the optically active polymer (A). It is measured similarly by the method. In addition to GPC, it can be measured by a measuring method such as GC-MS, FAB-MS, ESI-MS, or TOF-MS.
- GPC gel permeation chromatograph
- the amount of the stabilizer (B) added is preferably 0.01 to 10 parts by weight with respect to 100 parts by weight of the optically active polymer (A). Further, in order to obtain higher reliability (specifically, reliability in a reliability test of 500 hours described later), the addition amount is more preferably 0.7 parts by weight or more. In particular, when aliphatic carbodiimide is used as a stabilizer, it is more preferably contained in an amount of 0.01 to 2.8 parts by weight from the viewpoint of transparency. When the addition amount is in the above range, the reliability of the piezoelectric material can be improved without significantly impairing the noise inside the polymer piezoelectric layer in the present invention.
- the said addition amount shows those total amounts, when using 2 or more types of stabilizers (B) together.
- the amount of the stabilizer (B) added is 100 parts by weight of the aliphatic polyester (A) having optical activity. 0.01 to 1.2 parts by weight is preferable, 0.01 to 0.7 parts by weight is further preferable, and 0.01 to 0.6 parts by weight is even more preferable.
- the polymer piezoelectric layer in the present invention is a known resin represented by other components (for example, polyvinylidene fluoride, polyethylene resin and polystyrene resin) other than the optically active polymer described above, as long as the effects of the present invention are not impaired. And inorganic fillers such as silica, hydroxyapatite and montmorillonite, and known crystal nucleating agents such as phthalocyanine).
- the polymer piezoelectric layer in the present invention is an optically active polymer as described above (that is, a helical having an optical activity having a weight average molecular weight (Mw) of 50,000 to 1,000,000, as long as the effects of the present invention are not impaired.
- Mw weight average molecular weight
- a helical chiral polymer other than (chiral polymer) may be included.
- the polymer piezoelectric layer in the present invention may contain at least one inorganic filler.
- an inorganic filler such as hydroxyapatite may be nano-dispersed in the polymer piezoelectric layer in order to make the polymer piezoelectric layer a transparent film in which voids such as bubbles are suppressed.
- voids such as bubbles are suppressed.
- a large energy is required for crushing the aggregate, and when the inorganic filler is not nano-dispersed, the transparency of the film may be lowered.
- the content of the inorganic filler with respect to the total mass of the polymer piezoelectric layer is preferably less than 1% by mass.
- the content of components other than the optically active polymer is preferably 20% by mass or less based on the total mass of the polymer piezoelectric layer. More preferably, it is 10 mass% or less.
- the polymeric piezoelectric layer in the present invention may contain at least one crystal accelerator (crystal nucleating agent).
- the crystal accelerator (crystal nucleator) is not particularly limited as long as the effect of promoting crystallization is recognized, but is a substance having a crystal structure having a face spacing close to the face spacing of the crystal lattice of the optically active polymer. It is desirable to select. This is because a substance with a close spacing is more effective as a nucleating agent.
- organic materials such as zinc phenylsulfonate, melamine polyphosphate, melamine cyanurate, zinc phenylphosphonate, calcium phenylphosphonate, magnesium phenylphosphonate, inorganic Examples thereof include talc and clay.
- zinc phenylphosphonate is most preferable because the plane spacing is most similar to the plane spacing of polylactic acid and provides a good crystal formation promoting effect.
- the commercially available crystal accelerator can be used. Specific examples include zinc phenylphosphonate; Eco Promote (manufactured by Nissan Chemical Industries, Ltd.) and the like.
- the content of the crystal nucleating agent is preferably 0.01 to 1.0 part by weight, more preferably 0.01 to 0.5 part by weight, with respect to 100 parts by weight of the optically active polymer.
- the amount is particularly preferably 0.02 to 0.2 parts by weight from the viewpoint of maintaining the degree of biomass.
- the content of the crystal nucleating agent is 0.01 parts by weight or more, the effect of promoting crystallization can be obtained more effectively.
- the content of the crystal nucleating agent is less than 1.0 part by weight, the crystallization rate can be more easily controlled.
- the method for producing the polymer piezoelectric layer in the present invention is not particularly limited as long as the crystallinity can be adjusted and the product of the normalized molecular orientation MORc and the crystallinity can be adjusted.
- the crystallinity can be adjusted to 20% to 80%, and the product of the normalized molecular orientation MORc and the crystallinity can be adjusted to 25 to 700.
- a method for producing the polymer piezoelectric layer in the present invention for example, a method of crystallizing and stretching (whichever is first) may be performed on an amorphous sheet containing the optically active polymer described above.
- crystallization is a concept including preliminary crystallization described later and annealing treatment described later.
- the non-crystalline sheet refers to a sheet obtained by heating an optically active polymer alone or a mixture containing an optically active polymer to a temperature equal to or higher than the melting point Tm of the optically active polymer and then rapidly cooling it.
- An example of the rapid cooling temperature is 50 ° C.
- the optically active polymer (polylactic acid polymer or the like) is used alone as a raw material for the polymer piezoelectric layer (or an amorphous sheet). It is also possible to use a mixture of two or more of the optically active polymers described above (polylactic acid polymers, etc.), or at least one of the optically active polymers described above and other components (for example, the aforementioned stabilizer A mixture of at least one of the above) may be used. The above mixture is preferably a mixture obtained by melt kneading.
- optically active polymers to be mixed are mixed with a melt kneader (manufactured by Toyo Seiki Co., Ltd., Laboplast Mixer) under conditions of mixer rotation speed 30 rpm to 70 rpm, 180 ° C. to 250 ° C.
- a melt kneader manufactured by Toyo Seiki Co., Ltd., Laboplast Mixer
- mixer rotation speed 30 rpm to 70 rpm 180 ° C. to 250 ° C.
- the polymer piezoelectric layer in the present invention is, for example, a first step of heating a non-crystalline sheet containing a helical chiral polymer to obtain a pre-crystallized sheet, and stretching the pre-crystallized sheet mainly in a uniaxial direction. And a second step of manufacturing. Specifically, it can be produced by the methods described in Japanese Patent No. 4934235 and International Publication No. 2010/104196 pamphlet.
- the polymeric piezoelectric layer in the present invention comprises a step of stretching a sheet containing an optically active polymer (preferably an amorphous sheet) mainly in a uniaxial direction, and a step of annealing the stretched sheet. It can manufacture also by the manufacturing method included in this order.
- the stretching conditions and annealing conditions are preferably such that the polymer piezoelectric layer to be produced has a crystallinity of 20% to 80%, and the product of the normalized molecular orientation MORc and the crystallinity. Is appropriately adjusted to be 25 to 700.
- the display device and the laminated optical film of the present invention include at least one optical compensation layer (for example, the above-described optical compensation layer 20) that satisfies the above-described formula 1.
- the optical compensation layer is not particularly limited as long as it satisfies the above-described formula 1.
- the member can be an optical compensation layer (that is, it is not necessary to provide an optical compensation layer separately from this member).
- Rth represents the retardation (nm) in the thickness direction of the optical compensation layer at a wavelength of 550 nm.
- the retardation Rth (nm) in the thickness direction of the optical compensation layer at a wavelength of 550 nm is defined by the following formula a.
- the in-plane retardation Re (nm) of the optical compensation layer at a wavelength of 550 nm is defined by the following formula b.
- nx is the refractive index in the slow axis direction in the plane of the optical compensation layer at a wavelength of 550 nm
- ny is the fast axis direction in the plane of the optical compensation layer at a wavelength of 550 nm
- Nz is the refractive index in the thickness direction of the optical compensation layer at a wavelength of 550 nm
- d2 is the thickness (nm) of the optical compensation layer.
- JP 2012-7110 A the description in JP 2012-7110 A can be referred to as appropriate.
- the Rth is preferably ⁇ 3000 nm to ⁇ 100 nm, and more preferably ⁇ 1500 nm to ⁇ 200 nm.
- the Re is not particularly limited, but is preferably 0 nm to 3000 nm, and more preferably 0 nm to 1500 nm.
- the thickness of the optical compensation layer in the present invention is not particularly limited, but can be, for example, 1 ⁇ m to 1000 ⁇ m.
- optical compensation layer in the present invention for example, a stretched film of a polymer film, a solidified layer or a cured layer of a liquid crystal composition can be used.
- the stretched polymer film preferably includes a polymer exhibiting negative intrinsic birefringence.
- the “polymer exhibiting negative intrinsic birefringence” refers to a polymer in which the major axis direction of the refractive index ellipsoid is generated in a direction orthogonal to the orientation direction of the polymer chain when the polymer is oriented.
- the polymer exhibiting negative intrinsic birefringence include a polymer in which a chemical bond having a large polarization anisotropy such as an aromatic ring or a carbonyl group and / or a substituent is introduced into a side chain.
- a methacrylate polymer, a styrene polymer, a maleimide polymer, or the like is preferably used. These can be used alone or in combination of two or more.
- the methacrylate polymer can be obtained, for example, by addition polymerization of a methacrylate monomer.
- the methacrylate monomer include methyl methacrylate, butyl methacrylate, cyclohexyl methacrylate and the like.
- the styrene polymer can be obtained, for example, by addition polymerization of a styrene monomer.
- styrene monomer examples include styrene, ⁇ -methylstyrene, o-methylstyrene, p-methylstyrene, p-chlorostyrene, p-nitrostyrene, p-aminostyrene, p-carboxystyrene, p-phenylstyrene, Examples include 2,5-dichlorostyrene and pt-butylstyrene.
- the maleimide polymer can be obtained, for example, by addition polymerization of a maleimide monomer.
- maleimide monomers include N-ethylmaleimide, N-cyclohexylmaleimide, N-phenylmaleimide, N- (2-methylphenyl) maleimide, N- (2-ethylphenyl) maleimide, N- (2-n- Propylphenyl) maleimide, N- (2-isopropylphenyl) maleimide, N- (2,6-dimethylphenyl) maleimide, N- (2,6-diethylphenyl) maleimide, N- (2,6-di-isopropylphenyl) ) Maleimide, N- (2-methyl-6-ethylphenyl) maleimide, N- (2-chlorophenyl) maleimide, N- (2,6-dibromophenyl) maleimide, N- (2-biphenyl) maleimide
- the polymer exhibiting negative intrinsic birefringence can be copolymerized with other monomers as long as a polymer exhibiting negative birefringence can be obtained.
- other monomers include olefins such as ethylene, propylene, 1-butene, isobutene, 1,3-butadiene, 2-methyl-1-butene, 2-methyl-1-pentene, and 1-hexene; ) Acrylonitrile; (meth) acrylates such as methyl acrylate and methyl methacrylate; maleic anhydride; vinyl esters such as vinyl acetate.
- the blending ratio of the styrene monomer is preferably 50 mol% to 80 mol%.
- the blending ratio of the maleimide monomer is preferably 2 mol% to 50 mol%.
- the polymer exhibiting negative birefringence is preferably a styrene-maleic anhydride copolymer, a styrene- (meth) acrylonitrile copolymer, a styrene- (meth) acrylate copolymer, or a styrene-maleimide copolymer.
- Vinyl ester-maleimide copolymer, olefin-maleimide copolymer, and the like are used. These can be used alone or in combination of two or more.
- These polymers exhibit high negative birefringence and can be excellent in heat resistance.
- These polymers are, for example, NOVA Chemicals Japan Ltd. It can also be obtained from Arakawa Chemical Industries, Ltd.
- the polymers described in paragraphs 0027 to 0028 of JP-A-2009-192611 can also be used.
- the weight average molecular weight (Mw) of the polymer exhibiting negative birefringence is preferably 20,000 to 500,000.
- the glass transition temperature (Tg) of the polymer exhibiting negative birefringence is preferably 110 to 185 ° C. With such a polymer, a polymer film exhibiting excellent thermal stability and excellent stretchability can be obtained.
- the weight average molecular weight (Mw) is a value measured by gel permeation chromatograph method (polystyrene standard) using a tetrahydrofuran solvent.
- the glass transition temperature (Tg) can be determined by a DSC method according to JIS K 7121.
- the optical compensation layer can be obtained by stretching the polymer film under any appropriate stretching condition. Specifically, it can be obtained by stretching the polymer film in the longitudinal direction or the transverse direction.
- the stretching method include a longitudinal uniaxial stretching method and a lateral uniaxial stretching method.
- Any appropriate stretching machine can be used as the stretching machine. Specific examples include a roll stretching machine, a tenter stretching machine, and a biaxial stretching machine.
- the stretching temperature is preferably (Tg-50) ° C to (Tg + 50) ° C, more preferably (Tg-30) ° C to (Tg + 30), where Tg (° C) is the glass transition temperature of the polymer forming the polymer film. ) ° C.
- the stretching temperature is typically 80 to 250 ° C, preferably 90 to 200 ° C, more preferably 100 to 180 ° C.
- the draw ratio is preferably 3.0 times or less, more preferably 1.1 to 3.0 times, and particularly preferably 1.2 to 2.8 times.
- the thickness of the stretched film is preferably 20 to 1000 ⁇ m, more preferably 100 to 700 ⁇ m, and particularly preferably 200 to 500 ⁇ m.
- the stretched polymer film for example, the first optical compensation layer described in JP-A-2009-192611 can be used.
- the optical compensation layer in the present invention may be a solidified layer or a cured layer of a liquid crystalline composition.
- the solidified layer or the cured layer of the liquid crystal composition include retardation films described in paragraphs 0072 to 0078 of JP-A-2006-268018.
- a solidified layer or cured layer of a liquid crystalline composition containing a liquid crystal compound that is homeotropically aligned is also suitable.
- homeotropic alignment means a state in which the liquid crystal compound contained in the liquid crystalline composition is aligned in parallel and uniformly with respect to the film normal direction.
- the solidified layer or cured layer of the liquid crystalline composition is a solidified layer or cured layer of a liquid crystalline composition containing a homeotropically aligned liquid crystal compound, wherein the liquid crystalline composition is a part of the molecular structure.
- a layer containing a low molecular liquid crystal having at least one polymerizable or crosslinkable functional group is particularly preferably, the liquid crystalline composition contains a low molecular liquid crystal having at least two polymerizable or crosslinkable functional groups in a part of the molecular structure.
- the mechanical strength of the solidified layer or the cured layer of the liquid crystalline composition is obtained by polymerizing (or crosslinking) a polymerizable (or crosslinking) functional group by a polymerization (or crosslinking) reaction.
- a solidified layer or a cured layer of a liquid crystal composition excellent in durability and dimensional stability can be obtained.
- Any appropriate functional group can be selected as the polymerizable functional group.
- acryloyl group, methacryloyl group, epoxy group, vinyl ether group and the like can be mentioned.
- an acryloyl group and a methacryloyl group are preferably used in that a retardation film having high reactivity and excellent transparency can be obtained.
- the thickness of this layer is preferably 0.6 ⁇ m to 20 ⁇ m, more preferably It is 0.8 ⁇ m to 10 ⁇ m, and most preferably 0.8 ⁇ m to 2.5 ⁇ m.
- ⁇ n ne ⁇ no is preferably ⁇ 0.20 to ⁇ 0.04, more preferably ⁇ 0.18 to ⁇ 0.05, and most preferably ⁇ 0.14 to -0.07.
- the transmittance of the solidified layer or cured layer of the liquid crystalline composition containing the homeotropically aligned liquid crystal compound measured with light having a wavelength of 550 nm at 23 ° C. is preferably 80% or more, and more preferably 85% or more. Yes, most preferably 90% or more.
- the solidified layer or the cured layer of the liquid crystalline composition containing the homeotropically aligned liquid crystal compound may further contain a polymer liquid crystal represented by the following general formula (I). Thereby, the orientation of a liquid crystal compound improves more.
- l is an integer of 14 to 20, and when the sum of m and n is 100, m is 50 to 70, and n is 30 to 50.
- the content of the polymer liquid crystal is preferably 10 to 40 parts by weight with respect to 100 parts by weight of the total solid content of the solidified layer or cured layer of the liquid crystalline composition containing a liquid crystal compound aligned in a homeotropic molecular arrangement. Parts by weight, more preferably 15 to 30 parts by weight.
- a solidified layer or a cured layer of a liquid crystalline composition containing a homeotropically aligned liquid crystal compound can be obtained, for example, through the following steps 1 to 3. Specifically, (Step 1) a step of subjecting the surface of the base material (also referred to as a support) to vertical alignment treatment; (Step 2) the surface of the base material that has been subjected to the vertical orientation treatment of the liquid crystalline composition A step of applying a solution or dispersion and homeotropically aligning the liquid crystal compound in the liquid crystalline composition; and (step 3) a step of drying and solidifying the liquid crystalline composition.
- the method for forming a retardation film includes (step 4) a step of irradiating with ultraviolet rays to cure the liquid crystalline composition after the steps 1 to 3.
- the substrate is peeled off before the retardation film is put into practical use.
- the solidified layer or the cured layer of the liquid crystalline composition for example, a positive C plate described in JP-A-2006-268018 can be used.
- the display device and the laminated optical film of the present invention include at least one linear polarizer (for example, the polarizing plate 14A described above).
- a linear polarizer for example, it is disclosed by the stretched film of the polymer film which has iodine or a dichroic dye and which has a polyvinyl alcohol resin as a main component; US Patent 5,523,863 An O-type polarizer obtained by aligning a liquid crystalline composition containing a dichroic substance and a liquid crystalline compound in a certain direction; a lyotropic liquid crystal as disclosed in US Pat. No. 6,049,428 And an E-type polarizer oriented in a certain direction.
- a stretched polymer film containing a polyvinyl alcohol resin as a main component and containing iodine or a dichroic dye is preferable.
- the linear polarizer for example, a polarizer described in JP-A-2006-268018 can be used.
- the display device and the laminated optical film of the present invention may include components other than the polymer piezoelectric layer, the optical compensation layer, and the linear polarizer.
- the display device of the present invention can be appropriately configured with a liquid crystal cell or an organic electroluminescence (organic EL) element.
- organic EL organic electroluminescence
- the “MD direction” is the direction in which the film flows (Machine Direction)
- the “TD direction” is the direction (Transverse Direction) perpendicular to the MD direction and parallel to the main surface of the film. .
- ⁇ Preparation of polymer piezoelectric layer (crystalline polymer piezoelectric layer)
- ⁇ ⁇ Preparation of polymer piezoelectric layer A> A polylactic acid polymer (registered trademark LACEA H-400 (weight average molecular weight Mw: 200,000)) manufactured by Mitsui Chemicals, Inc. as a helical chiral polymer (A) is placed in an extruder hopper, 220 ° C. to 230 ° C. It was extruded from a T die while being heated to ° C., and contacted with a cast roll at 55 ° C. for 0.5 minutes to form a 150 ⁇ m-thick pre-crystallization sheet (pre-crystallization step).
- LACEA H-400 weight average molecular weight Mw: 200,000
- the obtained pre-crystallized sheet was stretched by roll-to-roll while being heated to 70 ° C. at a stretching speed of 1650 mm / min, and uniaxially stretched in the MD direction up to 3.5 times (stretching step). Thereafter, the uniaxially stretched film was roll-rolled and brought into contact with a roll heated to 130 ° C. for 60 seconds and annealed (annealing process) to obtain a polymer piezoelectric layer A that was a crystalline polymer piezoelectric layer. .
- the sample solution was cooled to room temperature, neutralized by adding 20 mL of a 1.0 mol / L hydrochloric acid solution, and the Erlenmeyer flask was sealed and mixed well.
- 1.0 mL of the sample solution was divided into a 25 mL volumetric flask, and HPLC sample solution 1 was prepared with 25 mL of mobile phase.
- Measurement conditions 0.1 mL of the sample solution was introduced into the column at a solvent (chloroform), a temperature of 40 ° C. and a flow rate of 1 mL / min, and the sample concentration in the sample solution separated by the column was measured with a differential refractometer.
- the weight average molecular weight (Mw) of the helical chiral polymer (A) (polylactic acid) was calculated based on a universal calibration curve created with a polystyrene standard sample. The measurement results are shown in Table 1 below. In Table 1 below, “LA” represents LACEA H-400.
- the normalized molecular orientation MORc of the polymer piezoelectric layer A was measured by a microwave molecular orientation meter MOA-6000 manufactured by Oji Scientific Instruments.
- the reference thickness tc was set to 50 ⁇ m. The measurement results are shown in Table 2 below.
- internal haze refers to haze inside the polymer piezoelectric layer, and the measurement method is a general method. Specifically, the internal haze (hereinafter also referred to as internal haze (H1)) of the polymer piezoelectric layer A was measured by measuring the light transmittance in the thickness direction. More specifically, the haze (H2) is measured in advance by sandwiching only silicon oil (Shin-Etsu Silicone (trademark) manufactured by Shin-Etsu Chemical Co., Ltd., model number: KF96-100CS) between two glass plates.
- Si oil Shin-Etsu Silicone (trademark) manufactured by Shin-Etsu Chemical Co., Ltd., model number: KF96-100CS
- the haze (H2) and haze (H3) in the above formula were measured by measuring the light transmittance in the thickness direction using the following apparatus under the following measurement conditions.
- Measuring device Tokyo Denshoku Co., Ltd., HAZE METER TC-HIIIDPK Sample size: 30 mm wide x 30 mm long (see Table 2 for thickness)
- Measurement conditions Conforms to JIS-K7105 Measurement temperature: Room temperature (25 ° C)
- a 40 mm ⁇ 40 mm test piece (polymer piezoelectric layer A) having a conductive layer of Ag formed on both sides is formed by 32 mm and 45 ° in a direction of 45 ° with respect to the stretching direction (MD direction) of the polymer piezoelectric layer A.
- the film was cut to 5 mm in a direction perpendicular to the direction, and a rectangular film of 32 mm ⁇ 5 mm was cut out. This was used as a piezoelectric constant measurement sample.
- the thickness d ( ⁇ m) of the piezoelectric polymer layer A was measured using a digital length measuring device DIGIMICRO STAND MS-11C manufactured by Nikon Corporation. The measurement results are shown in Table 2 below.
- the stabilizer (B) shown in Table 1 is as follows.
- "SI” in Table 1 ... Tokyo Chemical Industry B2756 (trade name), bis-2,6-diisopropylphenylcarbodiimide (structure is as follows)
- “LA” in Table 1 Carbodilite LA-1 (trade name), poly (4,4′-dicyclohexylmethanecarbodiimide) (manufactured by Nisshinbo Chemical Co., Ltd.) (weight average molecular weight of about 2000, structure is as follows).
- ⁇ Preparation of optical compensation layer ⁇ ⁇ Preparation of optical compensation layer a> A commercially available polymethyl methacrylate (PMMA: Sumipex EX manufactured by Sumitomo Chemical Co., Ltd.) was hot pressed at 250 ° C. for 2 minutes and then pressed with a press set at 20 ° C. to obtain a quenched film. Two opposite sides of the quenched film were fixed with a clip, and stretched up to 2.0 times at 110 ° C. in a direction perpendicular to the two fixed sides to obtain an optical compensation layer a as a film having a thickness of 278 ⁇ m.
- PMMA Polymethyl methacrylate
- the in-plane direction retardation Re (nm) and the thickness direction retardation Rth (nm) were measured under the following measurement conditions. Table 4 shows the measurement results.
- ⁇ Preparation of optical compensation layer b> A commercially available polyethylene terephthalate film [trade name “S-27E” manufactured by Toray Industries, Inc. (thickness: 75 ⁇ m)] and an ethyl silicate solution [manufactured by Colcoat Co., Ltd. (mixed solution of ethyl acetate and isopropyl alcohol, 2% by weight)] It was coated with a gravure coater and dried in an air circulating constant temperature oven at 130 ° C. ⁇ 1 ° C. for 1 minute to form a glassy polymer film having a thickness of 0.1 ⁇ m on the surface of the polyethylene terephthalate film.
- This solution was coated on the glassy polymer film of the polyethylene terephthalate film using a rod coater, dried for 2 minutes in an air circulating constant temperature oven at 80 ° C. ⁇ 1 ° C., and then brought to room temperature (23 ° C.). Then, a solidified layer of a liquid crystalline composition having homeotropic alignment was formed on the surface of the polyethylene terephthalate film. Next, the solidified layer was irradiated with ultraviolet rays having an irradiation light amount of 400 mJ / cm 2 in an air atmosphere to cure the liquid crystalline composition by a polymerization reaction.
- optical compensation layer b As a cured layer of a liquid crystalline composition having a thickness of 5.5 ⁇ m and homeotropic alignment.
- in-plane direction retardation Re (nm) and thickness direction retardation Rth (nm) were measured by the same method as optical compensation layer a. The measurement results are shown in Table 4 below.
- a polymer film containing polyvinyl alcohol as a main component [trade name “9P75R (thickness: 75 ⁇ m, average polymerization degree: 2,400, saponification degree 99.9 mol%)” manufactured by Kuraray Co., Ltd.]] is 30 ° C. ⁇ 3 ° C.
- the film was uniaxially stretched 2.5 times while dyeing using a roll stretching machine.
- Examples 1 to 8 and Comparative Examples 1 to 6 Polymer piezoelectric layers and optical compensation layers having combinations shown in Table 5 below were prepared, and the following optical evaluation (presence or absence of light leakage) was performed. By this evaluation, the contrast of the display image when the polymer piezoelectric layer and the optical compensation layer are used for a display device or a laminated optical film for a display device is evaluated. Specifically, in the following optical evaluation, the fact that light leakage is visually recognized corresponds to a decrease in contrast of the display image.
- a laminated sample having a structure in which a polymer piezoelectric layer and an optical compensation layer are sandwiched between the two polarizing plates arranged in a crossed Nicol arrangement is prepared, and light leakage occurs when light from a fluorescent lamp is transmitted through the laminated sample.
- the presence or absence of was observed visually and evaluated according to the following evaluation criteria. This evaluation was performed when the laminated sample was viewed from the front (normal direction) and when the laminated sample was viewed obliquely (obliquely with respect to the normal direction) while rotating around the normal direction. .
- the evaluation results are shown in Table 5 below.
- B Although some light leakage was visually recognized, it was within a practical allowable range.
- C Light leakage was clearly visible and exceeded the practically acceptable range.
- Examples 1 to 8 As shown in Table 5, in Examples 1 to 8, light leakage was not visually recognized or was slight even when visually recognized and was within a practically acceptable range. Accordingly, the combination of the polymer piezoelectric layer and the optical compensation layer in Examples 1 to 8 is used for a display device or a laminated optical film for a display device, thereby reducing the contrast of the display image caused by the polymer piezoelectric layer. It turned out that it can suppress.
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Abstract
Description
例えば、ポリ乳酸の成型物を延伸処理することで、常温で、10pC/N程度の圧電率を示す高分子圧電材料が開示されている(例えば、特開平5-152638号公報参照)。
また、ポリ乳酸結晶を高配向にするために、鍛造法と呼ばれる特殊な配向方法により18pC/N程度の高い圧電性を出すことも報告されている(例えば、特開2005-213376号公報参照)。
また、液晶表示装置や有機エレクトロルミネッセンス表示装置等の表示装置では、直線偏光子が用いられることがある(例えば、特開2006-268018号公報、特開2009-192611号公報、及び特開2009-21408号公報参照)。
従って、本発明の課題は、表示画像のコントラスト低下が抑制された表示装置を提供すること、及び、表示装置に用いたときに表示画像のコントラスト低下を抑制できる積層光学フィルムを提供することである。
<1> 重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を含む結晶性高分子圧電層と、下記式1を満たす光学補償層と、直線偏光子と、を備えた、表示装置である。
(式1): |0.06×Xc×MORc×d+Rth| ≦ 500
〔式1において、Xcは、前記結晶性高分子圧電層の、DSC法で得られる結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の、マイクロ波透過型分子配向計で測定される基準厚さを50μmとしたときの規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕
<3> 前記結晶性高分子圧電層と前記光学補償層との間に直線偏光子が存在しない、<1>又は<2>に記載の表示装置である。
<4> 更に、液晶セル又は有機エレクトロルミネッセンス素子を備えた、<1>~<3>のいずれか1項に記載の表示装置である。
<5> 一対の直線偏光子と、該一対の直線偏光子間に配置された、液晶セル、前記結晶性高分子圧電層、及び前記光学補償層と、を備えた、<1>~<4>のいずれか1項に記載の表示装置である。
この<6>に係る表示装置によれば、特に、サングラス等の偏光子を通して表示画像を観察した場合の表示画像のコントラスト低下が抑制される。
この<8>に係る表示装置によれば、特に、サングラス等の偏光子を通して表示画像を観察した場合の表示画像のコントラスト低下が抑制される。
<10> 前記光学補償層が、下記式2を満たす、<1>~<9>のいずれか1項に記載の表示装置である。
(式2): |0.06×Xc×MORc×d+Rth| ≦ 250
〔式2において、Xcは、前記結晶性高分子圧電層の前記結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の前記規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕
<12> 前記安定化剤(B)が、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する安定化剤(B3)を含む、<11>に記載の表示装置である。
<13> 前記結晶性高分子圧電層の可視光線に対する内部ヘイズが50%以下であり、かつ、25℃において変位法で測定した圧電定数d14が1pm/V以上である、<1>~<12>のいずれか1項に記載の表示装置である。
<14> 前記ヘリカルキラル高分子(A)が、下記式(1)で表される繰り返し単位を含む主鎖を有するポリ乳酸系高分子である、<1>~<13>のいずれか1項に記載の表示装置である。
(式1): |0.06×Xc×MORc×d+Rth| ≦ 500
〔式1において、Xcは、前記結晶性高分子圧電層の、DSC法で得られる結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の、マイクロ波透過型分子配向計で測定される基準厚さを50μmとしたときの規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕
<17> 前記結晶性高分子圧電層が、更に、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる1種類以上の官能基を有する重量平均分子量が200~60000の安定化剤(B)を含み、前記ヘリカルキラル高分子(A)100重量部に対して前記安定化剤(B)が0.01重量部~10重量部含まれる、<15>又は<16>に記載の積層光学フィルムである。
<18> 前記安定化剤(B)が、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する安定化剤(B3)を含む、<17>に記載の積層光学フィルムである。
<19> 前記結晶性高分子圧電層の可視光線に対する内部ヘイズが50%以下であり、かつ、25℃において変位法で測定した圧電定数d14が1pm/V以上である、<15>~<18>のいずれか1項に記載の積層光学フィルムである。
<20> 前記ヘリカルキラル高分子(A)が、下記式(1)で表される繰り返し単位を含む主鎖を有するポリ乳酸系高分子である、<15>~<19>のいずれか1項に記載の積層光学フィルムである。
本発明の表示装置は、重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を含む結晶性高分子圧電層と、下記式1を満たす光学補償層と、直線偏光子と、を備えている。
また、本発明の積層光学フィルムは、上記高分子圧電層と上記光学補償層とを含む。
以下において、単なる「高分子圧電層」との用語は、結晶性高分子圧電層を意味する。
〔式1において、Xcは、前記結晶性高分子圧電層の、DSC法で得られる結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の、マイクロ波透過型分子配向計で測定される基準厚さを50μmとしたときの規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(レターデーション)(nm)を表す。〕
この表示画像のコントラスト低下の理由は以下のように推測される。
即ち、上述の高分子圧電層では、XcとMORcとの積が大きくなるにつれて(例えば、ヘリカルキラル高分子(A)の分子配向が大きくなるにつれて)圧電性能が向上する傾向となるが、それと同時に、この高分子圧電層内に比較的結晶性が高い部分と低い部分との粗密構造が生じ、この高分子圧電層を通過する光の屈折率などへの影響が大きくなる傾向があると考えられる。このため、直線偏光子を備えた表示装置の一部材として上述の高分子圧電層を用いると、この高分子圧電層の上記の結晶構造に起因して、直線偏光子から光漏れが生じる場合があり、この光漏れが表示画像のコントラスト低下の原因となると考えられる。
この点に関し、本発明者は、上述の結晶性高分子圧電層と上記式1を満たす光学補償層とを組み合わせることで、表示画像のコントラスト低下が抑制されることを見出し、本発明を完成させた。
例えば、本発明の表示装置において、高分子圧電層及び光学補償層が、直線偏光子よりも反視認側(視認側の反対側。以下同じ。)に存在している形態(即ち、直線偏光子が視認側である形態;例えば、後述の第1実施形態及び第3実施形態)では、この直線偏光子からの光漏れに起因する、表示画像のコントラスト低下が抑制される。
詳細には、この形態の表示装置から光学補償層を除いた場合、本来この直線偏光子によって遮断されるべき光が漏れ、表示画像のコントラストが低下する。
詳細には、この形態の表示装置から光学補償層を除いた場合、サングラス等の偏光子を通して表示画像を観察したときに、表示装置の直線偏光子を通過した光の偏光状態が高分子圧電層によって変化し、表示画像のコントラストが低下する。
上記左辺が500を超えると、表示画像のコントラストが低下する。
上記左辺は、400以下であることが好ましく、300以下であることがより好ましく、250以下であることが特に好ましい。
なお、上記左辺が250以下であることは、下記式2を満たすことを意味している。
〔式2において、Xc、MORc、d、及びRthは、それぞれ、式1におけるXc、MORc、d、及びRthと同義である。〕
例えば、公知の表示装置に上記高分子圧電層を加えた場合において、表示装置の構成部材のうち、上記式1を満たす部材が存在する場合には、かかる部材を光学補償層とすることができる(即ち、この部材とは別に、光学補償層を設ける必要はない)。
表示部の例としては、液晶セル、有機エレクトロルミネッセンス(以下、「有機EL」ともいう)素子が挙げられる。
これにより、補償前の光が直線偏光子に入射される現象が抑制され、その結果、表示画像のコントラスト低下をより抑制できる。
ここで、略平行とは、2つの軸のなす角度を0°以上90°以下の範囲で表したときに、この角度が0°以上3°以下(好ましくは0°以上1°以下)であることを指す。また、略垂直とは、2つの軸のなす角度を0°以上90°以下の範囲で表したときに、この角度が87°以上90°以下(好ましくは89°以上90°以下)であることを指す。
また、高分子圧電層の結晶軸とは、ヘリカルキラル高分子(A)の分子鎖の主たる配向方向に平行な軸を指す。ここで、ヘリカルキラル高分子(A)の分子鎖の主たる配向方向は、具体的には、規格化分子配向MORcを測定した際に、異方性が最も高く出る方向でもある。例えば、高分子圧電層が延伸によって得られたものである場合、高分子圧電層の結晶軸の方向は、この延伸における主たる延伸方向にほぼ等しい。特に、高分子圧電層が一軸延伸によって得られたものである場合、高分子圧電層の結晶軸は、この一軸延伸の方向にほぼ等しい。
第1実施形態に係る表示装置は、一対の直線偏光子と、該一対の直線偏光子間に配置された、液晶セル、前記高分子圧電層、及び前記光学補償層と、を備えた形態の表示装置(即ち、液晶表示装置)である。
この第1実施形態は、一対の直線偏光子と該一対の直線偏光子間に配置された液晶セルとを含む液晶パネルの内部に、前記高分子圧電層及び前記光学補償層が配置されている形態である。
図1に示すように、液晶表示装置100は、視認側Xからみて、直線偏光子である偏光板14A、本発明における光学補償層の一例である光学補償層20、本発明における高分子圧電層の一例である高分子圧電層18、液晶セル16、及び直線偏光子である偏光板14Bが順次配置されてなる液晶パネル30を備えている。更に、液晶表示装置100は、液晶パネル30からみて反視認側(視認側Xの反対側)に、光源12(例えばバックライト)を備えている。ここで、視認側の偏光板14Aは、「上部偏光板」と呼ばれることがあり、また、反視認側(光源側)の偏光板14Bは、「下部偏光版」と呼ばれることがある。
液晶セル16の構成としては、例えば、一対の基板間(例えば、薄膜トランジスタ(TFT)付き基板と、カラーフィルタ基板やモノクロフィルタ基板等の対向基板と、の間)に液晶分子が配置された公知の構成とすることができる。また、液晶表示装置のモードとしてはTN(Twisted Nematic)モード、STN(Super Twisted Nematic)モード、IPS(In-Plane Switching)モード、VA(Vertical Alignment)モード、OCB(Optically Compensated Bend)モードなどが挙げられる。
高分子圧電層18及び光学補償層20の詳細については後述する。
即ち、液晶表示装置100から光学補償層20を除いた場合、視認側Xから液晶パネル30の表示画像を観察したときに、(特に、黒表示時や中間調表示時に)本来は偏光板14Aによって遮断されるべき光が漏れ、表示画像のコントラストが低下する。
また、液晶表示装置100を製造する際、予め、高分子圧電層18及び光学補償層20を含む積層光学フィルムを準備し、準備した積層光学フィルムを用いて液晶表示装置100を製造してもよい。
各部材を接着させる接着剤としては、例えば、アクリル樹脂、ウレタン樹脂、セルロース系、酢酸ビニル樹脂、エチレン-酢酸ビニル樹脂、エポキシ樹脂、ナイロン-エポキシ系、塩化ビニル樹脂、クロロプレンゴム系、シアノアクリレート系、シリコーン系、変性シリコーン系、水性高分子-イソシアネート系、スチレン-ブタジエンゴム系、ニトリルゴム系、アセタール樹脂、フェノール樹脂、ポリアミド樹脂、ポリイミド樹脂、メラミン樹脂、ユリア樹脂、臭素樹脂、デンプン系、ポリエステル樹脂、ポリオレフィン樹脂等が用いられる。
その他、液晶表示装置100の構成は、公知の液晶表示装置の構成と同様である。
例えば、液晶表示装置100において、光学補償層20及び高分子圧電層18の位置を、視認側Xの偏光板14Aと液晶セル16との間から、液晶セル16と光源12側の偏光板14Bとの間に変更した例が挙げられる。
また、液晶表示装置100において、光学補償層20と高分子圧電層18との配置を入れ替えた例も挙げられる。
また、液晶表示装置100において、光源12が省略されるとともに液晶セル16内に反射電極が設けられ、(更に、場合により偏光板14Bも省略され、)反射型の液晶表示装置とされた例が挙げられる。
これらの変形例は適宜組み合わせることができる。
第2実施形態に係る表示装置は、一対の直線偏光子と、前記一対の直線偏光子間に配置された液晶セルと、前記一対の直線偏光子よりも視認側に配置された、前記高分子圧電層及び前記光学補償層と、を備えた形態の表示装置(即ち、液晶表示装置)である。
この第2実施形態は、一対の直線偏光子と該一対の直線偏光子間に配置された液晶セルとを含む液晶パネルの内部には、前記高分子圧電層及び前記光学補償層が含まれず、これらが液晶パネルの外部(視認側)に配置されている形態である。
図2に示すように、液晶表示装置110の構成は、前述の液晶表示装置100(図1)において、光学補償層20及び高分子圧電層18が液晶パネルに含まれず、液晶パネルよりも視認側に配置されていること以外は前述の液晶表示装置100と同様である(好ましい態様や変形例も同様である)。
即ち、液晶表示装置110から光学補償層20を除いた場合、視認側Xからサングラス等の偏光子を通して液晶パネル40の表示画像を観察したときに、(特に、黒表示時や中間調表示時に)表示装置の直線偏光子を通過した光の偏光状態が高分子圧電層18によって変化し、表示画像のコントラストが低下する。
液晶表示装置110によるコントラスト低下抑制の原理は、前述の液晶表示装置100によるコントラスト低下抑制の原理と同様である。即ち、液晶表示装置100における偏光板14Aは、液晶表示装置110ではサングラス等の偏光子に相当する。
第3実施形態に係る表示装置は、有機EL素子を備え、前記高分子圧電層及び前記光学補償層が、前記直線偏光子と前記有機EL素子との間に配置されている形態の表示装置(即ち、有機EL表示装置)である。
第3実施形態に係る表示装置によれば、第1実施形態に係る表示装置と同様の原理により、高分子圧電層の結晶構造に起因する表示画像のコントラスト低下が抑制される。
第3実施形態に係る表示装置(有機EL表示装置)において、上記構成以外の構成は、公知の有機EL表示装置(例えば、特開2009-21408号公報に記載の有機EL表示装置等)の構成を適宜参照することができる。
有機EL表示装置120は、視認側Xからみて、直線偏光子である偏光板54、1/4波長板55、本発明における光学補償層の一例である光学補償層20、本発明における高分子圧電層の一例である高分子圧電層18、上部ITO透明電極52、有機EL素子層56、及び金属反射電極58が配置されて構成されている。
この例では、偏光板54及び1/4波長板55の積層体が円偏光板として機能し、外光反射を抑制する。この際、液晶表示装置100の場合と同様に、高分子圧電層18の結晶構造に起因する表示画像のコントラスト低下が、光学補償層20を設けたことによって抑制される。
第4実施形態に係る表示装置は、有機EL素子を備え、前記高分子圧電層及び前記光学補償層が、前記直線偏光子よりも視認側に配置されている形態の表示装置(即ち、有機EL表示装置)である。
第4実施形態に係る表示装置(有機EL表示装置)によれば、第2実施形態に係る表示装置と同様の原理により、視認側からサングラス等の偏光子を通して表示画像を観察したときに、高分子圧電層の結晶構造に起因する表示画像のコントラスト低下が抑制される。
第4実施形態に係る表示装置(有機EL表示装置)において、上記構成以外の構成は、公知の有機EL表示装置(例えば、特開2009-21408号公報に記載の有機EL表示装置等)の構成を適宜参照することができる。
図4に示すように、有機EL表示装置130の構成は、前述の有機EL表示装置120(図3)において、光学補償層20及び高分子圧電層18の位置が、偏光板54よりも視認側に配置されていること以外は前述の有機EL表示装置120と同様である。
この例でも、偏光板54及び1/4波長板55の積層体が円偏光板として機能し、外光反射を抑制する。この際、液晶表示装置110の場合と同様に、サングラス等の偏光子を通して表示画像を観察したときに、高分子圧電層18の結晶構造に起因する表示画像のコントラスト低下が、光学補償層20を設けたことによって抑制される。
ここで、「主面」とは、高分子圧電層の表面の中で、最も面積の大きい面をいう。
前記電極としては、光透過性を有する電極が好ましく、例えば、ITO、ZnO、IZO(登録商標)、導電性ポリマー等が用いられる。前記電極としては、内部ヘイズが50%以下(全光線透過率が50%以上)である電極が好ましい。
この圧電デバイスを備えた形態では、高分子圧電層と光学補償層との間に電極が存在することとなるが、この形態であっても、高分子圧電層の結晶構造に起因する表示画像のコントラスト低下が、光学補償層を設けたことによって抑制される。
この形態であっても、光学補償層を設けることによって、表示画像のコントラスト低下が抑制される。
かかる積層圧電デバイスの例としては、電極と高分子圧電層とのユニットを繰り返し重ね、最後に電極で覆われていない高分子圧電層の主面を電極で覆ったものが挙げられる。具体的にはユニットの繰り返しが2回のものは、電極、高分子圧電層、電極、高分子圧電層、電極をこの順で重ねた積層圧電素子である。積層圧電素子に用いられる高分子圧電層はそのうち1層の高分子圧電層が本発明における高分子圧電層であればよく、その他の層は本発明における高分子圧電層でなくてもよい。
また、積層圧電デバイスに複数の本発明における高分子圧電層が含まれる場合は、ある層の本発明における高分子圧電層に含まれる光学活性高分子の光学活性がL体ならば、他の層の高分子圧電層に含まれる光学活性高分子はL体であってもD体であってもよい。高分子圧電層の配置は圧電素子の用途に応じて適宜調整することができる。
例えば、L体の光学活性高分子を主たる成分として含む高分子圧電層の第1の層が電極を介してL体の光学活性高分子を主たる成分として含む第2の高分子圧電層と積層される場合は、第1の高分子圧電層の一軸延伸方向(主たる延伸方向)を、第2の高分子圧電層の一軸延伸方向(主たる延伸方向)と交差、好ましくは直交させると、第1の高分子圧電層と第2の高分子圧電層との変位の向きを揃えることができ、積層圧電素子全体としての圧電性が高まるので好ましい。
一方、L体の光学活性高分子を主たる成分として含む高分子圧電層の第1の層が電極を介してD体の光学活性高分子を主たる成分として含む第2の高分子圧電層と積層される場合は、第1の高分子圧電層の一軸延伸方向(主たる延伸方向)を、第2の高分子圧電層の一軸延伸方向(主たる延伸方向)と略平行となるように配置すると第1の高分子圧電層と第2の高分子圧電層の変位の向きを揃えることができ、積層圧電素子全体としての圧電性が高まるので好ましい。
ここで、「光学活性高分子」とは、重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を指す(以下、同様である)。
本発明の表示装置及び積層光学フィルムは、重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を含む高分子圧電層(例えば、前述の高分子圧電層18)を少なくとも1層備える。
上記構成の高分子圧電層は、圧電性に優れ(即ち、圧電定数d14が大きく)、透明性に優れる。
本発明において、「変位法で測定した圧電定数d14」とは、32mm×5mmの高分子圧電層の両面に導電層が形成されてなる圧電定数測定用サンプルの一対の導電層間に10Hz、300Vppの正弦波の交流電圧を印加し、このときの変位の最大値と最小値の差分距離を変位量(mp-p)として測定し、測定された変位量(mp-p)を基準長30mmで割った値を歪量とし、この歪量をフィルムに印加した電界強度((印加電圧(V))/(フィルム厚))で割った値に2を乗じた値を指す。
この「変位法で測定した圧電定数d14」は、例えば、特許4934235号公報の段落0058~0059に記載の方法によって測定できる。
具体的には、25℃における変位法で測定した圧電定数d14は1pm/V以上が好ましく、3pm/V以上がより好ましく、4pm/V以上がさらに好ましい。また圧電定数の上限は特に限定されないが、後述する透明性などのバランスの観点からは、ヘリカルキラル高分子を用いた圧電材料では50pm/V以下が好ましく、30pm/V以下がより好ましい。
また、同様に透明性とのバランスの観点からは共振法で測定した圧電定数d14が15pC/N以下であることが好ましい。
本発明における高分子圧電層中では、光学活性高分子が配向している。
この配向を表す指標として、「分子配向度MOR」がある。
分子配向度MOR(Molecular Orientation Ratio)は、分子の配向の度合いを示す値であり、以下のようなマイクロ波測定法により測定される。すなわち、試料(フィルム)を、周知のマイクロ波分子配向度測定装置(マイクロ波透過型分子配向計ともいう)のマイクロ波共振導波管中に、マイクロ波の進行方向に前記試料面(フィルム面)が垂直になるように配置する。そして、振動方向が一方向に偏ったマイクロ波を試料に連続的に照射した状態で、試料をマイクロ波の進行方向と垂直な面内で0~360°回転させて、試料を透過したマイクロ波強度を測定することにより分子配向度MORを求める。
MORc = (tc/t)×(MOR-1)+1
(tc:補正したい基準厚さ、t:試料厚さ)
規格化分子配向MORcは、公知の分子配向計、例えば王子計測機器株式会社製マイクロ波方式分子配向計MOA-2012AやMOA-6000等により、4GHzもしくは12GHz近傍の共振周波数で測定することができる。
具体的には、レターデーションは大塚電子株式会社製RETS100を用いて測定することができる。またMORcとΔnとは大凡、直線的な比例関係にあり、かつΔnが0の場合、MORcは1になる。
高分子圧電層の結晶化度(Xc)は、DSC(Differential scanning calorimetry)法によって求められるものであり、本発明における高分子圧電層の結晶化度は20%~80%であることが好ましく、30%~70%であることがより好ましい。前記範囲に結晶化度があれば、高分子圧電層の圧電性、透明性のバランスがよく、また高分子圧電層を延伸するときに、白化や破断がおきにくく製造しやすい。
具体的には、結晶化度が20%以上であると、圧電性が向上する傾向がある。
また、結晶化度が80%以下であると、透明性が高くなる傾向がある。
高分子圧電層の透明性は、例えば、目視観察やヘイズ測定により評価することができる。
高分子圧電層は、可視光線に対する内部ヘイズが50%以下であることが好ましい。ここで内部ヘイズは、厚さ0.03mm~0.07mmの高分子圧電層に対して、JIS-K7105に準拠して、ヘイズ測定機〔(有)東京電色製、TC-HIII DPK〕を用いて25℃で測定したときの値であり、測定方法の詳細は実施例において詳述する。
高分子圧電層の前記内部ヘイズは、20%以下がより好ましく、5%以下が更に好ましく、3.0%以下が更に好ましく、2.0%以下が更に好ましく、1.0%以下が特に好ましい。
また、高分子圧電層の前記内部ヘイズは、低ければ低いほどよいが、圧電定数などとのバランスの観点からは、0.0%~50%であることが好ましく、0.01%~20%であることがさらに好ましく、0.01%~5%がさらに好ましく、0.01%~3.0%がさらに好ましく、0.01%~2.0%がさらに好ましく、0.01%~1.0%が特に好ましい。
なお、本願でいう「内部ヘイズ」とは、本発明における高分子圧電層の内部へイズをいう。内部へイズとは、実施例において後述するように高分子圧電層の外表面の形状によるヘイズを除外したヘイズである。
本発明における高分子圧電層は、規格化分子配向MORcが1.0~15.0であることが好ましく、4.0~10.0であることがより好ましい。
規格化分子配向MORcが大きいほど、具体的には1.0以上であれば、延伸方向に配列する光学活性高分子の分子鎖(例えばポリ乳酸分子鎖)が多く、その結果、配向結晶の生成する率が高くなり、より高い圧電性を発現することが可能となる。
本発明において、高分子圧電層の結晶化度と規格化分子配向MORcとの積は25~700であることが好ましい。この範囲に調整することで、高い圧電性及び高い透明性が維持される。
高分子圧電層の結晶化度と規格化分子配向MORcとの積が25以上であると、圧電性が大きくなる傾向がある。
高分子圧電層の結晶化度と規格化分子配向MORcとの積が700以下であると、透明性が高くなる傾向がある。
上記結晶化度とMORcとの積は、より好ましくは40~700、さらに好ましくは75~680、さらに好ましくは90~660、さらに好ましくは125~650、さらに好ましくは180~350である。上記結晶化度とMORcとの積が40~700の範囲にあれば、圧電性と透明性とのバランスがより良好であり、かつ寸法安定性もより良好である。
本発明では、例えば、高分子圧電層を製造する際の結晶化及び延伸の条件を調整することにより、高分子圧電層の結晶化度と規格化分子配向MORcとの積を調整することができる。
高分子圧電層の厚さ(d)には、特に制限はないが、例えば10μm~100μmとすることができ、20μm~90μmが好ましく、30μm~80μmがより好ましい。
高分子圧電層は、加熱下、特にタッチパネルなどの圧電デバイスや機器等に組み込まれ使用される環境下の温度での寸法変化率が低い方が好ましい。
高分子圧電層の寸法が圧電デバイスなどの使用環境下で変化すると、圧電デバイスに接続されている配線などの位置を動かし、誤作動を引き起こす恐れがあるからである。高分子圧電層の寸法安定性は、圧電デバイスなどの使用環境よりも少し高い温度である150℃で、10分間処理した前後の寸法変化率で評価される。寸法変化率は、10%以下が好ましく、5%以下がさらに好ましい。
本発明における高分子圧電層は、重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を少なくとも1種含む。
本発明において、光学活性を有するヘリカルキラル高分子とは、分子構造が螺旋構造である分子光学活性を有する高分子をいう。
本明細書中では、重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を、「光学活性高分子(A)」や単に「光学活性高分子」ともいう。
光学活性高分子としては、例えば、ポリペプチド、セルロース、セルロース誘導体、ポリ乳酸系高分子、ポリプロピレンオキシド、ポリ(β―ヒドロキシ酪酸)等を挙げることができる。前記ポリペプチドとしては、例えば、ポリ(グルタル酸γ-ベンジル)、ポリ(グルタル酸γ-メチル)等が挙げられる。前記セルロース誘導体としては、例えば、酢酸セルロース、シアノエチルセルロース等が挙げられる。
光学純度(%ee)=100×|L体量-D体量|/(L体量+D体量)
すなわち、『「光学活性高分子のL体の量〔質量%〕と光学活性高分子のD体の量〔質量%〕との量差(絶対値)」を「光学活性高分子のL体の量〔質量%〕と光学活性高分子のD体の量〔質量%〕との合計量」で割った(除した)数値』に、『100』をかけた(乗じた)値を、光学純度とする。
さらに、前記の各製造方法により得られた光学活性高分子(例えばポリ乳酸系高分子)は、光学純度を95.00%ee以上とするために、例えば、ポリ乳酸をラクチド法で製造する場合、晶析操作により光学純度を95.00%ee以上の光学純度に向上させたラクチドを、重合することが好ましい。
本発明における光学活性高分子は、重量平均分子量(Mw)が、5万~100万である。光学活性高分子の重量平均分子量の下限が、5万未満であると光学活性高分子を成型体としたときの機械的強度が不十分となる。光学活性高分子の重量平均分子量の下限は、10万以上であることが好ましく、15万以上であることがさらに好ましい。一方、光学活性高分子の重量平均分子量の上限が100万を超えると、光学活性高分子を成形すること(例えば、押出成型などによりフィルム形状などに成形すること)が難しくなる。
重量平均分子量の上限は、80万以下であることが好ましく、30万以下であることがさらに好ましい。
また、前記光学活性高分子の分子量分布(Mw/Mn)は、高分子圧電層の強度の観点から、1.1~5であることが好ましく、1.2~4であることがより好ましい。さらに1.4~3であることが好ましい。なお、ポリ乳酸系高分子の重量平均分子量Mwと、分子量分布(Mw/Mn)は、ゲル浸透クロマトグラフ(GPC)を用い、下記GPC測定方法により、測定される。
Waters社製GPC-100
-カラム-
昭和電工社製、Shodex LF-804
-サンプルの調製-
ポリ乳酸系高分子を40℃で溶媒(例えば、クロロホルム)へ溶解させ、濃度1mg/mLのサンプル溶液を準備する。
-測定条件-
サンプル溶液0.1mLを溶媒〔クロロホルム〕、温度40℃、1mL/分の流速でカラムに導入する。
本発明における高分子圧電層において、光学活性高分子の含有量(2種以上である場合には総含有量。以下同じ。)には特に制限はないが、高分子圧電層全質量中に対して、80質量%以上であることが好ましい。
上記含有量が80質量%以上であることにより、圧電定数がより大きくなる傾向がある。
本発明における高分子圧電層は、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群より選ばれる1種類以上の官能基を有する重量平均分子量が200~60000の安定化剤(B)を少なくとも1種含むことが好ましい。
これにより、前記光学活性高分子の加水分解性がより抑制され、高分子圧電層の耐湿熱性がより向上する。
前記光学活性高分子の加水分解性を抑制するために、ポリエステルなどのポリマー中の未反応モノマーや不純物、鎖状・環状のオリゴマー等の低分子量化合物を低減する方法(例えば、特開平9-12688号公報)や、芳香族カルボジイミドを添加する方法(例えば、特表2001-525473号公報)、オキサゾリン化合物を添加する方法(例えば、特開2007-77193号公報)など多数の方法が知られている。しかし、光学活性を有するヘリカルキラル高分子を含む高分子圧電層の信頼性を、その圧電特性や透明性を大きく損なうことなく、上記光学活性高分子の加水分解性を抑制することで向上させる方法は知られていなかった。
上記光学活性高分子の加水分解は、以下のスキームにて進行するものと推定される。よって、加水分解を抑制するためには、水分との接触をラミネートなどにより抑制するか、或いは、系中で加水分解した部分に架橋構造を形成するか、フリーのカルボキシ基を封鎖する方法が考えられる。そこで、水酸基及びカルボキシ基の両方の官能基と相互作用を形成しやすい官能基を有する安定化剤、より好ましくは、複数の水酸基やカルボキシ基と相互作用を形成しやすい官能基を有する安定化剤を用いることで、上記加水分解を抑制しうると考えられる。
これは、水酸基とカルボキシ基の双方と相互作用する官能基を有する安定化剤であって、特定の範囲内の分子量を持つ安定化剤を用いることで、上記光学活性高分子が結晶化する際に、この安定化剤が、結晶になりやすい部分(具体的には、分子鎖が切れていない領域)から結晶になりにくい部分(一部分子鎖が切れていて水酸基やカルボキシ基が生じている領域)に移動しやすい。このため、安定化剤は、結晶になりやすい部分の結晶化を阻害することなく、結晶性が高い部分よりも耐湿熱性が低い結晶性が低い部分に多く、かつ、均一に存在することになり、効率的に耐湿熱性を向上させることができると考えられる。
他方、光学活性高分子の安定化剤として知られているオキサゾリン基を有する化合物を用いた場合、オキサゾリン基は、カルボキシ基と反応するが、水酸基とは反応し難い。このため、光学活性高分子が結晶化する際に、結晶になりやすい部分にもオキサゾリンが存在して結晶化し難くなり、また、用いる化合物の構造によっては結晶成長の核となって局所的に大きな結晶が形成される可能性がある。そのため、高分子圧電層の透明性が低下する懸念がある。また、より結晶性が低い部分にオキサゾリンが移動し難いために、耐湿熱性改良効果を充分に得難いと考えられる。
上記安定化剤(B)として用いられる、カルボジイミド基を有するカルボジイミド化合物は、分子中に1個以上のカルボジイミド基を有する。カルボジイミド化合物(ポリカルボジイミド化合物を含む)としては、一般的に良く知られた方法で合成されたものを使用することができる。例えば、触媒として有機リン系化合物又は有機金属化合物を用い、各種イソシアネートを約70℃以上の温度で、無溶媒又は不活性溶媒中で、脱炭酸縮合反応に付することより合成することができるものを挙げることができる。
上記カルボジイミド化合物に含まれるモノカルボジイミド化合物としては、ジシクロヘキシルカルボジイミド、ジメチルカルボジイミド、ジイソブチルカルボジイミド、ジオクチルカルボジイミド、t-ブチルイソプロピルカルボジイミド、ジフェニルカルボジイミド、ジ-t-ブチルカルボジイミド、ジ-β-ナフチルカルボジイミド等を例示することができ、これらの中では、特に工業的に入手が容易であるという面から、ジシクロヘキシルカルボジイミド、またはビス-2,6-ジイソプロピルフェニルカルボジイミドが好適である。
カルボジイミド化合物としては、市販品を用いてもよく、例えば、東京化成製、B2756(商品名)、日清紡ケミカル社製、カルボジライトLA-1、ラインケミー社製、Stabaxol P、Stabaxol P400、Stabaxol I(いずれも商品名)等が挙げられる。
上記安定化剤(B)として用いられる、イソシアネート基を有する化合物(イソシアネート化合物)としては、ヘキシルイソシアネート、シクロヘキシルイソシアネート、ベンジルイソシアネート、フェネチルイソシアネート、イソシアナト酢酸ブチル、ドデシルイソシアネート、オクタデシルイソシアネート、イソシアン酸3-(トリエトキシシリル)プロピル、2,4-トリレンジイソシアネート、2,6-トリレンジイソシアネート、m-フェニレンジイソシアネート、p-フェニレンジイソシアネート、4,4'-ジフェニルメタンジイソシアネート、2,4'-ジフェニルメタンジイソシアネート、2,2'-ジフェニルメタンジイソシアネート、3,3'-ジメチル-4,4'-ビフェニレンジイソシアネート、3,3'-ジメトキシ-4,4'-ビフェニレンジイソシアネート、3,3'-ジクロロ-4,4'-ビフェニレンジイソシアネート、1,5-ナフタレンジイソシアネート、1,5-テトラヒドロナフタレンジイソシアネート、テトラメチレンジイソシアネート、1,6-ヘキサメチレンジイソシアネート、ドデカメチレンジイソシアネート、トリメチルヘキサメチレンジイソシアネート、1,3-シクロヘキシレンジイソシアネート、1,4-シクロヘキシレンジイソシアネート、キシリレンジイソシアネート、テトラメチルキシリレンジイソシアネート、水素添加キシリレンジイソシアネート、リジンジイソシアネート、イソホロンジイソシアネート、4,4'-ジシクロヘキシルメタンジイソシアネート、又は、3,3'-ジメチル-4,4'-ジシクロヘキシルメタンジイソシアネート、ジフェニルメタンジイソシアネート系ポリイソシアネート、1,6-ヘキサメチレンジイソシアネート系ポリイソシアネート、キシリレンジイソシアネート系ポリイソシアネート、イソホロンジイソシアネート系ポリイソシアネート等が挙げられる。
上記安定化剤(B)として用いられる、エポキシ基を有する化合物(エポキシ化合物)としては、N-グリシジルフタルイミド、オルソフェニルフェニルグリシジルエーテル、フェニルグリシジルエーテル、p-t-ブチルフェニルグリシジルエーテル、ヒドロキノンジグリシジルエーテル、レゾルシンジグリシジルエーテル、1,6-ヘキサンジオールジグリシジルエーテル、ジエチレングリコールジグリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、トリメチロールプロパントリグリシジルエーテル、ビスフェノールA-ジグリシジルエーテル、水添ビスフェノールA-ジグリシジルエーテル、フェノールノボラック型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂、エポキシ化ポリブタジエン等が挙げられる。
安定化剤(B)の好ましい態様としては、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群より選ばれる1種類以上の官能基を有し、かつ、数平均分子量が200~900の安定化剤(B1)と、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群よりばれる1種類以上の官能基を1分子内に2以上有し、かつ、重量平均分子量が1000~60000の安定化剤(B2)とを併用するという態様が挙げられる。なお、数平均分子量が200~900の安定化剤(B1)の重量平均分子量は、大凡200~900であり、安定化剤(B1)の数平均分子量と重量平均分子量とはほぼ同じ値となる。
ここで、安定化剤(B1)としては、具体的には、ジシクロヘキシルカルボジイミド、ビス-2,6-ジイソプロピルフェニルカルボジイミド、ヘキシルイソシアネート、オクタデシルイソシアネート、イソシアン酸3-(トリエトキシシリル)プロピル、N-グリシジルフタルイミド、オルソフェニルフェニルグリシジルエーテル、フェニルグリシジルエーテル、p-t-ブチルフェニルグリシジルエーテル等が挙げられる。
また、安定化剤(B2)としては、具体的には、ポリ(4,4’-ジシクロヘキシルメタンカルボジイミド)、ポリ(テトラメチルキシリレンカルボジイミド)、ポリ(N,N-ジメチルフェニルカルボジイミド)、ポリ(N,N’-ジ-2,6-ジイソプロピルフェニルカルボジイミド)、ジフェニルメタンジイソシアネート系ポリイソシアネート、1,6-ヘキサメチレンジイソシアネート系ポリイソシアネート、キシリレンジイソシアネート系ポリイソシアネート、イソホロンジイソシアネート系ポリイソシアネート、フェノールノボラック型エポキシ樹脂、クレゾールノボラック型エポキシ樹脂、エポキシ化ポリブタジエン等が挙げられる。
カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する化合物の重量平均分子量としては、200~2000が好ましく、200~1500がより好ましく、300~900がさらに好ましい。
カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する化合物の具体例としては、ジシクロヘキシルカルボジイミド、ビス-2,6-ジイソプロピルフェニルカルボジイミド、ヘキシルイソシアネート、オクタデシルイソシアネート、イソシアン酸3-(トリエトキシシリル)プロピル、N-グリシジルフタルイミド、オルソフェニルフェニルグリシジルエーテル、フェニルグリシジルエーテル、p-t-ブチルフェニルグリシジルエーテルが挙げられる。これらの中でも、ジシクロヘキシルカルボジイミド、ビス-2,6-ジイソプロピルフェニルカルボジイミドが好ましく、ビス-2,6-ジイソプロピルフェニルカルボジイミドがさらに好ましい。
また安定化剤(B3)と、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に2つ以上有する安定化剤(B4)(例えば前述の安定化剤(B2)が含まれる)を併用してもよい。安定化剤(B3)100重量部に対して、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に2つ以上有する安定化剤(B4)が5重量部~200重量部の範囲であることが、透明性、耐湿熱性及び寸法安定性バランスという観点から好ましく、10重量部~100重量部の範囲であることが、より好ましい。
上記安定化剤(B)の数平均分子量(Mn)と重量平均分子量(Mw)は、いずれも、光学活性高分子(A)の項にて記載したゲル浸透クロマトグラフ(GPC)を用いた測定方法により同様に測定される。なおGPC以外にもGC-MS,FAB-MS,ESI-MS,TOF-MSなどの測定方法でも測定することができる。
上記安定化剤(B)の添加量は、光学活性高分子(A)100重量部に対して0.01重量部~10重量部が好ましい。また、より高い信頼性を得るためには(具体的には後述する信頼性試験500時間での信頼性)、添加量は0.7重量部以上がより好ましい。特に、安定化剤として脂肪族カルボジイミドを用いる場合は0.01重量部~2.8重量部含まれるのが透明性という観点からはさらに好ましい。添加量が上記の範囲になることで、本発明における高分子圧電層の内部へイズを著しく損なうことなく、圧電材料の信頼性を高めることができる。
なお、上記添加量は、安定化剤(B)を2種以上併用する場合、それらの総量を示す。
一方、内部ヘイズを低くし、かつ圧電定数を高めるか又は維持するという観点からは、安定化剤(B)の添加量は、光学活性を有する脂肪族系ポリエステル(A)100重量部に対して0.01重量部~1.2重量部が好ましく、0.01重量部~0.7重量部がさらに好ましく、0.01重量部~0.6重量部がさらにより好ましい。
本発明における高分子圧電層は、本発明の効果を損なわない限度において、既述の光学活性高分子以外のその他の成分(例えば、ポリフッ化ビニリデン、ポリエチレン樹脂やポリスチレン樹脂に代表される公知の樹脂や、シリカ、ヒドロキシアパタイト、モンモリロナイト等の無機フィラー、フタロシアニン等の公知の結晶核剤等)を含有していてもよい。
また、本発明における高分子圧電層は、本発明の効果を損なわない限度において、既述の光学活性高分子(即ち、重量平均分子量(Mw)が5万~100万である光学活性を有するヘリカルキラル高分子)以外のヘリカルキラル高分子を含んでいてもよい。
本発明における高分子圧電層は、無機フィラーを少なくとも1種含有していてもよい。
例えば、高分子圧電層を、気泡等のボイドの発生を抑えた透明なフィルムとするために、高分子圧電層中に、ヒドロキシアパタイト等の無機フィラーをナノ分散してもよいが、無機フィラーをナノ分散させるためには、凝集塊の解砕に大きなエネルギーが必要であり、また、無機フィラーがナノ分散しない場合、フィルムの透明度が低下する場合がある。従って、本発明における高分子圧電層が無機フィラーを含有するときは、高分子圧電層全質量に対する無機フィラーの含有量は、1質量%未満とすることが好ましい。なお、高分子圧電層が光学活性高分子以外の成分を含む場合、光学活性高分子以外の成分の含有量は、高分子圧電層全質量中に対して、20質量%以下であることが好ましく、10質量%以下であることがより好ましい。
本発明における高分子圧電層は、結晶促進剤(結晶核剤)を少なくとも1種含有していてもよい。
結晶促進剤(結晶核剤)としては、結晶化促進の効果が認められるものであれば、特に限定されないが、光学活性高分子の結晶格子の面間隔に近い面間隔を持つ結晶構造を有する物質を選択することが望ましい。面間隔が近い物質ほど核剤としての効果が高いからである。例えば、光学活性高分子としてポリ乳酸系樹脂を用いた場合、有機系物質であるフェニルスルホン酸亜鉛、ポリリン酸メラミン、メラミンシアヌレート、フェニルホスホン酸亜鉛、フェニルホスホン酸カルシウム、フェニルホスホン酸マグネシウム、無機系物質のタルク、クレー等が挙げられる。それらのうちでも、最も面間隔がポリ乳酸の面間隔に類似し、良好な結晶形成促進効果が得られるフェニルホスホン酸亜鉛が好ましい。なお、使用する結晶促進剤は、市販されているものを用いることができる。具体的には例えば、フェニルホスホン酸亜鉛;エコプロモート(日産化学工業(株)製)等が挙げられる。
結晶核剤の上記含有量が0.01重量部以上であると、結晶促進の効果がより効果的に得られる。結晶核剤の上記含有量が1.0重量部未満であると、結晶化速度をより制御しやすい。
本発明における高分子圧電層を製造する方法としては、前記結晶化度を調整でき、かつ、前記規格化分子配向MORcと前記結晶化度との積を調整できる方法であれば特に制限されない。好ましくは、前記結晶化度を20%~80%に、前記規格化分子配向MORcと前記結晶化度との積を25~700に調整できる方法である。
本発明における高分子圧電層を製造する方法として、例えば、既述の光学活性高分子を含む非晶状態のシートに対して結晶化及び延伸(いずれが先であってもよい)を施す方法であって、前記結晶化及び前記延伸の各条件を調整することにより、前記結晶化度を調整し、かつ、前記規格化分子配向MORcと前記結晶化度との積を調整する方法を用いることができる。
なお、ここでいう「結晶化」は、後述の予備結晶化及び後述のアニール処理を包含する概念である。
上述の混合物は、溶融混練して得られた混合物であることが好ましい。
具体的には、例えば、2種類以上の光学活性高分子を混合する場合や、1種類以上の光学活性高分子にその他の成分(例えば上述の無機フィラーや結晶核剤)を混合する場合は、混合する光学活性高分子を(必要に応じその他の成分とともに)、溶融混練機〔東洋精機社製、ラボプラストミキサー〕を用い、ミキサー回転数30rpm~70rpm、180℃~250℃の条件で、5分~20分間溶融混練することで、複数種の光学活性高分子のブレンド体や光学活性高分子と無機フィラーなどの他の成分とのブレンド体を得ることができる。
また、本発明における高分子圧電層は、光学活性高分子を含むシート(好ましくは非晶状態のシート)を主として1軸方向に延伸する工程と、延伸されたシートをアニール処理する工程と、をこの順で含む製造方法によっても製造できる。
上記延伸の条件やアニール処理の条件は、好ましくは、製造される高分子圧電層の前記結晶化度が20%~80%となり、かつ、前記規格化分子配向MORcと前記結晶化度との積が25~700となるように適宜調整される。
本発明の表示装置及び積層光学フィルムは、前述の式1を満たす光学補償層(例えば、前述の光学補償層20)を少なくとも1層備える。
光学補償層は、前述の式1を満たす層であれば特に制限はない。
例えば、直線偏光子及び上記高分子圧電層を含む表示装置の構成部材のうち、直線偏光子及び上記高分子圧電層以外の部材として、前述の式1を満たす部材が存在する場合には、かかる部材を光学補償層とすることができる(即ち、この部材とは別に、光学補償層を設ける必要はない)。
詳細には、波長550nmにおける光学補償層の厚さ方向の位相差Rth(nm)は、下記式aで定義される。
また、波長550nmにおける光学補償層の面内の位相差Re(nm)は、下記式bで定義される。
式b: Re=(nx-ny)×d2
〔式a及び式bにおいて、nxは、波長550nmにおける前記光学補償層の面内の遅相軸方向の屈折率であり、nyは、波長550nmにおける前記光学補償層の面内の進相軸方向の屈折率であり、nzは、波長550nmにおける前記光学補償層の厚さ方向の屈折率であり、d2は、前記光学補償層の厚さ(nm)である。〕
また、本発明における光学補償層において、前記Reは特に制限はないが、0nm~3000nmであることが好ましく、0nm~1500nmであることがより好ましい。
前記高分子フィルムの延伸フィルムは、負の固有複屈折を示すポリマーを含むことが好ましい。
ここで、「負の固有複屈折を示すポリマー」とは、ポリマーを配向させた場合に、ポリマー鎖の配向方向と直交する方向に、屈折率楕円体の長軸方向が発生するポリマーをいう。
負の固有複屈折を示すポリマーとしては、例えば、芳香環やカルボニル基等の分極異方性の大きい化学結合および/または置換基が側鎖に導入されたポリマーが挙げられる。
負の固有複屈折を示すポリマーとしては、好ましくは、メタクリレート系ポリマー、スチレン系ポリマー、マレイミド系ポリマー等が用いられる。これらは単独でまたは2種以上組み合わせて用いることができる。
また、本発明における光学補償層は、液晶性組成物の固化層または硬化層であってもよい。
液晶性組成物の固化層または硬化層としては、例えば、特開2006-268018号の段落0072~0078に記載されている位相差フィルムが挙げられる。
また、液晶性組成物の固化層または硬化層として、ホメオトロピック配向させた液晶化合物を含む液晶性組成物の固化層または硬化層も好適である。
ここで、「ホメオトロピック配向」とは、液晶性組成物に含まれる液晶化合物がフィルム法線方向に対し、平行かつ一様に配向した状態をいう。
特に好ましくは、上記液晶性組成物が、分子構造の一部分に、少なくとも2つの重合性または架橋性官能基を有する低分子液晶を含む。
このような液晶化合物を用いれば、重合(または架橋)反応により、重合性(または架橋性)官能基を重合(または架橋)させることによって、液晶性組成物の固化層または硬化層の機械的強度が増し、耐久性、寸法安定性に優れた液晶性組成物の固化層または硬化層が得られ得る。
例えば、分子構造の一部分に1つのメソゲン基と2つの重合性官能基を有する低分子液晶としては、BASF社製商品名「PaliocolorLC242」(Δn=0.131)や、HUNTSUMAN社製 商品名「CB483」(Δn=0.080)などが挙げられる。
上記の範囲とすることによって、フィルムを成形する際の生産性や作業性に優れ、実用上十分な機械的強度を有し、光学均一性に優れたフィルムを得ることができる。
mは50~70であり、nは30~50である。
本発明の表示装置及び積層光学フィルムは直線偏光子(例えば、前述の偏光板14A等)を少なくとも1つ備える。
直線偏光子としては特に制限はないが、例えば、ヨウ素または二色性染料を含む、ポリビニルアルコール系樹脂を主成分とする高分子フィルムの延伸フィルム;米国特許5,523,863号に開示されているような、二色性物質と液晶性化合物とを含む液晶性組成物を一定方向に配向させたO型偏光子;米国特許6,049,428号に開示されているような、リオトロピック液晶を一定方向に配向させたE型偏光子;などが挙げられる。
なお、直線偏光子としては、例えば、特開2006-268018号に記載の偏光子を用いることができる。
例えば、本発明の表示装置は、液晶セル又は有機エレクトロルミネッセンス(有機EL)素子を備えて適宜構成することができる。
表示装置の構成やその構成要素については、例えば、特開2006-268018号公報、特開2009-192611号公報、特開2009-21408号公報等の記載を適宜参照することができる。
なお、以下において、「MD方向」とはフィルムの流れる方向(Machine Direction)であり、「TD方向」とは、前記MD方向と直交し、フィルムの主面と平行な方向(Transverse Direction)である。
<高分子圧電層Aの作製>
ヘリカルキラル高分子(A)としての三井化学(株)製ポリ乳酸系高分子(登録商標LACEA H-400(重量平均分子量Mw:20万))を押出成形機ホッパーに入れて、220℃~230℃に加熱しながらTダイから押し出し、55℃のキャストロールに0.5分間接触させて、厚さ150μmの予備結晶化シートを製膜した(予備結晶化工程)。
得られた予備結晶化シートを70℃に加熱しながらロールツーロールで、延伸速度1650mm/分で延伸を開始し、3.5倍までMD方向に一軸延伸した(延伸工程)。
その後、前記一軸延伸フィルムを、ロールツーロールで、130℃に加熱したロール上に60秒間接触させアニール処理し(アニール処理工程)、結晶性高分子圧電層である高分子圧電層Aを得た。
得られた高分子圧電層Aについて、下記の測定を行った。
測定結果を下記表1~3に示す。
50mLの三角フラスコに1.0gのサンプル(高分子圧電層A)を秤り込み、IPA(イソプロピルアルコール)2.5mLと、5.0mol/L水酸化ナトリウム溶液5mLとを加えた。次に、サンプル溶液が入った前記三角フラスコを、温度40℃の水浴に入れ、ポリ乳酸が完全に加水分解するまで、約5時間攪拌した。
得られた結果に基づき、光学純度(%ee)を求めた。結果を下記表1に示す。
-HPLC測定条件-
・カラム
光学分割カラム、(株)住化分析センター製 SUMICHIRAL OA5000
・測定装置
日本分光社製 液体クロマトグラフィ
・カラム温度
25℃
・移動相
1.0mM-硫酸銅(II)緩衝液/IPA=98/2(V/V)
硫酸銅(II)/IPA/水=156.4mg/20mL/980mL
・移動相流量
1.0mL/分
・検出器
紫外線検出器(UV254nm)
ゲル浸透クロマトグラフ(GPC)を用い、下記GPC測定方法により、高分子圧電層Aに含まれるヘリカルキラル高分子(A)の重量平均分子量(Mw)及び分子量分布(Mw/Mn)を測定した。
-GPC測定方法-
・測定装置
Waters社製GPC-100
・カラム
昭和電工社製、Shodex LF-804
・サンプルの調製
高分子圧電層Aを、40℃で溶媒〔クロロホルム〕へ溶解させ、濃度1mg/mLのサンプル溶液を準備した。
・測定条件
サンプル溶液0.1mLを溶媒(クロロホルム)、温度40℃、1mL/分の流速でカラムに導入し、カラムで分離されたサンプル溶液中のサンプル濃度を示差屈折計で測定した。
ヘリカルキラル高分子(A)(ポリ乳酸)の重量平均分子量(Mw)は、ポリスチレン標準試料にて作成されたユニバーサル検量線に基づき、算出した。
測定結果を下記表1に示す。
なお、下記表1において、「LA」はLACEA H-400を表す。
高分子圧電層Aを10mg正確に秤量し、示差走査型熱量計(パーキンエルマー社製DSC-1)を用い、昇温速度10℃/分の条件で測定し、融解吸熱曲線を得た。得られた融解吸熱曲線から融点Tmおよび結晶化度Xc(%)を得た。
測定結果を下記表2に示す。
高分子圧電層Aの規格化分子配向MORcを、王子計測機器株式会社製マイクロ波方式分子配向計MOA-6000により測定した。基準厚さtcは、50μmに設定した。
測定結果を下記表2に示す。
本願でいう「内部ヘイズ」とは高分子圧電層の内部へイズのことをいい、測定方法は一般的な方法で測定される。
具体的には、高分子圧電層Aの内部ヘイズ(以下、内部ヘイズ(H1)ともいう)は、厚さ方向の光透過性を測定することにより、測定した。より詳細には、予めガラス板2枚の間に、シリコンオイル(信越化学工業株式会社製信越シリコーン(商標)、型番:KF96-100CS)のみを挟んでヘイズ(H2)を測定し、次にシリコンオイルで表面を均一に塗らしたフィルム(高分子圧電層A)を、ガラス板2枚で挟んでヘイズ(H3)を測定し、下記式のようにこれらの差をとることで、高分子圧電層Aの内部ヘイズ(H1)を得た。測定結果を下記表2に示す。
内部ヘイズ(H1)=ヘイズ(H3)-ヘイズ(H2)
測定装置:東京電色社製、HAZE METER TC-HIIIDPK
試料サイズ:幅30mm×長さ30mm(厚さは下記表2参照)
測定条件:JIS-K7105に準拠
測定温度:室温(25℃)
両面にAgの導電層が形成された40mm×40mmの試験片(高分子圧電層A)を、高分子圧電層Aの延伸方向(MD方向)に対して45°なす方向に32mm、45°なす方向に直交する方向に5mmにカットして、32mm×5mmの矩形のフィルムを切り出した。これを、圧電定数測定用サンプルとした。得られたサンプルに、10Hz、300Vppの正弦波の交流電圧を印加したときの、フィルムの変位の最大値と最小値の差分距離を、キーエンス社製レーザ分光干渉型変位計SI-1000により計測した。計測した変位量(mp-p)を、フィルムの基準長30mmで割った値を歪量とし、この歪量をフィルムに印加した電界強度((印加電圧(V))/(フィルム厚))で割った値に2を乗じた値を圧電定数d14(pm/V)とした。なお、上記の計測は25℃の条件下で行った。
測定結果を下記表2に示す。
高分子圧電層Aの厚さd(μm)を、ニコン社製デジタル測長機DIGIMICRO STAND MS-11Cを用いて測定した。
測定結果を下記表2に示す。
上記MORcと上記結晶化度Xc(%)との積(「MORc×結晶化度」)を算出した。
結果を下記表3に示す。
上記MORcと上記結晶化度Xc(%)と上記厚さd(μm)と0.06との積(「0.06×結晶化度×MORc×d(μm)」)を算出した。
結果を下記表3に示す。
高分子圧電層Aの作製において、LACEA H-400を押出成形機ホッパーに入れる操作を、LACEA H-400(100重量部)及び表1に示す種類及び量の安定化剤(B)を押出成形機ホッパーに入れる操作に変更したこと、並びに、一軸延伸の延伸倍率を表2に示す延伸倍率としたこと以外は高分子圧電層Aの作製と同様にして、結晶性高分子圧電層である高分子圧電層B~Eをそれぞれ作製した。
得られた高分子圧電層B~Eについて、それぞれ、高分子圧電層Aと同様の測定(及び算出)を行った。測定結果を表1~表3に示す。
・表1中の「SI」 … 東京化成製、B2756(商品名)、ビス-2,6-ジイソプロピルフェニルカルボジイミド(構造は以下の通りである)
・表1中の「LA」 … 日清紡ケミカル社製、カルボジライトLA-1(商品名)、ポリ(4,4’-ジシクロヘキシルメタンカルボジイミド)(重量平均分子量約2000、構造は以下の通りである)。
<光学補償層aの作製>
市販のポリメタクリル酸メチル(PMMA:住友化学製スミペックスEX)を250℃で熱プレスを2分間行った後、20℃に設定したプレス機でプレスして急冷フィルムを得た。
前記急冷フィルムの対向する2辺をクリップで固定し、固定した2辺と直交する方向に、110℃で2.0倍まで延伸し、厚さ278μmのフィルムとして、光学補償層aを得た。
得られた光学補償層aについて、面内方向の位相差Re(nm)、及び、厚さ方向の位相差Rth(nm)を、それぞれ以下の測定条件で測定した。測定結果を表4に示す。
・測定波長 … 550nm
・測定装置 … 大塚電子社製 位相差フィルム・光学材料検査装置RETS-100
市販のポリエチレンテレフタレートフィルム[東レ(株)製 商品名「S-27E」(厚み:75μm)]にエチルシリケート溶液[コルコート(株)製(酢酸エチル、イソプロピルアルコールの混合溶液、2重量%)]をグラビアコータで塗工し、130℃±1℃の空気循環式恒温オーブンで1分間乾燥させて、上記ポリエチレンテレフタレートフィルムの表面に厚み0.1μmのガラス質高分子膜を形成した。
次いで、下記式(II)で表される高分子液晶(重量平均分子量:5000)を5重量部、分子構造の一部分に2つの重合性官能基を有するカラミチック液晶化合物[BSAF社製、商品名「PaliocolorLC242」(ne=1.654、no=1.523)]20重量部、および光重合開始剤[チバスペシャリティケミカルズ(株)製、商品名「イルガキュア907」]1.25重量部を、シクロヘキサノン75重量部に溶解して、液晶性組成物の溶液を調製した。この溶液を、上記ポリエチレンテレフタレートフィルムのガラス質高分子膜上にロッドコータを用いて塗工し、80℃±1℃の空気循環式恒温オーブンで2分間乾燥させた後、室温(23℃)にまで徐々に冷却させて、上記ポリエチレンテレフタレートフィルムの表面に、ホメオトロピック配向させた液晶性組成物の固化層を形成した。次いで、この固化層に、400mJ/cm2の照射光量の紫外線を空気雰囲気下で照射して、上記液晶性組成物を重合反応により硬化させた。
上記ポリエチレンテレフタレートフィルムを剥離して、厚み5.5μmのホメオトロピック配向させた液晶性組成物の硬化層として、光学補償層bを得た。
得られた光学補償層bについて、光学補償層aと同様の方法で、面内方向の位相差Re(nm)、及び、厚さ方向の位相差Rth(nm)を測定した。
測定結果を下記表4に示す。
ポリビニルアルコールを主成分とする高分子フィルム[クラレ(株)製商品名「9P75R(厚み:75μm、平均重合度:2,400、ケン化度99.9モル%)」]を30℃±3℃に保持したヨウ素とヨウ化カリウム配合の染色浴にて、ロール延伸機を用いて、染色しながら2.5倍に一軸延伸した。次いで、60±3℃に保持したホウ酸とヨウ化カリウム配合の水溶液中で、架橋反応を行いながら、ポリビニルアルコールフィルムの元長の6倍となるように一軸延伸した。得られたフィルムを50℃±1℃の空気循環式恒温オーブン内で30分間乾燥させて、水分率23%、厚み28μm、偏光度99.9%、単体透過率43.5%の偏光板(直線偏光子)を得た。
この偏光板を2枚準備した。
下記表5に示す組み合わせの高分子圧電層及び光学補償層を準備し、以下の光学評価(光漏れの有無)を行った。
この評価により、高分子圧電層及び光学補償層を、表示装置又は表示装置用の積層光学フィルムに用いた場合の、表示画像のコントラストが評価される。具体的には、以下の光学評価において、光漏れが視認されることは、表示画像のコントラストが低下することに対応する。
クロスニコルの配置とした上記2枚の偏光板間に、高分子圧電層及び光学補償層を挟んだ構造の積層サンプルを準備し、この積層サンプルに蛍光灯の光を透過させたときの光漏れの有無を目視で観察し、下記評価基準に従って評価した。
この評価は、積層サンプルを正面(法線方向)から見た場合、及び、積層サンプルを法線方向を軸に回転させながら斜め(法線方向に対し斜め)から見た場合について、それぞれ行った。
評価結果を下記表5に示す。
-評価基準-
A: 光漏れが視認されなかった。
B: 光漏れが若干視認されたが、実用上の許容範囲内であった。
C: 光漏れが明確に視認され、実用上の許容範囲を超えていた。
なお、面内に遅相軸が検出されない光学補償層bを用いた実施例4~8では、光学補償層bと高分子圧電層との配置は、どのような配置であっても、評価には影響しない。
本明細書に記載された全ての文献、特許出願、および技術規格は、個々の文献、特許出願、および技術規格が参照により取り込まれることが具体的かつ個々に記された場合と同程度に、本明細書中に参照により取り込まれる。
Claims (20)
- 重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を含む結晶性高分子圧電層と、
下記式1を満たす光学補償層と、
直線偏光子と、
を備えた、表示装置。
(式1): |0.06×Xc×MORc×d+Rth| ≦ 500
〔式1において、Xcは、前記結晶性高分子圧電層の、DSC法で得られる結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の、マイクロ波透過型分子配向計で測定される基準厚さを50μmとしたときの規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕 - 前記結晶性高分子圧電層は、前記結晶化度が20%~80%であり、かつ、前記規格化分子配向と前記結晶化度との積が25~700である、請求項1に記載の表示装置。
- 前記結晶性高分子圧電層と前記光学補償層との間に直線偏光子が存在しない、請求項1又は請求項2に記載の表示装置。
- 更に、液晶セル又は有機エレクトロルミネッセンス素子を備えた、請求項1又は請求項2に記載の表示装置。
- 一対の直線偏光子と、
該一対の直線偏光子間に配置された、液晶セル、前記結晶性高分子圧電層、及び前記光学補償層と、
を備えた、請求項1又は請求項2に記載の表示装置。 - 一対の直線偏光子と、
前記一対の直線偏光子間に配置された液晶セルと、
前記一対の直線偏光子よりも視認側に配置された、前記結晶性高分子圧電層及び前記光学補償層と、
を備えた、請求項1又は請求項2に記載の表示装置。 - 更に、有機エレクトロルミネッセンス素子を備え、
前記結晶性高分子圧電層及び前記光学補償層が、前記直線偏光子と前記有機エレクトロルミネッセンス素子との間に配置されている、請求項1又は請求項2に記載の表示装置。 - 更に、有機エレクトロルミネッセンス素子を備え、
前記結晶性高分子圧電層及び前記光学補償層が、前記直線偏光子よりも視認側に配置されている、請求項1又は請求項2に記載の表示装置。 - 前記直線偏光子の吸収軸と前記結晶性高分子圧電層の結晶軸とが、略平行または略垂直である、請求項1又は請求項2に記載の表示装置。
- 前記光学補償層が、下記式2を満たす、請求項1又は請求項2に記載の表示装置。
(式2): |0.06×Xc×MORc×d+Rth| ≦ 250
〔式2において、Xcは、前記結晶性高分子圧電層の前記結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の前記規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕 - 前記結晶性高分子圧電層が、更に、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる1種類以上の官能基を有する重量平均分子量が200~60000の安定化剤(B)を含み、前記ヘリカルキラル高分子(A)100重量部に対して前記安定化剤(B)が0.01重量部~10重量部含まれる、請求項1又は請求項2に記載の表示装置。
- 前記安定化剤(B)が、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する安定化剤(B3)を含む、請求項11に記載の表示装置。
- 前記結晶性高分子圧電層の可視光線に対する内部ヘイズが50%以下であり、かつ、25℃において変位法で測定した圧電定数d14が1pm/V以上である、請求項1又は請求項2に記載の表示装置。
- 重量平均分子量が5万~100万である光学活性を有するヘリカルキラル高分子(A)を含む結晶性高分子圧電層と、
下記式1を満たす光学補償層と、
を含む、積層光学フィルム。
(式1): |0.06×Xc×MORc×d+Rth| ≦ 500
〔式1において、Xcは、前記結晶性高分子圧電層の、DSC法で得られる結晶化度(%)を表し、MORcは、前記結晶性高分子圧電層の、マイクロ波透過型分子配向計で測定される基準厚さを50μmとしたときの規格化分子配向を表し、dは、前記結晶性高分子圧電層の厚さ(μm)を表し、Rthは、波長550nmにおける前記光学補償層の厚さ方向の位相差(nm)を表す。〕 - 前記結晶性高分子圧電層は、前記結晶化度が20%~80%であり、かつ、前記規格化分子配向と前記結晶化度との積が25~700である、請求項15に記載の積層光学フィルム。
- 前記結晶性高分子圧電層が、更に、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる1種類以上の官能基を有する重量平均分子量が200~60000の安定化剤(B)を含み、前記ヘリカルキラル高分子(A)100重量部に対して前記安定化剤(B)が0.01重量部~10重量部含まれる、請求項15又は請求項16に記載の積層光学フィルム。
- 前記安定化剤(B)が、カルボジイミド基、エポキシ基、及びイソシアネート基からなる群から選ばれる官能基を1分子内に1つ有する安定化剤(B3)を含む、請求項17に記載の積層光学フィルム。
- 前記結晶性高分子圧電層の可視光線に対する内部ヘイズが50%以下であり、かつ、25℃において変位法で測定した圧電定数d14が1pm/V以上である、請求項15又は請求項16に記載の積層光学フィルム。
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CN104981760A (zh) | 2015-10-14 |
US20150362647A1 (en) | 2015-12-17 |
JP5819548B2 (ja) | 2015-11-24 |
EP2953011A1 (en) | 2015-12-09 |
CN104981760B (zh) | 2018-01-02 |
EP2953011A4 (en) | 2016-10-26 |
JPWO2014119577A1 (ja) | 2017-01-26 |
KR101789896B1 (ko) | 2017-10-25 |
KR20150100899A (ko) | 2015-09-02 |
US10126473B2 (en) | 2018-11-13 |
EP2953011B1 (en) | 2019-04-17 |
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