WO2022016464A1 - 一种旋光材料的制备方法及应用 - Google Patents

一种旋光材料的制备方法及应用 Download PDF

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WO2022016464A1
WO2022016464A1 PCT/CN2020/103858 CN2020103858W WO2022016464A1 WO 2022016464 A1 WO2022016464 A1 WO 2022016464A1 CN 2020103858 W CN2020103858 W CN 2020103858W WO 2022016464 A1 WO2022016464 A1 WO 2022016464A1
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optically active
active material
salt
nanorod
metal
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PCT/CN2020/103858
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French (fr)
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孟鸿
艾琳
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北京大学深圳研究生院
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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors

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  • the invention relates to the field of backlight luminescent materials, in particular to a preparation method and application of an optically active material.
  • LCD displays generally use white backlight and three-color color filters as the color display mechanism.
  • the incident light needs to be rotated by the upper and lower polarizers, but the intensity of the incident light at this time is when it passes through the lower polarizer.
  • the direct loss is 50%, and the loss after passing through each film layer is more serious, and the final light output rate is less than 5%, resulting in the brightness of the LCD display screen has always been a thorny problem in the field.
  • the resolution is constantly increasing, and the aperture ratio is gradually decreasing. How to improve the brightness is the focus of attention of various enterprises.
  • the existing solution is to use quantum dot nanorods as a backlight film. Since the anisotropic rods have optical rotation, the incident light does not need to undergo downward polarization treatment, and the light intensity is not lost, which greatly improves the brightness.
  • the brightness of LCD displays has always been criticized by the industry and buyers due to the presence of toxic elements such as lead and mercury in quantum dots.
  • the present invention provides a preparation method and application of an optically active material.
  • metal dot nanorods Dissolve metal salt in solvent, add alkyl acid and ligand, and prepare metal dot nanorod material by one-pot water bath method;
  • the metal salt is at least one of copper salts, gold salts, silver salts, platinum salts, iron salts, zinc salts, nickel salts, and cobalt salts;
  • the solvent is at least one of ethanol, toluene, paraffin, dibenzyl ether, dimethylformamide, dimethyl sulfoxide, and tetrahydrofuran.
  • the alkyl acid is at least one of citric acid, serine, and tryptophan.
  • the ligand is at least one of POSS, POSS whose amino group is substituted by a thiol group, and a POSS derivative.
  • the molar ratio of the ligand to the metal salt is 5:1 to 10:1.
  • the glue material is PSA glue material or PMMA glue material.
  • the metal dot nanorod material and the glue material are mixed after being heated and melted.
  • the metal dot nanorod material is mixed with a polymer, and then UV-cured after spreading.
  • the present invention also provides an LCD module, comprising a backlight film, and the backlight film is made of the aforementioned optically active material.
  • the invention constructs metal point nanorods, has excellent fluorescence performance, good optical activity, low metal point toxicity, simple synthesis, stable material, can be mass-produced, and is especially suitable for commercial application.
  • Anisotropic growth makes it have better optical rotation. It is used for LCD backlight film, which greatly improves the light utilization rate, improves the brightness of the display screen, reduces energy consumption, and becomes a favorable replacement material for the backlight of a new generation of display screens.
  • Fig. 1 is the preparation process schematic diagram of metal nanorods
  • Fig. 2 is the luminescence spectrum of metal dot nanorods of different sizes
  • Fig. 3 is the optical rotation schematic diagram of metal dot nanorod
  • FIG. 4 is a schematic diagram of a film material of a metal dot nanorod optically active material
  • FIG. 5 is a structural comparison diagram of an LCD module
  • 5(a) is an LCD module with a lower polarizer
  • 5(b) is an LCD module using an optically active material backlight film.
  • the optically active material is used as the backlight luminescent material, which reduces the loss of 50% of the polarization effect of the lower polarizer on the incident light, greatly improves the light utilization rate of the backlight, and reduces the energy loss. , enhance light efficiency and reduce costs.
  • the invention comprises a one-pot method for preparing metal dot nanorods (usually ⁇ 1000 nm) of different sizes, preparing the metal dot nanorods into a backlight film, and integrating the backlight film in a backlight LCD module.
  • metal dot nanorods usually ⁇ 1000 nm
  • the light utilization rate of the backlight is improved, and the excitation light intensity is 100% used, which improves the light utilization rate and the display brightness, especially the large-size TV brightness can be greatly improved.
  • the metal salt is dissolved in a solvent, an alkyl acid and a ligand are added, and a metal dot nanorod material is prepared by a water bath one-pot method.
  • the metal salt used is at least one of copper salt, gold salt, silver salt, platinum salt, iron salt, zinc salt, nickel salt and cobalt salt, and the metal salt can be used alone or mixed and added.
  • the solvent used is at least one in ethanol, toluene, paraffin, dibenzyl ether, dimethylformamide (DMF), dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), and the solvent can be used alone, or Can be mixed and added.
  • the metal salt is dissolved in the solvent to form a reaction bottom liquid of 0.01M-0.5M, and the preferred concentration range is 0.05-0.2M.
  • auxiliary means such as ultrasound and stirring can be used to promote the dissolution of the metal salt to form the reaction bottom liquid.
  • the metal salt can be copper chloride, chloroauric acid, silver nitrate, copper nitrate, copper acetate, copper acetylacetonate, copper sulfate, ferric chloride, ferric nitrate, chloride One of zinc, zinc nitrate, platinum chloride, nickel chloride, cobalt acetate and silver acetate.
  • Citric acid can also be substituted with amino acids such as serine and tryptophan.
  • the ligand is at least one of POSS, POSS in which the amino group is substituted by a thiol group, and a POSS derivative.
  • the molar ratio of the ligand to the metal salt is 5:1 to 10:1.
  • the fluorescence is blue, green, and red, respectively.
  • the luminescence spectra of metal dot nanorods of different sizes are shown in Figure 2. And among the metal nanoparticles of the same scale, the luminescence peak position is further controllable with the change of the metal species.
  • the material Due to the anisotropy of the metal dot nanorods, the material has optically active properties, which can emit polarized light under ultraviolet excitation, as shown in Figure 3. Therefore, the lower polarizer filter is no longer needed when used for LCD backlighting.
  • the optically active material is obtained by mixing the metal dot nanorod material with the glue material, and spin coating and spreading.
  • the adhesive material used is polymethyl methacrylate (PMMA) adhesive material or pressure sensitive adhesive (PSA) adhesive material.
  • PMMA polymethyl methacrylate
  • PSA pressure sensitive adhesive
  • the method of mixing the metal dot nanorod material with the glue material includes, but is not limited to, hot-melt method and ultraviolet curing method.
  • the general process of the hot-melting method includes: the metal dot nanorod material and the glue material are mixed after heating and melting, and the spreading method is preferably spin coating, which is convenient for forming.
  • the general process of the ultraviolet curing method includes: mixing the metal dot nanorods with the polymer monomer, and then performing ultraviolet curing after spreading to obtain the photosensitizing material.
  • the polymer monomers are multifunctional monomers, mainly polyhydric alcohol acrylates.
  • the spreading method is preferably spin coating spreading, which is convenient for UV curing.
  • 5(a) is an LCD module with a lower polarizer
  • 5(b) is an LCD module using an optically active material backlight film.
  • the backlight film emits polarized light under ultraviolet excitation, so the entire LCD backlight does not need a lower polarizer to filter light.
  • This patent constructs metal dot nanorods, which have excellent fluorescence properties, good optical activity, low metal dot toxicity, simple synthesis, stable materials, mass production, and are especially suitable for commercial applications.
  • Anisotropic growth makes it have better optical rotation. It is used for LCD backlight film, which greatly improves the light utilization rate, improves the brightness of the display screen, reduces energy consumption, and becomes a favorable replacement material for the backlight of a new generation of display screens.

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  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • Mathematical Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Liquid Crystal (AREA)

Abstract

一种旋光材料的制备方法，包括如下步骤：S1.金属点纳米棒的制备：将金属盐溶于溶剂，加入烷基酸和配体，水浴一锅法制备得到金属点纳米棒材料；S2.与胶材复合：将所述金属点纳米棒材料与胶材混合，旋涂铺开后即得所述旋光材料。将金属点纳米棒制备成背光膜片，将背光膜片集成在背光LCD模组中。利用金属点纳米棒的旋光性能，将背光的光利用率提升，激发光强度100％利用上，提升了光利用率，提升了显示亮度，成为新一代显示屏背光的有利取代材料。

Description

一种旋光材料的制备方法及应用 技术领域
本发明涉及背光发光材料领域，具体涉及一种旋光材料的制备方法及应用。
背景技术
LCD显示屏一般采用白背光以及三色彩色滤光片作为色彩显示的机制，控制色彩灰度时需要通过上下偏光片对入射光做旋光处理，但是此时的入射光在通过下偏光片时强度直接损失50％，并且再经过各膜层之后的损失更严重，最后出光率不足5％，导致LCD显示屏的亮度一直是领域内的棘手问题。尤其是现在大屏高清显示需求，分辨率不断提升，开口率逐渐下降，如何提升亮度是各企业尤为关注的焦点。
目前已有的解决方案为量子点纳米棒作为背光膜片，由于各向异性的棒材具有旋光性，所以入射光不需要经过下偏的旋光处理，光强没有损失，极大的提亮了LCD显示屏的亮度，但是由于量子点内含有铅、汞等毒性元素，历来被业界及买家所诟病。
发明内容
针对量子点纳米棒材料以上诸多不足，本发明提供一种旋光材料的制备方法及应用。
本发明的技术方案通过如下方式实现：提供一种旋光材料的制备方法，包括如下步骤：
S1.金属点纳米棒的制备：将金属盐溶于溶剂，加入烷基酸和配体，水浴一锅法制备得到金属点纳米棒材料；
S2.与胶材复合：将所述金属点纳米棒材料与胶材混合，旋涂铺开后即得所述旋光材料。
在本发明一个优选实施例中，所述步骤S1中，所述金属盐为铜盐、金盐、银盐、铂盐、铁盐、锌盐、镍盐、钴盐中的至少一种；所述溶剂为乙醇、甲苯、 石蜡、二卞醚、二甲基甲酰胺、二甲基亚砜、四氢呋喃中的至少一种。
在本发明一个优选实施例中，所述步骤S1中，所述烷基酸为柠檬酸、丝氨酸、色氨酸中的至少一种。
在本发明一个优选实施例中，所述步骤S1中，所述配体为POSS、氨基被巯基取代的POSS、POSS衍生物中的至少一种。
在本发明一个优选实施例中，所述步骤S1中，配体与金属盐的摩尔比为5：1～10：1。
在本发明一个优选实施例中，所述步骤S2中，胶材为PSA胶材或者PMMA胶材。
在本发明一个优选实施例中，所述步骤S2中，所述金属点纳米棒材料与所述胶材，加热融化后混合。
在本发明一个优选实施例中，所述步骤S2中，将所述金属点纳米棒材料与聚合物混合，铺开后进行紫外光固化。
本发明还提供一种LCD模组，包括背光膜片，所述背光膜片使用前述旋光材料制成。
有益效果如下：
本发明构筑了金属点纳米棒，荧光性能优异，旋光性好，且金属点毒性低，合成简易，材料稳定，可批量生产，特别适宜商业化应用，通过亲疏水配体的选择，控制纳米点各向异性生长，使其具有较好的旋光性，用于LCD背光膜片，大大提升了光利用率，提升显示屏亮度，降低能耗，成为新一代显示屏背光的有利取代材料。
附图说明
图1为金属纳米棒的制备过程示意图；
图2为不同尺寸金属点纳米棒的发光光谱；
图3为金属点纳米棒的旋光性示意图；
图4为金属点纳米棒旋光材料的膜材示意图；
图5为LCD模组结构对比图，5(a)为具有下偏振片的LCD模组，5(b)为使用旋光材料背光膜片的LCD模组。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合本发明具体实施例及相应的附图对本发明技术方案进行清楚、完整地描述。显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
下面结合附图和实施例对本发明进一步详细的说明。
为了提升LCD显示屏亮度，从光利用率入手，采用旋光材料作为背光发光材料，这样减少下偏振片对入射光做偏振效应50％的损失，大大提高了背光的光利用率，减少能耗损失，增强光效，降低成本。
本发明包含一锅法制备不同尺寸金属点纳米棒(通常<1000nm)，将金属点纳米棒制备成背光膜片，将背光膜片集成在背光LCD模组中。利用金属点纳米棒的旋光性能，将背光的光利用率提升，激发光强度100％利用上，提升了光利用率，提升了显示亮度，特别可以使大尺寸TV亮度大幅提升。其详细的制备方法如下：
1.不同尺寸金属点纳米棒的制备
将金属盐溶于溶剂，加入烷基酸和配体，水浴一锅法制备得到金属点纳米棒材料。
使用的金属盐为铜盐、金盐、银盐、铂盐、铁盐、锌盐、镍盐、钴盐中的至少一种，金属盐可以一种单独使用，也可以混合添加。使用的溶剂为乙醇、甲苯、石蜡、二卞醚、二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)、四氢呋喃(THF)中的至少一种，溶剂可以一种单独使用，也可以混合添加。金属盐溶于溶剂形成0.01M～0.5M的反应底液，优选浓度范围0.05～0.2M，反应底液制备过程中可以使用超声、搅拌等辅助手段，促进金属盐的溶解形成反应底液。
反应底液中随后加入柠檬酸和配体，配体与金属盐的摩尔比为5：1～10：1，水浴50-120℃一锅法搅拌10～40min即可得到不同尺寸不同金属中心的金属点纳米棒材料(制备路径如图1)，金属盐可以是氯化铜、氯金酸、硝酸银、硝酸铜、醋酸铜、乙酰丙酮铜、硫酸铜、氯化铁、硝酸铁、氯化锌、硝酸锌、氯化铂、氯化镍、醋酸钴、醋酸银其中的一种。柠檬酸也可以被丝氨酸、色氨酸等氨基酸取代。配体为POSS、氨基被巯基取代的POSS、POSS衍生物中的至少一种。
上述金属点的制备过程中，比较重要的是通过改变配体的比例可以改变棒材的尺寸，配体与金属盐的摩尔比为5：1～10：1。例如，柠檬酸：POSS＝1:5、1:10、1:20可以分别得到长度为50纳米、100纳米、200纳米的金属棒。365纳米激发下，其荧光分别为蓝光、绿光、红光。不同尺寸金属点纳米棒的发光光谱如图2所示。且其中同一种尺度的金属纳米粒子随着金属种类的变化，发光峰位进一步可控。
2.金属点纳米棒背光膜片制备
由于金属点纳米棒的各向异性使材料具有旋光性能，可以在紫外激发下发出偏振光，如图3。所以用于LCD背光时不再需要下偏振片滤光。
将所述金属点纳米棒材料与胶材混合，旋涂铺开后即得所述旋光材料。使用的胶材为聚甲基丙烯酸甲酯(PMMA)胶材或者压敏胶(PSA)胶材。金属点纳米棒材料与胶材混合的方法包括但不限于热融法、紫外固化法。
热融法的大体过程包括：金属点纳米棒材料与胶材，加热融化后混合，铺开的方式优选旋涂铺开，便于成型。
紫外固化法的大体过程包括：将金属点纳米棒与聚合物单体混合，铺开后进行紫外光固化，即得所述光敏化材料。聚合物单体为多官能基单体，主要是多羟基醇丙烯酸酯。铺开的方式优选旋涂铺开，便于紫外固化。
3.含金属点纳米棒的背光LCD模组
将背光膜片集成在背光架构里并组成模组，如图5所示。5(a)为具有下偏振片的LCD模组，5(b)为使用旋光材料背光膜片的LCD模组。该背光膜片在紫外激发下发出偏振光，所以整个LCD背光时不再需要下偏振片滤光。
本专利构筑了金属点纳米棒，荧光性能优异，旋光性好，且金属点毒性低，合成简易，材料稳定，可批量生产，特别适宜商业化应用，通过亲疏水配体的选择，控制纳米点各向异性生长，使其具有较好的旋光性，用于LCD背光膜片，大大提升了光利用率，提升显示屏亮度，降低能耗，成为新一代显示屏背光的有利取代材料。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。

Claims (9)

  1. 一种旋光材料的制备方法，其特征在于，包括如下步骤：
    S1.金属点纳米棒的制备：将金属盐溶于溶剂，加入烷基酸和配体，水浴一锅法制备得到金属点纳米棒材料；
    S2.与胶材复合：将所述金属点纳米棒材料与胶材混合，旋涂铺开后即得所述旋光材料。
  2. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S1中，所述金属盐为铜盐、金盐、银盐、铂盐、铁盐、锌盐、镍盐、钴盐中的至少一种；所述溶剂为乙醇、甲苯、石蜡、二卞醚、二甲基甲酰胺、二甲基亚砜、四氢呋喃中的至少一种。
  3. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S1中，所述烷基酸为柠檬酸、丝氨酸、色氨酸中的至少一种。
  4. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S1中，所述配体为POSS、氨基被巯基取代的POSS、POSS衍生物中的至少一种。
  5. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S1中，配体与金属盐的摩尔比为5：1～10：1。
  6. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S2中，胶材为PSA胶材或者PMMA胶材。
  7. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S2中，所述金属点纳米棒材料与所述胶材，加热融化后混合。
  8. 根据权利要求1所述的旋光材料的制备方法，其特征在于，所述步骤S2中，将所述金属点纳米棒材料与聚合物混合，铺开后进行紫外光固化。
  9. 一种LCD模组，其特征在于，包括背光膜片，所述背光膜片使用权利要求1-8中旋光材料制成。
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