CN116925638A - 一种纳米复合彩色滤光涂层液和滤光片的制备方法 - Google Patents
一种纳米复合彩色滤光涂层液和滤光片的制备方法 Download PDFInfo
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- CN116925638A CN116925638A CN202310690506.9A CN202310690506A CN116925638A CN 116925638 A CN116925638 A CN 116925638A CN 202310690506 A CN202310690506 A CN 202310690506A CN 116925638 A CN116925638 A CN 116925638A
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- selenide
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- metal oxide
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
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- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01G51/04—Oxides; Hydroxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/2272—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Optical Filters (AREA)
Abstract
一种纳米复合彩色滤光涂层液和滤光片的制备方法,涂层液包含A、B组分,A组分原料包括:70~90%聚氨酯丙烯酸酯预聚物;0~5.5%核壳型金属硒化物纳米粒子;0~5.5%核壳型金属氧化物纳米粒子;9.5~19%活性稀释剂;0.1~1%消泡剂;B组分为0.4~4%光引发剂。通过二异氰酸酯与二元醇和羟基丙烯酸酯的加聚反应,得到聚氨酯丙烯酸酯嵌段共聚物,然后再与具有特定光谱功能的纳米材料复合,在聚合物结构中引入反应性基团和金属硒化物、金属氧化物纳米粒子,利用不同纳米粒子在聚氨酯丙烯酸酯树脂中的光谱特性,可选择性透过所需波段光谱来精确调控滤光和颜色,具有滤光效果优异、光谱截击准确、色牢度高、抗老化性能好和色彩丰富的特点。
Description
技术领域
本发明属于滤光材料技术领域,具体涉及能精确调控滤光波段和涂层颜色的功能性滤光涂层液和滤光片的制备方法。
背景技术
纳米复合滤光材料,是光防控领域内具有优异光学性质和特殊功能的新材料,是用来选取所需辐射波段的一种光学元器件。广泛应用于激光器、传感器、滤波器、3D扫描、智能驾驶、生物医疗、荧光分析、生物识别、安防监控、激光雷达、航空航天、监控系统、红外相机、机器视觉、窗口材料和夜视仪等光学领域。滤光材料常用的有亚克力和光学玻璃,其制作工艺和物理性能差别比较大。亚克力滤光片一般是通过浇筑或者挤压的工艺在生产的过程中加入不同配比的颗粒料,使其具有不同的颜色透光效果,比如,通过红光、通过绿光等滤光片;玻璃滤光片通常是通过在光学玻璃表面镀膜来干涉镜片的透光属性,从而使特定波长透过或者截止,波长范围选择也更广泛,从紫外线到可见光、近红外、中远红外都可制作。
现有滤光片的常规制造技术包括印染色、高温掺杂和电泳沉积(EPD):(1)塑料片染色形成的滤光技术:把制造准确尺寸的塑料片经有机染料的热水中煮浮或通过染料与高分子粒子材料加温共混,颜色根据波段来选择。其不足是由于使用染色技术,滤光片的透光率较差,波谱带分布宽。(2)玻璃片掺杂金属氧化物形成的滤光技术,通过在玻璃中掺杂金属氧化物而成,根据不同滤光波段的要求,按照分量掺杂氧化钴、氧化铜制造蓝玻璃,掺杂氧化铁等过渡金属氧化物制造红色滤光玻璃。这种方法的不足之处耗能高、环境污染比较严重。(3)白片镀膜形成的滤光技术,通过镀膜沉积的方法设计截取波段范围,波谱带分布窄,但产品成本高,不良率高,大规模生产受到一定限制。
发明内容
针对现有技术的上述问题,本发明提供一种纳米复合彩色滤光涂层液的制备方法,通过二异氰酸酯与二元醇和羟基丙烯酸酯的加聚反应,得到聚氨酯丙烯酸酯嵌段共聚物,然后与具有特定光谱功能的纳米材料进行精细复配,在聚合物结构中引入反应性基团和金属硒化物、金属氧化物纳米粒子,利用不同纳米粒子在聚氨酯丙烯酸酯树脂中的光谱特性,可选择性透过或截止特定波段光谱来精确调控滤光和颜色,具有滤光效果优异、光谱截击准确、耐洗色牢度高、抗老化性能好和色彩丰富的特点,可用于多种不同材料基材,为滤光产品的应用提供更广泛的材料选择范围。
为实现上述目的,本发明提供如下技术方案:
一种纳米复合彩色滤光涂层液的制备方法,该方法包括如下步骤:
I.配置纳米复合彩色滤光涂层液:
A组分:
70~90%聚氨酯丙烯酸酯预聚物;
0~5.5%核壳型金属硒化物纳米粒子;
0~5.5%核壳型金属氧化物纳米粒子;
9.5~19%活性稀释剂;
0.1~1%消泡剂;
其中,核壳型金属硒化物粒子和核壳型金属氧化物粒子的总量为(0.5~5.5)%;
该聚氨酯丙烯酸酯预聚物是将二异氰酸酯和聚酯多元醇进行加成反应,再用羟基丙烯酸酯进行封端制得;
该核壳型金属硒化物纳米粒子的内核为金属硒化物,外壳为表面活性剂,内核与外壳的质量比为1∶(0.1~0.3),核壳型金属硒化物纳米粒子的粒径为3~10nm;
该核壳型金属氧化物粒子的内核为金属氧化物,外壳为表面活性剂,内核与外壳的质量比为1∶(0.1~0.5),核壳型金属氧化物纳米粒子的粒径4~10nm;
将核壳型金属硒化物纳米粒子和核壳型金属氧化物纳米粒子溶解于活性稀释剂中,搅拌下加入到聚氨酯丙烯酸酯预聚物中,随后加入消泡剂,得到A组分;
B组分:
0.4~4%光引发剂;
II.涂布前将A组分和B组分混合,超声搅拌5-10min,使A组分与B组分完全溶解,得到所需的彩色滤光涂层液。
如上所述的制备方法,优选地,所述金属硒化物为硒化镉、硒化锌、硒化铜、硒化钡、硒化铟和硒化锆中的至少一种;
如上所述的制备方法,优选地,所述金属氧化物为氧化镉、氧化锌、氧化铜、氧化钴、氧化铟、氧化铁、氧化铒、氧化锰、氧化钛和氧化钡中的至少一种;
如上所述的制备方法,优选地,所述核壳型金属硒化物粒子的表面活性剂为:月桂酰两性醋酸钠、月桂醇硫酸钠、月桂酰谷氨酸和脂肪醇聚氧乙烯醚中的至少一种;
如上所述的制备方法,优选地,所述核壳型金属氧化物粒子的表面活性剂为:硬脂酸、烷基葡糖苷、十二烷基苯磺酸钠、脂肪酸甘油酯和聚山梨酯中的至少一种。
如上所述的制备方法,优选地,所述活性稀释剂为苄基丙烯酸酯、乙氧基苯酚丙烯酸酯、联苯甲醇丙烯酸酯、邻苯基苯氧乙基丙烯酸酯、1,6-己二醇二丙烯酸酯、季戊四醇三丙烯酸酯或三羟甲基丙烷三丙烯酸酯中的至少一种;
如上所述的制备方法,优选地,所述消泡剂为T-1000A型消泡剂、DS100硅油性消泡剂、AT350聚醚型消泡剂和D90丙烯酸聚合型消泡剂中的至少一种;
如上所述的制备方法,优选地,所述光引发剂为自由基聚合光引发剂;更优选地,所述光引发剂选自:2-羟基-2-甲基-1-苯基丙酮(1173)、1-羟基环己基苯基甲酮(184)、2,2-二甲基-1-苯基-1-丙酮、2,4,6-三甲基苯甲酰基苯基膦酸乙酯(TPO-L)、2-二甲氨基-2-苄基-1-丁酮、2-羟基-2-甲基-1-丙酮和2,4,6-三甲基苯甲酰基-二苯基氧化膦(TPO);更优选地,所述光引发剂为2-羟基-2-甲基-1-苯基丙酮。
如上所述的制备方法,优选地,所述二异氰酸酯选自甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六亚甲基二异氰酸酯和/或赖氨酸二异氰酸酯;
所述聚酯多元醇选自聚己内酯二醇、聚己二酸乙二醇、苯酐聚酯二元醇和/或聚碳酸酯二醇;
如上所述的制备方法,优选地,所述羟基丙烯酸酯选自丙烯酸羟乙酯、丙烯酸羟丙酯和/或甲基丙烯酸羟乙酯。
如上所述的制备方法,优选地,所述聚氨酯丙烯酸酯预聚物采用如下方法制备:将聚酯二元醇加入到反应容器中,加入二异氰酸酯和溶剂,然后缓慢滴入二月桂酸二丁基锡催化剂,N2保护,温度控制在65-80℃反应60-90min,再加入羟基丙烯酸酯和扩链剂,降温到40-60℃,反应2-6h内取样检测-NCO含量,当检测到红外光谱2230~2240cm-1处-NCO的伸缩振动吸收峰消失,表明-NCO已经和-OH反应完全,即得到式I所示的聚氨酯丙烯酸酯预聚物;其中,羟基丙烯酸酯、二异氰酸酯、聚酯二元醇三者质量比为(1-3)∶(2-5)∶(8-10),聚酯多元醇与溶剂质量比为1∶(9-30)。
如上所述的制备方法,优选地,所述方法用于制备红色滤光涂层液,其中,所述金属硒化物为CdSe,所述金属氧化物为CoO;CdSe与CoO的质量比为4∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备红色滤光涂层液,其中,所述金属硒化物为CdSe和ZnSe,所述金属氧化物为Fe2O3;CdSe、ZnSe、Fe2O3三者的质量比为4∶(1~2)∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备蓝色滤光涂层液,其中,所述金属硒化物为CuSe,所述金属氧化物为CuO,CuSe,与CuO的质量比为3∶(3~7);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备紫色滤光涂层液,其中,所述金属硒化物为CdSe,所述氧化物为CoO和Fe2O3;CdSe、CoO、Fe2O3三者的质量比为1∶(3~5)∶(2~3);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备黄色滤光涂层液,其中,所述金属硒化物为ZnSe和BaSe,所述金属氧化物为TiO2;ZnSe、BaSe、TiO2三者的质量比为(2~3)∶1∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备绿色滤光涂层液,其中,所述金属硒化物为CuSe,所述金属氧化物为MnO2;CuSe与MnO2的质量比为1∶(3~7);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备青黄色滤光涂层液,其中,所述金属硒化物为ZnSe,所述金属氧化物为TiO2和MnO2;ZnSe、TiO2、MnO2三者的质量比为(1~2)∶1∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
如上所述的制备方法,优选地,所述方法用于制备蓝绿色色滤光涂层液,其中,所述金属硒化物为InSe,所述氧化物为MnO2;InSe与MnO2的质量比为(1~2)∶1;核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
另一方面,本发明提供一种纳米复合彩色滤光片的制备方法,所述方法用于包括如下步骤:采用如上所述的方法制备滤光涂层液,将涂层液经孔径0.1~10μm滤膜过滤脱气后,以2000~3000转/分钟速度旋涂到滤光片基材表面,然后将涂层片置于光照强度为160~300mW/cm2的UV-LED光固化机下照射20~50S,涂层完全固化得到彩色滤光片。
本发明的聚氨酯丙烯酸酯预聚物的制备方法是:将聚酯多元醇和二异氰酸酯进行反应,通过催化剂控制反应速率,再用丙烯酸羟乙酯(HEA)进行封端。
在本发明的优选实施方式中,采用了以下两种聚氨酯丙烯酸酯预聚物,并提供其制备方法,具体反应式如下:
1.聚氨酯丙烯酸酯预聚物(PUA-1)合成反应
其中,n为1~2500的整数。
2.聚氨酯丙烯酸酯预聚物(PUA-2)合成反应
聚氨酯丙烯酸酯(PUA)的合成是一个剧烈放热的过程,粘度增加较快,若体系粘度过大,则热量难以及时散发,会导致体系爆聚,因此,合成过程中通过加入溶剂来代替阻聚剂,一方面降低体系粘度,帮助热量及时散发,规避双键长时间的热聚合,防止自聚,另一方面,避免阻聚剂延长光固化时间的不利影响。
在本发明的优选实施方式中,所述核壳型金属硒化物纳米粒子采用如下方法制备:
a.将硼氢化钠加入到去离子水中,氮气保护,溶解后加入硒粉,硼氢化钠与硒粉的质量比为1∶(0.1~0.5),磁力搅拌反应至变成无色透明含硒溶液,溶液中硒的含量为(3~8)wt%;
b.将可溶性金属盐溶于去离子水中,滴加碱溶液调节PH值至9-11,然后氮气保护,得金属盐溶液,溶液中金属盐的浓度为(5~20)wt%;
c.把步骤a中制备的含硒溶液迅速加入到金属盐溶液中,搅拌加入相转移剂和表面活性剂,溶液中的硒、金属盐、相转移剂、表面活性剂的质量比为1∶(1.5~3.5)∶(0.1~0.3)∶(1.5~3),将该混合溶液加热回流1.5~4.5小时,得到硒化物纳米晶溶液;
d.用沉淀剂对制备好的硒化物纳米晶溶液进行沉淀,沉淀剂与步骤a硒粉的质量比为1∶(0.6~2),然后用去离子水和乙醇为洗涤剂进行洗涤、离心分离后,在恒温干燥箱内干燥得核壳型硒化物纳米晶粉末。
如上所述的制备方法,优选地,所述可溶性金属盐为氯化镉、氯化锌、氯化铜、氯化钴、氯化铟、氯化钡、醋酸镉、醋酸锌、醋酸铜、醋酸钴、醋酸钡或醋酸铟;
所述相转移剂选自醋酸钠、硫酸钠、氨水和山梨糖醇酐脂肪酸酯中的至少一种;
所述表面活性剂选自月桂酰两性醋酸钠、月桂醇硫酸钠、月桂酰谷氨酸和脂肪醇聚氧乙烯醚中的至少一种;
所述沉淀剂选自丙酮、甲基乙基酮、苯、乙酸乙酯和乙酸丁酯中的至少一种。
在本发明的优选实施方式中,所述核壳型金属氧化物纳米粒子采用如下方法制备:
将金属盐溶于去离子水中,配制成浓度为10-4~10mol/L的金属盐溶液;向金属盐溶液中加入表面活性剂水溶液和模板剂,金属盐、表面活性剂和模板剂的质量比为1∶(0.2~0.5)∶(0.03~0.1),搅拌30~120分钟,形成以金属氧化物纳米粒晶粒为核,以表面活性剂为壳的纳米粒子;再经脱水、烘干、得核壳型金属氧化物纳米粒子。
如上所述的制备方法,优选地,所述可溶性金属盐为金属镉、锌、铜、钴、铟、铁、铒、锰、钛和钡的可溶性金属盐;
所述表面活性剂选自硬脂酸、烷基葡糖苷、十二烷基苯磺酸钠、脂肪酸甘油酯和聚山梨酯中的至少一种;
所述模板剂能通过分子间的弱相互作用来维系模板作用力,从而精确控制纳米材料的尺寸与聚集,优选乙二胺和正丁胺等。
本发明的彩色滤光涂层液形成的滤光涂层由聚氨酯丙烯酸酯聚合物、核壳型金属硒化物纳米粒子和核壳型金属氧化物纳米粒子组成。纳米粒子的表面活性剂外壳使金属硒化物/金属氧化物在PUA中具有良好的分散性和融合度,同时表面活性剂与PUA、金属硒化物、金属氧化物协同实现特定区域光波的吸收。小于10纳米尺寸的硒化物和氧化物纳米粒子在具有特征滤光特性的同时,可以保证涂层良好的透光率。
聚氨酯丙烯酸酯预聚物具有聚酯多元醇形成的柔性链断,使聚合后的涂层软硬适度,且聚合前后伸缩率很小,适应各种滤光基片材料。预聚物的两端为丙烯酸羟乙酯(HEA)封端,端位的双键可作为光聚合反应位点。
本发明的有益效果在于:
(1)本发明的纳米复合彩色滤光涂层液组分中的无机纳米粒子通过复配,能使吸收谱线发生迁移,具有选择性透过或截止特定波长光谱的功能,所制滤光片色彩鲜艳、颜色丰富、色牢度高。
(2)本发明的纳米复合彩色滤光涂层液主体聚合物分子中含有三种化学结构的链段:二异氰酸酯形成的氨基甲酸酯嵌段,多元醇形成的主链和丙烯酸羟烷酯形成的链端。其中丙烯酸官能团透明度和透光率高,氨基甲酸酯粘附力和柔顺性好,对不同基材具有良好的附着力,与无机纳米粒子精细复合后也不影响涂层的牢固度,不会发生涂层剥离和龟裂。
(3)本发明的纳米复合彩色滤光涂层液组分中的无机纳米粒子通过简单的反应条件就可以制得,材料组成和制备工艺简便,这在一定程度上降低了应用的成本,制品集成不良率低。
附图说明
图1为具体实施方式中制备的CdSe纳米晶透射电子显微镜照片。
图2为具体实施方式中制备的CdSe纳米颗粒XRD图谱。
图3为实施例1制备的聚氨酯丙烯酸酯(PUA-1)红外光谱图。
图4为实施例5制备的聚氨酯丙烯酸酯(PUA-2)红外光谱图。
图5为不同含量CdSe纳米粒子在聚氨酯丙烯酸甲酯中的透过率光谱图。
图6为不同含量氧化铁纳米粒子在聚氨酯丙烯酸甲酯中的透过率光谱图。
图7为实施例1制备的滤光片透过率光谱图。
图8为实施例3制备的滤光片透过率光谱图。
图9为实施例4制备的滤光片透过率光谱图。
图10为实施例5制备的滤光片透过率光谱图。
图11为实施例6制备的滤光片透过率光谱图。
图12为实施例7制备的滤光片透过率光谱图。
图13为实施例8制备的滤光片透过率光谱图。
图14为实施例4制备的滤光片吸收光谱曲线图。
图15为实施例8制备的滤光片吸收光谱曲线图。
图16为具体实施方式中制备的氧化钴纳米晶透射电子显微镜照片。
图17为具体实施方式中制备的氧化钴纳米颗粒XRD图谱。
具体实施方式
下面通过具体实施例对本发明作进一步说明,但并不意味着对本发明保护范围的限制。
一、以下各实施例中的纳米硒化物是采用以下方法制备:
(1)制备核壳型硒化镉纳米粒子:
将420g硼氢化钠加入到1100g去离子水中,氮气保护,溶解后加入60g硒粉,磁力搅拌反应至无气泡产生,得无色透明含硒溶液;取140g氯化镉加入到盛有850g去离子水的反应容器中,滴加20%氢氧化钠碱溶液调节PH值至11,得含镉溶液;将无色透明含硒溶液加入到含镉溶液中,搅拌后加入9.5g山梨糖醇酐脂肪酸酯和135g月桂酰谷氨酸,将该溶液加热90℃并回流2.5小时;加入丙酮使CdSe出现絮状沉淀,分离、洗涤、干燥,得到核壳型CdSe纳米晶(PX01)。
将获得的核壳型CdSe纳米晶PX01用JEM-2100型透射电子显微镜观察,见图1,可见外观形貌呈立方晶的球形,所得纳米晶尺寸均匀,单分散性好,通过谢乐公式(D=K/βcosθ)和Zeta电位分析计算,得出CdSe纳米晶粒径约为4.6nm。
对制备的CdSe纳米晶进行XRD的测试,采用X射线衍射仪,结果如图2所示。观察到CdSe的强衍射峰在10-70°的2θ(衍射角)范围内,出现了3个主要衍射峰,峰位分别位于2θ≈25.3°、42.0°和49.6°,分别对应于立方相CdSe的(111)、(220)和(311)晶面,其中(111)方向上的衍射峰特别强。这些特征峰与CdSe纳米球所具有的衍射峰能够一一对应,且和标准卡片(JCPDS NO.65-2891)一致,表明样品CdSe具有立方晶体结构。
(2)制备其它核壳型硒化物纳米粒子:
采用上述同样方法,只是将氯化镉更换成等摩尔的其它金属氯化物,制备得核壳型ZnSe纳米晶(PX02)、CuSe纳米晶(PX03)、BaSe纳米晶(PX04)和InSe纳米晶(PX05)。
二、以下各实施例中的纳米氧化物是采用以下方法制备:
(1)制备核壳型氧化钴纳米粒子:
配制浓度为0.8mol/L亚硫酸钴的水溶液1850mL,搅拌中加入95mL浓度为1.8mol/L的表面活性剂十二烷基苯磺酸钠水溶液和12mL模板剂正丁胺。搅拌数分钟即有纳米粒子生成。经分离脱水烘干,得到核壳型CoO纳米晶(PS01)。
将获得的核壳型CoO纳米晶PS01用JEM-2100型透射电子显微镜观察,见图16,可见外观形貌为类球形,所得纳米晶尺寸均匀,通过谢乐公式(D=K/β cos θ)和Zeta电位分析计算,得出CoO纳米晶粒径约为6.6nm。
对制备的CoO纳米晶进行XRD的测试,采用X射线衍射仪,见图17,在2θ为19.0°、31.3°、36.8°、38.5°、44.8°、55.7°、59.4°和65.2°的位置处出现的特征衍射峰分别对应着CoO的(111)、(220)、(311)、(222)、(400)、(422)、(511)和(440)晶面,从而确定CoO为尖晶石结构。
(2)制备其它核壳型氧化物纳米粒子:
采用上述同样方法,只是将亚硫酸钴更换成等摩尔的其它难溶金属盐,制备得到核壳型CuO纳米晶(PS02)、Fe2O3纳米晶(PS03)、Er2O3纳米晶(PS04)、TiO2纳米晶(PS05)和MnO纳米晶(PS06)。
三、确定滤光片透过或截止波长范围
根据滤光光谱波段和光谱特性,从紫外线、可见光和红外线不同波段光谱进行分类,选定波段的光通过,通带以外的光截止。详见表一、表二。
表一不同波长滤光片透射设计
表二激光波长防护设计
四、纳米复合材料滤光功能设计与色度确认
确定并掌握硒化物、氧化物等不同无机纳米材料在树脂中的光谱特性以及颜色,选用2%含量纳米粒子胶体,将胶体涂覆到PC光学基材表面,对固化涂层进行测定,详见表三;发现纳米材料在树脂单体中含量与光谱谱线的红移关系;不同纳米材料在树脂单体中复配与光谱谱线的透射关系,通过对滤光涂层功能进行设计与色度匹配,得到所需彩色滤光片。图5为不同含量CdSe纳米粒子在聚氨酯丙烯酸酯中的涂层透过率光谱图,图6为不同含量氧化铁纳米粒子在聚氨酯丙烯酸酯中的涂层透过率光谱图。从图中可以看出,纳米粒子在树脂中的浓度影响吸收波段和吸收强度。
表三纳米复合涂层光谱特性
实施例1:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-1):
(1)向850g聚己二酸乙二醇中加入450g甲苯二异氰酸酯(TDI)和9Kg乙酸乙酯溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温65℃反应85min,依次加入15g1,4-丁二醇、12g3-甲基-1,5-戊二醇反应90min,再加入230g丙烯酸羟乙酯(HEA),降温到50℃,反应5小时8分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-1。
(2)上述步骤(1)制备的聚氨酯丙烯酸酯预聚物(PUA-1)进行了傅里叶变换红外光谱(FT-IR)测试,扫描范围:4000-500cm-1,从图3曲线分析可知,产物PUA-1在-NCO的吸收峰和-OH的伸缩振动峰消失,而在1740cm-1处出现了-C=O的吸收峰,在3325cm-1处出现了少量的-CO-NH-的伸缩振动吸收峰,1640cm-1处保留-C=C-的伸缩振动特征吸收峰。红外光谱的结果表明,羟基与异氰酸酯基反应,产生酯基,引入可供聚合基团碳碳双键。
(二)制备红色滤光涂层及滤光片
(1)取PX01(CdSe)1.2g和0.4gPS01(CoO)加入到4g苄基丙烯酸酯中,搅拌35分钟均匀分散并加入到上述步骤制备的40gPUA-1中,加入0.2gD90消泡剂,得到A组分。
(2)称取1.2g2-羟基-2-甲基-1-苯基丙酮1173加入到上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学PC基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射36S,涂层完全固化。滤光片透过率光谱图如图7所示,滤光片吸收紫外线和部分可见光,透过640-1250nm波长范围红光和近红外。
实施例2:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-1):
(1)向900g聚己二酸乙二醇中加入450g甲苯二异氰酸酯(TDI)和9Kg乙酸乙酯溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入13g1,4-丁二醇、10g3-甲基-1,5-戊二醇反应90min,再加入185g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时55分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-1。
(二)制备深红色滤光涂层及滤光片
(1)取PX01(CdSe)1.2g、PX02(ZnSe)0.4g和PS03(Fe2O3)0.5g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入到上述步骤制备的40gPUA-1中,加入0.2gD90消泡剂,得到A组分。
(2)称取1.2g2-羟基-2-甲基-1-苯基丙酮1173加入到上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学玻璃基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射38S,涂层完全固化。滤光片吸收紫外线和部分可见光,透过640-1250nm波长范围可见光和近红外。
实施例3:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-1):
(1)向800g聚己二酸乙二醇中加入450g甲苯二异氰酸酯(TDI)和9Kg乙酸乙酯溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入13g1,4-丁二醇、12g3-甲基-1,5-戊二醇反应90min,再加入280g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时54分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-1。
(二)制备蓝色滤光涂层及滤光片
(1)取PX03(CuSe)0.3g、PS02(CuO)0.5g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散后加入上述步骤制备的40gPUA-1中,加入0.2gD90消泡剂,得到A组分。
(2)称取1.2g2-羟基-2-甲基-1-苯基丙酮1173加入到上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学PC基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射28s,涂层完全固化。滤光片透过率光谱图如图8所示,滤光片吸收紫外线和520nm以上可见光,透过450-500nm波长范围可见光,吸收峰狭窄,色彩鲜明。
实施例4:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-1):
(1)向950g聚己二酸乙二醇中加入450g甲苯二异氰酸酯(TDI)和9Kg乙酸乙酯溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入15g1,4-丁二醇、1293-甲基-1,5-戊二醇反应90min,再加入220g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时50分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-1。
(二)制备紫色滤光涂层及滤光片
(1)取PX01(CdSe)0.3g、PS01(CoO)1.2g和PS03(Fe2O3)0.7g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入到上述步骤制备的40gPUA-1中,加入0.2gD90消泡剂,得到A组分。
(2)称取1.2g2-羟基-2-甲基-1-苯基丙酮1173加入到上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学玻璃基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射39S,涂层完全固化。滤光片透过率光谱图如图9所示,滤光片吸收光谱曲线图如图14所示,滤光片吸收488nm和514nm波段的激光束,吸光度>4A,透过630nm以上波长范围可见光。
实施例5:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-2):
(1)向380g聚碳酸酯二元醇(南通润丰石油化工有限公司,商品号:PCDL 355-6-9)中加入420g异佛尔酮二异氰酸酯(IPDI)和7.5Kg甲基乙基酮溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入15g1,4-丁二醇、12g3-甲基-1,5-戊二醇反应90min,再加入220g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时57分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-2。
(2)步骤(1)制备的聚氨酯丙烯酸酯预聚物(PUA-2)进行了傅里叶变换红外光谱测试,从图4中曲线分析可知,3320cm-1处为氨基甲酸酯中-NH伸缩振动峰,2955cm-1为-CH2的伸缩振动吸收峰,2360cm-1处峰消失,说明-NCO基团基本反应完全,1740cm-1处为C=0的伸缩振动吸收峰,所有这些峰表明IPDI中的-NCO与二元醇的中的羟基发生反应生成聚氨酯,1640cm-1处出现丙烯酸羟乙酯中的C=C双键的伸缩振动吸收峰,1240cm-1处为聚碳酸酯二元醇的O-C=O的反对称伸缩振动峰,而经紫外光固化后该峰消失,说明碳碳双键有效参与了固化交联反应。
(二)制备黄色滤光涂层及滤光片
(1)取PX02(ZnSe)0.7g、PX04(BaSe)0.3g和PS05(TiO2)0.5g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入到上述步骤制备的40gPUA-2中,加入0.2gT-A1000型消泡剂,得到A组分。
(2)称取1.2g1-羟基环己基苯基甲酮加入上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学玻璃基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射33s,涂层完全固化。滤光片透过率光谱图如图10所示,滤光片吸收480nm范围以下蓝光和紫外线,透过570-780nm波长范围的可见光。
实施例6:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-2):
(1)向380g聚碳酸酯二元醇中加入420g异佛尔酮二异氰酸酯(IPDI)和7.3Kg甲基乙基酮溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温75℃反应80min,依次加入26g3-甲基-1,5-戊二醇反应90min,再加入210g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时56分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-2。
(二)制备绿色滤光涂层及滤光片
(1)取PX03(CuSe)0.1g和PS06(MnO2)0.5g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入上述步骤制备的40gPUA-2中,加入0.2gT-A1000型消泡剂,得到A组分。
(2)称取1.2g1-羟基环己基苯基甲酮加入上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学玻璃基材表面,将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射28S,涂层完全固化。滤光片透过率光谱图如图11所示,滤光片吸收紫外线和400nm以下可见光,透过500-580nm波长范围可见光,吸收峰狭窄,色彩鲜明。
实施例7:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-2):
(1)向380g聚碳酸酯二元醇中加入420g六亚甲基二异氰酸酯(HDI)和7.4Kg甲基乙基酮溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入10g1,4-丁二醇、15g3-甲基-1,5-戊二醇反应90min,再加入230g丙烯酸羟乙酯(HEA),降温到50℃,反应5小时07分钟测定2236cm-1处-NCO伸缩振动吸收峰消失,蒸去除溶剂,即得PUA-2。
(二)制备青黄色滤光涂层及滤光片
(1)取PX02(ZnSe)0.5g、PS02(TiO2)0.3g和PS06(MnO2)0.4g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入到上述步骤制备的40gPUA-2中,加入0.2gT-A1000型消泡剂,得到A组分。
(2)称取1.2g1-羟基环己基苯基甲酮加入上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学PC基材表面,将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射32S,涂层完全固化。滤光片透过率光谱图如图12所示,滤光片吸收紫外线和400-450nm可见光,透过500-570nm波长范围可见光,吸收峰狭窄,色彩鲜明。
实施例8:制备聚氨酯丙烯酸酯预聚物、彩色涂层及滤光片
(一)聚氨酯丙烯酸酯预聚物(PUA-2):
(1)向380g聚碳酸酯二元醇中加入420g六亚甲基二异氰酸酯(HDI)和7.6Kg甲基乙基酮溶剂,缓慢滴入5g二月桂酸二丁基锡,25min滴完,氮气保护,控温70℃反应85min,依次加入15g1,4-丁二醇、12g3-甲基-1,5-戊二醇反应90min,再加入240g丙烯酸羟乙酯(HEA),降温到50℃,反应4小时49分钟测定2236cm-1处-NCO的伸缩振动吸收峰消失,蒸除溶剂,即得PUA-2。
(二)制备蓝绿色滤光涂层及滤光片
(1)取PX05(InSe)0.8g和PS04(MnO2)0.5g加入到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入上述步骤制备的40gPUA-2中,加入0.2gT-A1000型消泡剂,得到A组分。
(2)称取1.2g1-羟基环己基苯基甲酮加入上述A组分中,均匀混合后,得到预聚涂层液。
(3)将预聚涂层液经孔径0.5μm滤膜过滤脱气后,以2500转/分钟速度旋涂到光学玻璃基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射34S,涂层完全固化。滤光片透过率光谱图如图13所示,滤光片吸收光谱曲线图如图15所示,滤光片吸收660nm和690nm波段的激光束,吸光度>5A,透过500-580nm可见光,吸收峰狭窄,色彩鲜明。
对比例1:制备聚氨酯丙烯酸酯蓝光滤光片
根据实施例3步骤(二)相似的方法,(1)将0.0008g着色剂蓝2BLN分散到4.5g苄基丙烯酸酯中,搅拌30分钟均匀分散并加入到上述步骤制备的40gPUA-1中,加入0.2gD90消泡剂,得到A组分;
(2)称取1.2g2-羟基-2-甲基-1-苯基丙酮1173加入到上述A组分中,混合后得到预聚涂层液;
(3)将预聚涂层液过滤脱气后,以2500转/分钟速度旋涂到光学PC基材表面,然后将涂层片置于光照强度为200mW/cm2的UV-LED光固化机下照射28S,涂层完全固化,得到吸收蓝光滤光片。
实施例9:对涂层进行光学性能和色度检测实验
对实施例1-8制备的涂层分别进行光学性能检测,透光性是光学材料的最重要的性能之一,用透射比(透射率)来表示,检测选用上海元析仪器有限公司UV-8000紫外可见光光度计,检测方法:直接将样品放在紫外可见光光度计上测定透射比;颜色检测通过肉眼与选用标准色板进行比对。检测结果见表四和图7~图13。
表四检测样品透射比(tv)检测情况
实施例10:对滤光片涂层进行耐光色牢度检测
对实施例1-8、对比例1制备的滤光片分别进行耐光色牢度试验,采用上海典诺科技公司水冷氙灯试验箱,选择极限暴晒条件,辐照褪色色差达到肉眼可以分辨所需时间(h),结果见表五。
表五实施例样品耐光色牢度检测结果
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实施例11:对滤光片进行耐老化和剥离附着力实验
1.对实施例1-8和对比例1制备的滤光片分别进行耐老化试验,在耐老化试验箱中辐照24小时,对样品辐照前和辐照后进行紫外和可见光光谱检测,通过数据对比得知,实施例1-8检测样品未出现明显变化;传统印染滤光片对比例1样品出现1.4%的相对变化(见表六)。
表六实施例样品与对比例样品耐老化对比
2.对老化后样品进行胶带法十字穿插划格试验,检测方法:用刀片在镜片表面划痕,再从垂直角度划痕,最终在滤光片表面留下20个正方形小方块,用3M隐形胶带,粘在方格上,以稍快平稳的速度将胶带往后方向撕开,利用放大镜观察网格十字交点切割处涂层的脱落情况。划痕实验结果表明,全部滤光片涂层无脱落、剥离,附着力良好。
Claims (14)
1.一种纳米复合彩色滤光涂层液的制备方法,其特征在于,该方法包括如下步骤:
I.配置纳米复合彩色滤光涂层液:
A组分:
70~90%聚氨酯丙烯酸酯预聚物;
0~5.5%核壳型金属硒化物纳米粒子;
0~5.5%核壳型金属氧化物纳米粒子;
9.5~19%活性稀释剂;
0.1~1%消泡剂;
其中,核壳型金属硒化物粒子和核壳型金属氧化物粒子的总量为(0.5~5.5)%;
该聚氨酯丙烯酸酯预聚物是将二异氰酸酯和聚酯多元醇进行加成反应,再用羟基丙烯酸酯进行封端制得;
该核壳型金属硒化物纳米粒子的内核为金属硒化物,外壳为表面活性剂,内核与外壳的质量比为1∶(0.1~0.3),核壳型金属硒化物纳米粒子的粒径为3~10nm;
该核壳型金属氧化物粒子的内核为金属氧化物,外壳为表面活性剂,内核与外壳的质量比为1∶(0.1~0.5),核壳型金属氧化物纳米粒子的粒径4~10nm;
将核壳型金属硒化物纳米粒子和核壳型金属氧化物纳米粒子溶解于活性稀释剂中,搅拌下加入到聚氨酯丙烯酸酯预聚物中,随后加入消泡剂,得到A组分;
B组分:
0.4~4%光引发剂;
II.涂布前将A组分和B组分混合,超声搅拌5-10min,使A组分与B组分完全溶解,得到所需的彩色滤光涂层液。
2.如权利要求1所述的制备方法,其特征在于,所述金属硒化物为硒化镉、硒化锌、硒化铜、硒化钡、硒化铟和硒化锆中的至少一种;
所述金属氧化物为氧化镉、氧化锌、氧化铜、氧化钴、氧化铟、氧化铁、氧化铒、氧化锰、氧化钛和氧化钡中的至少一种;
所述核壳型金属硒化物粒子的表面活性剂为:月桂酰两性醋酸钠、月桂醇硫酸钠、月桂酰谷氨酸和脂肪醇聚氧乙烯醚中的至少一种;
所述核壳型金属氧化物粒子的表面活性剂为:硬脂酸、烷基葡糖苷、十二烷基苯磺酸钠、脂肪酸甘油酯和聚山梨酯中的至少一种。
3.如权利要求1所述的制备方法,其特征在于,所述活性稀释剂为苄基丙烯酸酯、乙氧基苯酚丙烯酸酯、联苯甲醇丙烯酸酯、邻苯基苯氧乙基丙烯酸酯、1,6-己二醇二丙烯酸酯、季戊四醇三丙烯酸酯或三羟甲基丙烷三丙烯酸酯中的至少一种;
所述消泡剂为T-1000A型消泡剂、DS100硅油性消泡剂、AT350聚醚型消泡剂和D90丙烯酸聚合型消泡剂中的至少一种;
所述光引发剂为自由基聚合光引发剂;优选地,所述光引发剂选自:2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、2,2-二甲基-1-苯基-1-丙酮、2,4,6-三甲基苯甲酰基苯基膦酸乙酯、2-二甲氨基-2-苄基-1-丁酮、2-羟基-2-甲基-1-丙酮和2,4,6-三甲基苯甲酰基-二苯基氧化膦;更优选地,所述光引发剂为2-羟基-2-甲基-1-苯基丙酮。
4.如权利要求1所述的制备方法,其特征在于,所述二异氰酸酯选自甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六亚甲基二异氰酸酯和/或赖氨酸二异氰酸酯;
所述聚酯多元醇选自聚己内酯二醇、聚己二酸乙二醇、苯酐聚酯二元醇和/或聚碳酸酯二醇;
所述羟基丙烯酸酯选自丙烯酸羟乙酯、丙烯酸羟丙酯和/或甲基丙烯酸羟乙酯。
5.如权利要求4所述的制备方法,其特征在于,所述聚氨酯丙烯酸酯预聚物采用如下方法制备:将聚酯二元醇加入到反应容器中,加入二异氰酸酯和溶剂,然后缓慢滴入二月桂酸二丁基锡催化剂,N2保护,温度控制在65-80℃反应60-90min,再加入羟基丙烯酸酯和扩链剂,降温到40-60℃,反应2-6h内取样检测-NCO含量,当检测到红外光谱2230~2240cm-1处-NCO的伸缩振动吸收峰消失,表明-NCO已经和-OH反应完全,即得到式I所示的聚氨酯丙烯酸酯预聚物;其中,羟基丙烯酸酯、二异氰酸酯、聚酯二元醇三者质量比为(1-3)∶(2-5)∶(8-10),聚酯多元醇与溶剂质量比为1∶(9-30)。
6.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备红色滤光涂层液,其中,所述金属硒化物为CdSe,所述金属氧化物为CoO;CdSe与CoO的质量比为4∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
7.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备红色滤光涂层液,其中,所述金属硒化物为CdSe和ZnSe,所述金属氧化物为Fe2O3;CdSe、ZnSe、Fe2O3三者的质量比为4∶(1~2)∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
8.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备蓝色滤光涂层液,其中,所述金属硒化物为CuSe,所述金属氧化物为CuO,CuSe,与CuO的质量比为3∶(3~7);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
9.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备紫色滤光涂层液,其中,所述金属硒化物为CdSe,所述氧化物为CoO和Fe2O3;CdSe、CoO、Fe2O3三者的质量比为1∶(3~5)∶(2~3);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
10.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备黄色滤光涂层液,其中,所述金属硒化物为ZnSe和BaSe,所述金属氧化物为TiO2;ZnSe、BaSe、TiO2三者的质量比为(2~3)∶1∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
11.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备绿色滤光涂层液,其中,所述金属硒化物为CuSe,所述金属氧化物为MnO2;CuSe与MnO2的质量比为1∶(3~7);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
12.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备青黄色滤光涂层液,其中,所述金属硒化物为ZnSe,所述金属氧化物为TiO2和MnO2;ZnSe、TiO2、MnO2三者的质量比为(1~2)∶1∶(1~2);核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
13.如权利要求1-5中任一项所述的制备方法,其特征在于,所述方法用于制备蓝绿色色滤光涂层液,其中,所述金属硒化物为InSe,所述氧化物为MnO2;InSe与MnO2的质量比为(1~2)∶1;核壳型金属硒化物粒子和核壳型金属氧化物粒子总量在涂层液中的质量百分含量为(0.5~4)%。
14.一种纳米复合彩色滤光片的制备方法,其特征在于,该方法包括如下步骤:采用如权利要求1-13中任一项所述的方法制备滤光涂层液,将涂层液经孔径0.1~10μm滤膜过滤脱气后,以2000~3000转/分钟速度旋涂到滤光片基材表面,然后将涂层片置于光照强度为160~300mW/cm2的UV-LED光固化机下照射20~50S,涂层完全固化得到彩色滤光片。
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CN1419151A (zh) * | 2002-12-06 | 2003-05-21 | 大连新世纪纳米科技股份有限公司 | 含金属氧化物纳米粒子的树脂光学透镜及制作方法 |
CN116023813A (zh) * | 2022-12-14 | 2023-04-28 | 江苏视科新材料股份有限公司 | 一种高折射率防蓝光改性环氧丙烯酸酯材料及滤光片的制备方法 |
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