CN113278176A - 一种反蛋白石型光子晶体可重复使用薄膜材料及其制备方法 - Google Patents
一种反蛋白石型光子晶体可重复使用薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明属于新材料领域,具体提供了一种反蛋白石型光子晶体可重复使用薄膜材料及其制备方法,所述的反蛋白石型光子晶体薄膜材料是通过分子印迹技术以高分子分散液或可聚合前驱液为基材制备,具有优异的自支撑性能;同时基于金属离子的可控沉积与解析,线性调控其折射率从而实现光子晶体纸颜色的精准调控,能够实现信息的全彩印刷及快速擦除,具有良好的循环稳定性。
Description
技术领域
本发明属于新材料领域,具体提供了一种反蛋白石型光子晶体可重复使用薄膜材料及其制备方法。
背景技术
资源与环境问题是当前乃至今后社会高质量发展的瓶颈问题。制浆造纸作为国民经济的支柱产业之一,也面临着瓶颈问题:纤维资源严重短缺,尤其是我国近年来限制固废(废纸)进口,纤维资源短缺问题更为严重。并且油墨、墨水、颜料及墨粉的生产过程中会消耗大量能源和有机溶剂,在印刷过程中会释放刺激性VOCs及细微颗粒墨粉,给环境及人体健康带来巨大损害。为缓解上述问题,发展环保型、无墨显色新型可重复使用光子晶体纸是缓解资源短缺、消除危害的有效途径。
目前,国内外研究团队针对可重复使用光子晶体纸的研究主要集中在如何将胶体光子晶体与刺激响应性材料结合,以特定的外界刺激(如溶剂、磁场、温度、pH及电场等)为印刷驱动力,调控响应区域的晶格常数及折射率,实现特定信息的无墨印刷显示效果。如承印材料吸收盐溶液(刺激源),体积发生变化,响应区域呈现绿色,实现字母的印刷;或以水为墨,实现文字与图案的显色;或通过施加磁场实现预置式信息的显示,但无法长期保存;或通过直接在特定基底上打印光子晶体的方式,实现绿色印刷;或通过外加电场控制压电材料PEDOT的氧化还原态,结合锂离子的掺杂调控其微观形态及折射率,从而实现图案的印刷与显示。
传统响应性材料的体积或折射率变化与分子链浸润性转变及相转变密切相关,均在临界值处发生突变(如湿度、温度、pH等),且响应区间有限;电磁响应材料仅可实现特定外场条件下两种或几种存在形态间的转变。由于传统刺激响应机理的局限性,仅能实现无墨承印材料颜色的间断性调控,无中间颜色;且由于不可控的刺激源扩散或传导,造成图案出现毛刺毛边现象,导致信息显示的分辨率低下。
为克服上述问题,基于反蛋白石型光子晶体结构色材料引起了科学家广泛的关注,能否提供一种可重复使用的反蛋白石型光子晶体薄膜材料成为本领域亟待解决的问题之一。
发明内容
本发明针对现有技术的空白,提供了一种反蛋白石型光子晶体可重复使用薄膜材料及其制备方法,所述的反蛋白石型光子晶体薄膜材料是通过分子印迹技术以高分子分散液或可聚合前驱液为基材制备,具有优异的自支撑性能;同时基于金属离子的可控沉积与解析,线性调控其折射率从而实现光子晶体纸颜色的精准调控,能够实现信息的全彩印刷及快速擦除,具有良好的循环稳定性。
本发明的主要原理是:
以高分子基反蛋白石型光子晶体为基质材料,结合紫外光与聚多巴胺(Polydopamine,PDA)对金属离子的协同还原及解析特性,以紫外光为笔,精准控制金属离子在多孔结构中的沉积量及沉积位置,线性调控体系折射率,实现信息的印刷、颜色改变及擦除,从而得到自支撑可重复使用光子晶体纸。
基于上述原理,本发明的具体技术方案是:
一种反蛋白石型光子晶体可重复使用薄膜材料,所采用的薄膜材料的基底材料为聚醚砜、聚偏氟乙烯、聚甲基丙烯酸甲酯,聚丙烯酰胺及乙烯基环氧树脂中的一种;
所述薄膜材料通过多巴胺自聚合进行改性;改性后聚多巴胺层通过自聚合反应在反蛋白石型阵列结构表面沉积壳层,所形成的壳层厚度为10nm-50nm;
所获得的薄膜材料以紫外光为驱动实现信息印刷和擦除,其中印刷时的紫外光波长为365nm,擦除时的紫外光波长为254nm;
发明人采用了上述分子键能大,(键能范围200-600kJ/mol),分子链排列紧密,具有优异的结构强度的高分子树脂作为原料,最终获得的材料其抗弯折角度为150°以上。
发明人还提供了上述反蛋白石型光子晶体可重复使用薄膜材料的制备方法,包括(1)制备蛋白石型光子晶体模板阵列,(2)制备高分子反蛋白石薄膜和(3)高分子薄膜的改性;
其中高分子薄膜的改性方法为:
利用多巴胺的自聚合反应对制备获得的多孔薄膜进行改性,利用催化剂催化多巴胺的自聚合反应,实现聚多巴胺层厚度均匀且均匀的改性,得到光子晶体纸;
具体改性方法举例如下:
将制备高分子反蛋白石薄膜置于pH值为8.5、浓度为10mM的三羟甲基氨基甲烷-盐酸(Tris-HCl)的缓冲溶液中,加入盐酸多巴胺,在催化剂的作用下室温搅拌30min即可得到PDA改性的高分子反蛋白石光子晶体纸;其中盐酸多巴胺用量与缓冲液体积的比例为0.01-0.5g/ml;
上述过程中所采用的催化剂包括但不仅限于硫酸铜、过硫酸铵、过氧化氢中的一种或多种;其中优选采用硫酸铜和过氧化氢的组合,其中硫酸铜的浓度为10-50mmol/L,过氧化氢的浓度为5-20mmol/L;
采用上述催化剂组合时,反应速度快,且聚多巴胺层沉积的均匀度高;
更进一步的,上述的(1)制备蛋白石型光子晶体模板阵列,具体步骤为:
选取单分散微球,通过自组装方法,将单分散微球按固定的周期性规律组装成三维有序的光子晶体阵列;
其中所述的单分散微球包括但不仅限于二氧化硅、二氧化锆、碳酸钙、硫化锌、硫化镉及其他含硫无机微球,粒径为180nm-500nm;
上述单分散微球的质量分数为2wt%-20wt%,所采用的分散剂选自水、乙醇、无水乙醇、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺中的一种或多种;
所述的组装方法包括但不限于垂直沉积法、浸渍提拉法、双基片自组装法及加热水平自组装法、旋涂法;其中优选采用浸渍提拉法,均可参考现有技术中的技术方案;最终获得的蛋白石型光子晶体模板阵列具有有序排列的三维结构。
(2)制备高分子反蛋白石薄膜,具体步骤为:
将聚合物分散液或可聚合前驱液均匀渗入步骤(1)中制备的蛋白石阵列中,经过固化或聚合过程,然后除去蛋白石模板,得到高分子基反蛋白石型多孔柔性薄膜;
其中所述的聚合物分散液或可聚合前驱液选自但不限于聚醚砜、聚偏氟乙烯、聚甲基丙烯酸甲酯,聚丙烯酰胺及乙烯基环氧树脂中的一种;
所述分散液或前驱液的固含量为4wt%-10wt%;
固化的方式为热聚合或磁聚合或紫外光聚合;
除去蛋白石模板的方法优选为刻蚀法;具体选用酸刻蚀、碱刻蚀或者是高温刻蚀中至少一种;
通过上述高分子薄膜的改性方法获得的光子晶体纸;可以用于印刷,具体步骤为:
首先选取合适的金属盐溶液,将其涂覆在待印刷区域,然后利用365nm的综合紫外光对其进行照射,通过调节上述盐溶液浓度,涂覆厚度、光照强度和时间等,控制金属沉积量,从而获得目标色彩印刷区域;
优选的,所采用的盐溶液浓度为0.01mmol/L-0.1mmol/L;
所采用的紫外光的强度为50μW/cm2-500μW/cm2;
紫外光的作用时长为5s-100s;
紫外光的光斑直径大小20μm-1000μm;
上述的金属盐选自但不限于:硝酸银、硝酸铜、高氯酸金、硝酸锌、硝酸铁中的一种;
对应的上述光子晶体纸上印刷物的擦除方法,具体步骤为:
将印刷有信息的光子晶体纸置于水中,利用254nm的紫外光对光子晶体纸进行照射,通过调节光照强度和时间控制金属离子从光子晶体纸上脱落,从而实现印刷物的擦除;
综上所述,本发明所提供的反蛋白石型光子晶体可重复使用薄膜材料具有如下有益效果:
(1)基于高分子反蛋白石型光子晶体纸具有优异的自支撑性能及柔性,其抗弯折角度为150°以上;
(2)利用紫外光(365nm)精准控制金属离子沉积量及沉积位置,实现光子晶体纸晶格常数局部差异化,信息的高分辨率印刷;
(3)采用254nm紫外光对以印刷信息的紫外光进行照射,可实现信息的擦除,该可重复使用纸具有良好的使用稳定性,并可按需存储信息。
与现有的特定的外界刺激为印刷驱动力的材料相比,本发明的高分子反蛋白石型光子晶体纸可以快速实现信息的高分辨率印刷,并且信息不会随刺激源的撤除而消失,同时可以按需要控制信息的存储时间。
附图说明
图1为本发明所提供的薄膜材料信息印刷及擦除过程示意图;
以紫外光(365nm)为笔,精准控制金属离子在光子晶体纸上的沉积量及沉积位置,实现信息的印刷,另外使用更短波长的(254nm)紫外光为驱动力,可使金属颗粒实现解析,光子晶体纸恢复到原来的状态;
图2为本发明所提供的薄膜材料的扫描电子显微镜照片;
其是以300nm二氧化硅微球为模板制备的反蛋白石光子晶体纸,其孔洞尺寸为300nm,PDA沉积在孔洞结构的表面,沉积的PDA壳层结构厚度为20nm。
具体实施方式
为了更好的理解本发明,下面结合实施例进一步阐明本发明的内容,此处所描述的本发明,仅用以解释本发明,并不用于限定本发明。
实施例1
一种反蛋白石型光子晶体可重复使用薄膜材料的制备方法,具体步骤如下:
(1)制备蛋白石型光子晶体模板阵列:
选直径为200nm的单分散二氧化硅纳米微球,以制备蛋白石型光子晶体阵列;通过浸渍提拉自组装方法,将单分散二氧化硅微球组装成三维有序的光子晶体阵列;其中所述的单分散二氧化硅纳米微球为二氧化硅/乙醇分散液,质量分数为8%;
(2)制备高分子反蛋白石薄膜:
选用的柔性高分子材料为:聚偏氟乙烯/N,N-二甲基甲酰胺分散液,质量分数为8wt%;
将上述聚偏氟乙烯/N,N-二-甲基甲酰胺分散液均匀地渗入到步骤(1)获得的二氧化硅光子晶体阵列中,经氢氟酸刻蚀途径,氢氟酸溶液的质量分数为4%,除去蛋白石模板,得到高分子基反蛋白石型多孔柔性薄膜;
(3)高分子薄膜的改性:
利用多巴胺的自聚合反应对多孔薄膜进行改性,将制备高分子反蛋白石结构色膜置于pH值为8.5、浓度为10mM的三羟甲基氨基甲烷-盐酸(Tris-HCl)的缓冲溶液中,加入核算量的盐酸多巴胺,以硫酸铜与过氧化氢作为催化剂,硫酸铜终浓度为25mmol/L,过氧化氢终浓度为15mmol/L,室温下搅拌30min即可得到PDA改性的高分子反蛋白石光子晶体纸;
优选的壳层厚度为30nm,盐酸多巴胺用量与缓冲液体积的比例为0.01g/ml,通过硫酸铜与过氧化氢协同催化,实现聚多巴胺对聚偏氟乙烯均匀的改性,得到光子晶体纸;
获得上述光子晶体纸后,发明人进一步实现了光子晶体纸上信息的印刷:
基于紫外光与多巴胺对金属离子的协同沉积作用,本实施例中以紫外光(365nm)为笔,精准控制金属离子沉积量及沉积区域,体系折射率出现区域差异化,实现信息的印刷;
金属盐选用硝酸银,该盐溶液浓度为0.05mmol/L,光斑直径为200μm,强度为100μW/cm2,作用时间为20s,30s,40s,50s,60s,70s,80s,90s,100s,呈现出九种不同的颜色;
光子晶体纸上信息的擦除:以254nm的紫外光为驱动力,可以使金属离子脱落,实现信息的擦除,作用时间为200s,采用大面积辐射模式;经测试,上述获得的光子晶体纸印刷和擦除次数高于500次,其抗弯折角度为150°以上。
实施例2
一种反蛋白石型光子晶体可重复使用薄膜材料的制备方法,具体步骤如下:
(1)制备蛋白石型光子晶体模板阵列:
选直径为250nm的单分散硫化镉纳米微球,以制备蛋白石型光子晶体阵列;通过垂直沉积自组装方法,将单分散硫化镉微球组装成三维有序的光子晶体阵列;其中所述的单分散硫化镉纳米微球为硫化镉/无水乙醇分散液,质量分数为10%;
(2)制备高分子反蛋白石薄膜:
柔性高分子材料为:聚醚砜/N,N-二甲基乙酰胺分散液,质量分数为10wt%;
将上述聚醚砜/N,N-二甲基乙酰胺分散液均匀地渗入到步骤(1)获得的硫化镉光子晶体阵列中,经质量分数为20%的稀硫酸刻蚀途径,除去蛋白石模板,得到高分子基反蛋白石型多孔柔性薄膜;
(3)高分子薄膜的改性:
利用多巴胺的自聚合反应对多孔薄膜进行改性,将制备高分子反蛋白石结构色膜置于pH值为8.5、浓度为10mM的三羟甲基氨基甲烷-盐酸(Tris-HCl)的缓冲溶液中,加入核算量的盐酸多巴胺,以终浓度为24mmol/L的过硫酸铵作为催化剂,室温下搅拌25min即可得到PDA改性的高分子反蛋白石光子晶体纸;优选的壳层厚度为20nm,盐酸多巴胺用量与缓冲液体积的比例为0.02g/ml;
获得上述光子晶体纸后,发明人进一步实现了光子晶体纸上信息的印刷:
基于紫外光与多巴胺对金属离子的协同沉积作用,本实施例中以紫外光(365nm)为笔,精准控制金属离子沉积量及沉积区域,体系折射率出现区域差异化,实现信息的印刷;
金属盐选用高氯酸金,该盐溶液浓度为0.01mmol/L,光斑直径为100μm,强度为200μW/cm2,作用时间为5s,10s,15s,20s,25s,30s,35s,40s,45s,呈现出九种不同的颜色;
光子晶体纸上信息的擦除:并以254nm的紫外光为驱动力,可以使金属离子脱落,实现信息的擦除,作用时间为200s,采用大面积辐射模式;经测试,上述获得的光子晶体纸印刷和擦除次数高于400次,其抗弯折角度为150°以上。
实施例3
一种反蛋白石型光子晶体可重复使用薄膜材料的制备方法,具体步骤如下:
(1)制备蛋白石型光子晶体模板阵列:
选直径为220nm的单分散硫化锌纳米微球,以制备蛋白石型光子晶体阵列;通过旋涂自组装方法,将单分散硫化锌微球组装成三维有序的光子晶体阵列;
其中所述的单分散硫化锌纳米微球为硫化锌/无水乙醇分散液,质量分数为12%;
(2)制备高分子反蛋白石薄膜:
选用的柔性高分子材料为:聚甲基丙烯酸甲酯/四氢呋喃分散液,质量分数为6wt%;
将上述聚甲基丙烯酸甲酯/四氢呋喃分散液均匀地渗入到步骤(3)获得的硫化锌光子晶体阵列中,经质量分数为10%的盐酸刻蚀途径除去蛋白石模板,得到高分子基反蛋白石型多孔柔性薄膜;
(3)高分子薄膜的改性:
利用多巴胺的自聚合反应对多孔薄膜进行改性,将制备高分子反蛋白石结构色膜置于pH值为8.5、浓度为10mM的三羟甲基氨基甲烷-盐酸(Tris-HCl)的缓冲溶液中,加入核算量的盐酸多巴胺,以终浓度为26mmol/L的过硫酸铵与终浓度为15mmol/L过氧化氢作为催化剂,室温下搅拌40min即可得到PDA改性的高分子反蛋白石光子晶体纸。
盐酸多巴胺用量与缓冲液体积的比例为0.02g/ml,通过过硫酸铵与过氧化氢协同催化,实现聚多巴胺对聚甲基丙烯酸甲酯均匀的改性,得到光子晶体纸;
获得上述光子晶体纸后,发明人进一步实现了光子晶体纸上信息的印刷:
基于紫外光与多巴胺对金属离子的协同沉积作用,本实施例中以紫外光(365nm)为笔,精准控制金属离子沉积量及沉积区域,体系折射率出现区域差异化,实现信息的印刷;
金属盐选用硝酸铜,该盐溶液浓度为0.1mmol/L,光斑直径为150μm,强度为300μW/cm2,作用时间为3s,6s,9s,12s,15s,18s,21s,24s,27s,呈现出九种不同的颜色;
光子晶体纸上信息的擦除:并以254nm的紫外光为驱动力,可以使金属离子脱落,实现信息的擦除,作用时间为200s,采用大面积辐射模式;经测试,上述获得的光子晶体纸印刷和擦除次数高于500次,其抗弯折角度为150°以上。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,依据本发明的技术实质,对以上实施例所做的任何修改、等同替换或改进等,均人数与本发明技术方案的保护范围之内。
Claims (8)
1.一种反蛋白石型光子晶体可重复使用薄膜材料,其特征在于:所采用的薄膜材料的基底材料为聚醚砜、聚偏氟乙烯、聚甲基丙烯酸甲酯,聚丙烯酰胺及乙烯基环氧树脂中的一种;
所述薄膜材料通过多巴胺自聚合进行改性;改性后聚多巴胺层通过自聚合反应在反蛋白石型阵列结构表面沉积壳层。
2.根据权利要求1所述的反蛋白石型光子晶体可重复使用薄膜材料,其特征在于:所形成的壳层厚度为10nm-50nm。
3.根据权利要求1所述的反蛋白石型光子晶体可重复使用薄膜材料,其特征在于:所获得的薄膜材料以紫外光为驱动实现信息印刷和擦除,其中印刷时的紫外光波长为365nm,擦除时的紫外光波长为254nm。
4.权利要求1所述反蛋白石型光子晶体可重复使用薄膜材料的制备方法,包括(1)制备蛋白石型光子晶体模板阵列,(2)制备高分子反蛋白石薄膜和(3)高分子薄膜的改性;其特征在于:
高分子薄膜的改性方法为:
将制备高分子反蛋白石薄膜置于pH值为8.5、浓度为10mM的三羟甲基氨基甲烷-盐酸(Tris-HCl)的缓冲溶液中,加入盐酸多巴胺,在催化剂的作用下室温搅拌30min即可得到PDA改性的高分子反蛋白石光子晶体纸;其中盐酸多巴胺用量与缓冲液体积的比例为0.01-0.5g/ml;
上述过程中所采用的催化剂包括但不仅限于硫酸铜、过硫酸铵、过氧化氢中的一种或多种。
5.根据权利要求4所述反蛋白石型光子晶体可重复使用薄膜材料的制备方法,其特征在于:
(1)制备蛋白石型光子晶体模板阵列,具体步骤为:
选取单分散微球,通过自组装方法,将单分散微球按固定的周期性规律组装成三维有序的光子晶体阵列;
其中所述的单分散微球包括但不仅限于二氧化硅、二氧化锆、碳酸钙、硫化锌、硫化镉及及其他含硫无机微球,粒径为180nm-500nm;
上述单分散微球的质量分数为2wt%-20wt%,所采用的分散剂选自水、乙醇、无水乙醇、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺中的一种或多种;
所述的组装方法包括但不限于垂直沉积法、浸渍提拉法、双基片自组装法及加热水平自组装法、旋涂法。
6.根据权利要求4所述反蛋白石型光子晶体可重复使用薄膜材料的制备方法,其特征在于:(2)制备高分子反蛋白石薄膜,具体步骤为:
将聚合物分散液或可聚合前驱液均匀渗入步骤(1)中制备的蛋白石阵列中,经过固化或聚合过程,然后除去蛋白石模板,得到高分子基反蛋白石型多孔柔性薄膜;
其中所述的聚合物分散液或可聚合前驱液选自但不限于聚醚砜、聚偏氟乙烯、聚甲基丙烯酸甲酯,聚丙烯酰胺及乙烯基环氧树脂中的一种;
所述分散液或前驱液的固含量为4wt%-10wt%;
固化的方式为热聚合或磁聚合或紫外光聚合;
除去蛋白石模板的方法选用酸刻蚀、碱刻蚀或者是高温刻蚀中至少一种。
7.权利要求1所述反蛋白石型光子晶体可重复使用薄膜材料在印刷中的应用,其特征在于:印刷具体步骤为:
首先选取合适的金属盐溶液,将其涂覆在待印刷区域,然后利用365nm的综合紫外光对其进行照射,通过调节上述盐溶液浓度,涂覆厚度、光照强度和时间等,控制金属沉积量,从而获得目标色彩印刷区域;
优选的,所采用的盐溶液浓度为0.01mmol/L-0.1mmol/L;
所采用的紫外光的强度为50μW/cm2-500μW/cm2;
紫外光的作用时长为5s-100s;
紫外光的光斑直径大小20μm-1000μm;
上述的金属盐选自但不限于:硝酸银、硝酸铜、高氯酸金、硝酸锌、硝酸铁中的一种。
8.根据权利要求7所述反蛋白石型光子晶体可重复使用薄膜材料在印刷中的应用,其特征在于:擦除具体步骤为:
将印刷有信息的光子晶体纸置于水中,利用254nm的紫外光对光子晶体纸进行照射,通过调节光照强度和时间控制金属离子从光子晶体纸上脱落,从而实现印刷物的擦除。
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