CN113549377A - 一种跨尺度结构光学吸收涂层材料及涂层制备工艺 - Google Patents

一种跨尺度结构光学吸收涂层材料及涂层制备工艺 Download PDF

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CN113549377A
CN113549377A CN202110750043.1A CN202110750043A CN113549377A CN 113549377 A CN113549377 A CN 113549377A CN 202110750043 A CN202110750043 A CN 202110750043A CN 113549377 A CN113549377 A CN 113549377A
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王啸
李朝龙
朴明星
史浩飞
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Chongqing Institute of Green and Intelligent Technology of CAS
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Abstract

本发明的目的是提供一种跨尺度结构光学吸收涂层材料及涂层制备工艺。即针对现有光学涂层吸收率较低、吸收波段较窄的缺陷,提供一种能在紫外、可见光、近红外和中远红外全波段范围内进行超高光学吸收的涂层及其制备方法。该涂层同时具有微米和纳米跨尺度多孔光学吸收结构,多样的跨尺度结构尺寸能与不同波段光的波长相匹配,实现全波段的超高光学吸收。

Description

一种跨尺度结构光学吸收涂层材料及涂层制备工艺
技术领域
本发明涉及光学吸收涂层材料。
背景技术
光学吸收涂层是一种能够实现较高光学吸收、较低光学反射的功能材料,是许多光学器件的核心材料,在航空航天、军工计量等领域具有重要的应用价值,现有的商业化光学吸收涂层的光学吸收率大多为95-97%(漫反射率3-5%),难以满足不断发展的航天空间技术对高吸收率涂层的性能需求,制备超高光学吸收涂层已经十分迫切。同时,现有光学涂层往往只具有单一尺度的光学吸收结构,只能针对紫外、可见光、近红外和中远红外中某些较窄的波段进行较高的光学吸收,限制了涂层的工作范围和应用场景,而如何制备全波段下超高光学吸收的涂层需要进一步的探索。
发明内容
本发明的目的是提供一种跨尺度结构光学吸收涂层材料,其特征在于:包括作为基底表面的底漆材料,以及作为吸收剂的面漆材料;
所述底漆材料为聚四氟乙烯;
所述面漆材料是包括碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂的混合物。
本发明要求保护一种跨尺度结构光学吸收涂层的制备工艺,其特征在于,包括以下步骤:
(1)基底表面预处理;
将基底表面进行喷砂或者磨砂处理,洗净干燥后,对基底进行预热。
(2)底漆的喷涂:将聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的基底表面,干燥后形成底漆,并冷却至室温。
(3)面漆的制备:将碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂混合均匀后获得面漆。
(4)面漆的喷涂:将所述面漆喷涂并覆盖底漆表面,表干后,在基底表面形成涂层;
(5)涂层热处理:将步骤(4)中得到的涂层进行热处理,获得跨尺度结构光学吸收涂层。
进一步,基底材料为形变温度大于280℃的金属、陶瓷或者高分子材料。
进一步,所述的聚四氟乙烯乳液的固含量为30-70%,所述的聚四氟乙烯的平均粒径为50-350nm。
进一步,所述的碳纳米管的直径为4-100nm,长度为0.2-50μm,所述的碳黑粒径为5-200nm,该粒径是指原生一次结构碳黑粒子的粒径。进一步,面漆的原料及其配比为:
碳纳米管1-300份
碳黑1-300份
聚四氟乙烯乳液50-990份
N-甲基吡咯烷酮1-800份
进一步,步骤(1)中,将基底表面进行喷砂或者磨砂处理,洗净干燥后,对基底进行预热,预热温度为30-80℃。
进一步,步骤(2)中,将聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的基底表面,经过高温干燥后形成底漆,然后自然冷却至室温;干燥温度为30-150℃;底漆厚度为10-50μm。
进一步,步骤(3)中,将碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂混合,搅拌后经过超声处理得到面漆喷涂液,超声时间为5-120分钟;步骤(4)中,面漆的厚度为10-500μm。
进一步,步骤(5)中,热处理条件为:在150-200℃保温20-120分钟,然后升温至280-300℃并保温30-120分钟,热处理后涂层随烘箱冷却至室温。
本发明的技术效果是毋庸置疑的,本发明在聚四氟乙烯中添加碳纳米管和碳黑,通过混合喷涂的方式构建具有“微米-纳米”跨尺度光学吸收结构的功能涂层,该涂层同时拥有纳米级和微米级尺寸的多孔吸光结构,使得不同波段的光在该结构内部中经多次反射被高效吸收,吸收范围覆盖0.1~25μm全波段,该发明有效地提高了涂层的光学吸收率,并且实现了全波段的高效光学吸收,大幅拓展了涂层的使用范围,在杂散光抑制、计量与校准、航天黑体定标等领域具有广泛的应用前景。
附图说明
图1是根据本发明的方法制备的具有“微米-纳米”跨尺度光学吸收结构的涂层表面的扫描电子显微镜(SEM)照片,其中,放大倍数为500倍,显示了微米尺度的光学吸收结构;
图2是根据本发明的方法制备的具有“微米-纳米”跨尺度光学吸收结构的涂层表面的扫描电子显微镜(SEM)照片,其中,放大倍数为30000倍,显示了纳米尺度的光学吸收结构;。
具体实施方式
下面结合实施例对本发明作进一步说明,但不应该理解为本发明上述主题范围仅限于下述实施例。在不脱离本发明上述技术思想的情况下,根据本领域普通技术知识和惯用手段,做出各种替换和变更,均应包括在本发明的保护范围内。
实施例1:
一种跨尺度结构光学吸收涂层,采用管径为10nm、长度为20μm的碳纳米管和粒径为50nm的碳黑为吸收剂,粒径为150nm的聚四氟乙烯为基体树脂,N-甲基吡咯烷酮为溶剂制备而成,其制备方法如下:(1)基底的处理:
选取铝片作为基底,对其表面进行喷砂处理,洗净干燥后,对铝片进行预热,预热温度为60℃。
(2)底漆的喷涂:
将固含量为50%的聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的铝片表面,经过130℃干燥后形成底漆,然后自然冷却至室温,底漆的厚度为30μm。
(3)面漆的制备:
按照以下重量份称取原料:碳纳米管-6份,碳黑-6份,固含量为50%的聚四氟乙烯乳液-100份,N-甲基吡咯烷酮-20份;在室温下混合搅拌后经过30分钟超声处理得到面漆喷涂液。
(4)面漆的喷涂:
在室温下,将步骤(3)中制备的面漆喷涂液均匀喷涂并覆盖底漆表面,经过自然表干后形成面漆,面漆的厚度为50μm。
(5)涂层热处理:
将步骤(4)中得到的涂层置于烘箱中进行高温热处理,热处理过程为:在160℃保温30分钟,然后升温至280℃并保温30分钟,热处理后涂层随烘箱冷却至室温,制得跨尺度结构光学吸收涂层。
跨尺度结构光学吸收涂层与铝片基底结合力优异,涂层的漫反射率为2.3%,吸收率为97.7%。
实施例2:
一种跨尺度结构光学吸收涂层,采用管径为10nm、长度为20μm的碳纳米管和粒径为50nm的碳黑为吸收剂,粒径为150nm的聚四氟乙烯为基体树脂,N-甲基吡咯烷酮为溶剂制备而成,其制备方法如下:(1)基底的处理:
选取铝片作为基底,对其表面进行喷砂处理,洗净干燥后,对铝片进行预热,预热温度为60℃。
(2)底漆的喷涂:
将固含量为50%的聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的铝片表面,经过130℃干燥后形成底漆,然后自然冷却至室温,底漆的厚度为30μm。
(3)面漆的制备:
按照以下重量份称取原料:碳纳米管-8份,碳黑-8份,固含量为50%的聚四氟乙烯乳液-100份,N-甲基吡咯烷酮-40份;在室温下混合搅拌后经过30分钟超声处理得到面漆喷涂液。
(4)面漆的喷涂:
在室温下,将步骤(3)中制备的面漆喷涂液均匀喷涂并覆盖底漆表面,经过自然表干后形成面漆,面漆的厚度为50μm。
(5)涂层热处理:
将步骤(4)中得到的涂层置于烘箱中进行高温热处理,热处理过程为:在160℃保温30分钟,然后升温至280℃并保温30分钟,热处理后涂层随烘箱冷却至室温,制得跨尺度结构光学吸收涂层。
跨尺度结构光学吸收涂层与铝片基底结合力优异,涂层的漫反射率为1.8%,吸收率为98.2%。
实施例3:
一种跨尺度结构光学吸收涂层,采用管径为10nm、长度为20μm的碳纳米管和粒径为50nm的碳黑为吸收剂,粒径为150nm的聚四氟乙烯为基体树脂,N-甲基吡咯烷酮为溶剂制备而成,其制备方法如下:(1)基底的处理:
选取铝片作为基底,对其表面进行喷砂处理,洗净干燥后,对铝片进行预热,预热温度为60℃。
(2)底漆的喷涂:
将固含量为50%的聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的铝片表面,经过130℃干燥后形成底漆,然后自然冷却至室温,底漆的厚度为30μm。
(3)面漆的制备:
按照以下重量份称取原料:碳纳米管-12份,碳黑-12份,固含量为50%的聚四氟乙烯乳液-100份,N-甲基吡咯烷酮-80份;在室温下混合搅拌后经过30分钟超声处理得到面漆喷涂液。
(4)面漆的喷涂:
在室温下,将步骤(3)中制备的面漆喷涂液均匀喷涂并覆盖底漆表面,经过自然表干后形成面漆,面漆的厚度为50μm。
(5)涂层热处理:
将步骤(4)中得到的涂层置于烘箱中进行高温热处理,热处理过程为:在160℃保温30分钟,然后升温至280℃并保温30分钟,热处理后涂层随烘箱冷却至室温,制得跨尺度结构光学吸收涂层。
跨尺度结构光学吸收涂层与铝片基底结合力优异,涂层的漫反射率为1.3%,吸收率为98.7%。
实施例4:
一种跨尺度结构光学吸收涂层,采用管径为15nm、长度为40μm的碳纳米管和粒径为50nm的碳黑为吸收剂,粒径为150nm的聚四氟乙烯为基体树脂,N-甲基吡咯烷酮为溶剂制备而成,其制备方法如下:(1)基底的处理:
选取铝片作为基底,对其表面进行喷砂处理,洗净干燥后,对铝片进行预热,预热温度为60℃。
(2)底漆的喷涂:
将固含量为50%的聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的铝片表面,经过130℃干燥后形成底漆,然后自然冷却至室温,底漆的厚度为30μm。
(3)面漆的制备:
按照以下重量份称取原料:碳纳米管-12份,碳黑-12份,固含量为50%的聚四氟乙烯乳液-100份,N-甲基吡咯烷酮-80份;在室温下混合搅拌后经过30分钟超声处理得到面漆喷涂液。
(4)面漆的喷涂:
在室温下,将步骤(3)中制备的面漆喷涂液均匀喷涂并覆盖底漆表面,经过自然表干后形成面漆,面漆的厚度为50μm。
(5)涂层热处理:
将步骤(4)中得到的涂层置于烘箱中进行高温热处理,热处理过程为:在160℃保温30分钟,然后升温至280℃并保温30分钟,热处理后涂层随烘箱冷却至室温,制得跨尺度结构光学吸收涂层。
跨尺度结构光学吸收涂层与铝片基底结合力优异,涂层的漫反射率为0.9%,吸收率为99.1%。

Claims (10)

1.一种跨尺度结构光学吸收涂层材料,其特征在于:包括作为所述基底表面的底漆材料,以及作为吸收剂的面漆材料;
所述底漆材料为聚四氟乙烯;
所述面漆材料是包括碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂的混合物。
2.一种跨尺度结构光学吸收涂层的制备工艺,其特征在于,包括以下步骤:
(1)基底表面预处理;
将基底表面进行喷砂或者磨砂处理,洗净干燥后,对基底进行预热。
(2)底漆的喷涂:将聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的基底表面,干燥后形成底漆,并冷却至室温。
(3)面漆的制备:将碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂混合均匀后获得面漆。
(4)面漆的喷涂:将所述面漆喷涂并覆盖底漆表面,表干后,在基底表面形成涂层;
(5)涂层热处理:将步骤(4)中得到的涂层进行热处理,获得跨尺度结构光学吸收涂层。
3.根据权利要求1或2所述的基底,其特征在于:基底材料为形变温度大于280℃的金属、陶瓷或者高分子材料。
4.根据权利要求1、2或3所述的底漆和面漆材料,其特征在于:所述的聚四氟乙烯乳液的固含量为30-70%,所述的聚四氟乙烯的平均粒径为50-350nm。
5.根据权利要求1或2所述的面漆材料,其特征在于:所述的碳纳米管的直径为4-100nm,长度为0.2-50μm,所述的碳黑粒径为5-200nm,该粒径是指原生一次结构碳黑粒子的粒径。
6.根据权利要求1或2所述的面漆材料,其特征在于:面漆的原料及其配比为:
碳纳米管1-300份
碳黑1-300份
聚四氟乙烯乳液50-990份
N-甲基吡咯烷酮1-800份。
7.根据权利要求2所述的跨尺度结构光学吸收涂层的制备工艺,其特征在于:
步骤(1)中,将基底表面进行喷砂或者磨砂处理,洗净干燥后,对基底进行预热,预热温度为30-80℃。
8.根据权利要求2所述的跨尺度结构光学吸收涂层的制备工艺,其特征在于:步骤(2)中,将聚四氟乙烯乳液均匀喷涂在步骤(1)中处理后的基底表面,经过高温干燥后形成底漆,然后自然冷却至室温;干燥温度为30-150℃;底漆厚度为10-50μm。
9.根据权利要求2所述的跨尺度结构光学吸收涂层的制备工艺,其特征在于:步骤(3)中,将碳纳米管、碳黑、聚四氟乙烯乳液和N-甲基吡咯烷酮溶剂混合,搅拌后经过超声处理得到面漆喷涂液,超声时间为5-120分钟;步骤(4)中,面漆的厚度为10-500μm。
10.根据权利要求2所述的跨尺度结构光学吸收涂层的制备工艺,其特征在于:步骤(5)中,热处理条件为:在150-200℃保温20-120分钟,然后升温至280-300℃并保温30-120分钟,热处理后涂层随烘箱冷却至室温。
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