CN111363399A - 一种红外吸收复合涂层的制备方法 - Google Patents
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Abstract
本发明公开了一种红外吸收复合涂层的制备方法,属于表面工程技术领域,本发明所述方法以纳米氧化铜(CuO)和纳米碳化硼(CB4)的混合物为基料,水性聚氨酯和聚乙烯醇为粘结剂;纳米氧化铜与纳米碳化硼的质量比为3:1~5:1,粘结剂为水性聚氨酯+聚乙烯醇,使基料均匀分散在粘结剂中,涂覆在经过预处理的Cu基体上。本发明所述方法制备的红外吸收涂层在1000‑4000cm‑1范围内红外吸收率达95%以上,抗热震性次数达30次未出现裂纹,表明所制备的涂层具有良好的韧性;此外,该方法还具有环保无毒,工艺简单,生产周期短等特点。
Description
技术领域
本发明公开一种红外吸收复合涂层的制备方法,属于表面工程技术领域。
背景技术
红外吸收材料是指在红外辐射的波谱范围内红外吸收率较高的一种材料。红外吸收涂层的应用是从60年代末的日本开始的,红外吸收涂层因其独特的优良特性在全世界都已经备受关注,越来越多的科研工作者致力于红外吸收涂层的研究与开发。与此同时,我国也将它归为国家的重点研究和发展的项目之一。随着时间的推移,红外吸收技术已经被用于越来越多的领域。而且现在红外技术慢慢的可以代表一个国家的军事装备现代化的水平。红外吸收涂层常常应用在复杂恶劣的环境中。超细超薄化、成分复合化是红外吸收涂层发展的一个重要方向。
红外吸收涂层常用的基料非常多,如氧化铜、氧化锆、碳化硅、三氧化二铁、碳化硼等,但单独使用其中的某种材料都会有一定的缺陷,而成分复合化后的材料能够在温度与波长均不同的情况下,其辐射特性能够相互互补并增强,但是制备复合涂层也存在涂层容易剥落,容易出现裂纹,韧性不好等问题。
发明内容
本发明的目的在于提供一种高韧性红外吸收复合涂层的制备方法,通过合理选择基料与粘结剂,在进行基体的预处理,将混合均匀的涂料进行涂覆与烧结;经过工艺优化后,所制备的红外吸收涂层在1000-4000cm-1范围内红外吸收率达95%以上,抗热震性次数达30次未出现裂纹,满足要求,说明所制备的涂层具有良好的韧性,具体步骤如下:
(1)基体预处理:用砂纸对铜片进行表面的粗化处理,洗净、吹干后备用。
(2)将纳米氧化铜与纳米碳化硼按质量比为3:1~5:1的比例研磨混合均匀得到基料。
(3)将水性聚氨酯稀释到质量百分比浓度为原溶液的10%~15%,聚乙烯醇加水配制为质量百分比浓度为0.5%~0.8%的聚乙烯醇水溶液,然后将两者混合,将步骤(2)制备的基料均匀分散在粘结剂溶液中得到涂料。
(4)涂覆与烧结:将步骤(3)制备的涂料均匀涂覆到步骤(1)粗化后的铜基体上进行烧结。
优选的,本发明所述基体预处理过程中砂纸的型号为500目。
优选的,本发明步骤(2)所述纳米氧化铜为球形,粒径为37~42nm、纯度≥99.5%;纳米碳化硼粒径为48~52nm,纯度≥99%。
优选的,本发明步骤(3)所述涂料中稀释后水性聚氨酯的质量分数为80%~90%、聚乙烯醇水溶液的质量分数为3%~8%、基料的质量分数为4%~6%。
优选的,本发明步骤(4)中烧结温度为125-150℃,烧结时间为10~30min。
本发明的有益效果:
(1)本发明充分利用纳米技术,使得涂层吸收率高,材料利用率高。其原因在于涂层的颗粒超细化后,粒子间的平均间距增大,单位体积内的粒子数减少,因此其密度降低,从而提高了物体的红外辐射的透射深度以及降低了其折射指数和吸收指数,达到了提高其吸收率的效果。
(2)本发明所述方法使用环保无毒的有机粘结剂制备高韧性的红外吸收涂层,在保证红外吸收率的情况下还提升了其韧性,使其满足其在复杂环境下的使用寿命。
(3)本发明所述方法以水性聚氨酯为主要粘结剂,为增强涂层的柔韧性加入少量的聚乙烯醇溶液;经实验工艺参数优化后,在满足较高的红外吸收率的前提下,该方法制备的涂层在具有良好的韧性;此外,该方法绿色环保、工艺简单、制备周期短。
附图说明
图1为本发明的工艺流程图。
图2为实施例1基料配比优化透射率曲线。
图3为实施例2聚氨酯浓度优化反射率曲线。
图4为实施例2烧结温度优化透反射率曲线。
图5为实施例3涂层附着力测试。
图6为实施例4涂层的显微组织形貌。
图7为实施例4涂层的显微组织形貌。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1
(1)基体预处理:用型号为500目的砂纸对铜片进行表面的粗化处理,将砂纸在铜片上用同等的力度均匀处理,将粗化后的铜片先进行油渍的清洗,然后用等离子水冲洗铜基表面,然后吹干。
(2)红外吸收基料制备:将纳米氧化铜与纳米碳化硼通过研磨混合均匀制成的基料;其中,纳米氧化铜与纳米碳化硼的配比如表1所示。
表1红外吸收涂层基料配比
实验号 | 纳米碳化硼质量(%) | 纳米氧化铜质量(%) |
1 | 25 | 75 |
2 | (1/6)*100 | (5/6)*100 |
3 | (1/9)*100 | (8/9)*100 |
4 | 0 | 100 |
5 | 100 | 0 |
(3)将水性聚氨酯稀释到质量百分比浓度为原溶液的10%,聚乙烯醇加水配制为质量百分比浓度为0.5%的聚乙烯醇水溶液,然后将两者混合,再将步骤(2)制备的基料均匀分散在粘结剂溶液中得到涂料;所述涂料中稀释后水性聚氨酯的质量分数为90%、聚乙烯醇水溶液的质量分数为5%、基料的质量分数为5%。
(4)涂覆与烧结:将步骤(3)制备的涂料均匀涂覆到步骤(1)粗化后的铜基体上进行烧结,烧结温度为130℃,烧结时间为20min。
对本实施例制备得到的5个样品进行透射率测试,测试结果如图2所示;从图中可以看出透射率最低的是2号样品,物体的反射率、透射率与吸收率之和等于1,并且粉末的反射率可以忽略不计,因此透射率越低的粉末代表其吸收率越高,由此可以看出在表1所设计的五个比例的样品中,实验号为2的样品吸收率最高,其次为1号样品,由此可见纳米氧化铜与纳米碳化硼按一定比例混合可提高涂层的吸收率。
实施例2
(1)基体预处理:用型号为500目的砂纸对铜片进行表面的粗化处理,将砂纸在铜片上用同等的力度均匀处理,将粗化后的铜片先进行油渍的清洗,然后用等离子水冲洗铜基表面,然后吹干。
(2)红外吸收基料制备:将纳米氧化铜与纳米碳化硼通过研磨混合均匀制成的基料;其中,纳米氧化铜与纳米碳化硼的配比5∶1。
(3)将水性聚氨酯稀释,浓度如表2所示,聚乙烯醇加水配制为质量百分比浓度为0.5%的聚乙烯醇水溶液,然后将两者混合,再将步骤(2)制备的基料均匀分散在粘结剂溶液中得到涂料,将涂料在磁力搅拌机上搅拌30分钟,使基料均匀分散在粘结剂中;所述涂料中稀释后水性聚氨酯的质量分数为90%、聚乙烯醇水溶液的质量分数为5%、基料的质量分数为5%。
(4)涂覆与烧结:将步骤(3)制备的涂料均匀涂覆到步骤(1)粗化后的铜基体上进行烧结,涂层的涂覆厚度控制在25-30μm之间,烧结温度如表1所示,烧结时间为20min。
表2本实施中聚氨酯浓度与烧结温度
试样号 | 聚氨酯浓度(%) | 烧结温度(℃) |
1# | 10 | 125 |
2# | 10 | 150 |
3# | 10 | 175 |
4# | 15 | 125 |
5# | 15 | 150 |
6# | 15 | 175 |
7# | 20 | 125 |
8# | 20 | 150 |
9# | 20 | 175 |
选取1#、4#、7#试样来分析聚氨酯浓度对红外吸收性能的影响,涂层在400-4000cm-1范围内的红外吸收光谱;如图3所示,物体的反射率、透射率与吸收率之和等于1,并且涂层的透射率可以忽略不计,因此反射率越低的涂层代表其吸收率越高,从图3可知在波数在400-4000cm-1范围内,不同粘结剂浓度的红外吸收涂层均呈现良好的红外吸收性能,吸收率均在95%以上,但其含量的多少对红外吸收性能有一定的影响,随着水性聚氨酯浓度的增加吸收率呈下降趋势,聚氨酯浓度在波数为500-800cm-1范围内的影响较为明显。聚氨酯浓度为10%、15%时,红外吸收性能较为接近,当聚氨酯浓度为20%时,红外吸收性能明显不如前两者。
选取1#、2#、3#试样来分析烧结温度对红外吸收性能的影响,涂层在400-4000cm-1范围内的红外吸收光谱如图4所示;从图4可知波数在1000-4000cm-1范围内,不同烧结温度的红外吸收涂层均呈现良好的红外吸收性能,吸收率均在90%以上。随着烧结温度的增加吸收率呈下降趋势,同样烧结温度的影响在波数为500-1100cm-1范围内的影响较为明显。烧结温度为125℃、150℃时,吸收率较为接近,当烧结温度为175℃时,吸收率下降较为明显,故烧结温度为125℃-150℃时红外吸收性能较好。
实施例3
(1)涂层的抗热震性能分析
抗热震性是指材料承受温度急剧变化而不被破坏的能力。涂层材料与基材的热膨胀系数及弹性模量等性能差异,通过影响温度变化时的涂层热应力,从而影响涂层与基材的结合强度。对样品1#、4#、7#进行了抗热震性的检测,检测方法是将样品在液氮下保持1min左右,然后取出加热至85℃并保温1-2min,上述过程重复30次后,三组试样显检未见裂纹、鼓泡等异常现象。综上所述,同一粘结剂配比、不同烘干温度下得到的样品均有较好的抗热震性。
(2)涂层的附着力分析
影响涂层附着力的因素主要有粘结剂的配比、涂层表面的清洁度和平整度,涂层的厚度,基体的预处理工艺等。本发明对涂层附着力的分析采用的是划格法,划格法是国标GB/T9286-1998,《色漆和清漆漆膜的划格实验》规定的测试方法,具体操作方法是用尖轨的硬质工具刀划边长为1毫米的方格,观察方格内的涂层是否脱落。对样品1#、4#、7#进行附着力分析,实验结果如图5所示,由图可以看出,随着粘结剂中水性聚氨酯浓度的增加,红外吸收涂层与铜基体结合变得更好,表面也会比较光亮,但是会比较难干燥,而且涂层的均匀性没有低浓度的水性聚氨酯的好。
实施例4
微观形貌对材料的红外吸收性能有较大影响,首先分析烧结温度对材料吸收率的影响。选择1#、2#、3#样品进行分析,由图6(a)可以看出在聚合物界面嵌有小的纳米颗粒,烧结致密,形状不规则,聚合物尺寸不超过5μm,随着烧结温度的升高,轮廓变得模糊,聚合物间尺寸增大,当烧结温度达175℃时图6(c),聚合物尺寸明显较小,无清晰的轮廓,涂层的反射率增加,故红外吸收率有所降低。
选取1#、4#、7#样品分析聚氨酯浓度对涂层表面形态的影响,由图7(a)(b)可以看出,1#、4#涂层的表面差异不大,聚氨酯的浓度进一步加大时图7(c),团聚物无清晰轮廓,暗区面积加大,纳米颗粒在高浓度聚氨酯下分散性很差,故红外吸收性能不如1#、4#试样。
Claims (5)
1.一种红外吸收复合涂层的制备方法,其特征在于,具体包括以下步骤:
(1)基体预处理:用砂纸对铜片进行表面的粗化处理,洗净、吹干后备用;
(2)将纳米氧化铜与纳米碳化硼按质量比为3:1~5:1的比例研磨混合均匀得到基料;
(3)将水性聚氨酯稀释到质量百分比浓度为原溶液的10%~15%,聚乙烯醇加水配制为质量百分比浓度为0.5%~0.8%的聚乙烯醇水溶液,然后将两者混合,将步骤(2)制备的基料均匀分散在粘结剂溶液中得到涂料;
(4)涂覆与烧结:将步骤(3)制备的涂料均匀涂覆到步骤(1)粗化后的铜基体上进行烧结。
2.根据权利要求1所述的红外吸收复合涂层的制备方法,其特征在于:基体预处理过程中砂纸的型号为500目。
3.根据权利要求1所述的红外吸收复合涂层的制备方法,其特征在于:步骤(2)所述纳米氧化铜为球形,粒径为37~42nm、纯度≥99.5%;纳米碳化硼粒径为48~52nm,纯度≥99%。
4.根据权利要求1所述的红外吸收复合涂层的制备方法,其特征在于:步骤(3)所述涂料中稀释后水性聚氨酯的质量分数为80%~90%、聚乙烯醇水溶液的质量分数为3%~8%、基料的质量分数为4%~6%。
5.根据利要求1所述的红外吸收复合涂层的制备方法,其特征在于:步骤(4)中烧结温度为125-150℃,烧结时间为10~30min。
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