CN117117516A - 一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法 - Google Patents
一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法 Download PDFInfo
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Abstract
本发明属于B5G技术领域,具体为一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法。本发明提出的制备方法,是将碱式碳酸盐包覆在缓释膜中,再与酸性聚合物一起,分散到热熔胶中,搅拌,然后置于热转印机中,热压成膜,室温放置一段时间,得有机/无机杂化型亚太赫兹吸波薄膜。本发明具有以下优点:(1)在B5G技术亚太赫兹频段的吸收效能大于40dB,而反射效能小于0.01dB,避免了反射电磁波耦合干扰;(2)薄膜厚度可调,适合于B5G电路板有限空间的电磁兼容;(3)利用缓释膜控制酸碱反应速率,将水固定在薄膜中,在亚太赫兹波辐照下,产生共振或弛豫,达到强吸波、低反射的效果。
Description
技术领域
本发明属于B5G技术领域,具体涉及一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法。
背景技术
5G由移动互联网拓展到物联网领域,开启了产业互联网新时代,5G的成功商用将成为B5G(Beyond 5G)发展的基础,但部分应用场景的性能需求超过了5G能力。
美国国家标准研究院指出,B5G是指未来几代移动无线通信***,这些下一代***的愿景是实现开创性的移动应用,除了大容量(超过1000倍)和连接(数十亿用户和机器)外,还需要高质量的低延迟视觉、触觉和音频临场感。下一代移动通信已经开始利用毫米波(0.03–0.3THz)的可用频率,在这种频率下,高功率发射机可以使用数十到数百个天线(通常称为大规模MIMO天线)来恢复高传播损耗。天线的数量越大,通过组合每个天线的单独功率(也称为波束形成)可以实现的发射功率越高。业界已经在探索使用大规模MIMO天线阵列,以增加同时传输容量;毫米波频谱,以缓解当前频带中的频谱紧缩;以及超密集网络,以允许短距离、高速数据传输(https://www.nist.gov/programs-projects/5g-beyond)。
B5G研究主要集中在毫米波(0.03~0.3THz)频段,与亚太赫兹频段(0.1~0.3THz)及6G频段(0.1~3.0 THz )有重叠。
美国伍斯特理工学院的Titova LV等以溶液法制备了柔性MXene (Ti3C2Ty)薄膜[Nano Letters, 2020, 20, 636-643.],有极高的导电率和太赫兹电磁屏蔽效能,且屏蔽效能可以调制,Ti3C2Ty与各种衬底的兼容性,使得这类二维材料在太赫兹技术和电磁屏蔽中有广泛应用。波兰华沙工业大学的Zeranska-Chudek K等利用太赫兹时域光谱研究了0.7mm厚的PDMS、PDMS/石墨烯(1 wt%)、PDMS/MXene(1 wt%)的太赫兹屏蔽性能[Journal ofApplied Polymer Science, 2021,138: e49962],PDMS的屏蔽效能约6dB,PDMS/MXene约11dB,PDMS/石墨烯为21.9~54.9 dB,复合材料的介电损耗均较低。美国加州大学河边分校的Balandin AA 等研究了填充型石墨烯环氧树脂复合材料的电磁屏蔽性能[ACS AppliedMaterials&Interfaces, 2020, 12: 28635-28644],在0.22~0.30THz频段,石墨烯负载量为8wt%时,1mm厚的环氧树脂复合薄膜的电阻率为1.51×105Ω.cm,最大屏蔽效能为70dB,但对应的频带较窄,频率较低。湖南大学谭勇文教授等将MXene与氧化石墨烯混合,用离子扩散诱导凝胶化的方法制备85μm厚的MXene泡沫[ACS Nano, 2020, 14:2109-2117],其中MXene片被多价金属离子和氧化石墨烯交联以形成定向多孔结构,该泡沫导电率为5671.8S/m,在0.2~0.3THz频段的最大电磁屏蔽效能为51dB,为研制高性能太赫兹屏蔽材料提供了新的思路。电子科技大学文岐业教授、肖旭教授等将聚氨酯泡沫浸渍在Ti3C2Tx溶液中,制备10mm厚的MXene海绵泡沫(MSF)[Advanced Optical Materials, 2020, 8: 2001120],在0.3THz的吸收率超过99.99%(屏蔽效能>40dB),该泡沫在雷达隐身、电磁屏蔽和B5G通信等领域具有潜在应用。
总之,目前的亚太赫兹吸波材料大多是导电粒子填充型材料,而绝缘粒子填充型吸波材料比较少。绝缘型薄膜材料在B5G电子器件中可以实现 “封装-吸波”一体化,节约电路板上空间,提升电路板集成度,具有极大的应用价值。
发明内容
本发明目的是提出一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法。
本发明提出有机/无机杂化型亚太赫兹吸波薄膜的制备方法,其特征在于,将1~3g碱式碳酸盐、10~15g取代甲基纤维素、50~100ml乙醇水溶液混合,搅拌30~45分钟,加热,蒸除溶剂,固体粉碎,过筛,得800~1000目的甲基纤维素包覆碱式碳酸盐粉末;将3~5g甲基纤维素包覆碱式碳酸盐粉末、1~3g酸性聚合物,分散到50~80g热熔胶中,搅拌,然后置于热转印机中,于120~150℃热压成膜,室温冷却6~12小时,得有机/无机杂化型亚太赫兹吸波薄膜。
其中,碱式碳酸盐为碱式碳酸铜、碱式碳酸钙、碱式碳酸锌、碱式碳酸镁或碱式碳酸铋中的任意一种。
其中,取代甲基纤维素为羟甲基纤维素或羟丙基甲基纤维素中的任意一种。
其中,乙醇水溶液的溶质为乙醇,溶剂为水,质量百分比浓度为20%~30%。
其中,酸性聚合物为聚丙烯酸或聚苯乙烯磺酸中的任意一种。
其中,热熔胶为乙烯-醋酸乙烯酯共聚物、聚氨基甲酸酯、聚己二酰己二胺或聚丁二酸乙二醇酯中的任意一种。
上述有机/无机杂化型亚太赫兹吸波薄膜样品吸波效能测试是通过太赫兹时域光谱***实现的,测试波长为0.1~0.3 THz;分别采用了透射模式和反射模式两种光路,对薄膜样品的总屏蔽效能和反射效能进行检测,吸收效能为总屏蔽效能减去反射效能。测得该薄膜在0.1~0.3THz频段的吸收效能为43.2~53.1dB,反射效能为0.007~0.01dB;用膜厚仪测得薄膜厚度为0.01~0.05mm。
因此,本发明具有以下优点:
(1)在B5G亚太赫兹频段(0.1~0.3THz)的吸收效能大于40dB,可用于民用电子元件及电路板电磁兼容(民用标准为≥30dB)。
(2)反射效能≤0.01dB,能极大降低反射电磁波耦合干扰,从源头上降低辐射源的自损伤。
(3)利用取代甲基纤维素为缓释膜,控制碱式碳酸盐与酸性聚合物的接触反应,保持吸波薄膜的水含量,在亚太赫兹波辐射下,类似微波炉效应,水产生共振弛豫,将电磁波能量转化为热能,极大提升吸收效能,降低反射效能。
附图说明
图1为有机/无机杂化型亚太赫兹吸波薄膜的扫描电镜照片图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细描述。
实施例1
将1g碱式碳酸铜、10g羟甲基纤维素、50ml质量百分比浓度为30%的乙醇水溶液混合,搅拌30分钟,加热,蒸除溶剂,固体粉碎,过筛,得800目的羟甲基纤维素包覆碱式碳酸铜粉末;将3g羟甲基纤维素包覆碱式碳酸铜粉末、1g聚丙烯酸,分散到50g乙烯-醋酸乙烯酯共聚物热熔胶中,搅拌,然后置于热转印机中,于120℃热压成膜,室温冷却6小时,得有机/无机杂化型亚太赫兹吸波薄膜。将薄膜样品被裁剪为1 cm ×1 cm平面大小,利用太赫兹时域光谱***测得薄膜样品在0.1~0.3THz频段的总屏蔽效能为43.21~51.32dB,反射效能为0.007~0.009dB,计算得到吸收效能为43.203~51.311dB;用膜厚仪测得薄膜厚度为0.01mm。
实施例2
将3g碱式碳酸钙、15g羟丙基甲基纤维素、100ml质量百分比浓度为20%的乙醇水溶液混合,搅拌45分钟,加热,蒸除溶剂,固体粉碎,过筛,得1000目的羟丙基甲基纤维素包覆碱式碳酸钙粉末;将5g羟丙基甲基纤维素包覆碱式碳酸钙粉末、3g聚苯乙烯磺酸,分散到80g聚氨基甲酸酯热熔胶中,搅拌,然后置于热转印机中,于150℃热压成膜,室温冷却12小时,得有机/无机杂化型亚太赫兹吸波薄膜。将薄膜样品被裁剪为1 cm × 1 cm平面大小,利用太赫兹时域光谱***测得薄膜样品在0.1~0.3THz频段的总屏蔽效能为45.63~53.10dB,反射效能为0.009~0.01dB,计算得到吸收效能为45.621~53.09dB;用膜厚仪测得薄膜厚度为0.05mm。
实施例3
将2g碱式碳酸锌、12g羟甲基纤维素、80ml质量百分比浓度为25%的乙醇水溶液混合,搅拌40分钟,加热,蒸除溶剂,固体粉碎,过筛,得900目的羟甲基纤维素包覆碱式碳酸锌粉末;将4g羟甲基纤维素包覆碱式碳酸锌粉末、2g聚丙烯酸,分散到60g聚己二酰己二胺热熔胶中,搅拌,然后置于热转印机中,于140℃热压成膜,室温冷却8小时,得有机/无机杂化型亚太赫兹吸波薄膜。将薄膜样品被裁剪为1 cm × 1 cm平面大小,利用太赫兹时域光谱***测得薄膜样品在0.1~0.3THz频段的总屏蔽效能为44.98~52.17dB,反射效能为0.007~0.008dB,计算得到吸收效能为44.973~51.162dB;用膜厚仪测得薄膜厚度为0.03mm。
实施例4
将2.5g碱式碳酸镁、13g羟丙基甲基纤维素、70ml质量百分比浓度为20%的乙醇水溶液混合,搅拌35分钟,加热,蒸除溶剂,固体粉碎,过筛,得800目的羟丙基甲基纤维素包覆碱式碳酸镁粉末;将4.5g羟丙基甲基纤维素包覆碱式碳酸镁粉末、2.5g聚苯乙烯磺酸,分散到65g聚丁二酸乙二醇酯热熔胶中,搅拌,然后置于热转印机中,于145℃热压成膜,室温冷却7小时,得有机/无机杂化型亚太赫兹吸波薄膜。将薄膜样品被裁剪为1 cm × 1 cm平面大小,利用太赫兹时域光谱***测得薄膜样品在0.1~0.3THz频段的总屏蔽效能为43.33~51.88dB,反射效能为0.008~0.009dB,计算得到吸收效能为43.322~51.871dB;用膜厚仪测得薄膜厚度为0.04mm。
实施例5
将1.5g碱式碳酸铋、14g羟甲基纤维素、60ml质量百分比浓度为25%的乙醇水溶液混合,搅拌35分钟,加热,蒸除溶剂,固体粉碎,过筛,得1000目的羟甲基纤维素包覆碱式碳酸铋粉末;将5g羟甲基纤维素包覆碱式碳酸铋粉末、1.5g聚苯乙烯磺酸,分散到70g乙烯-醋酸乙烯酯共聚物热熔胶中,搅拌,然后置于热转印机中,于130℃热压成膜,室温冷却8小时,得有机/无机杂化型亚太赫兹吸波薄膜。将薄膜样品被裁剪为1 cm × 1 cm平面大小,利用太赫兹时域光谱***测得薄膜样品在0.1~0.3THz频段的总屏蔽效能为44.45~51.96dB,反射效能为0.009~0.01dB,计算得到吸收效能为44.441~51.95dB;用膜厚仪测得薄膜厚度为0.02mm。
Claims (3)
1.一种有机/无机杂化型亚太赫兹吸波薄膜的制备方法,其特征在于,具体步骤如下:
(1)复合:将1~3g碱式碳酸盐、10~15g取代甲基纤维素、50~100ml乙醇水溶液混合,搅拌30~45分钟,加热,蒸除溶剂,固体粉碎,过筛,得800~1000目的甲基纤维素包覆碱式碳酸盐粉末;其中,碱式碳酸盐为碱式碳酸铜、碱式碳酸钙、碱式碳酸锌、碱式碳酸镁或碱式碳酸铋中的任意一种;其中,取代甲基纤维素为羟甲基纤维素或羟丙基甲基纤维素中的任意一种;其中,乙醇水溶液的溶质为乙醇,溶剂为水,质量百分比浓度为20%~30%;
(2)成膜:将3~5g 800~1000目的甲基纤维素包覆碱式碳酸盐粉末、1~3g酸性聚合物,分散到50~80g热熔胶中,搅拌,然后置于热转印机中,于120~150℃热压成膜,室温冷却6~12小时,得有机/无机杂化型亚太赫兹吸波薄膜;其中,酸性聚合物为聚丙烯酸或聚苯乙烯磺酸中的任意一种;其中,热熔胶为乙烯-醋酸乙烯酯共聚物、聚氨基甲酸酯、聚己二酰己二胺或聚丁二酸乙二醇酯中的任意一种。
2.根据权利要求1所述的有机/无机杂化型亚太赫兹吸波薄膜的制备方法,其特征在于,有机/无机杂化型亚太赫兹吸波薄膜的吸收效能测试是通过太赫兹时域光谱***实现的,测试波长为0.1~0.3 THz;分别采用了透射模式和反射模式两种光路,对总屏蔽效能和反射效能进行检测,吸收效能为总屏蔽效能减去反射效能。
3.根据权利要求1所述的有机/无机杂化型亚太赫兹吸波薄膜的制备方法,其特征在于,有机/无机杂化型亚太赫兹吸波薄膜在0.1~0.3THz频段的吸收效能为43.2~53.1dB,反射效能为0.007~0.01dB;用膜厚仪测得有机/无机杂化型亚太赫兹吸波薄膜的厚度为0.01~0.05mm。
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