CN110039841A - 一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法 - Google Patents
一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，涉及电磁隐身复合材料技术领域，该方法以硝酸钴和明胶为原料，通过水热法合成具有蝴蝶结形状的钴离子‑明胶聚合物前驱体；然后热处理制备得到一种具有蝴蝶结形状分级结构的Co/C纳米复合吸波材料。将制备得到的Co/C纳米吸波材料填充到周期性芳纶蜂窝的蜂窝中，并在填充蜂窝的上下侧分别覆盖玻璃纤维增强树脂基复合材料蒙皮和碳纤维增强树脂基复合材料蒙皮，得到蝴蝶结状Co/C纳米复合吸波材料填充的蜂窝夹芯吸波复合材料。在解决了传统吸波材料有效吸收频带窄，力学承载能力差的技术难题。
Description
技术领域
本发明涉及电磁隐身复合材料技术领域，特别是涉及一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法。
背景技术
军用领域随着现代雷达探测技术的发展，以军用战斗机为代表的武器装备受到越来越频繁的跟踪和侦测；同时，在民用领域，无线电通讯技术的发展在带给人们便捷生活的同时也带来了严重的电磁辐射污染问题。因而，能够将电磁波能量转化为热能损耗掉从而显著降低电磁波反射的电磁波吸收材料作为解决上述问题的最有效解决方案收到越来越多的关注。由于实际使用环境的限制，理想的电磁波吸收材料性能特点包括：有效吸收频带宽、材料密度轻、材料厚度薄、力学强度高。磁性钴及其氧化物和碳基体复合吸波材料由于同时对电磁波具有介电损耗和磁滞损耗。成为目前研究最广泛的吸波剂之一，磁性Co/C纳米复合材料的碳基体对电磁波具有优异的介电损耗性能，而畴壁共振和自然共振是其钴及其氧化物最主要的磁损耗吸收机理。磁性Co/C纳米复合材料具有磁矫顽力高、吸波强度高、制备简单等优点，且作为双损耗介质，对电磁波既有磁损耗又有介电损耗，但其相对密度大、吸收频带窄等缺点难以满足优秀吸波剂“薄、轻、宽、强”的要求，限制了其进一步的应用。同时传统磁性Co/C 纳米复合材料多呈粉末状使用工艺以和涂料混合制成吸波涂料为主，使用过程易磨损脱落，难以满足现代飞行器对于雷达吸波材料结构承载和电磁吸波功能一体化的要求。
发明内容
为了克服上述传统磁性Co/C纳米复合材料多呈粉末状使用工艺以和涂料混合制成吸波涂料为主，相对密度大、吸收频带窄，力学承载能力差、使用过程易磨损脱落，难以满足现代飞行器对于雷达吸波材料结构承载和电磁吸波功能一体化的要求等现有技术的不足，本发明提供了一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法。
本发明所采用的技术方案是：以硝酸钴、明胶、尿素为原料三步法制成，首先以硝酸钴和明胶为原料，通过溶液热法制备出长链状钴离子-明胶分子金属离子聚合物有机框架；然后以尿素作为辅助沉淀剂，通过高压反应釜高温水热法合成具有蝴蝶结形状的金属离子-聚合物配合前驱体；然后经过干燥处理后采用高温热处理的方法，将Co金属离子和明胶聚合物配合前驱体，制备成为一种具有蝴蝶结形状分级结构的Co/C纳米复合吸波材料。将制备得到的蝴蝶结状Co/C纳米复合吸波材料填充到周期性芳纶蜂窝的蜂窝孔中，并在填充蜂窝的上下侧分别覆盖玻璃纤维增强树脂基复合材料蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米复合吸波材料填充的蜂窝夹芯吸波复合材料。采用国军标GJB 2038A-2011 弓形框法对复合材料板2-18GHz电磁波反射率进行测试，3mm厚度下反射损耗低于-10dB的有效吸收频带宽度9.8GHz，最大吸收强度达到-49.9dB。
具体为：
(1)将硝酸钴、尿素溶解在去离子水中，搅拌溶解，得液体A；将明胶加热、搅拌溶解在去离子水中，得液体B；然后将液体A和液体B混合，加热反应，得到钴离子-明胶分子金属离子聚合物有机框架胶状混合溶液。
(2)取(1)中得到的胶状混合溶液加入聚四伏乙烯内胆反应釜中，高温水热反应得到蝴蝶结状前驱体，离心收集沉淀，干燥。
(3)将(2)中得到的干燥后的蝴蝶结状前驱体样品，置于管式炉中，保护性气体下高温热处理2h得到蝴蝶结形状的Co/C纳米吸波材料。
(4)将(3)中制备的蝴蝶结形状的Co/C纳米吸波材料填充到周期性芳纶蜂窝板中，采用胶膜粘结的方法在蜂窝板上下分别加盖1mm厚玻璃纤维增强树脂基复合材料透波蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料。
优选的，步骤(1)中硝酸钴与尿素的质量比为1:1；硝酸钴、尿素溶解在去离子水中，硝酸钴与去离子水的质量体积比(g/mL)为1:16；明胶加热温度为50℃；明胶溶解在去离子水中，明胶与去离子水的质量体积比(g/mL)为1:5-1:10；所述液体A与液体B混合，液体 A中硝酸钴与液体B中明胶的质量比为1:0.5-1:2；液体A与液体B混合后加热搅拌反应，温度为60℃-80℃，时间为1h。
优选的，步骤(2)所述高温水热反应温度为100℃-110℃，反应时间为6-10h；离心时间为5-15min，离心条件为7000-9000rpm；所述干燥，温度不得超过80℃。
优选的，步骤(3)所述保护气体为氮气或氩气；所述高温热处理，温度为400℃-600℃。
优选的，步骤(4)所述周期性芳纶蜂窝板，孔径为2mm-10mm；填充后的蜂窝板上表面覆盖的玻璃纤维增强树脂基复合材料透波蒙皮的树脂基体是环氧树脂或氰酸酯树脂。
与现有技术相比，本发明的有益效果是
(1)采用水热法合成了具有特殊蝴蝶结形状的钴离子明胶金属有机框架前驱体，并通过热处理得到了Co/C磁性纳米复合吸波材料，通过对水热反应时间的控制可以实现对产物蝴蝶结状形貌饱和度的有效调控。
(2)采用Co/C磁性纳米复合材料吸波剂和蜂窝夹芯结构复合的方法，制备了具有力学承载能力的宽频吸波复合材料，通过调整纤维增强树脂基复合材料蒙皮中纤维的铺层方案可以有效控制复合材料的力学强度，实现吸波复合材料结构承载和吸波功能的一体化设计。
(3)与其他材料复合，提高了结构承载和吸波性能。通过Co/C纳米复合吸波材料和特殊结构的复合，实现了宽频吸波效果的同时，降低了材料厚度，提升了材料整体力学强度。
附图说明
图1为实施例1制备的蝴蝶结状Co-明胶金属有机框架前驱体SEM照片；
图2为实施例1制备的蝴蝶结状磁性Co/C纳米复合材料SEM照片；
图3为实施例1制备的蝴蝶结状Co/C纳米材料填充的蜂窝夹芯结构复合材料示意图；
图4为实施例1制备的蝴蝶结状Co/C纳米材料填充的蜂窝夹芯结构复合材料板2-18GHz 的电磁波反射率。
具体实施方式
下面结合附图对本发明进一步说明。
实施例1
(1)将硝酸钴、尿素溶解在去离子水中速磁力搅拌30min至全部溶解，得到液体A；将明胶 50℃加热、中速磁力搅拌条件下溶解在去离子水中，保持搅拌状态30min，得到液体B；然后将硝酸钴和尿素混合溶液和明胶溶液(即液体A和液体B)加入250mL单口烧瓶中混合，加热条件下磁力搅拌反应，得到钴离子-明胶分子金属离子聚合物有机框架紫色胶状混合溶液。
(2)取(1)中得到的紫色胶状混合溶液加入100mL聚四伏乙烯内胆反应釜中，水热反应一定时间得到蝴蝶结状前驱体(见附图1)，离心收集沉淀，干燥24h待用。
(3)将(2)中得到的干燥后的蝴蝶结状前驱体样品，置于管式炉中，保护性气体下热处理得到蝴蝶结形状的Co/C纳米吸波材料(见附图2)。
(4)将50g(3)中制备的蝴蝶结形状的Co/C纳米吸波材料填充到外形尺寸为 300mm×300mm×3mm的周期性芳纶蜂窝板中，采用胶膜粘结的方法在蜂窝板上下分别加盖 1mm厚玻璃纤维增强树脂基复合材料透波蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料(见附图3)。
步骤(1)中硝酸钴与尿素的质量比为1:1；硝酸钴、尿素溶解在去离子水中，硝酸钴与去离子水的质量体积比(g/mL)为1:16；明胶加热温度为50℃；明胶溶解在去离子水中，明胶与去离子水的质量体积比(g/mL)为1:8；所述液体A与液体B混合，液体A中硝酸钴与液体B中明胶的质量比为1:2；液体A与液体B混合后加热搅拌反应，温度为70℃，时间为1h。步骤(2)所述高温水热反应温度为100℃，反应时间为6h；离心时间为10min，离心条件为9000rpm；所述干燥，温度80℃。
步骤(3)所述保护气体为氮气；所述高温热处理，温度为800℃。
步骤(4)所述周期性芳纶蜂窝板，孔径为4mm；填充后的蜂窝板上表面覆盖的玻璃纤维增强树脂基复合材料透波蒙皮的树脂基体是环氧树脂。
(5)采用国军标GJB 2038A-2011电磁吸波材反射率弓形框法，对制得的蝴蝶结状Co/C 纳米材料填充的蜂窝夹芯结构复合材料板2-18GHz电磁波反射率进行测试，3mm厚度下反射损耗低于-10dB的有效吸收频带宽度9.8GHz，最大吸收强度达到-49.9dB(见附图4)。
实施例2
(1)将硝酸钴、尿素溶解在去离子水中速磁力搅拌30min至全部溶解，得到液体A；将明胶 50℃加热、中速磁力搅拌条件下溶解在去离子水中，保持搅拌状态30min，得到液体B；然后将硝酸钴和尿素混合溶液和明胶溶液(即液体A和液体B)加入250mL单口烧瓶中混合，加热条件下磁力搅拌反应，得到钴离子-明胶分子金属离子聚合物有机框架紫色胶状混合溶液。
(2)取(1)中得到的紫色胶状混合溶液加入100mL聚四伏乙烯内胆反应釜中，水热反应一定时间得到蝴蝶结状前驱体，离心收集沉淀，干燥24h待用。
(3)将(2)中得到的干燥后的蝴蝶结状前驱体样品，置于管式炉中，保护性气体下热处理得到蝴蝶结形状的Co/C纳米吸波材料。
(4)将50g(3)中制备的蝴蝶结形状的Co/C纳米吸波材料填充到外形尺寸为 300mm×300mm×3mm的周期性芳纶蜂窝板中，采用胶膜粘结的方法在蜂窝板上下分别加盖 1mm厚玻璃纤维增强树脂基复合材料透波蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料。
步骤(1)中硝酸钴与尿素的质量比为1:1；硝酸钴、尿素溶解在去离子水中，硝酸钴与去离子水的质量体积比(g/mL)为1:16；明胶加热温度为50℃；明胶溶解在去离子水中，明胶与去离子水的质量体积比(g/mL)为1:5；所述液体A与液体B混合，液体A中硝酸钴与液体B中明胶的质量比为1:0.5；液体A与液体B混合后加热搅拌反应，温度为60℃，时间为1h。步骤(2)所述高温水热反应温度为100℃，反应时间为6h；离心时间为5min，离心条件为7000rpm；所述干燥，温度80℃。
步骤(3)所述保护气体为氩气；所述高温热处理，温度为400℃。
步骤(4)所述周期性芳纶蜂窝板，孔径为2mm；填充后的蜂窝板上表面覆盖的玻璃纤维增强树脂基复合材料透波蒙皮的树脂基体是氰酸酯树脂。
(5)采用国军标GJB 2038A-2011电磁吸波材反射率弓形框法，对制得的蝴蝶结状Co/C 纳米材料填充的蜂窝夹芯结构复合材料板2-18GHz电磁波反射率进行测试，3mm厚度下反射损耗低于-10dB的有效吸收频带宽度8.5GHz，最大吸收强度达到-38dB。
实施例3
(1)将硝酸钴、尿素溶解在去离子水中速磁力搅拌30min至全部溶解，得到液体A；将明胶 50℃加热、中速磁力搅拌条件下溶解在去离子水中，保持搅拌状态30min，得到液体B；然后将硝酸钴和尿素混合溶液和明胶溶液(即液体A和液体B)加入250mL单口烧瓶中混合，加热条件下磁力搅拌反应，得到钴离子-明胶分子金属离子聚合物有机框架紫色胶状混合溶液。
(2)取(1)中得到的紫色胶状混合溶液加入100mL聚四伏乙烯内胆反应釜中，水热反应一定时间得到蝴蝶结状前驱体，离心收集沉淀，干燥24h待用。
(3)将(2)中得到的干燥后的蝴蝶结状前驱体样品，置于管式炉中，保护性气体下热处理得到蝴蝶结形状的Co/C纳米吸波材料。
(4)将50g(3)中制备的蝴蝶结形状的Co/C纳米吸波材料填充到外形尺寸为 300mm×300mm×3mm的周期性芳纶蜂窝板中，采用胶膜粘结的方法在蜂窝板上下分别加盖 1mm厚玻璃纤维增强树脂基复合材料透波蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料。
步骤(1)中硝酸钴与尿素的质量比为1:1；硝酸钴、尿素溶解在去离子水中，硝酸钴与去离子水的质量体积比(g/mL)为1:16；明胶加热温度为50℃；明胶溶解在去离子水中，明胶与去离子水的质量体积比(g/mL)为1:10；所述液体A与液体B混合，液体A中硝酸钴与液体B中明胶的质量比为1:2；液体A与液体B混合后加热搅拌反应，温度为80℃，时间为1h。步骤(2)所述高温水热反应温度为110℃，反应时间为10h；离心时间为15min，离心条件为9000rpm；所述干燥，温度70℃。
步骤(3)所述保护气体为氮气；所述高温热处理，温度为800℃。
步骤(4)所述周期性芳纶蜂窝板，孔径为10mm；填充后的蜂窝板上表面覆盖的玻璃纤维增强树脂基复合材料透波蒙皮的树脂基体是氰酸酯树脂。
(5)采用国军标GJB 2038A-2011电磁吸波材反射率弓形框法，对制得的蝴蝶结状Co/C 纳米材料填充的蜂窝夹芯结构复合材料板2-18GHz电磁波反射率进行测试，3mm厚度下反射损耗低于-10dB的有效吸收频带宽度7.6GHz，最大吸收强度达到-35dB。
Claims (9)
1.一种蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，其特征在于：以硝酸钴、明胶、尿素为原料三步法制成；首先以硝酸钴和明胶为原料，通过溶液热法制备出长链状钴离子-明胶分子金属离子聚合物有机框架；然后以尿素作为辅助沉淀剂，通过高温水热法合成具有蝴蝶结形状的金属离子-聚合物配合前驱体；然后经过干燥处理后采用高温热处理的方法，将Co金属离子和明胶聚合物配合前驱体，制备成为一种具有蝴蝶结状Co/C纳米复合吸波材料；将制备得到的蝴蝶结状Co/C纳米复合吸波材料填充到周期性芳纶蜂窝的蜂窝孔中，并在填充蜂窝的上下侧分别覆盖玻璃纤维增强树脂基复合材料蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米复合吸波材料填充的蜂窝夹芯吸波复合材料。
2.根据权利要求1所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，其特征在于，该方法的具体步骤为：
(1)将硝酸钴、尿素溶解在去离子水中，搅拌溶解，得液体A；将明胶加热、搅拌溶解在去离子水中，得液体B；然后将液体A和液体B混合，加热反应，得到钴离子-明胶分子金属离子聚合物有机框架胶状混合溶液；
(2)取(1)中得到的胶状混合溶液进行高温水热反应得到蝴蝶结状前驱体，离心收集沉淀，干燥；
(3)将(2)中得到的干燥后的蝴蝶结状前驱体样品，置于管式炉中，保护性气体下高温热处理2h得到蝴蝶结形状的Co/C纳米吸波材料；
(4)将(3)中制备的蝴蝶结形状的Co/C纳米吸波材料填充到周期性芳纶蜂窝板中，采用胶膜粘结的方法在蜂窝板上下分别加盖1mm厚玻璃纤维增强树脂基复合材料透波蒙皮和碳纤维增强树脂基复合材料蒙皮，最终得到蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料。
3.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，其特征在于：步骤(1)中硝酸钴与尿素的质量比为1:1；硝酸钴、尿素溶解在去离子水中，硝酸钴与去离子水的质量体积比(g/mL)为1:16。
4.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，其特征在于：步骤(1)所述明胶加热温度为50℃；明胶溶解在去离子水中，明胶与去离子水的质量体积比(g/mL)为1:5-1:10。
5.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料的制备方法，其特征在于：步骤(1)所述液体A与液体B混合，液体A中硝酸钴与液体B中明胶的质量比为1:0.5-1:2；液体A与液体B混合后加热搅拌反应，温度为60℃-80℃，时间为1h。
6.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料制备方法，其特征在于：步骤(2)所述高温水热反应温度为100℃-110℃，反应时间为6-10h。
7.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料制备方法，其特征在于：步骤(2)所述离心时间为5-15min，离心条件为7000-9000rpm；所述干燥，温度不得超过80℃。
8.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料制备方法，其特征在于：步骤(3)所述保护气体为氮气或氩气；所述高温热处理，温度为400℃-800℃。
9.根据权利要求2所述的蝴蝶结状Co/C纳米吸波材料填充的蜂窝夹芯结构吸波复合材料制备方法，其特征在于：步骤(4)所述周期性芳纶蜂窝板，孔径为2mm-10mm；填充后的蜂窝板上表面覆盖的玻璃纤维增强树脂基复合材料透波蒙皮的树脂基体是环氧树脂或氰酸酯树脂。
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