CN112521155A - 一种新型陶瓷吸波微球材料及其制备方法 - Google Patents
一种新型陶瓷吸波微球材料及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种新型陶瓷吸波微球材料及其制备方法。所述制备方法包括以下步骤:磁性粉末与PSA液体的混合,混合物连续相中乳化;乳液固化;前体微球与连续相的分离;磁性聚合物的陶瓷化处理。本发明实施例示例的新型陶瓷吸波微球材料的制备方法,工艺简单,易于在简易的条件下制备,同时可以实现大规模工业化生产。本发明实施例示例的新型陶瓷吸波微球材料的制备方法制备得到的吸波材料具有良好的球形形貌,聚硅乙炔具有活性反应位点,成分结构可调,可与磁性物质反应交联,通过调节磁性物质的成分和含量形成不同的微观结构,改变制备得到的吸波材料对电磁波的吸收和反射能力。
Description
技术领域
本发明涉及陶瓷吸波材料及其制备方法,尤其涉及新型的陶瓷吸波微球材料及其制备方法。
背景技术
随着现代技术的发展,电磁波被广泛用于无线通信系统,数据传输,卫星发射和雷达隐身技术领域。然而,电磁波造成的电磁污染严重威胁着人类的健康,工作和生活。因此有效屏蔽或吸收电磁波是当前信息化中迫切需要解决的问题。同时,电磁吸收材料的应用已成为军事领域的主要方向。因此,开发具有显着电磁吸收和宽工作频率的先进吸收材料是非常紧迫的,具有重要意义。
现代吸收材料正朝着介电和磁性轻质复合材料的方向发展。综合性能满足吸收材料“薄,宽,轻,强”的要求。磁性金属/合金颗粒因其出色的电磁性能而被公认为是电磁波吸收(EMA)的最有希望的候选者。在高于居里点的温度下,铁氧体和羰基铁基磁性吸收剂的磁性会消失,并且电磁吸收性能也会丧失。另外,由于它们较低的铁磁共振频率,它们不能在高频下使用。作为铁氧体的替代品,磁性合金具有高居里点以确保即使在高温下也具有活性,例如Co-Fe,Fe-Si和Co-Si合金。陶瓷材料由于具有热稳定性,抗辐射性和良好的机械性能而具有电磁吸收的潜力,尤其是聚合物衍生的陶瓷(PDC)。通过PDC,电磁吸收材料在成分,形貌和结构上具有很大的可变性。与其他陶瓷相比,SiCO陶瓷具有合适的阻抗匹配,良好的机械性能以及即使在空气中1000°C下仍具有较高的热稳定性。
发明内容
本发明的目的在于提供一种新型的陶瓷吸波微球材料及其制备方法,本发明通过将聚硅乙炔和磁性物质的混合物乳化制备了陶瓷吸波微球材料,聚硅乙炔作为SiCO陶瓷先驱体制备的吸波材料具有较好的高温稳定性,制备的微球吸波材料具有良好的球形形貌,提供良好的界面效果,磁性成分的引入提高材料磁损耗,制备的磁性陶瓷微球具有较强的吸波性能。
第一方面,本申请实施例提供了一种新型的陶瓷吸波微球材料的制备方法,包括以下步骤:将磁性粉末加入到PSA液体中,然后将混合物滴入二甲基硅油中搅拌乳化;烘箱中固化乳液;然后将前体微球与二甲基硅油分离;磁性聚合物的陶瓷化处理。
优选的:所述磁性物质选自氯化铁、氯化钴、氯化镍、硝酸铁、硝酸钴、硝酸镍、乙酰丙酮铁、乙酰丙酮钴、乙酰丙酮镍、铁钴镍金属粉中的一种以上。
优选的:所述聚硅乙乙炔溶液中乙酰丙酮铁、乙酰丙酮钴、乙酰丙酮镍的质量比为1%-20%。
优选的:所述聚硅乙炔可以用聚碳硅烷、聚硅氧烷替代。
优选的:所述乳化具体步骤如下:连续相可以用二甲基硅油、甘油,二甲基硅油的粘度为350-50000mP∙s,搅拌速度为400-1500转/分钟。
优选的:所述乳液固化具体步骤如下:将混合后的乳液进行加热固化,固化温度选择在180-300℃,并保温2-6小时。
优选的:所述前体微球与二甲基硅油分离具体步骤如下:将前体微球与二甲基硅油的乳液溶解分散于正己烷、四氢呋喃或二甲苯溶液中,超声分散30-60分钟,然后在5000-10000转/分钟转速下离心5-20分钟取下层粉末,重复上述过程2-5次得到磁性聚合物微球。
优选的:所述磁性聚合物微球陶瓷化具体步骤如下:将聚合物微球分散于正己烷或四氢呋喃溶液中,超声处理10-20分钟,烘干后在氮气或者氩气气氛下进行烧结,烧结温度为800-1400℃,保温1-4小时,升温速率为1-5℃/min。
第二方面,本申请实施例提供了一种由上述任一所述的制备方法制备得到的陶瓷吸波微球材料。
综上所述,本发明提供了一种先驱体转化碳化硅陶瓷及其制备方法。本发明的方案具有以下优点:
1、本发明实施例示例的新型的陶瓷吸波微球材料的制备方法,工艺简单,易于在简易的条件下制备,同时可以实现大规模工业化生产;
2、本发明实施例示例的陶瓷吸波微球的制备方法制备得到的吸波微球具有良好的球形形貌,可以提供较好的界面效应;
3、本发明实施例示例的聚硅乙炔具有较好的流动性和溶解性,可溶解于正己烷、无水乙醇、四氢呋喃;
4、本发明实施例示例的聚硅乙炔具有活性反应位点,成分结构可调,可与磁性物质反应交联,通过调节磁性物质的成分和含量形成不同的微观结构,改变制备得到的吸波材料对电磁波的吸收和反射能力。
附图说明
图1为本发明实施例示例的吸波微球热固化后的红外图。
图2为本发明实施例示例的加入乙酰丙酮铁、乙酰丙酮钴、乙酰丙酮镍后陶瓷吸波微球的XRD图。
图3为本发明实施例示例的含钴的陶瓷吸波微球的吸波性能图。
具体实施方式
为了更好的说明本发明的技术方案,下面结合附图和具体实施例对本发明制备陶瓷吸波微球作进一步详细介绍。
实施例1
将乙酰丙酮铁粉末(1g)加入到聚硅乙炔液体(9g)中,同时加入适量的四氢呋喃,使乙酰丙酮铁粉末完全溶解并通过搅拌混合。将混合物滴入二甲基硅油中,并以1000rpm搅拌。搅拌2小时后,在烘箱中200℃固化4小时,然后通过离心将前体微球与二甲基硅油分离;
分离后获得的含铁树脂微球的红外图如图1所示,在2165cm-1 2040 cm-1处的峰分别是-Si-H键和-C≡C-拉伸振动的峰,1260 cm-1和1420 cm-1是由于Si-CH3振动引起的。尤其是PSA的Si-H键与乙酰丙酮铁反应,生成了一个新的Si-O-Fe键,对应于1023至1016 cm-1的范围,这使-Si-O-在1037 cm-1处的峰变宽,同时在2165 cm-1处的Si-H键减弱,在1571 cm-1处的乙酰丙酮的-C=O键同时出现。
实施例2
首先,将乙酰丙酮镍粉末(1g)加入到PSA液体(9g)中,同时加入适量的四氢呋喃,使乙酰丙酮镍粉末完全溶解并通过搅拌混合。将混合物滴入二甲基硅油中,并以1000rpm搅拌。搅拌2小时后,按照以下步骤在烘箱中固化乳液:180℃保温1小时,200℃保温1小时,220℃保温2小时。然后通过离心将前体微球与二甲基硅油分离。分离后,在高温氧化铝管式炉中在超高纯氮气氛下进行聚合物的热解。以3℃/ min的加热速率将管式炉从室温加热至1000℃,再保持2小时。制备的陶瓷吸波微球的XRD图如图2所示。样品在35.54°,59.92°和71.69°处出现了SiC相的峰,分别对应于晶格平面(111),(220)和(311)。Fe3Si在27.33°和45.30°处出现的峰,分别对应于晶格平面(111)和(220)。
实施例3
首先,将乙酰丙酮钴粉末(2g)加入到PSA液体(8g)中,同时加入适量的丙酮,使乙酰丙酮钴粉末完全溶解并通过搅拌混合。将混合物滴入二甲基硅油中,并以1000rpm搅拌。搅拌2小时后,按照以下步骤在烘箱中固化乳液:160℃保温1小时,190℃保温1小时,200℃保温2小时。然后通过离心将前体微球与二甲基硅油分离。分离后,在高温氧化铝管式炉中在高纯氮气氛下进行聚合物的热解。以5℃/ min的加热速率将管式炉从室温加热至1200℃,再保持4小时。制备的陶瓷吸波微球的吸波性能如图3所示。
实施例4
第一步,将乙酰丙酮钴粉末(2g)加入到聚硅氧烷液体(8g)中 同时加入适量的丙酮溶液,使乙酰丙酮钴粉末完全溶解于丙酮并搅拌均匀。将混合物滴加进甘油中,并以800rpm搅拌。搅拌2小时后,按照以下步骤在烘箱中固化乳液:90℃保温2小时,100℃保温2小时。然后通过将乳液与水混合搅拌,通过抽滤的方法将前体微球与甘油分离。分离后,在氧气气氛下进行聚合物的热解。以3℃/ min的加热速率将管式炉从室温加热至800℃,再保持2小时。
以上描述仅为本申请的较佳实施例以及对所运用技术原理的说明。本领域技术人员应当理解,本申请中所设计的发明范围,并不限于上述技术特征的特定组合而成的技术方案,同时也应涵盖在不脱离所属发明构思的情况下,有上述技术特征或其同特征进行任意组合而形成的其他技术方案。例如上述特征与本申请中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。
Claims (9)
1.一种新型陶瓷吸波微球材料的制备方法,其特征是:包括以下步骤:将磁性粉末加入到PSA液体中,然后将混合物滴入二甲基硅油中搅拌乳化;烘箱中固化乳液;然后将前体微球与二甲基硅油分离;磁性聚合物的陶瓷化处理。
2.如权利要求1所述的制备方法,其特征是:所述磁性物质选自氯化铁、氯化钴、氯化镍、硝酸铁、硝酸钴、硝酸镍、乙酰丙酮铁、乙酰丙酮钴、乙酰丙酮镍、铁钴镍金属粉中的一种以上。
3.如权利要求1所述的制备方法,其特征是:所述聚硅乙乙炔溶液中乙酰丙酮铁、乙酰丙酮钴、乙酰丙酮镍的质量比为1%-20%。
4.如权利要求1所述的制备方法,其特征是:所述聚硅乙炔可以用聚碳硅烷、聚硅氧烷替代。
5.如权利要求1所述的制备方法,其特征是:所述乳化具体步骤如下:连续相可以用二甲基硅油、甘油,二甲基硅油的粘度为350-50000mP∙s,搅拌速度为400-1500转/分钟。
6.如权利要求1所述的制备方法,其特征是:所述乳液固化具体步骤如下:将混合后的乳液进行加热固化,固化温度选择在180-300℃,并保温2-6小时。
7.如权利要求1所述的制备方法,其特征是:所述前体微球与二甲基硅油分离具体步骤如下:将前体微球与二甲基硅油的乳液溶解分散于正己烷、四氢呋喃或二甲苯溶液中,超声分散30-60分钟,然后在5000-10000转/分钟转速下离心5-20分钟取下层粉末,重复上述过程2-5次得到磁性聚合物微球。
8.如权利要求1所述的制备方法,其特征是:所述磁性聚合物微球陶瓷化具体步骤如下:将聚合物微球分散于正己烷或四氢呋喃溶液中,超声处理10-20分钟,烘干后在氮气或者氩气气氛下进行烧结,烧结温度为800-1400℃,保温1-4小时,升温速率为1-5℃/min。
9.一种如权利要求1-8任一项所述的制备方法制得的新型陶瓷吸波微球材料。
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