CN102977366B - 一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法 - Google Patents
一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法 Download PDFInfo
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Abstract
本发明提供一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法。本发明先以硝酸盐、正硅酸乙酯和无水乙醇等为原料，采用溶胶-凝胶法制备出NiCoZn铁氧体-SiO2复合粉体，再以NiCoZn铁氧体-SiO2复合粉体、十二烷基苯磺酸（DBSA）、吡咯单体为原料，采用原位聚合法制备出NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料。该复合材料主要克服了传统吸波材料“吸收弱、频带窄、密度大、厚度厚”的问题，在隐身技术、电磁屏蔽等领域具有重要的应用价值。
Description
技术领域
本发明属于电磁波吸收材料制备领域，特别涉及一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法。
背景技术
现阶段制备的铁氧体/导电聚合物微波吸收剂，存在一些缺陷，比如饱和磁化强度不高，电导率较低等，难以满足吸波材料“吸收频带宽、吸收强度强、密度轻、厚度薄”的要求。
Co2+作为软磁铁氧体中一种比较常用的添加剂而在实际生产中经常采用，溶胶-凝胶法具有制备温度低、工艺简单且易于控制反应条件等特点在铁氧体制备中广泛应用。聚吡咯(PPy)作为最常见的导电聚合物之一，由于具有结构多样、密度低、电磁参数易于调节、中低温性良好等特点，同时又具备空气稳定性好、易于电化学聚合制备成膜、无毒等优点，有着广阔的应用前景。本发明通过对DBSA掺杂的聚吡咯基质中加入NiCoZn铁氧体-SiO2复合粉体，使复合吸波材料表现出优良的磁性能和导电性能，从而制得综合性能优越的微波吸收材料。
发明内容
本发明的目的是提供一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯微波吸收剂的制备方法，可以克服现阶段制备的铁氧体/导电聚合物微波吸收材料存在饱和磁化强度不高、电导率较低等不足。
本发明是这样来实现的，其制备方法如下：
（1）NiCoZn铁氧体-SiO2复合粉体的制备
按照化学元素计量比为Ni0.3Co0.2Zn0.5Fe2O4称取0.87g Ni(NO3)2·6H2O、0.58gCo(NO3)2·6H2O、1.49g Zn(NO3)2·6H2O、8.08g Fe(NO3)3·9H2O溶解于35mL无水乙醇中，60℃恒温水浴30min混合均匀。控制NiCoZn铁氧体与SiO2质量比7:3，将正硅酸乙酯(TEOS)1.10mL，缓慢滴加到上述硝酸盐的醇溶液中，60℃恒温水浴至溶液成凝胶，再80℃真空干燥处理12h。然后将干凝胶研磨后，950℃保温2h，再次研磨后得到NiCoZn铁氧体-SiO2复合粉体。
（2）NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料的制备
将X g（X=0.75～4.50）的NiCoZn铁氧体-SiO2复合粉体加入25mL无水乙醇中，超声分散30min，再将2.0g吡咯单体、1.0g DBSA分别滴加入上述体系中，增力搅拌10min，40℃恒温水浴保持30min，不断搅拌下30min内加入2.0g过硫酸氨，再在0～5℃聚合反应6h。将上述反应产物 抽滤，并用去离子水、无水乙醇洗涤至滤液无色，80℃真空干燥滤饼24h后，研磨得到NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料。
用H-600透射电子显微镜对NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的颗粒形态及尺寸进行观测，操作电压为75kV。以NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合物（X=0.75）为例，复合物呈球状，粒径约为100nm。
用日立HITACHI/SU1510扫描电子显微镜对NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的颗粒形态及尺寸进行观测。以NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合物（X=0.75）为例，复合物呈球形颗粒，粒径约为100nm。
用四探针电导仪对NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的电导率进行测定。以NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合物（X=0.75）为例，复合物电导率为2.59×10-4S/cm。
用振动样品磁强计(VSM)对NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料进行磁性能测试。以NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合物（X=0.75）为例，测试结果为：矫顽力为4535.430Oe，饱和磁化强度为65.95emu·g-1，剩余磁化强度为58.09emu·g-1。
采用安捷伦8722ES矢量网络分析仪测试NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料在2～18GHz的反射率。以NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合物（X=4.50）为例，测试结果为：7.2GHz处出现最大吸收峰，峰值为-39dB，反射率损失值低于-10dB的吸收频带宽达10.3GHz。本发明所制备的NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料在2～18GHz内反射率损失值低于-10dB的频带宽度达10.3～14.5GHz，最小反射率损失值可达-35～-39dB。
本发明的优点是：在制备过程中，先以硝酸盐、正硅酸乙酯和无水乙醇等为原料，采用溶胶-凝胶法制备出NiCoZn铁氧体-SiO2复合粉体，该复合材料中同时含有Ni、Co、Zn三种金属的NiCoZn铁氧体，拓宽了吸收频带宽度，同时SiO2的掺入使得该NiCoZn铁氧体-SiO2晶体比单一的铁氧体晶体平均晶粒尺寸大，晶面各向异性增加，磁滞损耗增强。接着再以NiCoZn铁氧体-SiO2复合粉体、十二烷基苯磺酸（DBSA）、吡咯单体为原料，采用原位聚合法制备出NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料，该复合材料中导电聚合物聚吡咯经DBSA掺杂后，使其导电性增强，复合材料的整体电阻损耗增强。通过改变NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料中NiCoZn铁氧体-SiO2的含量可以调节吸收频带宽度，以达到预期的应用范围。因此，该NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料兼具电、磁性能，在隐身技术、电磁屏蔽等领域具有重要的应用价值。
具体实施方式
下面通过实施例对本发明作进一步说明。
实施例1
（1）按照化学元素计量比为Ni0.3Co0.2Zn0.5Fe2O4称取0.87g Ni(NO3)2·6H2O、0.58gCo(NO3)2·6H2O、1.49g Zn(NO3)2·6H2O、8.08g Fe(NO3)3·9H2O溶解于35mL无水乙醇中，60℃恒温水浴30min，按照NiCoZn铁氧体与SiO2质量比7:3量取正硅酸乙酯(TEOS)1.10mL，并缓慢滴加到上述硝酸盐的醇溶液中，继续60℃恒温水浴至成凝胶，80℃真空干燥12h成干凝胶，研磨，950℃保温2h，再次研磨，得到NiCoZn铁氧体-SiO2复合粉体。
（2）将0.75g NiCoZn铁氧体-SiO2复合粉体加入25mL无水乙醇中，超声分散30min，将2.0g吡咯单体、1.0g DBSA分别滴加入上体系中，增力搅拌10min，40℃恒温水浴保持30min，不断搅拌下30min内加入2.0g过硫酸氨，0～5℃聚合反应6h，抽滤，滤饼用去离子水、无水乙醇洗涤至滤液无色，80℃真空干燥24h后，研磨得到NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料（X=0.75）。所制备的复合材料在2～18GHz内反射率损失值低于-10dB的频带宽度达14.5GHz，最小反射率损失值可达-35dB。
实施例2
NiCoZn铁氧体-SiO2复合粉体的制备方法同实施例1的步骤（1）。称取2.00g NiCoZn铁氧体-SiO2复合粉体用以制备NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料，其制备方法同实施例1的步骤（2），得到NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料（X=2.00）。所制备的复合材料在2～18GHz内反射率损失值低于-10dB的频带宽度达12.3GHz，最小反射率损失值可达-37dB。
实施例3
NiCoZn铁氧体-SiO2复合粉体的制备方法同实施例1的步骤（1）。称取4.50g NiCoZn铁氧体-SiO2复合粉体用以制备NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料，其制备方法同实施例1的步骤（2），得到NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料（X=4.50）。所制备的复合材料在2～18GHz内反射率损失值低于-10dB的频带宽度达10.3GHz，最小反射率损失值可达-37dB。
Claims (2)
1.一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法，其特征在于该材料的制备包含两部分，即NiCoZn铁氧体-SiO2复合粉体的制备和NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料的制备，具体过程：
（1）NiCoZn铁氧体-SiO2复合粉体的制备
按照化学元素计量比为Ni0.3Co0.2Zn0.5Fe2O4称取0.87g Ni(NO3)2·6H2O、0.58gCo(NO3)2·6H2O、1.49g Zn(NO3)2·6H2O、8.08g Fe(NO3)3·9H2O溶解于35mL无水乙醇中，60℃恒温水浴30min混合均匀；
控制NiCoZn铁氧体与SiO2质量比7:3，将正硅酸乙酯(TEOS)1.10mL，缓慢滴加到上述硝酸盐的醇溶液中，60℃恒温水浴至溶液成凝胶，再80℃真空干燥处理12h；
然后将干凝胶研磨后，950℃保温2h，再次研磨后得到NiCoZn铁氧体-SiO2复合粉体；
（2）NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料的制备
将X g（X=0.75～4.50）的NiCoZn铁氧体-SiO2复合粉体加入25mL无水乙醇中，超声分散30min，再将2.0g吡咯单体、1.0g DBSA分别滴加入上述体系中，增力搅拌10min，40℃恒温水浴保持30min，不断搅拌下30min内加入2.0g过硫酸氨，再在0～5℃聚合反应6h；
将上述反应产物进行抽滤，并用去离子水、无水乙醇洗涤至滤液无色，80℃真空干燥24h后，研磨得到NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合材料。
2.根据权利要求1所述的一种NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料的制备方法，其特征在于：所制备的NiCoZn铁氧体-SiO2/DBSA掺杂聚吡咯复合吸波材料在2～18GHz内反射率损失值低于-10dB的频带宽度达10.3～14.5GHz，最小反射率损失值可达-35～-39dB。
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634016A (zh) * | 2012-04-05 | 2012-08-15 | 南昌航空大学 | 一种镧钕掺杂钡铁氧体-聚吡咯复合微波吸收剂的制备方法 |
Non-Patent Citations (5)
| Title |
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| JP特开2002-234988A 2002.08.23 |
| 十二苯磺酸-聚吡咯纳米复合材料的合成与表征;林生岭等;《材料开发与应用》;20090430;39-41，47 * |
| 华杰等.用Sol-gel法制备NiCoZn铁氧体/SiO2纳米复合材料的结构与磁性.《兵器材料科学与工程》.2009,第23卷(第1期),64-66. |
| 林生岭等.十二苯磺酸-聚吡咯纳米复合材料的合成与表征.《材料开发与应用》.2009,39-41，47. |
| 用Sol-gel法制备NiCoZn铁氧体/SiO2纳米复合材料的结构与磁性;华杰等;《兵器材料科学与工程》;20090131;第23卷(第1期);64-66 * |
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| CN102977366A (zh) | 2013-03-20 |
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