CN116947475B - 一种自偏置环行器用高性能复合铁氧体的制备方法 - Google Patents

一种自偏置环行器用高性能复合铁氧体的制备方法 Download PDF

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CN116947475B
CN116947475B CN202311020957.8A CN202311020957A CN116947475B CN 116947475 B CN116947475 B CN 116947475B CN 202311020957 A CN202311020957 A CN 202311020957A CN 116947475 B CN116947475 B CN 116947475B
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泮敏翔
杨杭福
俞能君
吴琼
葛洪良
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Abstract

本发明公开了一种自偏置环行器用高性能复合铁氧体的制备方法，属于磁性材料技术领域。该制备方法包括：（1）首先分别制备BaM铁氧体初始粉体和NiCuZnSn铁氧体初始粉体；（2）按比例将BaM铁氧体初始粉体NiCuZnSn铁氧体初始粉体和去离子水混合均匀并在高能球磨机内球磨，然后通过一次预烧、二次预烧及二次球磨处理后获得混合粉末；（3）随后通过低温磁场取向成型技术及磁场热处理，最终获得自偏置环行器用高性能复合铁氧体。本发明较好的通过复合BaM铁氧体粉体和NiCuZnSn铁氧体粉体，并通过高能球磨技术、低温磁场取向成型技术及磁场热处理技术增加了饱和磁化强度，改善了双相复合铁氧体的微结构与磁特性。

Description

一种自偏置环行器用高性能复合铁氧体的制备方法
技术领域
本发明涉及磁性材料技术领域，尤其涉及一种自偏置环行器用高性能复合铁氧体的制备方法。
背景技术
随着有源相控阵雷达在现代电子对抗中的广泛应用，具备高频、小尺寸、低损耗等特质的微波器件成为微波、毫米波技术的研究重点。微波环行器是Transmit/Receive（T/R）组件中不可或缺的重要元器件，而传统环行器需内置尺寸较大的永磁体来提供直流偏置场，以致收发系统难以实现整机的小型化。单轴六角铁氧体具有大的磁晶各向异性和高饱和磁化强度等特性，基于单轴六角铁氧体设计制备的微波环行器具备自偏置场，无需永磁体，这对实现微波环行器乃至T/R组件的小型化和平面化具有重要意义。
旋磁材料在微波领域的应用非常广泛，但随着微波器件及应用技术的提高，对旋磁材料的要求也越来越高，进一步提高旋磁材料的性能就显得极为迫切，尤其是宽带温度稳定性好同时损耗又小的材料。本专利创造性的通过复合BaM铁氧体粉体和NiCuZnSn铁氧体粉体，并通过高能球磨技术、低温磁场取向成型技术及磁场热处理技术，有效调控晶粒晶界特性，提高取向度，增加了饱和磁化强度，配合其他元素的掺入，改善了双相复合铁氧体的微结构与磁特性。
发明内容
针对现有技术中存在的问题，本发明目的在于提供一种自偏置环行器用高性能复合铁氧体的制备方法。
本发明的自偏置环行器用高性能复合铁氧体的制备方法，包括如下步骤：
（1）BaM铁氧体初始粉体制备：以BaCO3、La2O3、Fe2O3为原料，按照“5~15 mol%BaCO3、2~12 mol%La2O3、73~93 mol%Fe2O3”的比例称料，混料，得到BaM铁氧体初始粉体；
（2）NiCuZnSn铁氧体初始粉体制备：以NiO、ZnO、CuO、SnO2、Co2O3、Fe2O3为原料，按照“20~40 mol%NiO、5~30 mol%ZnO、2~10 mol%CuO、1~5 mol%SnO2、4~10 mol%Co2O3、5~68 mol%Fe2O3”的比例称料，混料，得到NiCuZnSn铁氧体初始粉体；
（3）将步骤（1）获得的BaM铁氧体初始粉体、步骤（2）获得的NiCuZnSn铁氧体初始粉体和去离子水按照质量比为1:0.1~1:3~5的比例混合均匀后获得混合粉体浆料，随后混合粉体浆料在高能球磨机内混合均匀，高能球磨的时间为1~3 h；
（4）将步骤（3）获得的球磨料粉体烘干，过筛，随后对粉体进行一次预烧和二次预烧处理后到混合粉末；
（5）将步骤（4）获得的混合粉末和去离子水按照质量比为1:3~5的比例混合均匀并进行二次高能球磨后获得粉体浆料，高能球磨的时间为0.5~1.5 h；
（6）将步骤（5）获得的粉体浆料进行低温磁场取向成型技术制备压坯，所述低温磁场取向成型技术的温度为50~150 ℃，压力为40~150 MPa，磁场强度为2~4 T；
（7）将步骤（6）获得的压坯进行磁场热处理，最终获得自偏置环行器用高性能复合铁氧体。
进一步的，步骤（4）中所述的一次预烧的烧结温度为1050~1350 ℃，升温速率为1~3 ℃/min，保温时间为2~7 h；所述的二次预烧的烧结温度为800~1000 ℃，升温速率为1~3℃/min，保温时间为1~4 h。
进一步的，步骤（7）中所述的磁场热处理的磁场强度为1~2 T，热处理温度为800~1100 ℃，升温速率为1~3 ℃/min，保温时间为2~6 h，随后急冷至室温。
与现有的技术相比，本发明具有如下优点和有益效果：本专利创造性的通过复合BaM铁氧体粉体和NiCuZnSn铁氧体粉体，并通过高能球磨技术、低温磁场取向成型技术及磁场热处理技术，有效调控晶粒晶界特性，提高取向度，增加了饱和磁化强度，配合其他元素的掺入，改善了双相复合铁氧体的微结构与磁特性。
实施方式
下面将结合实施例对本发明做进一步的详细说明，但本发明并不仅仅局限于以下实施例。
实施例1
（1）BaM铁氧体初始粉体制备：以BaCO3、La2O3、Fe2O3为原料，按照“5 mol%BaCO3、10mol%La2O3、85 mol%Fe2O3”的比例称料，混料，得到BaM铁氧体初始粉体；
（2）NiCuZnSn铁氧体初始粉体制备：以NiO、ZnO、CuO、SnO2、Co2O3、Fe2O3为原料，按照“20 mol%NiO、5 mol%ZnO、2 mol%CuO、1 mol%SnO2、4 mol%Co2O3、68 mol%Fe2O3”的比例称料，混料，得到NiCuZnSn铁氧体初始粉体；
（3）将步骤（1）获得的BaM铁氧体初始粉体、步骤（2）获得的NiCuZnSn铁氧体初始粉体和去离子水按照质量比为1:0.3:3的比例混合均匀后获得混合粉体浆料，随后混合粉体浆料在高能球磨机内混合均匀，高能球磨的时间为1 h；
（4）将步骤（3）获得的球磨料粉体烘干，过筛，随后对粉体进行一次预烧和二次预烧处理后到混合粉末，所述的一次预烧的烧结温度为1050 ℃，升温速率为1 ℃/min，保温时间为6 h；所述的二次预烧的烧结温度为1000 ℃，升温速率为3 ℃/min，保温时间为1 h；
（5）将步骤（4）获得的混合粉末和去离子水按照质量比为1:3的比例混合均匀并进行二次高能球磨后获得粉体浆料，高能球磨的时间为0.5 h；
（6）将步骤（5）获得的粉体浆料进行低温磁场取向成型技术制备压坯，所述低温磁场取向成型技术的温度为50 ℃，压力为150 MPa，磁场强度为2 T；
（7）将步骤（6）获得的压坯进行磁场热处理，磁场强度为1 T，热处理温度为1000℃，升温速率为3 ℃/min，保温时间为6 h，随后急冷至室温，最终获得复合铁氧体。
采用本发明制备的复合铁氧体经磁性能和矢量网络分析仪测试，饱和磁化强度4πMs为4850 Gs、剩磁比Mr/Ms为0.89、矫顽力Hc为4010 Oe、铁磁共振线宽ΔH为368 Oe、各向异性场Ha为14.10 kOe。
实施例2
（1）BaM铁氧体初始粉体制备：以BaCO3、La2O3、Fe2O3为原料，按照“10 mol%BaCO3、8mol%La2O3、82 mol%Fe2O3”的比例称料，混料，得到BaM铁氧体初始粉体；
（2）NiCuZnSn铁氧体初始粉体制备：以NiO、ZnO、CuO、SnO2、Co2O3、Fe2O3为原料，按照“30 mol%NiO、15 mol%ZnO、5 mol%CuO、3 mol%SnO2、7 mol%Co2O3、40 mol%Fe2O3”的比例称料，混料，得到NiCuZnSn铁氧体初始粉体；
（3）将步骤（1）获得的BaM铁氧体初始粉体、步骤（2）获得的NiCuZnSn铁氧体初始粉体和去离子水按照质量比为1:0.5:4的比例混合均匀后获得混合粉体浆料，随后混合粉体浆料在高能球磨机内混合均匀，高能球磨的时间为2 h；
（4）将步骤（3）获得的球磨料粉体烘干，过筛，随后对粉体进行一次预烧和二次预烧处理后到混合粉末，所述的一次预烧的烧结温度为1150 ℃，升温速率为2 ℃/min，保温时间为4 h；所述的二次预烧的烧结温度为900 ℃，升温速率为2 ℃/min，保温时间为2 h；
（5）将步骤（4）获得的混合粉末和去离子水按照质量比为1:4的比例混合均匀并进行二次高能球磨后获得粉体浆料，高能球磨的时间为1 h；
（6）将步骤（5）获得的粉体浆料进行低温磁场取向成型技术制备压坯，所述低温磁场取向成型技术的温度为100 ℃，压力为100 MPa，磁场强度为3 T；
（7）将步骤（6）获得的压坯进行磁场热处理，磁场强度为1.5 T，热处理温度为900℃，升温速率为2 ℃/min，保温时间为4 h，随后急冷至室温，最终获得复合铁氧体。
采用本发明制备的复合铁氧体经磁性能和矢量网络分析仪测试，饱和磁化强度4πMs为4910 Gs、剩磁比Mr/Ms为0.90、矫顽力Hc为4100 Oe、铁磁共振线宽ΔH为350 Oe、各向异性场Ha为13.93 kOe。
实施例3
（1）BaM铁氧体初始粉体制备：以BaCO3、La2O3、Fe2O3为原料，按照“15 mol%BaCO3、5mol%La2O3、80 mol%Fe2O3”的比例称料，混料，得到BaM铁氧体初始粉体；
（2）NiCuZnSn铁氧体初始粉体制备：以NiO、ZnO、CuO、SnO2、Co2O3、Fe2O3为原料，按照“40 mol%NiO、25 mol%ZnO、8 mol%CuO、5 mol%SnO2、9 mol%Co2O3、13 mol%Fe2O3”的比例称料，混料，得到NiCuZnSn铁氧体初始粉体；
（3）将步骤（1）获得的BaM铁氧体初始粉体、步骤（2）获得的NiCuZnSn铁氧体初始粉体和去离子水按照质量比为1:1:5的比例混合均匀后获得混合粉体浆料，随后混合粉体浆料在高能球磨机内混合均匀，高能球磨的时间为3 h；
（4）将步骤（3）获得的球磨料粉体烘干，过筛，随后对粉体进行一次预烧和二次预烧处理后到混合粉末，所述的一次预烧的烧结温度为1350 ℃，升温速率为3℃/min，保温时间为2 h；所述的二次预烧的烧结温度为800 ℃，升温速率为1 ℃/min，保温时间为4 h；
（5）将步骤（4）获得的混合粉末和去离子水按照质量比为1:5的比例混合均匀并进行二次高能球磨后获得粉体浆料，高能球磨的时间为1.5 h；
（6）将步骤（5）获得的粉体浆料进行低温磁场取向成型技术制备压坯，所述低温磁场取向成型技术的温度为150 ℃，压力为60 MPa，磁场强度为4 T；
（7）将步骤（6）获得的压坯进行磁场热处理，磁场强度为2 T，热处理温度为800℃，升温速率为1 ℃/min，保温时间为2 h，随后急冷至室温，最终获得复合铁氧体。
采用本发明制备的复合铁氧体经磁性能和矢量网络分析仪测试，饱和磁化强度4πMs为4978 Gs、剩磁比Mr/Ms为0.91、矫顽力Hc为4250 Oe、铁磁共振线宽ΔH为340 Oe、各向异性场Ha为13.55 kOe。

Claims (2)

1.一种自偏置环行器用高性能复合铁氧体的制备方法，其特征在于包括如下步骤：
（1）BaM铁氧体初始粉体制备：以BaCO3、La2O3、Fe2O3为原料，按照“5~15 mol%BaCO3、2~12mol%La2O3、73~93 mol%Fe2O3”的比例称料，混料，得到BaM铁氧体初始粉体；
（2）NiCuZnSn铁氧体初始粉体制备：以NiO、ZnO、CuO、SnO2、Co2O3、Fe2O3为原料，按照“20~40 mol%NiO、5~30 mol%ZnO、2~10 mol%CuO、1~5 mol%SnO2、4~10 mol%Co2O3、40~68 mol%Fe2O3”的比例称料，混料，得到NiCuZnSn铁氧体初始粉体；
（3）将步骤（1）获得的BaM铁氧体初始粉体、步骤（2）获得的NiCuZnSn铁氧体初始粉体和去离子水按照质量比为1:0.1~1:3~5的比例混合均匀后获得混合粉体浆料，随后混合粉体浆料在高能球磨机内混合均匀，高能球磨的时间为1~3 h；
（4）将步骤（3）获得的球磨料粉体烘干，过筛，随后对粉体进行一次预烧和二次预烧处理后到混合粉末；所述的一次预烧的烧结温度为1050~1350 ℃，升温速率为1~3 ℃/min，保温时间为2~7 h；所述的二次预烧的烧结温度为800~1000 ℃，升温速率为1~3 ℃/min，保温时间为1~4 h；
（5）将步骤（4）获得的混合粉末和去离子水按照质量比为1:3~5的比例混合均匀并进行二次高能球磨后获得粉体浆料，高能球磨的时间为0.5~1.5 h；
（6）将步骤（5）获得的粉体浆料进行低温磁场取向成型技术制备压坯，所述低温磁场取向成型技术的温度为50~150 ℃，压力为40~150 MPa，磁场强度为2~4 T；
（7）将步骤（6）获得的压坯进行磁场热处理，最终获得自偏置环行器用高性能复合铁氧体。
2. 根据权利要求1 所述的一种自偏置环行器用高性能复合铁氧体的制备方法，其特征在于：步骤（7）中所述的磁场热处理的磁场强度为1~2 T，热处理温度为800~1100 ℃，升温速率为1~3 ℃/min，保温时间为2~6 h，随后急冷至室温。
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