CN106630992A - 一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法 - Google Patents

一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法 Download PDF

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CN106630992A
CN106630992A CN201610865455.9A CN201610865455A CN106630992A CN 106630992 A CN106630992 A CN 106630992A CN 201610865455 A CN201610865455 A CN 201610865455A CN 106630992 A CN106630992 A CN 106630992A
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刘银
赵莉
郑林义
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Anhui University of Science and Technology
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Abstract

本发明涉及一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法。该复合铁氧体材料的化学结构式为xSrFe12O19/yCoFe2O4，其中0＜x＜1，0＜y＜1，x+y＝1。该复合铁氧体材料的制备方法：包括步骤：混料、预烧、压片、烧结处理。本发明利用六角型铁氧体SrFe12O19和尖晶石型铁氧体CoFe2O4自身的优越磁性能，使得铁氧体SrFe12O19与铁氧体CoFe2O4二者之间产生磁交换耦合作用，进而使得SrFe12O19/CoFe2O4复合铁氧体材料具有高的饱和磁化强度(Ms)和矫顽力(Hc)，有效改善了单一铁氧体材料的缺陷，拓展了其应用领域。

Description

一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法
技术领域
本发明属于铁氧体材料领域，具体是涉及一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法。
背景技术
铁氧体作为一种磁性材料，由于其具有低成本、环境稳定、高饱和磁化强度等优点一直以来备受关注。铁氧体材料广泛应用于永磁电机、磁选设备、磁纪录、以及微波等领域。其中作为磁铅石型的铁氧体AFe12O19(在A位通常是Ba、Sr，或两者都有)，国际上对其需求一直很大。六角型铁氧体SrFe12O19作为硬磁材料，具有很高的矫顽力(Hc)，为改善此类硬磁材料的磁性能，其复合材料的交换耦合作用的研究成为一大热点。比如在SrFe12O19/(Ni,Zn)Fe2O4复合铁氧体材料的研究中，发现随着(Ni,Zn)Fe2O4的添加，SrFe12O19材料的矫顽力不断减小。可见研究结果并不理想，对于如何通过复合来提高单一铁氧体材料的性能，还有待于科研人员的进一步研究。
发明内容
为了解决上述技术问题，本发明提供一种高性能SrFe12O19/CoFe2O4复合铁氧体材料及制备方法。
为了实现本发明的目的，本发明采用了以下技术方案：
一种高性能SrFe12O19/CoFe2O4复合铁氧体材料，该复合铁氧体材料的化学结构式为xSrFe12O19/yCoFe2O4，其中0＜x＜1，0＜y＜1，x+y＝1。
进一步的，所述的复合铁氧体材料的制备方法：包括以下步骤：
S1、混料：按所述化学结构式中的组成要求配置两组混合料，其中第一组混合料由Fe2O3与Co2O3二者的原料粉末混合得到，第二组混合料由Fe2O3与SrCO3二者的原料粉末混合得到；将上述两组混合料分别进行湿磨后予以烘干处理；
S2、预烧：将上述步骤中烘干处理后所得的第一组混合料在950～1050℃保温3.5～4.5h得到尖晶石型铁氧体CoFe2O4粉体，将上述步骤中烘干处理后所得的第二组混合料在1050～1150℃保温1.5～2.5h得到六角形铁氧体SrFe12O19粉体；
S3、造粒：将所述CoFe2O4粉体、SrFe12O19粉体、粘结剂进行混合造粒得到粒料；
S4、压片：将所述粒料进行压片处理得到片型料；
S5、烧结：将所述片型料生坯在1170～1260℃下，保温3.5～4.5h得到最终样品。
进一步的，步骤S1中湿磨时所加的球磨介质为水和氧化锆球；湿磨时转速为180r/min，湿磨时间为5h；所述烘干处理是在100℃下烘干24h。
进一步的，步骤S2中第一组混合料在1000℃保温4h，第二组混合料在1100℃保温2h。
进一步的，步骤S3中粘结剂为质量浓度为8％的聚乙烯醇。
进一步的，步骤S4中压片处理时压力为20MPa，片型料直径为12.98mm、厚度为2mm。
进一步的，步骤S5中保温时间为4h。
本发明的有益效果在于：
(1)本发明SrFe12O19/CoFe2O4复合铁氧体材料改善了单一铁氧体磁性材料的缺陷，提高了其相应的饱和磁化强度与矫顽力，改善了铁氧体材料的综合磁性能。本发明利用六角型铁氧体SrFe12O19和尖晶石型铁氧体CoFe2O4自身的优越磁性能，使得铁氧体SrFe12O19与铁氧体CoFe2O4二者之间产生磁交换耦合作用，进而使得SrFe12O19/CoFe2O4复合铁氧体材料具有高的饱和磁化强度(Ms)和矫顽力(Hc)，有效改善了复合铁氧体材料的磁性能，拓展了其应用领域。
(2)本发明SrFe12O19/CoFe2O4复合铁氧体材料采用传统的固相反应法制备，成本低，工艺简单，周期短，而且能在大量生产的情况下不对环境造成影响。本发明通过调整两种铁氧体的含量，即可方便得到任何配比的复合铁氧体材料，另外本发明可以通过传统烧结得到同一化学计量比不同烧结温度，或者同一烧结温度不同化学计量比的复合铁氧体材料，从而确定最佳的烧结温度、最佳的化学计量比，进而确定具有最佳磁性能的样品，以满足不同的应用需求。
(3)本发明提供了最佳混料条件与预烧条件，其中水、氧化锆在湿磨时可以进一步提高原料粉末的混合均匀性，以便于预烧后得到纯度更高的铁氧体SrFe12O19与铁氧体CoFe2O4，所述预烧过程中第一组混合物发生的化学反应式为:6Fe2O3+SrCO3→+SrFe12O19+CO2,所述预烧过程中第二组混合物发生的化学反应式为：4Fe2O3+2Co2O3→4CoFe2O4+O2。在造粒过程中，为了方便造粒，在CoFe2O4粉体、SrFe12O19粉体混合物中加入了质量浓度为8％的聚乙烯醇作为粘结剂，该粘结剂在烧结后不存留于复合铁氧体材料中，且无有毒物质产生，其在为复合铁氧体材料制备提供便利的同时也非常环保。压片可以使得片型料在烧结过程中自身受热更均匀，利于得到磁性能更好的复合铁氧体材料。
附图说明
图1为SrFe12O19/CoFe2O4复合铁氧体材料的衍射峰随X射线扫描范围变化的XRD图谱。
图2为SrFe12O19/CoFe2O4复合铁氧体材料的TEM照片。
图3为SrFe12O19/CoFe2O4复合铁氧体材料的外加磁场与磁化强度关系的磁滞回线。
具体实施方式
本发明通过Archimedes方法测定样品的烧结性能。采用岛津X-射线衍射仪分析样品物相，测试条件：CuKα靶，扫描范围20～90°。采用美振动样品磁强计(VSM)测量样品的磁滞回线，采用永磁B-H测量仪测量永磁特征参量。
下面结合实施例对本发明技术方案做出更为具体的说明：
实施例1
分别按SrFe12O19与CoFe2O4的化学计量比称量分析纯氧化铁(Fe2O3)、三氧化二钴(Co2O3)、碳酸锶(SrCO3)。分别置于聚四氟乙烯球磨罐中以转速180r/min球磨5h，然后将球磨混合浆料置于干燥箱中干燥24h。置于高温箱式烧结炉中至1000℃下保温4h得到CoFe2O4粉体；置于高温箱式烧结炉中至1100℃下保温2h得到SrFe12O19粉体。
分别称取SrFe12O19粉体5.481g，CoFe2O4粉体0.519g，于研钵内混合均匀，然后加入适量的混合料质量浓度为8％的聚乙烯醇(PVA)作为粘结剂，混合造粒得到粒料，在20MPa下压成片型料(直径Φ＝12.98mm、厚度d≈2mm)。
片型料置于高温箱式烧结炉中至1170℃后保温4h，冷却后即得到最终的样品。
本实施例制备的SrFe12O19/CoFe2O4的铁氧体复合材料饱和磁化强度为47.63A·m2·g-1，矫顽力为1217Oe，剩磁为2067Gs。
实施例2
分别按SrFe12O19与CoFe2O4的化学计量比称量分析纯氧化铁(Fe2O3)、三氧化二钴(Co2O3)、碳酸锶(SrCO3)。分别置于聚四氟乙烯球磨罐中以转速180r/min球磨5h，然后将球磨混合浆料置于干燥箱中干燥24h。置于高温箱式烧结炉中至1000℃下保温4h得到CoFe2O4粉体；置于高温箱式烧结炉中至1100℃下保温2h得到SrFe12O19粉体。
分别称取SrFe12O19粉体5.481g，CoFe2O4粉体0.519g，于研钵内混合均匀，然后加入适量的混合料质量浓度为8％的聚乙烯醇(PVA)作为粘结剂，混合造粒得到粒料，在20MPa下压成片型料(直径Φ＝12.98mm、厚度d≈2mm)。
片型料置于高温箱式烧结炉中至1230℃后保温4h，冷却后即得到最终的样品。
本实施例制备的SrFe12O19/CoFe2O4的铁氧体复合材料饱和磁化强度为51.13A·m2·g-1，矫顽力为774Oe，剩磁为1907Gs。
实施例3
分别按SrFe12O19与CoFe2O4的化学计量比称量分析纯氧化铁(Fe2O3)、三氧化二钴(Co2O3)、碳酸锶(SrCO3)。分别置于聚四氟乙烯球磨罐中以转速180r/min球磨5h，然后将球磨混合浆料置于干燥箱中干燥24h。置于高温箱式烧结炉中至1000℃下保温4h得到CoFe2O4粉体；置于高温箱式烧结炉中至1100℃下保温2h得到SrFe12O19粉体。
分别称取SrFe12O19粉体2.007g，CoFe2O4粉体3.993g，于研钵内混合均匀，然后加入适量的混合料质量浓度为8％的聚乙烯醇(PVA)作为粘结剂，混合造粒得到粒料，在20MPa下压成片型料(直径Φ＝12.98mm、厚度d≈2mm)。
片型料置于高温箱式烧结炉中至1230℃后保温4h，冷却后即得到最终的样品。
本实施例制备的SrFe12O19/CoFe2O4的铁氧体复合材料饱和磁化强度为64.84A·m2·g-1，矫顽力为932Oe，剩磁为1927Gs。
实施例4
分别按SrFe12O19与CoFe2O4的化学计量比称量分析纯氧化铁(Fe2O3)、三氧化二钴(Co2O3)、碳酸锶(SrCO3)。分别置于聚四氟乙烯球磨罐中以转速180r/min球磨5h，然后将球磨混合浆料置于干燥箱中干燥24h。置于高温箱式烧结炉中至950℃下保温4.5h得到CoFe2O4粉体；置于高温箱式烧结炉中至1050℃下保温2.5h得到SrFe12O19粉体。
分别称取SrFe12O19粉体2.007g，CoFe2O4粉体3.993g，于研钵内混合均匀，然后加入适量的混合料质量浓度为8％的聚乙烯醇(PVA)作为粘结剂，混合造粒得到粒料，在20MPa下压成片型料(直径Φ＝12.98mm、厚度d≈2mm)。
片型料置于高温箱式烧结炉中至1230℃后保温3.5h，冷却后即得到最终的样品。
本实施例制备的SrFe12O19/CoFe2O4的铁氧体复合材料饱和磁化强度为63.84A·m2·g-1，矫顽力为920Oe，剩磁为1900Gs。
实施例5
分别按SrFe12O19与CoFe2O4的化学计量比称量分析纯氧化铁(Fe2O3)、三氧化二钴(Co2O3)、碳酸锶(SrCO3)。分别置于聚四氟乙烯球磨罐中以转速180r/min球磨5h，然后将球磨混合浆料置于干燥箱中干燥24h。置于高温箱式烧结炉中至1050℃下保温3.5h得到CoFe2O4粉体；置于高温箱式烧结炉中至1150℃下保温1.5h得到SrFe12O19粉体。
分别称取SrFe12O19粉体2.007g，CoFe2O4粉体3.993g，于研钵内混合均匀，然后加入适量的混合料质量浓度为8％的聚乙烯醇(PVA)作为粘结剂，混合造粒得到粒料，在20MPa下压成片型料(直径Φ＝12.98mm、厚度d≈2mm)。
片型料置于高温箱式烧结炉中至1200℃后保温4.5h，冷却后即得到最终的样品。
本实施例制备的SrFe12O19/CoFe2O4的铁氧体复合材料饱和磁化强度为66.32A·m2·g-1，矫顽力为950Oe，剩磁为1985Gs。
不同x与y值条件下所得样品的剩磁化、矫顽力、饱和磁化强度、磁能积参数值，如下表1所示：
如图，随着CoFe2O4含量的增加，SrFe12O19与铁氧体CoFe2O4二者之间产生磁交换耦合作用，从而使得复合材料的饱和磁化强度(Ms)与磁感应矫顽力均增大。其中铁氧体CoFe2O4与SrFe12O19两相的结合，使混乱取向的磁矩处于平行排列，从而导致磁矩沿外磁场方向的分量增加，产生剩磁增强效应，磁能积随之增加，从而使复合材料具有更好的磁性能。

Claims (7)

1.一种高性能SrFe12O19/CoFe2O4复合铁氧体材料，其特征在于：该复合铁氧体材料的化学结构式为xSrFe12O19/yCoFe2O4，其中0＜x＜1，0＜y＜1，x+y＝1。
2.如权利要求1所述的复合铁氧体材料的制备方法：包括以下步骤：
S1、混料：按所述化学结构式中的组成要求配置两组混合料，其中第一组混合料由Fe2O3与Co2O3二者的原料粉末混合得到，第二组混合料由Fe2O3与SrCO3二者的原料粉末混合得到；将上述两组混合料分别进行湿磨后予以烘干处理；
S2、预烧：将上述步骤中烘干处理后所得的第一组混合料在950～1050℃保温3.5～4.5h得到尖晶石型铁氧体CoFe2O4粉体，将上述步骤中烘干处理后所得的第二组混合料在1050～1150℃保温1.5～2.5h得到六角形铁氧体SrFe12O19粉体；
S3、造粒：将所述CoFe2O4粉体、SrFe12O19粉体、粘结剂进行混合造粒得到粒料；
S4、压片：将所述粒料进行压片处理得到片型料；
S5、烧结：将所述片型料生坯在1170～1260℃下，保温3.5～4.5h得到最终样品。
3.如权利要求2所述的复合铁氧体材料的制备方法，其特征在于：步骤S1中湿磨时所加的球磨介质为水和氧化锆球；湿磨时转速为180r/min，湿磨时间为5h；所述烘干处理是在100℃下烘干24h。
4.如权利要求2所述的复合铁氧体材料的制备方法，其特征在于：步骤S2中第一组混合料在1000℃保温4h，第二组混合料在1100℃保温2h。
5.如权利要求2所述的复合铁氧体材料的制备方法，其特征在于：步骤S3中粘结剂为质量浓度为8％的聚乙烯醇。
6.如权利要求2所述的复合铁氧体材料的制备方法，其特征在于：步骤S4中压片处理时压力为20MPa，片型料直径为12.98mm、厚度为2mm。
7.如权利要求2所述的复合铁氧体材料的制备方法，其特征在于：步骤S5中保温时间为4h。
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