CN109265155A - 一种锶铁氧体磁性材料及其制备方法 - Google Patents
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Abstract
本发明的目的是为了解决现有的M型锶铁氧体材料磁学性能差的问题。对锶铁氧体进行离子掺杂及工艺改进。本发明M型锶铁氧体磁性材料的分子式为:Sr1‑xGdxFe12‑xMnxO19。制备方法为按照分子式中元素质量比称取原料;混合均匀后压片;进行第一次烧结;对第一次烧结得到的样品研磨、压片;进行第二次烧结;本发明M型锶铁氧体磁性材料制备方法成本较低,制备工艺简单、耗能低,适合于工业化生产,且制备的M型锶铁氧体磁性材料磁学性能优越。
Description
技术领域
本发明属于磁性材料技术领域,具体涉及一种锶铁氧体磁性材料及其制备方法。
背景技术
M型六角铁氧体作为一种高性能永磁材料,具有较宽的磁滞回线、较高的矫顽力、磁能积、单轴磁晶各向异性和高剩余磁化强度等特点,同时具有较高的性价比,因此成为应用最广泛的永磁材料、微波吸收材料和高密度垂直磁记录器件等领域中,是电子、军事工业一种重要的基础功能材料。近年来,随着人们对电子产品的性能方面要求日益严格,工业发展水平日益提高,M型铁氧体的性能也在不断的被探索。研究者主要从制备方法、工艺参数、配方改进方面进行研究。
M型锶铁氧体具有磁铅石结构,一个晶胞中含有两个分子,其中24个Fe3+分布在5种不同的氧离子空位当中,2a,12k,4f2为八面体间隙,2b为六面体间隙,4f1属于四面体间隙,且不同位置的Fe3+的磁矩排列方向也不同,2a,12k,2b空位上的磁矩排列向上与4f1和4f2空位上的磁矩反向平行排列,两个方向上的磁矩未能完全抵消,剩余的磁矩使整个分子具有亚磁性,也是铁氧体磁性的来源。为提高磁性能可以掺杂适量的例子取代Sr2+或Fe3+减小排列方向向下的离子磁矩,从而提高净磁矩。
发明内容
本发明目的是为了解决现有的M型锶铁氧体材料磁学性能差的问题,而提出了一种M型锶铁氧体磁性材料及其制备方法。
本发明所述M型锶铁氧体磁性材料的分子式为:Sr1-xGdxFe12-xMnxO19,分子式中:0<x<0.1。
本发明制备分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料的方法按以下步骤进行:
步骤一:按照分子式Sr1-xGdxFe12-xMnxO19中的化学计量比称取Gd2O3、MnCO3、SrCO3和Fe2O3做为原料,分子式Sr1-xGdxFe12-xMnxO19中:0<x<0.1;
步骤二:将步骤一中称取的原料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料1h~2h得到混合粉体,将得到的混合粉体烘干后置于压片的模具中,在3MPa~5MPa的压力下压制得到片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为80~150℃,烘干时间为3h~6h;
步骤三:把步骤二得到的片状样品放入高温箱式电阻炉中,以5℃/min~10℃的升温速率升温至1200℃~1250℃,然后保温2h~8h后随炉冷却至室温,得到预烧料;
步骤四:将步骤三得到的预烧料用钢钵进行粗破碎并研磨,然后将研磨后的预烧料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料2h~3h,将混料烘干后置于压片的模具中,在3MPa~5MPa的压力下压制得到预烧料片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为80℃~150℃,烘干时间为3h~6h;
步骤五:将步骤四得到的预烧料片状样品置于高温箱式电阻炉中,以5℃/min ~10℃/min的升温速率升温至1150℃~1250℃,然后保温2h~4h后随炉冷却至室温,最终得到分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料。
本发明具备如下有益效果:
1、本发明所用原料SrCO3、MnCO3和Fe2O3价格低廉,Gd2O3原料易得且用量较低,故综合成本较低,适合于工业化生产,并且本发明方法制备工艺简单、能耗较低;
2、本发明制备出的分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料磁学性能优于相同工艺条件下制备的M型锶铁氧体磁性材料SrFe12O19,剩余磁化强度Br增加8.52%~41.33%,矫顽力Hc增加27.65%~65.49%,饱和磁化强度Ms增加6.98%~10.56%,即本发明配方体系和方法获得了性能优良的M型锶铁氧体磁性材料。
附图说明
图1为施实例一制备的M型锶铁氧体磁性材料的X射线衍射图谱;
图2为施实例一制备的M型锶铁氧体磁性材料的SEM图;
图3为施实例二制备的M型锶铁氧体磁性材料的X射线衍射图谱;
图4为施实例二制备的M型锶铁氧体磁性材料的SEM图。
具体实施方式
本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意合理组合。
具体实施方式一:本实施方式一种M型锶铁氧体磁性材料,该M型锶铁氧体磁性材料的分子式为:Sr1-xGdxFe12-xMnxO19,分子式中:0<x<0.1。
本实施方式的Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料磁学性能优于相同工艺条件下制备的M型锶铁氧体磁性材料SrFe12O19,剩余磁化强度Br增加6.18%~36.11%,矫顽力Hc增加25.35%~42.70%,饱和磁化强度Ms增加8.03%~10.03%,即本实施方式配方体系获得了性能优良的M型锶铁氧体磁性材料。
具体实施方式二:制备分子式为Sr1-xLnxFe12-xMnxO19的M型锶铁氧体磁性材料的方法按以下步骤进行:
步骤一:按照分子式Sr1-xLnxFe12-xMnxO19中的化学计量比称取Gd2O3、MnCO3、SrCO3和Fe2O3做为原料,分子式Sr1-xGdxFe12-xMnxO19中:0<x<0.1;
步骤二:将步骤一中称取的原料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料1h~2h得到混合粉体,将得到的混合粉体烘干后置于压片的模具中,在3MPa~5MPa的压力下压制得到片状样品;
步骤三:把步骤二得到的片状样品放入高温箱式电阻炉中,以5℃/min~10℃的升温速率升温至1200℃~1250℃,然后保温2h~8h后随炉冷却至室温,得到预烧料;
步骤四:将步骤三得到的预烧料用钢钵进行粗破碎并研磨,然后将研磨后的预烧料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料2h~3h,烘干后将混料置于压片的模具中,在3MPa~5MPa的压力下压制得到预烧料片状样品;
步骤五:将步骤四得到的预烧料片状样品置于高温箱式电阻炉中,以5℃/min ~10℃/min的升温速率升温至1150℃~1250℃,然后保温2h~4h后随炉冷却至室温,最终得到分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料。
1、本实施方式所用原料SrCO3、MnCO3和Fe2O3价格低廉,Gd2O3原料易得且用量较低,故综合成本较低,适合于工业化生产,并且本实施方式方法制备工艺简单、能耗较低;
2、本实施方式制备出的分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料磁学性能优于相同工艺条件下制备的M型锶铁氧体磁性材料SrFe12O19,剩余磁化强度Br增加8.52%~41.33%,矫顽力Hc增加27.65%~65.49%,饱和磁化强度Ms增加6.98%~10.56%,即本实施方式配方体系和方法获得了性能优良的M型锶铁氧体磁性材料。
具体实施方式三:本实施方式与具体实施方式二不同的是:步骤二所述磨球为氧化镐磨球。其他步骤和参数与具体实施方式二相同。
具体实施方式四:本实施方式与具体实施方式二或三不同的是:步骤二所述磨球、原料和无水乙醇的质量比为10:1:0.5。其他步骤和参数与具体实施方式二或三相同。
具体实施方式五:本实施方式与具体实施方式二至四之一不同的是:步骤二所述烘干的温度为80℃~150℃,烘干时间为3h~6h。其他步骤和参数与具体实施方式二至四之一相同。
具体实施方式六:本实施方式与具体实施方式二至五之一不同的是:步骤四所述磨球为氧化镐磨球。其他步骤和参数与具体实施方式二至五之一相同。
具体实施方式七:本实施方式与具体实施方式二至六之一不同的是:步骤四所述磨球、原料和无水乙醇的质量比为10:1:0.5。其他步骤和参数与具体实施方式二至六之一相同。
具体实施方式八:本实施方式与具体实施方式二至六之一不同的是:步骤四所述烘干的温度为80℃~150℃,烘干时间为3h~6h。其他步骤和参数与具体实施方式二至八之一相同。
用以下实施例验证本发明的有益效果:
实施例1:
本实施例所述M型锶铁氧体磁性材料的分子式为:Sr0.95 Gd0.05Fe11.95Mn0.05O19;
本实施例所述M型锶铁氧体磁性材料的制备方法按以下步骤进行:
步骤一:按照分子式Sr0.95 Gd0.05Fe11.95Mn0.05O19中的化学计量比称取Gd2O3、MnCO3、SrCO3和Fe2O3做为原料;
步骤二:将步骤一中称取的原料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为400r/min下混料2h得到混合粉体,将得到的混合粉体烘干后置于压片的模具中,在3MPa的压力下压制得到片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为120℃,烘干时间为6h;
步骤三:把步骤二得到的片状样品放入高温箱式电阻炉中,以5℃/min的升温速率升温至1250℃,然后保温6h后随炉冷却至室温,得到预烧料;
步骤四:将步骤三得到的预烧料用钢钵进行粗破碎并研磨,然后将研磨后的预烧料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为400r/min下混料3h,将混料烘干后置于压片的模具中,在3MPa的压力下压制得到预烧料片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为120℃,烘干时间为6h;
步骤五:将步骤四得到的预烧料片状样品置于高温箱式电阻炉中,以5℃/min的升温速率升温至1250℃,然后保温4h后随炉冷却至室温,最终得到分子式为Sr0.95Gd0.05Fe11.95Mn0.05O19的M型锶铁氧体磁性材料。
对本实施例制备的M型锶铁氧体磁性材料进行XRD衍射测试,测试结果如图1所示,由图可见:当取代量x=0.05时,粉体在衍射角2θ=30.4°,31.0°,32.36°,34.2°等处出现强烈的衍射峰,对应六方晶相(110)晶面、(008)晶面、(107)晶面(114)晶面,跟纯M型锶铁氧体SrFe12O19标准卡片及按实施例一制备方法制得的纯M型锶铁氧体SrFe12O19 的XRD衍射图比对基本吻合,没有发现其他杂峰,表明此时的粉体为单一的M型锶铁氧体相。
对本实施例制备的M型锶铁氧体磁性材料进行SEM扫描,结果如图2所示,由图可见,样品中的晶粒尺寸在1μm~3μm之间,且晶粒尺寸大小较均匀,分布也较为均匀,且界面清晰,呈六角片状结构,样品中存在一定的孔洞,说明样品的密度仍有提升的空间。
对本实施例制备的分子式为Sr0.95 Gd0.05Fe11.95Mn0.05O19的M型锶铁氧体磁性材料进行VSM测试:剩余磁化强度Br=32.75emu/g,饱和磁化强度Ms=57.16emu/g,矫顽力Hc=43.27kA/m;按照本实施例的方法和工艺参数制备分子式为SrFe12O19 的M型锶铁氧体磁性材料并通过VSM测试得到剩余磁化强度Br=28.89emu/g,Ms=53.36emu/g,Hc=32.58kA/m,由此可知,本实施例制备的分子式为Sr0.95Gd0.05Fe11.95Mn0.05O19的M型锶铁氧体磁性材料与现有的分子式为SrFe12O19 的M型锶铁氧体磁性材料相比,剩余磁化强度Br增加13.36%,饱和磁化强度Ms增加7.12%,矫顽力Hc增加32.8%。
实施例2:
本实施例所述M型锶铁氧体磁性材料的分子式为:Sr0.9Gd 0.1Fe11.9Mn0.1O19;
本实施例所述M型锶铁氧体磁性材料的制备方法按以下步骤进行:
步骤一:按照分子式Sr0.9Gd0.1Fe11.9Mn0.1O19中的化学计量比称取Gd2O3、MnCO3、SrCO3和Fe2O3做为原料;
步骤二:将步骤一中称取的原料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为400r/min下混料2h得到混合粉体,将得到的混合粉体烘干后置于压片的模具中,在3MPa的压力下压制得到片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为120℃,烘干时间为6h;
步骤三:把步骤二得到的片状样品放入高温箱式电阻炉中,以5℃/min的升温速率升温至1200℃,然后保温6h后随炉冷却至室温,得到预烧料;
步骤四:将步骤三得到的预烧料用钢钵进行粗破碎并研磨,然后将研磨后的预烧料、磨球和无水乙醇置于行星球磨机的陶瓷球磨罐中,在转速为400r/min下混料3h,将混料烘干后置于压片的模具中,在3MPa的压力下压制得到预烧料片状样品;所述磨球为氧化镐磨球;所述磨球、原料和无水乙醇的质量比为10:1:0.5;所述烘干的温度为120℃,烘干时间为6h;
步骤五:将步骤四得到的预烧料片状样品置于高温箱式电阻炉中,以10℃/min的升温速率升温至1250℃,然后保温4h后随炉冷却至室温,最终得到分子式为Sr0.9Gd 0.1Fe11.9Mn0.1O19的M型锶铁氧体磁性材料。
对本实施例制备的M型锶铁氧体磁性材料进行XRD衍射测试,测试结果如图3所示,由图可见:粉体在衍射角2θ=30.4°,31.0°,32.36°,34.2°等处出现强烈的衍射峰,对应六方晶相(110)晶面、(008)晶面、(107)晶面(114)晶面,跟纯M型锶铁氧体SrFe12O19标准卡片及按实施例一制备方法制得的纯M型锶铁氧体SrFe12O19 的XRD衍射图比对基本吻合,没有发现其他杂峰,表明此时的粉体为单一的M型锶铁氧体相。
对本实施例制备的M型锶铁氧体磁性材料进行SEM扫描,结果如图4所示,由图可见,样品中的晶粒尺寸在2μm~4μm之间,且晶粒尺寸大小均匀,分布也较均匀,晶粒界面清晰,呈六角片状结构,样品中存在一定的孔洞,说明样品的密度仍有提升的空间。
对本实施例制备的分子式为Sr0.9Gd 0.1Fe11.9Mn0.1O19的M型锶铁氧体磁性材料进行VSM测试:剩余磁化强度Br=39.43emu/g,饱和磁化强度Ms=57.87emu/g,矫顽力Hc=52.72kA/m;按照本实施例的方法和工艺参数制备分子式为SrFe12O19 的M型锶铁氧体磁性材料并通过VSM测试得到剩余磁化强度Br=28.89emu/g,饱和磁化强度Ms=53.36emu/g,矫顽力Hc=32.58kA/m,由此可知,本实施例制备的分子式为Sr0.9Gd 0.1Fe11.9Mn0.1O19的M型锶铁氧体磁性材料与现有的分子式为SrFe12O19 的M型锶铁氧体磁性材料相比,剩余磁化强度Br增加36.48%,饱和磁化强度Ms增加8.45%,矫顽力Hc增加61.82%。
Claims (8)
1.一种锶铁氧体磁性材料,其特征在于该锶铁氧体磁性材料的分子式为:Sr1-xGdxFe12- xMnxO19,分子式中:0<x<0.1。
2.一种制备如权利要求1所述的M型锶铁氧体磁性材料的方法,其特征在于该方法按照以下步骤进行:
步骤一:按照分子式Sr1-xGdxFe12-xMnxO19中的化学计量比称取Gd2O3、MnCO3、SrCO3和Fe2O3做为原料,分子式Sr1-xLnxFe12-xMnxO19中:0<x<0.1;
步骤二:将步骤一中称取的原料、磨球和乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料1h~2h得到混合粉体,将得到的混合粉体烘干后置于压片的模具中,在3MPa~5MPa的压力下压制得到片状样品;
步骤三:把步骤二得到的片状样品放入高温箱式电阻炉中,以5~10℃/min的升温速率升温至1200℃~1250℃,然后保温2h~8h后随炉冷却至室温,得到预烧料;
步骤四:将步骤三得到的预烧料用钢钵进行粗破碎并研磨,然后将研磨后的预烧料、磨球和乙醇置于行星球磨机的陶瓷球磨罐中,在转速为300r/min~500r/min下混料2h~3h,烘干后将混料置于压片的模具中,在3MPa~5MPa的压力下压制得到预烧料片状样品;
步骤五:将步骤四得到的预烧料片状样品置于高温箱式电阻炉中,以5℃/min ~10℃/min的升温速率升温至1150℃~1250℃,然后保温2h~4h后随炉冷却至室温,最终得到分子式为Sr1-xGdxFe12-xMnxO19的M型锶铁氧体磁性材料。
3.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤二所述磨球为氧化锆磨球。
4.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤二所述磨球、原料和乙醇的质量比为10:1:0.5。
5.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤二所述烘干的温度为80℃~150℃,烘干时间为3h~6h。
6.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤四所述磨球为氧化锆磨球。
7.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤四所述磨球、原料和无水乙醇的质量比为10:1:0.5。
8.根据权利要求2所述的M型锶铁氧体磁性材料的制备方法,其特征在于步骤四所述烘干的温度为80℃~150℃,烘干时间为3h~6h。
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