非晶纳米晶软磁材料的制备及其性能研究

【作者】 宋翀旸；

【导师】 陈学定；

【作者基本信息】 兰州理工大学 ， 材料加工工程， 2003， 硕士

【摘要】 本文研制了铜辊直径450mm,宽度150mm的单辊熔体自旋设备，其径向跳动为±15μm，循环水冷却，密封良好，最大线速度达35.37m/s。从设计、加工、安装过程中保证了该设备所需精度，完成了实验室条件下制备非晶薄带，并为产业化创造了条件。本文选取Fe₇₈Si₉B₁₃、Fe_73.5Cu₁Nb₃Si_13.5B₉、Fe₇₄Cu₁Mo₂Nb₁Si₁₃B₉、Co₆₆Fe₄NiB₁₄Si₁₅和Fe₁₆Ni₆₀Cr₄B₁₆Si₄五种成分的合金作为研究对象，运用差热分析（DTA）、X衍射（XRD）、振动样品磁强计（VSM）、扫描电镜（SEM）等多种测试手段和设备对其性能进行分析，获得了非晶纳米晶软磁合金最佳综合性能的热处理工艺。 研究表明，非晶态合金随着热处理温度升高，均发生不同程度的晶化，一定成分的Fe基非晶合金在最佳温度范围内退火处理后可获得由非晶和纳米晶组成的复相组织，晶粒尺寸可达到8～16nm。另外，处于热力学亚稳态的非晶软磁合金在退火过程中发生结构重排，导致条带变脆，通过调整热处理工艺可以改善脆性，实现非晶合金延性与磁性较佳的配合。结果表明Fe₇₈Si₉B₁₃、Fe_73.5Cu₁Nb₃Si_13.5B₉、Fe₇₄Cu₁Mo₂Nb₁Si₁₃B₉合金分别在753K、813K、773K退火1h后合金材料具有优良的综合性能。同时Cu、Nb、Mo等元素的加入有助于提高晶化温度，稳定非晶相组织。其中Cu原子对α Fe-Si相纳米晶粒的形核有重要影响。Nb与B等元素有着择优键合作用，形成团簇结构直接影响着非晶相的热稳定性、Fe₂B的析出和纳米结构α Fe-Si晶粒的长大。 通过对比五种合金非晶晶化行为发现，833K退火1h后，Fe_73.5Cu₁Nb₃Si_13.5B₉合金与Co₆₆Fe₄NiB₁₄Si₁₅合金具有相似的软磁性能，Co₆₆Fe₄NiB₁₄Si₁₅合金晶化后晶粒较大，耐腐蚀性不如Fe_73.5Cu₁Nb₃Si_13.5B₉合金。773K退火1h后，Fe₁₆Ni₆₀Cr₄B₁₆Si₄合金晶粒长大达1μm，其软磁性能介于Fe₇₈Si₉B₁₃合金和Co₆₆Fe₄NiB₁₄Si₁₅合金之间。Fe基纳米晶软磁合金Fe_73.5Cu₁Nb₃Si_13.5B₉退火后晶化相稳定，晶粒细小可达8～11nm，磁性的温度稳定性和时间稳定性较高，因此具有更广阔的应用前景。更多还原

【Abstract】 An experimental melt spinning equipment with the copper roller 450mm in diameter, 150mm in width and ±15μm in radial vibration, which has circulating cooling and good airproof and 35.37m/s in the max wheel speed has been fabricated. In the process of designning, processing and installing, the precision of this equipment has been improved. The amorphous ribbons have been prepared with rapid solidification technology in experimental condition. Also it will be used to industrialization. The properties of Fe78Si9B13 , Fe73.5Cu1Nb3Si13.5B9, Fe74Cu1Mo2Nb1Si13B9, Co66Fe4NiB14S15 and Fe16Ni60Cr4B16Si4 alloys have been investigated mostly by means of differential thermal analysis(DTA),X-ray diffraction meter(XRD), Vabrating sample magnetometer(VSM), scanning electron microscope(SEM) et al. techniques. The optimal comprehensive properties have been obstained by the proper heat treatment process.It would be found that amorphous alloys would be crystallization at different degree with the temperature increase of heat treatment. The two phases structure of amorphous and nanocrystalline could be obstained by Fe-based amorphous alloys of some elements within best temperature rage. The average grain size was in the range of 8~16nm. Especially, Amorphous soft magnetic alloys which were thermodynamical metastable state would take place atom recognition in the process of annealed treatment resulted in the brittleness. The excellent coopertation of tenacity and magnetism was achieved by adjusting the heat treatment technologies. In this paper, the optimal comprehensive properties of alloys could be obstained by FeygSi9B13, Fe73.5Cu1Nb3Si13.5B9, Fe74Cu1Mo2Nb1Si13B9 alloys after 1h anneald at 753K, 813K, 773K respectively. At the same time, the addition of Cu, Nb, Mo elements could be benefit to improve crystallization temperature and stabilize amorphous structure. The addition of Cu atoms had significant effect on the nucleation process of a Fe-Si phase. The Nb atoms would preferently intetact with the B atoms and form relatively stable clustetrs. Thus, the clusters might influence on the thermal stabilities, the precipitation of the Fe2B, and the growth of the a Fe-Si nanocrystallities.Comparing with the crystallization of above alloys indicated that the soft magnetic properties of Fe735Cu1Nb3Si135B9 alloy was as well as Co66Fe4NiB14Si15 alloy after 1h annealed at 833K. Yet the average grain size of Co66Fe4NiB14Si15 alloy was larger, its resistance to corrosion was less than Fe73.5Cu1Nb3Si13.5B9 alloy. The average grain size of Fe16Ni6oCr4B16Si4 alloy accessed to lμm after Ih annealed at 773K, And its soft magnetic properties was between Co66Fe4NiB14Si15 alloy and Fe78Si9B13 alloy. The crystalline phases of Fe735Cu1Nb3Si13.5B9 alloys was stabilized, The Fe735Cu1Nb3Si135B9 alloy with 8-11nm crystalline grain was good thermal stability and time stability, Thus this kind of alloy would be an extensive application.更多还原