摘要
非晶态合金具有长程无序、短程有序的结构特点，使其具有一系列独特的优良性能，如高强度、高硬度、耐腐蚀和耐磨损等。近年来一系列大块非晶合金的发现，更使其成为目前材料科学的热点领域之一。磁性材料是应用最为广泛的一种功能材料，具有优异磁性能的大块非晶合金的研究也备受人们的关注。本论文对Fe-Nd-Al系非晶合金的磁性能、非晶形成能力和晶化行为做了较为深入的研究，重点研究了该系列非晶合金在铸态和晶化后的微观结构和磁性能的变化规律。探索了在合金居里温度附近，外加脉冲磁场退火处理对具有铁磁性大块非晶合金磁性能的影响，研究了其晶化过程中磁性能与相组成和微观结构的变化关系。主要实验结果和结论如下：
在Fe_xNd_(90-x)Al_(10)(x=30-55)合金中提高Fe元素的相对含量，合金的饱和磁化强度提高，但其非晶形成能力有所下降。其中Fe_(53)Nd_(37)Al_(10)合金是非晶形成能力较好、饱和磁化强度较高的Fe基合金。Fe_(53)Nd_(37)Al_(10)合金的吸铸样品为软磁性，而条带样品为硬磁性，该现象与Nd基合金的磁性能恰好相反。通过HRTEM观察到Fe_(53)Nd_(37)Al_(10)条带中的非晶相含有A_x有序相(α=0．549nm面心立方结构的相)，这些具有各向异性的有序相通过交互耦合作用使得非晶相具有硬磁性，从而使Fe_(53)Nd_(37)Al_(10)淬态条带为硬磁性。而Fe_(53)Nd_(37)Al_(10)吸铸样品中的非晶相是完全无序的，所以表现为软磁性。Fe_(53)Nd_(37)Al_(10)条带样品中含有大量的短程有序自旋玻璃态的磁有序结构，而Fe_(53)Nd_(37)Al_(10)吸铸样品则主要是由长程有序的铁磁态结构组成。
在研究Fe_(53)Nd_(37)Al_(10)合金的过程中，得到了一种新的Nd基非晶合金Fe_(28)Nd_(59)Al_(13)。该合金具有很好的非晶形成能力，吸铸样品为硬磁性，条带样品为软磁性。通过对Fe_(28)Nd_(59)Al_(13)合金条带和吸铸样品结构和磁性能的分析，进一步证实了Nd基大块非晶合金的硬磁性来源于非晶相中的短程有序结构。
在(Fe_(0．53)Nd_(0．37)Al_(0．10))_(100-x)B_x合金中，随着B元素的相对含量增加，合金的非晶形成能力下降，当B含量增加到5at％时，合金中已基本不含有非晶相。随着B含量的增加，合金从软磁性转变为硬磁性，这是由于合金中出现了新的晶态相Nd_2Fe_(14)B的缘故。当(Fe_(0．53)Nd_(0．37)Al_(0.10))_(100-x)B_x(x=2，4)合金在晶化退火后，硬磁性相Nd_2Fe_(14)B的相对含量增加，合金的内禀矫顽力得到进一步的提高。
通过比较两种脉冲磁场退火工艺(工艺Ⅰ和Ⅱ)对合金磁性能的影响可知，在退火冷却阶段也外加磁场(工艺Ⅱ)，可以避免磁场退火中已经偏转的磁矩在冷却过程中发生偏转复位，磁性能可以更加显著得提高。将(Fe_(0．53)Nd_(0．37)Al_(0．1))_(96)B_4≈Fe_(51)Nd_(35)Al_(10)B_4合金在463K、523K下5T脉冲磁场退火后，获得比常规退火更好的综合磁性能。特别是523K下采用工艺Ⅱ脉冲磁场退火，与常规退火相比，合金的剩磁提高幅度达25．9％。即利用脉冲磁场在合金的居里温度以下进行退火，可以明显改善大块非晶磁性材料的磁性能。
适量Zr(6at％)的添加有效地提高合金[Fe_(0．51)Nd_(0.35)Al_(0.10)B_(0．04)]_(100-x)Zr_x的非晶形成能力，合金从硬磁性转变为软磁性。在对x=6合金的研究结果中，发现了一种新的具有较好非晶形成能力和软磁性能的大块非晶合金Fe_(47)Nd_(38)Al_(12)Zr_3。在[Fe_(0．51)Nd_(0．35)Al_(0.10)B_(0．04)]_(100-x)Nb_x合金中，适当Nb元素的添加(4at％-8at％)可以有效提高合金的非晶形成能力，而一定量(≥4at％)的Nb元素将会抑制硬磁相Nd_2Fe_(14)B的析出，使得合金从硬磁性转变成软磁性。少量Dy元素(1at％)的添加，使得合金[Fe_(0．51)Nd_(0．35)Al_(0.10)B_(0．04)]_(100-x)Dy_x的磁性能大幅度提高，使合金的剩磁从13．42 Am~2／kg提高到20．10Am~2／kg，内禀矫顽力从237．4kA／m提高到491．0kA／m。
The amorphous alloys have many unique characteristics such as high strength, high hardness, excellent corrosion resistance and good wear resistance due to the microstructure of long-range disorder and short-range order. Recently, the discoveries of multi-component bulk amorphous alloys have been one of the hottest topics in the materials science field. Ferromagnetic materials have the widest applications among the functional materials. Therefore, the bulk amorphous alloys with ferromagnetic properties have attracted much attention. In this work, the magnetic properties, glass forming ability and crystallization behavior of Fe-Nd-Al amorphous alloys have been investigated. Especially, the present investigations are mainly focused on the correlations between microstructure and magnetic properties of the as-cast bulk amorphous alloys and the annealed alloys. Pulsed magnetic field is employed when annealing temperature is around the Curie temperature of the alloy. The effects of the microstructure and magnetic properties for the ferromagnetic amorphous alloy have been studied in detail. Some of the main experimental results are listed as follows:
For Fe_xNd_(90-x)Al_(10) (x=30-55) alloys, the saturation magnetization increases and the glass forming ability decreases with the increasing Fe content. The Fe_(53)Nd_(37)Al_(10) alloy shows good glass forming ability and soft magnetic property with high saturation magnetization. The Fe_(53)Nd_(37)Al_(10) melt-spun ribbon exhibits high coercivity, while the bulk alloy prepared by suction casting shows soft magnetic property. The phenomenon is contrary to that of the Nd-based bulk amorphous alloy and ribbons. Ax phases (face-centered cubic structure a=0.549nm) can be observed in the amorphous phase of the Fe_(53)Nd_(37)Al_(10) ribbon by high resolution transmission electron microscopy (HRTEM). The hard magnetic property of the ribbon results from the magnetic exchange coupling interaction between A_x phases with large random anisotropy. The soft magnetic property of bulk Fe_(53)Nd_(37)Al_(10) alloy is attributed to the amorphous phase with the fully disordered microstructure. Furthermore, the existence of the spin-glass-like short-range magnetic order in the Fe_(53)Nd_(37)Al_(10) ribbon and the long-range ferromagnetic order in the bulk Fe_(53)Nd_(37)Al_(10) alloy can be validated.
From the SEM and EDS results of the bulk Fe_(53)Nd_(37)Al_(10) alloy, a new bulk Nd-rich amorphous alloy (Fe_(28)Nd_(59)Al_(13)) with good glass forming ability is obtained. The bulk amorphous alloy shows hard magnetic property, while the ribbon presents soft magnetic property. The microstructure and magnetic property investigations validate that the origin of hard magnetic property for Nd-based bulk amorphous alloy is the short-range order with large random anisotropy.
The glass forming ability significantly deceases with the addition of boron in the(Fe_(0.53)Nd_(0.37)Al_(0.10))_(100-x)B_x alloy and there is almost no amorphous phase in the x=5 alloy. The magnetic properties of the alloys change from soft magnetic property to hard magnetic property with the increasing boron content, which is due to the presence of the Nd_2Fe_(14)B phase. The proportion of Nd_2Fe_(14)B phase increases while the alloy annealed over crystallization temperatrue. Therefore, the intrinsic coercivity of the alloys increases markedly.
The bulk (Fe_(0.53)Nd_(0.37)Al_(0.1))_(96)B_4 alloy is annealed in a pulsed magnetic field with two different working processes (ProcessingⅠandⅡ). The results demonstrate that the magnetic property of the alloy can be further enhanced with pulsed magnetic field during the furnace cooling (ProcessingⅡ). It may be ascribed as the pulsed magnetic field can keep the magnetic moment alignment. The alloy has better magnetic property when annealed in a 5T pulsed magnetic field at 463K and 523K. The optimal magnetic property of the alloy is obtained by annealing at 523K using Processing II. The remanence is enhanced by 25.9% compared with that of sample without magnetic field annealing. It can provide a new way to improve the magnetic properties of ferromagnetic bulk amorphous alloys with pulsed magnetic field annealing below the Curie temperature of the alloy.
The proper addition of Zr (6%) is very effective in improving the glass forming ability of [Fe_(0.51)Nd_(0.35)Al_(0.10)B_(0.04)]_(100-x)Zr_x alloys and the magnetic properties of the alloys change from hard magnetic property to soft magnetic property. From the results of SEM and EDS, a new bulk amorphous alloy (Fe_(47)Nd_(38)Al_(12)Zr_3) with good glass forming ability is prepared by suction casting and it shows soft magnetic property. The addition of Nb (4at%-8at%) could effectively enhance the glass forming ability of the [Fe_(0.41)Nd_(0.35)Al_(0.10)B_(0.04)]_(100-x)Nb_x alloys. However, the precipitation of hard magnetic phase Nd_2Fe_(14)B would be depressed by the certain addition of Nb (≥4at%). Therefore, the magnetic properties of the alloys change from hard magnetic property to soft magnetic property. The minor Dy addition is effective in improving the magnetic properties of the [Fe_(0.41)Nd_(0.35)Al_(0.10)B_(0.04)]_(100-x)Dy_x alloys. With the addition of Dy=lat%, the remanence (M_r) changes from 13.42Am~2/kg to 20.10Am~2/kg and the coercivity (iH_c) changes from 237.4kA/m to 491.0kA/m, respectively.
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