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以硫脲为硫源、硼酸为缓冲剂、柠檬酸三钠为络合剂及糖精和1,4丁炔二醇为添加剂的酸性镀液中电沉积了Fe-Ni-S非晶合金薄膜。采用差示扫描量热(DSC)、X射线衍射(XRD)和扫描电镜(SEM)研究了该合金的晶化行为和表面微观形貌。结果表明,镀态Fe-Ni-S合金呈非晶态结构,250℃热处理出现了Fe_7Ni_3(I_(mam))微晶,320.4℃开始晶化出现NiS(R_(3m))相和FeNi_3(P_(m3m))相,417.9℃下大量晶化生成NiS(R_(3m))相和FeNi_3(P_(m3m))相,500℃时合金完全晶化生成许多粒径约为100-200 nm均匀颗粒。研究了热处理对合金薄膜的磁性能、显微硬度和耐腐蚀性能的影响。250℃以下,随着退火温度升高,薄膜的磁性能、显微硬度和耐腐蚀性能不断提高,然后下降。250℃热处理时,合金薄膜饱和磁化强度、硬度和电化学阻抗达到最大(Ms≈1201.1 kA/m,Hv≈425.4 kg/mm~2,Z′≈400Ω),而矫顽力最小(H_C≈2.1 kA/m)。因此250℃热处理的合金镀层软磁性能最佳,耐腐蚀最好。
Fe-Ni-S amorphous alloy films were electrodeposited in acid bath containing thiourea as sulfur source, boric acid as buffer, trisodium citrate as complexing agent, saccharin and 1,4-butynediol as additive. The crystallization behavior and surface morphology of the alloy were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that the as-deposited Fe-Ni-S alloy has an amorphous structure, Fe_7Ni_3 (I_ (mam)) crystallites appear at 250 ℃ and NiS (R_3m) and FeNi_3 (P_ (3m) phase and FeNi_3 (Pm (m3m)) phase at 417.9 ℃. The alloy was completely crystallized at 500 ℃ to form many homogeneous particles with the size of about 100-200 nm . The effects of heat treatment on the magnetic properties, microhardness and corrosion resistance of the alloy films were investigated. Below 250 ℃, with the annealing temperature increases, the magnetic properties of the film, microhardness and corrosion resistance continue to increase, and then decline. At 250 ℃, the saturation magnetization, hardness and electrochemical impedance of the alloy film reach the maximum (Ms≈1201.1 kA / m, Hv≈425.4 kg / mm ~ 2, Z’≈400Ω), while the coercive force is the smallest (H_C≈2.1 kA / m). Therefore, 250 ℃ heat treatment alloy coating best soft magnetic properties, the best corrosion resistance.