以还原铁粉为基体粉末,探究氧化促进剂Na2MoO4、NaNO2及其复合添加对铁粉在NaH2PO4磷化液中磷化反应的影响,通过扫描电镜、X射线衍射仪、傅里叶红外光谱仪,振动样品磁强计以及软磁交流测量仪对磷化前后的铁粉和铁粉芯进行结构与性能表征。结果表明:铁粉在质量分数为5%的NaH2PO4磷化液中反应速度过快,无法生成完整均匀的包覆层,铁粉芯的软磁损耗虽有降低,但磁导率的频率稳定性不佳,铁粉经NaH2PO4磷化的表面磷化层主要由Fe3(PO4)2、FePO4组成。在NaH2PO4磷化液中添加NaNO2,虽然促进了磷酸盐的生成,但包覆不均匀,其包覆层主要由FePO4组成;在NaH2PO4磷化液中添加Na2MoO4或Na2MoO4+NaNO2复合氧化促进剂可以使铁粉表面生成均匀的包覆层,大幅度降低铁粉芯的涡流损耗,其包覆层主要由FePO4和Fe2(MoO4)3组成。其中Na2MoO4+NaNO2复合添加对磷化反应的改善效果最好,400 ℃热处理后的铁粉芯电阻率为194.2 μΩ·m,在测试励磁场强度Bm=50 mT,测试频率f=100 kHz条件下,铁粉芯的磁导率为92.5,软磁损耗为142.0 W/kg。
[1] TAGHVAEI A H, EBRAHIMI A, GHEISARI K, et al.Analysis of the magnetic losses in iron-based soft magnetic composites with MgO insulation produced by sol-gel method[J]. Journal of Magnetism and Magnetic Materials, 2010, 322(23): 3748-3754.
[2] HSIANG H I, FAN L F, HUNG J J.Phosphoric acid addition effect on the microstructure and magnetic properties of iron-based soft magnetic composites[J]. Journal of Magnetism and Magnetic Materials, 2018, 447: 1-8.
[3] YI Y, PENG Y, XIA C, et al.Influence of heat treatment on microstructures and magnetic properties of Fe-based soft magnetic composites prepared by co-precipitation method[J]. Journal of Magnetism and Magnetic Materials, 2019, 476: 100-105.
[4] LI K, CHENG D, YU H, et al.Process optimization and magnetic properties of soft magnetic composite cores based on phosphated and mixed resin coated Fe powders[J]. Journal of Magnetism and Magnetic Materials, 2020, 501: 166455.
[5] ZHENG J, ZHENG H, LE J, et al.Magnetic properties and microstructure of iron-based soft magnetic composites with Al2O3 insulating coating by one-pot synthesis method[J]. Journal of Magnetism and Magnetic Materials, 2020, 499: 166255.
[6] WU S, SUN A, ZHAI F, et al.Annealing effects on magnetic properties of silicone coated iron-based soft magnetic composites[J]. Journal of Magnetism and Magnetic Materials, 2012, 324(5): 818-822.
[7] LI L, GAO Z, LI A, et al.Fabrication of carbonyl iron powder/ SiO2-reduced iron powder/SiO2 soft magnetic composites with a high resistivity and low core loss[J]. Journal of Magnetism and Magnetic Materials, 2018, 464: 161-167.
[8] GAO Z, LI L, GE Y, et al.Enhanced AC magnetic properties of Fe-based soft magnetic composites coated with an electrically insulated SiO2-ZrO2 layer[J]. Journal of Materials Science- Materials in Electronics, 2021, 32(11): 14944-14955.
[9] ZHOU M M, HAN Y, GUAN W W, et al.Magnetic properties and loss mechanism of Fe-6.5wt%Si powder core insulated with magnetic Mn-Zn ferrite nanoparticles[J]. Journal of Magnetism and Magnetic Materials, 2019, 482: 148-154.
[10] 李腊, 蔡一湘, 刘辛, 等. 磷酸浓度对Fe-6.5%Si磁粉芯组织及磁特性的影响[J]. 粉末冶金材料科学与工程, 2016, 21(6): 899-906.
LI La, CAI Yixiang, LIU Xin, et al.Effect of phosphoric acid concentration on microstructure and magnetic properties of Fe- 6.5%Si magnetic powder core[J]. Journal of Materials Science and Engineering for Powder Metallurgy, 2016, 21(6): 899-906.
[11] 李发长, 冯晓鹏, 李一, 等. 热处理工艺对铁基软磁复合材料电磁性能的影响[J]. 粉末冶金材料科学与工程, 2015, 20(2): 319-324.
LI Fachang, FENG Xiaopeng, LI Yi, et al.Effect of heat treatment process on electromagnetic properties of iron-based soft magnetic composites[J]. Journal of Materials Science and Engineering of Powder Metallurgy, 2015, 20(2): 319-324.
[12] CHEN Z, LIU X, KAN X, et al.Phosphate coatings evolution study and effects of ultrasonic on soft magnetic properties of FeSiAl by aqueous phosphoric acid solution passivation[J]. Journal of Alloys and Compounds, 2019, 783: 434-440.
[13] 刘菲菲, BAKER A P, 翁履谦, 等. 铁粉基软磁复合材料绝缘包覆层的研究[J]. 材料开发与应用, 2007, 22(5): 11-15.
LIU Feifei, BAKER A P, WENG Lüqian, et al.Study on insulating coating of iron powder based soft magnetic composites[J]. Development and Application of Materials, 2007, 22(5): 11-15.
[14] HUANG M, WU C, JIANG Y, et al.Evolution of phosphate coatings during high-temperature annealing and its influence on the Fe and FeSiAl soft magnetic composites[J]. Journal of Alloys and Compounds, 2015, 644: 124-130.
[15] 鲁维国, 李淑英. 磷化促进剂[J]. 表面技术, 2002, 31(6): 12-14, 23.
LU Wei Guo, LI Shuying.Phosphatizing accelerator[J]. Surface Technology, 2002(6): 12-14, 23.
[16] 唐思哲, 胡家秀, 赵健, 等. 新型无机复配缓蚀剂对钠基膨润土中Q235钢的缓蚀作用[J]. 化工进展, 2018, 37(12): 4806-4813.
TANG Sizhe, HU Jiaxiu, ZHAO Jian, et al.Corrosion inhibition effect of new inorganic compound corrosion inhibitor on Q235 steel in sodium bentonite[J]. Chemical Industry and Engineering Progress, 2018, 37(12): 4806-4813.
[17] 王瑛, 柴明成, 王宇友. 钼酸盐与其他缓蚀剂协同缓蚀效应的研究[J]. 上海化工, 2003, 7: 23-25.
WANG Ying, CAI Mingcheng, WANG Yuyou.Study on synergistic inhibition effect of molybdate and other corrosion inhibitors[J]. Shanghai Chemical Industry, 2003, 7: 23-25.
[18] 李红兵, 李爱农, 林志峰, 等. 钼酸盐复配体系对碳钢缓蚀作用研究[J]. 电镀与精饰, 2018, 40(5): 41-46.
LI Hongbing, LI Ainong, LIN Zhifeng,et al.Study on corrosion inhibition of carbon steel by molybdate complex system[J]. Plating & Finishing, 2018, 40(5): 41-46.
[19] 唐春华. 金属表面磷化技术[M]. 北京: 化学工业出版社, 2009: 1-29.
TANG Chunhua.Phosphating Technology for Metal Surface[M]. Beijing: Chemical Industry Press, 2009: 1-29.
[20] LI G Y, LIAN J S, NIU L Y, et al.Effect of zinc- phosphate-molybdate conversion precoating on performance of cathode epoxy electrocoat on AZ91D alloy[J]. Surface Engineering, 2007, 23(1): 56-61.
[21] 胡秀英, 傅建, 马迪. 促进剂对钢铁常温磷化的影响及机理[J]. 电镀与精饰, 2017, 39(9): 5-9.
HU Xiuying, FU Jian, MA Di.Effect and mechanism of accelerator on phosphating of iron and steel at room temperature[J]. Plating and Finishing, 2017, 39(9): 5-9.
[22] STRECKOVA M, FUEZER J, MEDVECKY L, et al.Characterization of composite materials based on Fe powder (core) and phenol-formaldehyde resin (shell) modified with nanometer-sized SiO2[J]. Bulletin of Materials Science, 2014, 37(2): 167-177.
[23] ZHAO N, HE C, LIU J, et al.Dependence of catalytic properties of Al/Fe2O3 thermites on morphology of Fe2O3 particles in combustion reactions[J]. Journal of Solid State Chemistry, 2014, 219: 67-73.
[24] 张圣麟, 陈华辉, 李红玲, 等. 常温磷化处理技术的研究现状及展望[J]. 材料保护, 2006, 39(7): 42-47.
ZHANG Shenglin, CHEN Huahui, LI Hongling, et al.Research status and prospect of phosphating technology at room temperature[J]. Journal of Materials Protection, 2006, 39(7): 42-47.
[25] ZHAO G, WU C, YAN M.Evolution of the insulation matrix and influences on the magnetic performance of Fe soft magnetic composites during annealing[J]. Journal of Alloys and Compounds, 2016, 685: 231-236.