CN116504526A - 铁氧体微纳复合软磁粉体及其制备方法 - Google Patents
铁氧体微纳复合软磁粉体及其制备方法 Download PDFInfo
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Abstract
本发明提供一种铁氧体微纳复合软磁粉体及其制备方法,制备方法包括:将金属盐溶液、羰基铁粉及还原剂混合均匀,在惰性气体保护下加热至60‑80℃,反应30‑60分钟,得到金属纳米粒子悬浮液;将铁氧体前驱体溶液与表面活性剂混合均匀,在惰性气体保护下加热后,反应30‑60分钟,得到铁氧体纳米粒子悬浮液;将所述金属纳米粒子悬浮液和所述铁氧体纳米粒子悬浮液混合均匀,加热后,反应60‑90分钟,得到包覆有铁氧体粒子的复合粉末悬浮液;将所述复合粉末悬浮液进行离心、洗涤、干燥后,得到铁氧体微纳复合软磁粉体。通过本发明的制备方法能够快速、简便地制备出尺寸均匀、结构稳定、性能优异的铁氧体微纳复合软磁粉体。
Description
技术领域
本发明涉及软磁材料领域,尤其涉及一种铁氧体微纳复合软磁粉体及其制备方法。
背景技术
随着现代电子器件小型化、高频化的发展,要求磁芯具有高的饱和磁化强度、高磁导率、优良的高频性能。传统的软磁铁氧体材料由于其低电阻率,导致在高频下产生较大的涡流损耗,限制了其应用范围。金属软磁材料虽然具有较高的饱和磁化强度和低损耗,但是其易受外界环境影响而产生氧化、腐蚀等问题,影响其稳定性和可靠性。
为了克服上述问题,近年来出现了一种新型的软磁复合材料,即以金属为核心、以铁氧体为绝缘包覆层的复合粉末。这种复合粉末结合了金属和铁氧体两者的优点,既具有较高的饱和磁化强度和低损耗,又具有较好的抗氧化、抗腐蚀能力。然而,目前常用的制备方法主要是机械球磨法或雾化法,这些方法存在以下不足:一是球磨法需要长时间的机械处理,容易造成金属核心过度碎裂或包覆层过厚不均匀;二是雾化法需要较高温度下进行反应或还原处理,容易造成金属核心晶粒长大或包覆层结构变形;三是以上两种方法都难以控制复合粉末尺寸分布,在微米级以上波动较大。
因此,在现有技术水平下仍存在着提供一种能够快速、简便地制备出尺寸均匀、结构稳定、性能优异的铁氧体微纳复合软磁粉体及其制备方法等技术问题。
发明内容
本发明目的在于提供一种能够快速、简便地制备出尺寸均匀、结构稳定、性能优异的铁氧体微纳复合软磁粉体及其制备方法。
为实现上述目的,本发明提供了一种铁氧体微纳复合软磁粉体的制备方法,用于制备铁氧体微纳复合软磁粉体,所述制备方法包括:
S1:将金属盐溶液、羰基铁粉及还原剂混合均匀,在惰性气体保护下加热至60-80℃,反应30-60分钟,得到金属纳米粒子悬浮液;
S2:将铁氧体前驱体溶液与表面活性剂混合均匀,在惰性气体保护下加热至100-150℃,反应30-60分钟,得到铁氧体纳米粒子悬浮液;
S3:将所述金属纳米粒子悬浮液和所述铁氧体纳米粒子悬浮液混合均匀,加热至120-140℃,反应60-90分钟,得到包覆有铁氧体粒子的复合粉末悬浮液;
S4:将所述复合粉末悬浮液进行离心、洗涤、干燥后,得到铁氧体微纳复合软磁粉体。
作为本发明进一步地改进,所述金属盐溶液至少包括硝酸钴、硝酸亚铁、硝酸镍、硝酸锰、硝酸钴中的一种。
作为本发明进一步地改进,所述还原剂至少包括乙二胺、乙二胺四乙酸钠、甘油中的一种。
作为本发明进一步地改进,所述铁氧体前驱体溶液包括硝酸铁、硫酸亚铁、碳酸钠中的一种。
作为本发明进一步地改进,所述表面活性剂包括聚乙二醇、聚丙烯酸钠、十二烷基苯磺酸钠中的一种。
作为本发明进一步地改进,步骤S3中所述金属纳米粒子悬浮液和所述铁氧体纳米粒子悬浮液的比例为3:7。
本发明的另一个目的在于提供一种铁氧体微纳复合软磁粉体。
为实现上述目的,本发明提供了一种铁氧体微纳复合软磁粉体,所述铁氧体微纳复合软磁粉体应用上述制备方法制备获得。
本发明的有益效果是:与现有技术相比,本发明的铁氧体微纳复合软磁粉体结合羰基铁粉高饱和磁化强度、铁氧体高电阻率高使用频率的特点,获得了高频磁导率稳定的优异特征。同时,铁氧体包覆层均匀致密,颗粒粒径均匀,球形度高,且铁氧体包覆层为磁性相,有效减少了软磁复合材料中的磁稀释效应,通过本发明的制备方法能够快速、简便地制备出尺寸均匀、结构稳定、性能优异的铁氧体微纳复合软磁粉体。
附图说明
图1是本发明的铁氧体微纳复合软磁粉体的微米量级扫描电镜图。
具体实施方式
为了使本发明的目的、技术方案和优点更加清楚,下面结合附图和具体实施例对本发明进行详细描述。
在此,需要说明的是,为了避免因不必要的细节而模糊了本发明,在附图中仅仅示出了与本发明的方案密切相关的结构和/或处理步骤,而省略了与本发明关系不大的其他细节。
另外,还需要说明的是,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
实施例1
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸钴溶液、0.4mol/L的乙二胺四乙酸钠溶液按1:2的体积比混合得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至70℃,反应45分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至130℃,反应45分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按3:7的体积比混合均匀,在氮气保护下加热至130℃,反应75分钟,得到包覆有铁氧体纳米粒子的复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为200nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属钴和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实施例2
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硫酸亚铁溶液与0.4mol/L的甘油溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至80℃,反应60分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至140℃,反应60分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按5:5的体积比混合均匀,在氮气保护下加热至140℃,反应90分钟,得到包覆有铁氧体纳米粒子的铁微纳复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为300nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属铁和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实施例3
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸镍溶液与0.4mol/L的乙二胺溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至60℃,反应30分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至130℃,反应30分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按4:6的体积比混合均匀,在氮气保护下加热至120℃,反应60分钟,得到包覆有铁氧体纳米粒子的复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为250nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属镍和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实施例4
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸锰溶液与0.4mol/L的乙二胺四乙酸钠溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至50℃,反应15分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至110℃,反应15分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按6:4的体积比混合均匀,在氮气保护下加热至110℃,反应45分钟,得到包覆有铁氧体纳米粒子的复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为150nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属锰和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实施例5
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸钴溶液与0.4mol/L的乙二胺四乙酸钠溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至40℃,反应10分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至120℃,反应10分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按7:3的体积比混合均匀,在氮气保护下加热至100℃,反应30分钟,得到包覆有铁氧体纳米粒子的钴微纳复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为100nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属钴和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实验数据如下:
实施例6
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸镍溶液与0.4mol/L的乙二胺四乙酸钠溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至50℃,反应15分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至150℃,反应15分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按8:2的体积比混合均匀,在氮气保护下加热至120℃,反应60分钟,得到包覆有铁氧体纳米粒子的镍微纳复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为80nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属镍和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实验数据如下:
实施例7
制备铁氧体微纳复合软磁粉体的方法如下:
将0.2mol/L的硝酸锌溶液与0.4mol/L的乙二胺四乙酸钠溶液按1:2的体积比混合均匀得到混合溶液,加入羰基铁粉后搅拌均匀,羰基铁粉在混合溶液中的浓度为0.1g/L,在氮气保护下加热至60℃,反应20分钟,得到金属纳米粒子悬浮液;
将0.5mol/L的硝酸铁溶液与0.5mol/L的碳酸钠溶液按1:1的体积比混合均匀,在氮气保护下加热至100℃,反应20分钟,得到铁氧体纳米粒子悬浮液;
将金属纳米粒子悬浮液和铁氧体纳米粒子悬浮液按9:1的体积比混合均匀,在氮气保护下加热至140℃,反应90分钟,得到包覆有铁氧体纳米粒子的锌微纳复合粉末悬浮液;
将复合粉末悬浮液进行离心、洗涤、干燥等后处理,得到铁氧体微纳复合软磁粉体。
通过扫描电镜观察发现,所制备的铁氧体微纳复合软磁粉体具有球形或近似球形结构,平均尺寸约为60nm。通过X射线衍射分析发现,所制备的铁氧体微纳复合软磁粉体由金属锌和尖晶石型铁氧体两种相组成。通过交流阻抗谱仪测试发现,所制备的铁氧体微纳复合软磁粉体在100kHz-10MHz范围内具有较低的损耗角正切值。
实验数据如下:
综上所述,本发明的铁氧体微纳复合软磁粉体结合羰基铁粉高饱和磁化强度、铁氧体高电阻率高使用频率的特点,具有高频磁导率稳定的优异特征。同时,铁氧体包覆层均匀致密,颗粒粒径均匀,球形度高,且铁氧体包覆层为磁性相,有效减少了软磁复合材料中的磁稀释效应,通过本发明的制备方法能够快速、简便地制备出尺寸均匀、结构稳定、性能优异的铁氧体微纳复合软磁粉体。
以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围。
Claims (7)
1.一种铁氧体微纳复合软磁粉体制备方法,其特征在于,所述制备方法包括:
S1:将金属盐溶液、羰基铁粉及还原剂混合均匀,在惰性气体保护下加热至60-80℃,反应30-60分钟,得到金属纳米粒子悬浮液;
S2:将铁氧体前驱体溶液与表面活性剂混合均匀,在惰性气体保护下加热至100-150℃,反应30-60分钟,得到铁氧体纳米粒子悬浮液;
S3:将所述金属纳米粒子悬浮液和所述铁氧体纳米粒子悬浮液混合均匀,加热至120-140℃,反应60-90分钟,得到包覆有铁氧体粒子的复合粉末悬浮液;
S4:将所述复合粉末悬浮液进行离心、洗涤、干燥后,得到铁氧体微纳复合软磁粉体。
2.根据权利要求1所述的制备方法,其特征在于:所述金属盐溶液至少包括硝酸钴、硝酸亚铁、硝酸镍、硝酸锰、硝酸钴中的一种。
3.根据权利要求1所述的制备方法,其特征在于:所述还原剂至少包括乙二胺、乙二胺四乙酸钠、甘油中的一种。
4.根据权利要求1所述的制备方法,其特征在于:所述铁氧体前驱体溶液包括硝酸铁、硫酸亚铁、碳酸钠中的一种。
5.根据权利要求1所述的制备方法,其特征在于:所述表面活性剂包括聚乙二醇、聚丙烯酸钠、十二烷基苯磺酸钠中的一种。
6.根据权利要求1所述的制备方法,其特征在于:步骤S3中所述金属纳米粒子悬浮液和所述铁氧体纳米粒子悬浮液的比例为3:7。
7.一种铁氧体微纳复合软磁粉体,其特征在于,应用权利要求1~6任意一项所述的制备方法制备获得。
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