CN111411325A - 钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法 - Google Patents

钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法 Download PDF

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CN111411325A
CN111411325A CN201910007062.8A CN201910007062A CN111411325A CN 111411325 A CN111411325 A CN 111411325A CN 201910007062 A CN201910007062 A CN 201910007062A CN 111411325 A CN111411325 A CN 111411325A
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董元
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Abstract

本发明涉及涉及一种稀土氮化物粘结永磁材料,具体为一种钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法。针对现有钐铁氮或钕铁氮各向异性粘结磁粉颗粒外包覆的都是有机防氧化膜的现状,提供一种包覆金属防氧化膜的钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法。所述制备方法是由如下步骤实现的:1)制备钐铁氮或钕铁氮各向异性磁粉;2)在10‑1‑‑10‑4Pa真空下,以气相沉积的方法在钐铁氮或钕铁氮各向异性磁粉的颗粒表面镀一层防氧化金属膜,所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金;金属的用量为钐铁氮或钕铁氮各向异性磁粉重量的0.5‑4.5%。

Description

钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法
技术领域
本发明涉及稀土粘结永磁材料领域,特别涉及一种稀土氮化物粘结永磁材料,具体为一种钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法。
背景技术
粘结磁体具有可成型复杂形状、成型尺寸精度高、无需二次加工、材料利用率高、生产效率高、成本低、磁性能优良等特点,在硬盘驱动器、光盘驱动器、办公自动化、消费电子、家用电器、汽车工业等领域得到广泛应用。
目前粘结磁粉主要是钕铁硼HDDR粉末,但由于其居里温度低,限制了其使用的范围。
Sm2Fe17Nx( 简称钐铁氮 ) 与 Nd2Fe17Nx( 简称钕铁氮 )具有优异的内禀磁性,可与钕铁硼媲美,同时,其居里温度高达470℃,高于钕铁硼。因此,钐铁氮与钕铁氮在制备各向异性粘结磁体(粉)方面得到关注。
钐铁氮或钕铁氮各向异性磁粉粒度在3μm以下,不能在空气中存在,成粉后需马上制成粘结磁体,或在磁粉颗粒外包覆一层防氧化膜而成为粘结磁粉。目前,防氧化膜都是有机膜,未见金属防氧化膜及其制备方法的相关报道。
发明内容
本发明针对现有钐铁氮或钕铁氮各向异性粘结磁粉颗粒外包覆的都是有机防氧化膜的现状,提供一种包覆金属防氧化膜的钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法。
本发明是采用如下技术方案实现的:钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,是由如下步骤实现的:
1)制备钐铁氮或钕铁氮各向异性磁粉;
2)在10-1--10-4Pa真空下,以气相沉积的方法在钐铁氮或钕铁氮各向异性磁粉的颗粒表面镀一层防氧化金属膜,所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金;金属的用量为钐铁氮或钕铁氮各向异性磁粉重量的0.5-4.5%。
进一步地,步骤1)的钐铁氮或钕铁氮各向异性磁粉是由如下步骤制备的:
1-1)制备钐铁合金(Sm2Fe17)或钕铁合金(Nd2Fe17);
1-2)将钐铁合金或钕铁合金粗破碎到平均粒度0.5mm以下;
1-3)再气流粉碎到平均粒度2-3微米;
1-4)在如下条件下进行氮化处理而得到钐铁氮或钕铁氮各向异性磁粉:氮气分压50KPa-200KPa,氢气分压0KPa-50KPa,温度350℃--550℃,时间0.5-10小时。
更进一步,步骤1-4)的氮化处理和步骤2)是在同一个处理设备中完成;步骤1-4)完成后,待得到的钐铁氮或钕铁氮各向异性磁粉冷却到100-200℃,接着进行步骤2)。将氮化处理和表面镀膜巧妙地设计在同一个工位内完成,可靠、廉价的实现了氮化处理和表面包覆,为钐铁氮、钕铁氮各向异性粘结磁粉的广泛使用创造了可能。
钐铁氮或钕铁氮各向异性粘结磁粉,是在各向异性钐铁氮磁粉颗粒或钕铁氮磁粉颗粒的表面包覆防氧化金属膜,而得到在空气中不被氧化的钐铁氮或钕铁氮各向异性粘结磁粉;所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金。防氧化金属膜的厚度为0.5-20纳米;防氧化金属膜的厚度低于0.5纳米不能可靠完整的包覆,高于20纳米会影响粘结磁体的磁性能。
本发明给出了包覆防氧化金属膜的钐铁氮或钕铁氮各向异性粘结磁粉及其制备方法,填补了钐铁氮或钕铁氮各向异性粘结磁粉的空白,丰富了钐铁氮或钕铁氮各向异性粘结磁粉的种类。创造性地给出了制备方法涉及的精确技术参数,和粘接磁粉的层结构特征。
具体实施方式
钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,是由如下步骤实现的:
1)制备钐铁氮或钕铁氮各向异性磁粉;
2)在10-1--10-4Pa真空下(如,可选用0.1Pa、0.05Pa、0.01Pa、0.001Pa、0.0006Pa、0.0001Pa),以气相沉积的方法在钐铁氮或钕铁氮各向异性磁粉的颗粒表面镀一层防氧化金属膜,所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金;金属的用量为钐铁氮或钕铁氮各向异性磁粉重量的0.5-4.5%(0.5%、1.0%、2.5%、3.0%、4.0%、4.5%)。所述气相沉积的方法具体是金属真空蒸汽镀,金属加热蒸发温度400-2000℃(如,选用400℃、600℃、800℃、1000℃、1200℃、1500℃、2000℃,根据所镀金属的饱和蒸汽压而定)。加热方式为电阻热场加热、电子束加热或等离子轰击。
步骤1)的钐铁氮或钕铁氮各向异性磁粉是由如下步骤制备的:
1-1)制备钐铁合金(Sm2Fe17)或钕铁合金(Nd2Fe17);具体采用速凝法制备成厚度为0.05-0.4mm(选用0.05 mm、0.1 mm、0.2 mm、0.3 mm、0.35 mm、0.4 mm)的钐铁合金或钕铁合金薄片;
1-2)将钐铁合金或钕铁合金粗破碎到平均粒度0.5mm以下;
1-3)再气流粉碎到平均粒度2-3微米;
1-4)在如下条件下进行氮化处理而得到钐铁氮或钕铁氮各向异性磁粉:氮气分压50KPa-200KPa,(如,选用50KPa、100KPa、150 KPa、200KPa)氢气分压0KPa-50KPa,(如,选用0KPa、20KPa、50KPa),温度350℃--550℃(如,选用350℃、370℃、400℃、450℃、480℃、500℃、550℃),时间0.5-10小时(如,选用0.5小时、1小时、2小时、3.5小时、5小时、8小时、9.5小时、10小时)。
步骤1-4)的氮化处理和步骤2)是在同一个处理设备中完成;步骤1-4)完成后,待得到的钐铁氮或钕铁氮各向异性粘结磁粉冷却到100-200℃,接着进行步骤2)。所述的处理设备采用旋转式真空镀膜机;旋转速度0.5-15转/分钟。
防氧化金属膜镀完后,充入惰性气体N2或Ar,冷却到室温。
步骤1)所述的钐铁氮或钕铁氮各向异性磁粉也可以采用以还原扩散、渗氮法制得的钐铁氮或钕铁氮各向异性磁粉。
一种钐铁氮或钕铁氮各向异性粘结磁粉,是在各向异性钐铁氮磁粉颗粒或钕铁氮磁粉颗粒的表面包覆防氧化金属膜,而得到在空气中不被氧化的钐铁氮或钕铁氮各向异性粘结磁粉;所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金。防氧化金属膜的厚度为0.5-20纳米(0.5纳米、1.0纳米、5.0纳米、8纳米、10纳米、15纳米、20纳米)。
实施例
按照 Sm2Fe17原子比配置炉料,并增加总重量百分比1-5%Sm,用于抵消真空熔炼的挥发。熔炼并速凝冷却,得到0.05-0.4mm的薄带。
在锤式破碎机中破碎,至粒度小于0.5mm。
用气流磨粉碎到3微米。
在密封并于氮气饱和的条件下装入旋转式真空镀膜机内,并加入Sm2Fe17粉末重量1.5%的金属Zn到坩埚内。
抽真空到0.1Pa,升温到480℃,充高纯氮气至压力120KPa,转速2转/分,保持200分钟。
冷却到200℃,抽真空到0.1Pa,将坩埚温度升到800℃开始镀锌膜。40分钟镀膜结束。充氮气,压力150KPa。冷却到室温后,出炉。
实测磁粉磁性能:Br1.38T,Hcj 1800KA/m,(BH)max 358KJ/m3

Claims (10)

1.一种钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,是由如下步骤实现的:
1)制备钐铁氮或钕铁氮各向异性磁粉;
2)在10-1--10-4Pa真空下,以气相沉积的方法在钐铁氮或钕铁氮各向异性磁粉的颗粒表面镀一层防氧化金属膜,所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金。
2.根据权利要求1所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,金属的用量为钐铁氮或钕铁氮各向异性磁粉重量的0.5-4.5%。
3.根据权利要求1或2所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,步骤1)的钐铁氮或钕铁氮各向异性磁粉是由如下步骤制备的:
1-1)制备钐铁合金或钕铁合金;
1-2)将钐铁合金或钕铁合金粗破碎到平均粒度0.5mm以下;
1-3)再气流粉碎到平均粒度2-3微米;
1-4)在如下条件下进行氮化处理而得到钐铁氮或钕铁氮各向异性磁粉:氮气分压50KPa-200KPa,氢气分压0KPa-50KPa,温度350℃--550℃,时间0.5-10小时。
4.根据权利要求3所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,气相沉积的方法具体是金属真空蒸汽镀,金属加热蒸发温度400-2000℃。
5.根据权利要求3所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,采用速凝法制备成厚度为0.05-0.4mm的钐铁合金或钕铁合金薄片。
6.根据权利要求3所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,步骤1-4)的氮化处理和步骤2)是在同一个处理设备中完成。
7.根据权利要求6所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,步骤1-4)完成后,待得到的钐铁氮或钕铁氮各向异性粘结磁粉冷却到100-200℃,接着进行步骤2)。
8.根据权利要求1或2所述的钐铁氮或钕铁氮各向异性粘结磁粉的制备方法,其特征在于,步骤1)所述的钐铁氮或钕铁氮各向异性磁粉采用以还原扩散、渗氮法制得的钐铁氮或钕铁氮各向异性磁粉。
9.一种钐铁氮或钕铁氮各向异性粘结磁粉,其特征在于,是在各向异性钐铁氮磁粉颗粒或钕铁氮磁粉颗粒的表面包覆防氧化金属膜,而得到在空气中不被氧化的钐铁氮或钕铁氮各向异性粘结磁粉;所述金属为Ir、Ti、Au、Ag、Ni、Cu、Al、Zn、Sn中的一种或多种以任意比例制成的合金。
10.根据权利要求9所述的钐铁氮或钕铁氮各向异性粘结磁粉,其特征在于,防氧化金属膜的厚度为0.5-20纳米。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022107462A1 (ja) * 2020-11-19 2022-05-27 日亜化学工業株式会社 リン酸塩被覆SmFeN系異方性磁性粉末の製造方法、およびボンド磁石

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Application publication date: 20200714