CN106531385B - 一种梯度型烧结钕铁硼磁体及其制备方法 - Google Patents

一种梯度型烧结钕铁硼磁体及其制备方法 Download PDF

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CN106531385B
CN106531385B CN201611173766.5A CN201611173766A CN106531385B CN 106531385 B CN106531385 B CN 106531385B CN 201611173766 A CN201611173766 A CN 201611173766A CN 106531385 B CN106531385 B CN 106531385B
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丁开鸿
李文超
彭众杰
徐明锋
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Yantai Dongxing magnetic material Co.,Ltd.
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Yantai Shougang Magnetic Materials Inc
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    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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    • B22F2003/248—Thermal after-treatment

Abstract

本发明公开了一种梯度型烧结钕铁硼磁体及其制备方法，其特点是磁体的边部到芯部的稀土总量呈梯度分布，逐渐增加，增加值范围为0.5%‑5%重量百分比；所述磁体各元素重量百分比为：R为32%～35%，R包含Pr和Nd两种元素，B为0.8%～1.2%，Al为0.1%～1%，Co为0.2%～3%，Cu为0.1%～0.3%，Ga为0.1%～0.7%，余量为铁，成分中不含重稀土元素或重稀土元素重量百分比低于0.2%；通过调整元素配比，使用平均粒径2.0～5.0μm的磁粉制备烧结钕铁硼磁体，控制制备条件，控制磁体的尺寸为a×b×c，a范围为10～100mm，b范围为10～60mm，c范围为10～40mm，磁体边部到芯部的稀土总量呈梯度分布逐渐增加，矫顽力逐渐增加。

Description

一种梯度型烧结钕铁硼磁体及其制备方法
技术领域：
本发明涉及钕铁硼磁体技术领域，具体地讲是一种梯度型烧结钕铁硼磁体及其制备方法，通过调整磁体中添加元素的配比，同时控制磁体制备过程中各项工艺参数实现的。
背景技术：
钕铁硼磁体因其优异的磁性能，现已广泛应用在计算机、通讯技术、电子、电声、汽车工业、自动化技术、风力发电等领域。钕铁硼磁体是当代最强永磁体，Nd2Fe14B的各向异性场，即矫顽力的理论极限为80Koe，然而烧结钕铁硼的实际矫顽力仅能达到理论值的30%，因此提高烧结钕铁硼的矫顽力大有潜力。
目前，已经有报道通过晶界扩散技术来提高烧结钕铁硼的矫顽力，同时避免了磁体剩磁和磁能积的大幅下降；同时可以降低磁体中镝和铽的含量，降低原材料成本。但该方法存在以下缺点：这些扩散的磁体厚度不能太厚，超过10mm后芯部的矫顽力基本不增长，对于大尺寸产品性能达不到使用要求。
发明内容：
本发明的目的是克服现有技术的不足，而提供一种梯度型烧结钕铁硼磁体。
本发明的另一目的是提供一种梯度型烧结钕铁硼磁体的制备方法。
本发明主要解决现有的烧结钕铁硼的实际矫顽力低及晶界扩散技术提高矫顽力对于磁体厚度和尺寸受限等问题。
本发明的技术方案是：一种梯度型烧结钕铁硼磁体，其特殊之处在于，所述的磁体的边部到芯部的稀土总量逐渐增加，呈梯度分布，其增加值为0.5%-5%重量百分比；所述的磁体的元素重量百分比为：R为32%～35%，R包含Pr和Nd两种元素，B为0.8%～1.2%，Al为0.1%～1%，Co为0.2%～3%，Cu为0.1%～0.3%，Ga为0.1%～0.7%，余量为铁；成分中不含重稀土元素或重稀土元素重量百分比低于0.2%；所述磁体的尺寸为a×b×c，a为非取向方向，范围为10～100mm，b为高度方向，范围为10～60mm，c为取向方向，范围为10～40mm。
进一步的，所述的磁体由平均粒径2.0～5.0μm的磁粉制成。
本发明的梯度型烧结钕铁硼磁体的制备方法，其特殊之处在于，包括如下工艺步骤：
a按照配比配料，用速凝薄带工艺制备合金片，合金片的厚度为0.2～0.6mm；
b将所得薄片进行氢爆处理，吸氢时间为1-5小时，在500-600℃进行脱氢，得到合金粉末；
c在氢处理后的合金片中加入质量百分数为0.05～0.3%的润滑剂，随后将合金片研磨至D50=2.0～5.0μm；
d在制备的粉体中加入质量百分数为0.05～0.3%的润滑剂，并混合均匀；
e选择不同尺寸的模具在磁场取向条件下进行压制成型，取向磁场为2.0T，然后通过等静压方式进一步使磁体密实，等静压压力为200Mpa；
f将等静压后的生坯在真空烧结炉中进行烧结，烧结温度为880℃～1050℃，烧结保温时间为3～15小时，保温过程中烧结炉真空度为5×10-2Pa以下；待冷却后在850℃进行一级回火处理，保温时间为3小时；最后在480～720℃进行二级回火，保温时间为1～5小时。
本发明所述的一种梯度型烧结钕铁硼磁体及其制备方法，与已有技术相比具有突出的实质性特点和显著进步，1、本发明的梯度钕铁硼磁体的主要特点是磁体的边部到芯部的稀土总量呈梯度分布，逐渐增加，增加值为0.5%-5%重量百分比，是一种适合作为晶界扩散基体的梯度钕铁硼的方法；2、在磁体制备过程中，不添加任何重稀土元素，而是通过优化磁体显微结构的方式，通过控制配料成分、粉体粒度、热处理工艺等因素制备高性能梯度钕铁硼磁体，有效降低了生产成本，避免了重稀土元素的消耗，节约了资源。
附图说明：
图1是实施例3的1#位置放大200倍的扫描电镜图像；
图2是实施例3的3#位置放大200倍的扫描电镜图像；
图3是实施例3的1#位置放大1000倍的扫描电镜图像；
图4是实施例3的3#位置放大1000倍的扫描电镜图像；
图5是进行性能测试的圆柱取样示意图。
具体实施方式：
为了更好地理解与实施，下面结合实施例详细说明本发明。所举实施例仅用于解释本发明，并非用于限制本发明的范围。
实施例1、2、3、4、5、6的梯度型烧结钕铁硼磁体的制备方法如下：
a按照元素重量百分比为：R为32%～35%，R包含Pr和Nd两种元素，B为0.8%～1.2%，Al为0.1%～1%，Co为0.2%～3%，Cu为0.1%～0.3%，Ga为0.1%～0.7%，余量为铁；成分中不含重稀土元素或重稀土元素重量百分比低于0.2 %，进行配比配料；用速凝薄带工艺制备合金片，合金片的厚度为0.2～0.6mm；
b将所得薄片进行氢爆处理，吸氢时间为1-5小时，在500-600℃进行脱氢，得到合金粉末；
c在氢处理后的合金片中加入质量百分数为0.05～0.3%的常规润滑剂；随后使用气流磨将合金片研磨至D50=2.0～5.0μm；
d在气流磨制备的粉体中加入质量百分数为0.05～0.3%的常规润滑剂，，并用混料机混合均匀；
e随后选择尺寸不同的模具在磁场取向条件下进行压制成型，取向磁场为2.0T，然后通过等静压方式进一步使磁体密实，等静压压力为200Mpa；
f将等静压后的生坯在真空烧结炉中进行烧结，烧结温度为880℃～1050℃，烧结保温时间为3～15小时，保温过程中烧结炉真空度为5×10-2Pa以下；待冷却后在850℃进行一级回火处理，保温时间为3小时；最后在480～720℃进行二级回火，保温时间为1～5小时；保温过程中烧结炉真空度为5×10-2Pa以下；制得梯度型烧结钕铁硼磁体，磁体的边部到芯部的稀土总量逐渐增加，呈梯度分布，其增加值为0.5%-5%重量百分比。
实施例1、2、3、4、5、6的元素配比及工艺条件见表1；磁体成份及性能对比见表2。
表1：
表2
步骤a中各实施例按照表1所述配比进行配料；步骤b中实施例5吸氢时间为1小时，脱氢温度为500℃，实施例6吸氢时间为5小时，脱氢温度为600℃，其它实施例吸氢时间均为3小时，脱氢温度均为600℃；步骤c中实施例1的润滑剂比例为0.05%，实施例5的润滑剂比例为0.3%，其余都为0.1%；步骤d中实施例5的润滑剂比例为0.05%，实施例6的润滑剂比例为0.3%，其它实施例的润滑剂比例都为0.15%；步骤f中实施例5的烧结时间为15h，实施例6的烧结时间为3h，其它实施例的烧结时间都为6h。
时效后在毛坯体心沿取向方向加工φ10mm圆柱，如图5所示，将圆柱四等分后分别在1#、2#、3#、4#、5#位置加工直径φ10mm，高度1.5mm的圆柱进行性能测试，之后再做成分分析，得到结果见表2，从边部到芯部ΣRe逐渐增加、Hcj逐渐升高。
图1、图3和图2、图4分别是实施例3的1#和3#位置的扫描电镜图像，图中白色区域是Re，明显看出图2的Re的含量比图1的高，图4的Re的含量比图3的高，磁体的ΣRe从边部到芯部逐渐增加。
以上所述，仅代表本发明的较好实施例，并非对本发明在任何形式上的限制，凡是依据本发明技术实质对本实施例进行的修改，均落入本发明的保护范围。

Claims (3)

1.一种梯度型烧结钕铁硼磁体，其特征在于，所述的磁体的边部到芯部的稀土总量逐渐增加，呈梯度分布，其增加值为0.5%-5%重量百分比；所述的磁体的元素重量百分比为：R为32%～35%，R包含Pr和Nd两种元素，B为0.8%～1.2%，Al为0.1%～1%，Co为0.2%～3%，Cu为0.1%～0.3%，Ga为0.1%～0.7%，余量为铁；成分中不含重稀土元素或重稀土元素重量百分比低于0.2%；所述磁体的尺寸为a×b×c，a为非取向方向，范围为10～100mm，b为高度方向，范围为10～60mm，c为取向方向，范围为10～40mm；制备方法，，包括如下工艺步骤：
a按照配比配料，用速凝薄带工艺制备合金片，合金片的厚度为0.2～0.6mm；
b将所得薄片进行氢爆处理，吸氢时间为1-5小时，在500-600℃进行脱氢，得到合金粉末；
c在氢处理后的合金片中加入质量百分数为0.05～0.3%的润滑剂，随后将合金片研磨至D50=2.0～5.0μm；
d在制备的粉体中加入质量百分数为0.05～0.3%的润滑剂，并混合均匀；
e选择不同尺寸的模具在磁场取向条件下进行压制成型，取向磁场为2.0T，然后通过等静压方式进一步使磁体密实，等静压压力为200Mpa；
f将等静压后的生坯在真空烧结炉中进行烧结，烧结温度为880℃～1050℃，烧结保温时间为3～15小时，保温过程中烧结炉真空度为5×10-2Pa以下；待冷却后在850℃进行一级回火处理，保温时间为3小时；最后在480～720℃进行二级回火，保温时间为1～5小时。
2.根据权利要求1所述的一种梯度型烧结钕铁硼磁体，其特征在于，所述的磁体由平均粒径2.0～5.0μm的磁粉制成。
3.根据权利要求1或2所述的梯度型烧结钕铁硼磁体的制备方法，其特征在于，包括如下工艺步骤：
a按照配比配料，用速凝薄带工艺制备合金片，合金片的厚度为0.2～0.6mm；
b将所得薄片进行氢爆处理，吸氢时间为1-5小时，在500-600℃进行脱氢，得到合金粉末；
c在氢处理后的合金片中加入质量百分数为0.05～0.3%的润滑剂，随后将合金片研磨至D50=2.0～5.0μm；
d在制备的粉体中加入质量百分数为0.05～0.3%的润滑剂，并混合均匀；
e选择不同尺寸的模具在磁场取向条件下进行压制成型，取向磁场为2.0T，然后通过等静压方式进一步使磁体密实，等静压压力为200Mpa；
f将等静压后的生坯在真空烧结炉中进行烧结，烧结温度为880℃～1050℃，烧结保温时间为3～15小时，保温过程中烧结炉真空度为5×10-2Pa以下；待冷却后在850℃进行一级回火处理，保温时间为3小时；最后在480～720℃进行二级回火，保温时间为1～5小时。
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