CN106783128B - 制备低重稀土高矫顽力钕铁硼磁体的方法 - Google Patents

制备低重稀土高矫顽力钕铁硼磁体的方法 Download PDF

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CN106783128B
CN106783128B CN201611191110.6A CN201611191110A CN106783128B CN 106783128 B CN106783128 B CN 106783128B CN 201611191110 A CN201611191110 A CN 201611191110A CN 106783128 B CN106783128 B CN 106783128B
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neodymium iron
iron boron
rare earth
heavy rare
magnetic body
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CN106783128A (zh
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鲁飞
孙良成
刘小鱼
杨占峰
陈蓓新
刘树峰
邢正茂
张刚
李慧
白洋
王峰
李静雅
郑天仓
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Baotou Yun Jie Electric Furnace Factory
Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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Baotou Yun Jie Electric Furnace Factory
Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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Priority to PCT/CN2017/117641 priority patent/WO2018113717A1/zh
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Abstract

本发明公开了一种制备低重稀土高矫顽力钕铁硼磁体的方法，包括：配料、熔炼、速凝铸片；采用物理气相沉积方法，在惰性气氛下将重稀土粒子或者高熔质粒子沉积在钕铁硼薄片上；进行破碎制粉、取向成型、烧结热处理，制备钕铁硼磁体。本发明可使钕铁硼磁体矫顽力显著提高，细化磁体晶粒，大幅降低重稀土元素使用量。

Description

制备低重稀土高矫顽力钕铁硼磁体的方法
技术领域
本发明涉及一种稀土永磁材料制备技术，具体说，涉及一种制备低重稀土高矫顽力钕铁硼磁体的方法。
背景技术
钕铁硼永磁材料是我国稀土行业最为关注的稀土应用产业，随着科学技术的发展和技术的进步对高性能钕铁硼永磁材料的需求日益广泛。众所周知，为了提高钕铁硼的矫顽力和高温使用性，通常采用的方法是加入少量重稀土元素(如Dy、Tb等)或优化工艺细化磁体晶粒。
目前使用的降低重稀土使用量的方法主要包括双合金工艺和晶间扩散重稀土元素工艺。双合金工艺是分别熔炼主合金和包含重稀土元素的辅合金，破碎制粉，将主合金磁粉和辅合金粉按配比混合，取向压制，烧结，该工艺中重稀土元素使用量仍较高。晶间扩散重稀土元素工艺是通过涂抹、喷洒、浸渍和镀膜等方式在钕铁硼表面形成重稀土元素覆盖层，经高温晶间扩散将重稀土元素扩散至磁体内部以达到提高磁体矫顽力，少量使用重稀土的目的。但是该工艺仅限于制作较薄的磁件(厚度一般不超过5mm)，在制备大块磁体时矫顽力提升不明显。
目前通常采用的细化磁体晶粒的方法主要是在磁体成分中加入微量的W、Mo、V、Ti、Ta、Zr、Nb、Co、Cr、Ga等元素抑制磁体晶粒的长大，但此类元素在磁体中会发生偏析等不均匀分布，对晶粒长大的抑制效果有限，加入量过高则会对磁体性能产生严重的影响。
发明内容
本发明所解决的技术问题是提供一种制备低重稀土高矫顽力钕铁硼磁体的方法，可使钕铁硼磁体矫顽力显著提高，细化磁体晶粒，大幅降低重稀土元素使用量。
技术方案如下：
一种制备低重稀土高矫顽力钕铁硼磁体的方法，包括：
配料、熔炼、速凝铸片；
采用物理气相沉积方法，在惰性气氛下将重稀土粒子或者高熔质粒子沉积在钕铁硼薄片上；
进行破碎制粉、取向成型、烧结热处理，制备钕铁硼磁体。
进一步：重稀土粒子采用Dy或者Tb元素的粒子，高熔质粒子采用W、Mo、V、Ti、Ta、Zr、Nb、Co、Cr或者Ga元素的粒子。
进一步：惰性气氛采用真空、充入氩气或充入氦气。
进一步：物理气相沉积的温度为300～500℃，沉积速率为0.01～50μm/min。
进一步，沉积微量重稀土粒子的步骤包括：
选择所需重稀土靶材；
将钕铁硼合金薄片和重稀土靶材置于物理气相沉积装置内；
抽真空至真空度高于2.0×10-2Pa，充入氩气至0.2～1.0Pa；
调节参数，对钕铁硼薄片加热，加热温度300～500℃；
开启物理气相沉积装置，利用物理气相沉积将靶材粒子沉积在钕铁硼薄片上；
停止物理气相沉积，待钕铁硼薄片温度降至室温后取出；
将制得的钕铁硼薄片破碎制粉、取向压制成型、真空烧结、回火热处理，获得最终钕铁硼磁体。
进一步：物理气相沉积采用磁控溅射沉积、离子镀沉积或者蒸发源沉积；粒子沉积速率为0.01～50μm/min。
进一步：重稀土靶材为Dy或Tb中至少一种元素的纯金属、合金或氧化物。
进一步，沉积高熔质粒子的步骤包括：
选择所需高熔质靶材；
将钕铁硼合金薄片和高熔质靶材分别置于物理气相沉积装置内；
抽真空至真空度高于2.0×10-2Pa，充入氩气至0.2～1.0Pa；
调节参数，对钕铁硼薄片加热，加热温度300～500℃；
开启物理气相沉积装置，利用物理气相沉积将靶材粒子沉积在钕铁硼薄片上；
停止物理气相沉积，待钕铁硼薄片温度降至室温后取出；
将制得的钕铁硼薄片破碎制粉、取向压制成型、真空烧结、回火热处理，获得最终钕铁硼磁体。
进一步：高熔质靶材采用W、Mo、V、Ti、Ta、Zr、Nb、Co、Cr或者Ga中至少一种元素的纯金属、合金或氧化物。
进一步：物理气相沉积采用磁控溅射沉积、离子镀沉积或者蒸发源沉积，粒子沉积速率为0.01～50μm/min。
与现有技术相比，本发明技术效果包括：
1、本发明可使重稀土粒子或者高熔质粒子在磁体中均匀分散在晶界处，提高磁体矫顽力，细化磁体晶粒，减少重稀土使用量，剩磁和磁能积优异。采用本发明制备钕铁硼磁体，可使钕铁硼磁体矫顽力显著提高，细化磁体晶粒，大幅降低重稀土元素使用量，降低钕铁硼磁体制造成本，同时可降低磁体中氧含量。
2、经济效益显著。钕铁硼磁体生产企业都在力争用降低Dy/Tb等重稀土元素的使用量，在降低Dy/Tb用量的同时提高性能，使钕铁硼磁体的生产成本降下来。目前，在高性能钕铁硼磁体中，平均重量高于2％，特别是矫顽力大于30Koe的产品，Dy/Tb高达4％以上，按目前Dy/Tb价计算价格高达80元/Kg，影响成本达40-80元/Kg，每公斤钕铁硼Dy/Tb等重稀土元素的使用量一般在20g以上，成本影响大约在每公斤40元，按3万吨钕铁硼毛坯计算，成本影响达12-24亿元。
具体实施方式
下面参考示例实施方式对本发明技术方案作详细说明。然而，示例实施方式能够以多种形式实施，且不应被理解为限于在此阐述的实施方式；相反，提供这些实施方式使得本发明更全面和完整，并将示例实施方式的构思全面地传达给本领域的技术人员。
制备低重稀土高矫顽力钕铁硼磁体的方法，具体步骤如下：
步骤1：配料、熔炼、速凝铸片；
步骤2：采用物理气相沉积方法，在惰性气氛下将靶材粒子(微量重稀土粒子或者高熔质粒子)沉积在钕铁硼薄片上；
物理气相沉积的靶材粒子选用重稀土元素Dy或者Tb粒子，或者高熔质元素W、Mo、V、Ti，Ta、Zr、Nb，Co、Cr、Ga粒子中的一种或者多种粒子。惰性气氛为氩气或氦气或真空。
步骤3：进而进行破碎制粉、烧结制备钕铁硼磁体。
方案1：沉积微量重稀土粒子
步骤11：配料、熔炼、速凝铸片；
步骤12：选择所需重稀土靶材；
步骤13：将钕铁硼合金薄片和重稀土靶材分别置于物理气相沉积装置内；
重稀土靶材为Dy、Tb或Dy-Tb的至少一种纯金属、合金或氧化物。
步骤14：抽真空至真空度高于2.0×10-2Pa，充入氩气至0.2～1.0Pa；
步骤15：调节参数，对钕铁硼薄片加热，加热温度300～500℃；
步骤16：开启物理气相沉积装置，利用物理气相沉积将靶材粒子沉积在钕铁硼薄片上；
物理气相沉积包括磁控溅射沉积、离子镀沉积和蒸发源沉积。粒子沉积速率为0.01～50μm/min。
步骤17：停止物理气相沉积，待钕铁硼薄片温度降至室温后取出；
步骤18：将制得的钕铁硼薄片破碎制粉、取向压制成型、真空烧结、回火热处理，获得最终钕铁硼磁体。
方案2：沉积高熔质粒子
步骤21：配料、熔炼、速凝铸片；
步骤22：选择所需高熔质靶材；
步骤23：将钕铁硼合金薄片和高熔质靶材分别置于物理气相沉积装置内；
高熔质靶材为W、Mo、V、Ti、Ta、Zr、Nb、Co、Cr、Ga等元素的至少一种纯金属、合金或氧化物。
步骤24：抽真空至真空度高于2.0×10-2Pa，充入氩气至0.2～1.0Pa；
步骤25：调节参数，对钕铁硼薄片加热，加热温度300～500℃；
步骤26：开启物理气相沉积装置，利用物理气相沉积将靶材粒子沉积在钕铁硼薄片上；
物理气相沉积包括磁控溅射沉积、离子镀沉积和蒸发源沉积。粒子沉积速率为0.01～50μm/min。
步骤27：停止物理气相沉积，待钕铁硼薄片温度降至室温后取出；
步骤28：将制得的钕铁硼薄片破碎制粉、取向压制成型、真空烧结、回火热处理，获得最终钕铁硼磁体。
实施例1：
一种低重稀土高矫顽力钕铁硼磁体的制备方法，具体包括如下步骤：
(1)配料、熔炼、速凝铸片制备钕铁硼薄片；
(2)将所得钕铁硼薄片进行物理气相沉积：
选择Dy金属靶材，抽真空至2.0×10-2Pa，充入氩气至0.2Pa，采用磁控溅射，调整溅射功率，使Dy粒子沉积速率为0.01μm/min；
(3)将所得的钕铁硼薄片盘磨破碎、球磨制粉、取向成型、烧结、热处理，获得最终磁体。
采用磁性能测量仪测试本实施例制备的磁体磁能积和矫顽力，与传统方法制备的磁体进行对比，结果如表1所示。
表1
实施例2：
一种低重稀土高矫顽力钕铁硼磁体的制备方法，具体包括如下步骤：
(1)配料、熔炼、速凝铸片制备钕铁硼薄片；
(2)将所得钕铁硼薄片进行物理气相沉积：
选择Tb金属靶材，抽真空至5.0×10-3Pa，充入氦气至0.5Pa，将钕铁硼薄片加热到300℃，采用离子镀，调整氩气发射源电流，使Tb粒子沉积速率为50μm/min。
(3)将所得的钕铁硼薄片氢破碎、气流磨、取向成型、烧结、热处理，获得最终磁体。
采用磁性能测量仪测试本实施例制备的磁体磁能积和矫顽力，与传统方法制备的磁体进行对比，结果如表2所示。
表2
实施例3：
一种低重稀土高矫顽力钕铁硼磁体的制备方法，具体包括如下步骤：
(1)配料、熔炼、速凝铸片制备钕铁硼薄片；
(2)将所得钕铁硼薄片进行物理气相沉积：
选择CoZr金属靶材，抽真空至9.0×10-4Pa，将钕铁硼薄片加热到500℃
采用蒸发沉积，调整蒸发舟加热源功率，使CoZr原子气化蒸发，沉积速率为3μm/min。
(3)将所得的钕铁硼薄片氢破碎、气流磨、取向成型、烧结、热处理，获得最终磁体。
采用磁性能测量仪测试本实施例制备的磁体磁能积和矫顽力，与传统方法制备的磁体进行对比，结果如表3所示。
表3
实施例4：
一种低重稀土高矫顽力钕铁硼磁体的制备方法，具体包括如下步骤：
(1)配料、熔炼、速凝铸片制备钕铁硼薄片；
(2)将所得钕铁硼薄片进行物理气相沉积：
选择Dy2O3靶材，Mo靶材，抽真空至3.0×10-2Pa，充入氩气至0.3Pa，将钕铁硼薄片加热到420℃，采用磁控溅射，同时对两种靶材进行溅射，调整溅射功率，使粒子沉积速率为0.2μm/min。
(3)将所得的钕铁硼薄片氢破碎、气流磨、取向成型、烧结、热处理，获得最终磁体。
采用磁性能测量仪测试本实施例制备的磁体磁能积和矫顽力，与传统方法制备的磁体进行对比，结果如表4所示。
表4
本发明所用的术语是说明和示例性、而非限制性的术语。由于本发明能够以多种形式具体实施而不脱离发明的精神或实质，所以应当理解，上述实施例不限于任何前述的细节，而应在随附权利要求所限定的精神和范围内广泛地解释，因此落入权利要求或其等效范围内的全部变化和改型都应为随附权利要求所涵盖。

Claims (1)

1.一种低重稀土高矫顽力钕铁硼磁体的制备方法，包括如下步骤：
(1)配料、熔炼、速凝铸片制备钕铁硼薄片；
(2)将步骤(1)所得的钕铁硼薄片进行物理气相沉积：
选择Tb金属靶材，抽真空至5.0×10-3Pa，充入氦气至0.5Pa，将钕铁硼薄片加热到300℃，采用离子镀，调整氩气发射源电流，使Tb粒子沉积速率为50μm/min；
(3)将步骤(2)所得的钕铁硼薄片氢破碎、气流磨、取向成型、烧结和热处理，获得钕铁硼磁体；其中，钕铁硼磁体的内禀矫顽力为28.45kOe。
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