CN109698067B - 各向异性粘结磁体的制造方法 - Google Patents

各向异性粘结磁体的制造方法 Download PDF

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CN109698067B
CN109698067B CN201910030332.7A CN201910030332A CN109698067B CN 109698067 B CN109698067 B CN 109698067B CN 201910030332 A CN201910030332 A CN 201910030332A CN 109698067 B CN109698067 B CN 109698067B
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CN109698067A (zh
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董永安
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Taiyuan Kaiyuan Intelligent Equipment Co ltd
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Abstract

本发明涉及粘结磁体的制造方法，具体为各向异性粘结磁体的制造方法。解决现有制造方法在加热磁粉的条件下，粘结剂融化后进行磁场取向，生产效率低、模具结构复杂、工艺成本高，进而影响各向异性粘结磁体的广泛使用的问题。各向异性粘结磁体的制造方法，包括如下步骤：1）将各向异性磁粉和热固性粘结剂进行混合；2）将步骤1）的混合物加入模腔，在取向磁场下进行压力成型，然后退磁，得到生坯；3）将步骤2）的生坯放进真空炉内进行热固化；得到各向异性粘结磁体。本发明在常温或冷态下进行磁场成型，避免磁粉颗粒的相互粘连，提高了磁场取向效果，模具结构简单、易操作、效率高，进而成本低。

Description

各向异性粘结磁体的制造方法
技术领域
本发明涉及粘结磁体的制造方法，具体为各向异性粘结磁体的制造方法。
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、磁性能优良等的特点，在硬盘驱动器、光盘驱动器、办公自动化、消费电子、家用电器、汽车工业等得到广泛应用。
模压成型是粘结磁体的主要生产方式：将热固性粘结剂和各向异性磁粉混合，然后加入模腔，模腔升温到热固性粘结剂融化，开始施加取向磁场并施压成型，退磁后脱出模具，最后进行热固处理。由于很难做到磁粉颗粒之间没有粘连，所有磁场取向时必须待粘结剂液化，特别是为了性能和成本上的考量，加入1-3微米的钐铁氮、铁氧体等细磁粉时，互相粘连更是不可避免。在磁场成型时加热，生产效率低、工艺成本高，给各向异性粘结磁体的广泛使用带来了障碍。
发明内容
本发明解决现有制造方法在加热磁粉的条件下，粘结剂融化后进行磁场取向，生产效率低、模具结构复杂、工艺成本高，进而影响各向异性粘结磁体的广泛使用的问题，提供一种各向异性粘结磁体的制造方法，该方法采用常温磁场成型。
本发明是采用如下技术方案实现的：各向异性粘结磁体的制造方法，包括如下步骤：
1）将各向异性磁粉和热固性粘结剂进行混合；
2）将步骤1）的混合物加入模腔，在取向磁场下进行压力成型，然后退磁，得到生坯；
3）将步骤2）的生坯放进真空炉内进行热固化；得到各向异性粘结磁体。
对于需要更高性能、更高强度的磁体，在步骤2）和步骤3）之间增加热压步骤，即步骤2）得到的生坯在热固化之前，先放进真空炉内进行预热；预热完成后的生坯，从真空炉取出后，立即放入和预热温度相同的热压模具内进行热压，热压过程在氮气保护气氛中完成。
在冷态或常温下进行取向磁场下的压力成型，热固性粘结剂为非融化状态，确保每一个磁粉颗粒都是独立的，即使磁粉很细也是各自独立的，即磁粉颗粒间互不粘连，在磁场中极易取向，因此，极大地提高了磁场取向效果，进而提高各向异性粘结磁体的性能。由于磁场成型是在常温下进行，模具结构简单、易操作、效率高，进而成本低。
进一步地，步骤1）所述的热固性粘结剂为热固性粘结剂粉末。现有技术是通过丙酮将热固性粘结剂溶解，然后与各向异性磁粉混合，挥发丙酮，得到颗粒被粘结剂包覆的磁粉，一则磁粉颗粒间（即使在冷态或常温下也）容易粘连，影响磁场取向效果，二则颗粒被粘结剂包覆的磁粉很难填入成型模具特别是热态的成型模具，给加工带来困难。本发明将热固性粘结剂制成粉末与各向异性磁粉相混合，不但进一步避免了磁粉颗粒间的相互粘连，而且方便了加工。
另一种各向异性粘结磁体的制造方法，包括如下步骤：
1）配置聚氨酯粘结剂：将聚氨酯溶解于稀释剂；
2）将配置的聚氨酯粘结剂与各向异性磁粉混合，然后挥发掉稀释剂，得到颗粒被聚氨酯包覆的各向异性磁粉；
3）将颗粒被聚氨酯包覆的各向异性磁粉加入模腔，在取向磁场下进行压力成型，然后退磁，得到生坯；
4）将生坯进行固化处理得到成品。
固化前聚氨酯是粘性较低的液体状态，在磁场下各粉末颗粒能自由转动，不影响磁场取向效果。
本发明在常温或冷态下进行磁场成型，避免磁粉颗粒的相互粘连，提高了磁场取向效果，模具结构简单、易操作、效率高，进而成本低；同时，选择粉末态热固性粘结剂和聚氨酯粘结剂，进一步避免粘结剂对磁粉磁场取向的影响，使得本发明所述方法制得的各向异性粘结磁体的效率大幅度提高，降低了成本。
具体实施方式
实施例一
一种各向异性粘结磁体的制造方法，包括如下步骤：
1）将各向异性磁粉和热固性粘结剂进行混合；
2）将步骤1）的混合物加入模腔，在取向磁场下进行压力成型，然后退磁，得到生坯；
3）将步骤2）的生坯放进真空炉内进行热固化；得到各向异性粘结磁体。
步骤1)中，各向异性磁粉是各向异性钕铁硼磁粉、各向异性钐铁氮磁粉、各向异性铁氧体磁粉、各向异性钐钴磁粉的一种或多种任意比例的混合。热固性粘结剂采用热固性树脂。粘结剂也可替换为尼龙粘结剂。热固性粘结剂为热固性粘结剂粉末，尼龙粘结剂为尼龙粘结剂粉末；粘结剂粉末的粒度3-100微米（如，选用3微米、10微米、30微米、42微米、50微米、70微米、80微米、87微米、90微米、100微米），加入量为各向异性磁粉重量的2-4%（如，选用2%、2.5%、3%、3.7%、4%）。
步骤2）中，取向磁场大于1.2T，成型压力30MPa-100MPa（如，选用30MPa、50MPa、67MPa、75MPa、80MPa、90MPa、100MPa）。
步骤3）中，热固化温度120℃-160℃（如，选用120℃、130℃、145℃、153℃、160℃），1.5小时-3小时（如，选用1.5小时、2小时、2.3小时、3小时）；随后在氮气中自然冷却或强制风冷。
对于需要更高性能、更高强度的磁体，在步骤2）和步骤3）之间增加热压步骤，即步骤2）得到的生坯在热固化之前，先放进真空炉内进行预热；预热完成后的生坯，从真空炉取出后，立即放入和预热温度相同的热压模具内进行热压，热压过程在氮气保护气氛中完成。其中，预热温度90℃-200℃（如，选用90℃、100℃、135℃、150℃、177℃、190℃、200℃），10 -60分钟（如，选用10分钟、17分钟、25分钟、33分钟、46分钟、50分钟、60分钟），真空度1-200Pa（如，选用1、5、10、50、87、100、150、188、200）；热压压力300MPa-700MPa（如，选用300MPa、330MPa、450MPa、500MPa、620MPa、700MPa）。
如果步骤1）采用尼龙粘结剂，热压步骤后的生坯即为成品。
在步骤1）之前对各向异性磁粉进行如下处理：将偶联剂、表面活性剂、润滑剂用三者重量之和5-20倍的无水乙醇或丙酮进行稀释，得到稀释液，按各向异性磁粉重量的0.3-1.5%将稀释液加入各向异性磁粉，并混合均匀；偶联剂、表面活性剂、润滑剂的用量均是各向异性磁粉重量的1%-4.5%；表面活性剂选择吐温-80、壬基酚聚氧乙烯醚、二缩三乙二醇的其中一种；偶联剂选择硅烷类偶联剂（KH-570）、钛酸酯类、铝酸酯类、磷酸酯、锆酸酯、锡酸酯的一种；润滑剂选择硬脂酸乙酯。
实例：
1）粉末前处理：将质量百分比80%的各向异性钕铁硼磁粉+20%的各向异性钐铁氮磁粉在混料机混合5分钟，得到各向异性磁粉。将硅烷类偶联剂（KH-570）1.5%、表面活性剂吐温-80，3%；润滑剂硬脂酸乙酯，2%；用三者重量之和10倍的无水乙醇稀释，搅拌均匀，按各向异性磁粉重量的1%加入各向异性磁粉，在混合机混合均匀。
2）将1）前处理后的各向异性磁粉和磁粉重量的2%的环氧树脂粉末进行冷态混合，混合时间10min。
3）将2）得到的混合粉末加入模腔，进行磁场冷压成型和退磁，得到生坯，磁场1.2T，预成型压力50MPa。
4）将3）的生坯放进真空炉内预热，温度90℃，时间50min。
5）预热完成后的生坯，从真空炉取出后，立即放入和预热温度相同（或相近）的热压模具内进行热压，热压过程要求在氮气保护气氛中完成，施加600MPa的压力。
6）转移到真空烘干箱内热固化，固化温度150℃，时间2小时。随后充入氮气，冷却到室温。
得到密度6.25g/cm3，磁能积（BH)Max 24.5MGOe，矫顽力 14KOe的各向异性粘结磁体。
实施例二：
一种各向异性粘结磁体的制造方法，包括如下步骤：
1）配置聚氨酯粘结剂：将聚氨酯溶解于稀释剂；
2）将配置的聚氨酯粘结剂与各向异性磁粉混合，然后挥发掉稀释剂，得到颗粒被聚氨酯包覆的各向异性磁粉；
3）将颗粒被聚氨酯包覆的各向异性磁粉加入模腔，在取向磁场下进行压力成型，然后退磁，得到生坯；
4）将生坯进行固化处理得到成品。
步骤1）中，聚氨酯与稀释剂的重量比为1：1.5-4.0；同时配置的聚氨酯粘结剂中还有固化剂，固化剂的用量为聚氨酯重量的7-9%，如，固化剂选用缩二脲多异氰酸酯，稀释剂选择无水乙醇。
步骤2）中，配置的聚氨酯粘结剂的用量为各向异性磁粉重量的1.5-2.5%；各向异性磁粉是各向异性钕铁硼磁粉、各向异性钐铁氮磁粉、各向异性铁氧体磁粉、各向异性钐钴磁粉的一种或多种任意比例的混合。
步骤3）中，成型压力120-700MPa，取向磁场1.5T－2.0 T，取向时间10-20s。
步骤4）中，在温度60-100℃的烘箱内固化30-60分钟。
在步骤2）中，各向异性磁粉在与配置的聚氨酯粘结剂混合之前对各向异性磁粉进行如下处理：将偶联剂、表面活性剂、润滑剂用三者重量之和5-20倍的无水乙醇或丙酮进行稀释，得到稀释液，按各向异性磁粉重量的0.3-1.5%将稀释液加入各向异性磁粉，并混合均匀；偶联剂、表面活性剂、润滑剂的用量均是各向异性磁粉重量的1%-4.5%；表面活性剂选择吐温-80、壬基酚聚氧乙烯醚、二缩三乙二醇的其中一种；偶联剂选择硅烷类偶联剂（KH-570）、钛酸酯类、铝酸酯类、磷酸酯、锆酸酯、锡酸酯的一种；润滑剂选择硬脂酸乙酯。
实例：
1）粉末前处理：将质量百分比80%的各向异性钕铁硼磁粉+20%的各向异性钐铁氮磁粉在混料机混合5分钟，得到各向异性磁粉。将偶联剂磷酸酯2%、表面活性壬基酚聚氧乙烯醚，4%；润滑剂硬脂酸乙酯，2%；用三者重量之和15倍的丙酮稀释，搅拌均匀，按各向异性磁粉重量的1.5%加入各向异性磁粉，在混合机混合均匀。
2）配置聚氨酯粘结剂。聚氨酯+固化剂+稀释剂。聚氨酯：无水乙醇稀释剂=1：4，固化剂的用量为聚氨酯重量的8%，搅拌均匀。
3）将2）配置的聚氨酯粘结剂加入1）前处理后的各向异性磁粉，配置的聚氨酯粘结剂的用量为各向异性磁粉重量的2%，进行混合，随后抽真空挥发掉稀释剂。
4）将3）得到的粉末加入模腔，进行磁场压力成型和退磁。取向磁场1.5T，取向时间12s，600MPa。
5）在烘箱内80℃固化处理。
得到密度6.15g/cm3，磁能积（BH)Max 22.5MGOe，出矫顽力15KOe的各向异性粘结磁体。

Claims (7)

1.一种各向异性粘结磁体的制造方法，其特征在于，包括如下步骤：
1）将各向异性磁粉和粉末状的热固性粘结剂进行混合；
2）将步骤1）的混合物加入模腔，在常温下，在取向磁场下进行压力成型，然后退磁，得到生坯；
3）将步骤2）的生坯放进真空炉内进行热固化；得到各向异性粘结磁体。
2.根据权利要求1所述的各向异性粘结磁体的制造方法，其特征在于，步骤1)中，各向异性磁粉是各向异性钕铁硼磁粉、各向异性钐铁氮磁粉、各向异性铁氧体磁粉、各向异性钐钴磁粉的一种或多种任意比例的混合。
3.根据权利要求2所述的各向异性粘结磁体的制造方法，其特征在于，粘结剂粉末的粒度5-100微米；加入量为各向异性磁粉重量的2-4%。
4.根据权利要求1或2或3所述的各向异性粘结磁体的制造方法，其特征在于，在步骤2）和步骤3）之间增加热压步骤，即步骤2）得到的生坯在热固化之前，先放进真空炉内进行预热；预热完成后的生坯，从真空炉取出后，立即放入和预热温度相同的热压模具内进行热压，热压过程在氮气保护气氛中完成。
5.根据权利要求4所述的各向异性粘结磁体的制造方法，其特征在于，步骤1）采用尼龙粘结剂，热压步骤后的生坯即为成品。
6.根据权利要求4所述的各向异性粘结磁体的制造方法，其特征在于，在步骤1）之前对各向异性磁粉进行如下处理：将偶联剂、表面活性剂、润滑剂用三者重量之和5-20倍的无水乙醇或丙酮进行稀释，得到稀释液，按各向异性磁粉重量的0.3-1.5%将稀释液加入各向异性磁粉，并混合均匀。
7.根据权利要求4所述的各向异性粘结磁体的制造方法，其特征在于，
步骤2）中，取向磁场大于1.2T，成型压力30MPa-100MPa；
热压步骤中，预热温度90℃-200℃，时间10-60分钟，真空度1-200Pa；热压压力300MPa-700MPa；
步骤3）中，热固化温度120℃-160℃，时间 1.5小时-3小时。
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