CN110622261B - L10-FeNi磁粉及粘结磁铁 - Google Patents

L10-FeNi磁粉及粘结磁铁 Download PDF

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CN110622261B
CN110622261B CN201880031865.0A CN201880031865A CN110622261B CN 110622261 B CN110622261 B CN 110622261B CN 201880031865 A CN201880031865 A CN 201880031865A CN 110622261 B CN110622261 B CN 110622261B
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magnetic powder
feni
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藏裕彰
渡部英治
金甫根
小山内健太
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Denso Corp
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Abstract

L10‑FeNi磁粉(11)的平均粒径为50nm～1μm，通过以下的式(1)定义的球状度P的平均值为0.9以上，式(1)P＝Ls/Lr。在上述式(1)中，Lr为显微镜的图像中的上述L10‑FeNi磁粉的周长。在上述式(1)中，Ls为具有与算出上述Lr的上述L10‑FeNi磁粉的上述图像的面积相同面积的正圆的周长。

Description

L10-FeNi磁粉及粘结磁铁
关联申请的相互参照
本国际申请基于2017年5月17日在日本专利局申请的日本专利申请第2017-098205号而主张优先权，通过参照将日本专利申请第2017-098205号的全部内容援引于本国际申请中。
技术领域
本公开涉及L10-FeNi磁粉及粘结磁铁。
背景技术
以往，已知有粘结磁铁。粘结磁铁具备母材和分散于该母材中的磁粉。粘结磁铁被公开于专利文献1中。粘结磁铁可以通过注射成型等方法来制造。
现有技术文献
专利文献
专利文献1：日本特开平6-132107号公报
发明内容
发明者进行了详细的研究，结果发现以下的课题。在通过注射成型来制造粘结磁铁的情况下，需要确保原料的流动性。另外，需要提高磁粉的取向度。若提高粘结磁铁中的磁粉的填充率，则原料的流动性容易下降。因此，在以往的粘结磁铁中提高磁粉的填充率是困难的。若磁粉的填充率低，则粘结磁铁的磁铁性能下降。另外，若提高粘结磁铁中的磁粉的填充率，则磁粉的取向度也容易下降。
本公开的一方面优选提供能够提高粘结磁铁的磁铁性能的L10-FeNi磁粉及粘结磁铁。
本公开的一方面为一种L10-FeNi磁粉，其平均粒径为50nm～1μm，通过以下的式(1)定义的球状度P的平均值为0.9以上。
式(1) P＝Ls/Lr
在上述式(1)中，Lr为显微镜的图像中的上述L10-FeNi磁粉的周长。在上述式(1)中，Ls为具有与算出上述Lr的上述L10-FeNi磁粉的上述图像的面积相同面积的正圆的周长。
若使用作为本公开的一方面的L10-FeNi磁粉，则能够使粘结磁铁的磁铁性能提高。
本公开的另一方面为一种粘结磁铁，其具备母材和分散于上述母材中的磁粉。上述磁粉包含作为本公开的一方面的L10-FeNi磁粉和平均粒径为1～500μm的大径磁粉。上述磁粉中的5质量％以上为上述L10-FeNi磁粉。作为本公开的另一方面的粘结磁铁的磁铁性能高。
需要说明的是，权利要求书中记载的括弧内的符号为表示与作为一个方案在下文叙述的实施方式中记载的具体手段的对应关系的符号，并不限定本公开的技术范围。
附图说明
图1是表示Lr及Ls的说明图。
图2是表示粘结磁铁的构成的说明图。
具体实施方式
参照附图对本公开的例示的实施方式进行说明。
1.L10-FeNi磁粉的构成
L10-FeNi是指具有L10结构的FeNi。本公开的L10-FeNi磁粉为由L10-FeNi形成的磁粉。
L10-FeNi磁粉中的球状度P的平均值(以下记为平均值Pavg)为0.9以上。球状度P为通过以下的式(1)定义的值。
式(1) P＝Ls/Lr
如图1中所示的那样，上述式(1)中的Lr为显微镜图像中的L10-FeNi磁粉1的周长。在上述式(1)中，Ls为具有与算出Lr的L10-FeNi磁粉1的显微镜图像中的面积S相同的面积S的正圆3的周长。
平均值Pavg可以如以下那样算出。首先，取得显现L10-FeNi磁粉的SEM或TEM的图像(以下记为显微镜图像)。对于显微镜图像中的每个L10-FeNi磁粉，基于上述式(1)算出球状度P。接着，算出显微镜图像中的100个L10-FeNi磁粉的球状度P的平均值Pavg。
本公开的L10-FeNi磁粉的平均粒径Davg为50nm～1μm。平均粒径Davg的测定方法如下所述。首先，取得显现L10-FeNi磁粉的显微镜图像。对于每个L10-FeNi磁粉，算出以下的式(2)所表示的粒径D。
式(2) D＝Ls/π
在上述式(2)中，Ls为具有与应该算出粒径D的L10-FeNi磁粉的显微镜图像的面积相同面积的正圆的周长。将显微镜图像中的100个L10-FeNi磁粉的粒径D的平均值设定为L10-FeNi磁粉的平均粒径Davg。
本公开的L10-FeNi磁粉例如可以作为粘结磁铁中包含的磁粉来使用。本公开的L10-FeNi磁粉的剩余磁通密度大。另外，在将本公开的L10-FeNi磁粉与后述的大径磁粉一起作为粘结磁铁中包含的磁粉来使用的情况下，粘结磁铁的原料的流动性不易下降。因此，能够提高粘结磁铁中的磁粉的填充率。其结果是，在将本公开的L10-FeNi磁粉与大径磁粉一起作为粘结磁铁中包含的磁粉来使用的情况下，能够增大粘结磁铁的剩余磁通密度。需要说明的是，所谓磁粉的填充率是磁粉的质量相对于粘结磁铁的总质量的比率。
另外，在将本公开的L10-FeNi磁粉与大径磁粉一起作为粘结磁铁中包含的磁粉来使用的情况下，能够提高粘结磁铁中的磁粉的取向度。
本公开的L10-FeNi磁粉的平均粒径Davg优选为400nm～1μm。在本公开的L10-FeNi磁粉的平均粒径Davg为400nm～1μm的情况下，粘结磁铁的剩余磁通密度进一步变大，粘结磁铁中的磁粉的取向度进一步变高。
L10-FeNi磁粉例如可以通过在对作为原料的FeNi粒子进行激光照射法、热等离子体法及气体雾化法中的任一种以上后进行氮化脱氮处理的方法等来制造。
2.粘结磁铁
如图2中所示的那样，本公开的粘结磁铁5具备母材7和分散于母材7中的磁粉9。磁粉9包含本公开的L10-FeNi磁粉11和平均粒径为1～500μm的大径磁粉13。磁粉9中的5质量％以上为L10-FeNi磁粉11。
关于粘结磁铁5，不会使粘结磁铁5的原料的流动性大大下降，能够提高磁粉9的填充率。其结果是，能够增大粘结磁铁5的剩余磁通密度。另外，在粘结磁铁5中，即使磁粉9的填充率高，磁粉9的取向度也高。
作为母材7，可列举出例如树脂等。作为树脂，可列举出例如聚酰胺、氯化聚乙烯、ABS等。
大径磁粉13没有特别限定，可以使用适当选择的磁铁粉作为大径磁粉13。作为大径磁粉13，可列举出例如稀土类磁粉等。作为大径磁粉13的材质，可列举出例如SmFeN、NdFeB、SmCo等。大径磁粉13的球状度P的平均值Pavg优选为1.0～0.4的范围。
优选磁粉9中的10质量％以上为L10-FeNi磁粉11。在磁粉9中的10质量％以上为L10-FeNi磁粉11的情况下，能够进一步增大粘结磁铁5的剩余磁通密度。另外，在粘结磁铁5中，能够进一步提高磁粉9的取向度。
粘结磁铁5中的磁粉9的填充率优选为80质量％以上，进一步优选为90质量％以上。在磁粉9的填充率为80质量％以上的情况下，能够进一步增大粘结磁铁5的剩余磁通密度。
3.粘结磁铁的制造方法
本公开的粘结磁铁例如可以如以下那样操作来制造。首先，将本公开的L10-FeNi磁粉与母材以规定的质量比混合，进行真空混炼，制作预混合物。母材例如为树脂。真空混炼中的温度例如为140℃。真空混炼的时间例如为10小时。
接着，例如使用破碎机等，将预混合物破碎成例如1mm以下的大小。接着，将破碎的预混合物与大径磁粉使用例如掺合机等进行混合，真空混炼而制作复合混合物。真空混炼中的温度例如为140℃。真空混炼的时间例如为10小时。
接着，例如通过注射成形等方法，将复合混合物成型为规定的形状。作为规定的形状，可列举出例如圆柱等。接着，一边对成型品施加一定方向的磁场，一边进行热处理，完成粘结磁铁。热处理的温度例如为180℃。热处理的时间例如为4小时。
4.实施例
(4-1)磁粉C1、C2的制造
作为原料，准备FeNi球状粒子A。FeNi球状粒子A为Nisshin Engineering株式会社制的定制品。FeNi球状粒子A为通过公知的热等离子体法而制造的粒子。FeNi球状粒子A中的组成比为Fe：Ni＝50：50。组成比的单位为原子％(at.％)。
对上述的FeNi球状粒子A进行以下的激光照射法。
激光照射法：通过在硅酸钠系增稠剂水溶液中添加1质量％以下的FeNi球状粒子A的纳米粒子，使用超声波均化器使其分散，由此制备了悬浮液。就该悬浮液而言，FeNi球状粒子A的纳米粒子分散于水中。超声波均化器的输出功率为150W。
通过对该悬浮液照射1～4小时的YAG脉冲激光，使FeNi球状粒子A烧结/生长。其结果是，得到粒径为200～500nm的FeNi球状粒子B。YAG脉冲激光的波长为1064nm。YAG脉冲激光的激光强度为75mJ/Pulse。YAG脉冲激光的脉冲宽度为6nsec。YAG脉冲激光的重复频率为10Hz。通过变更YAG脉冲激光的照射时间，得到粒径不同的多种FeNi球状粒子B。
接着，对多种FeNi球状粒子B分别进行以下的氮化脱氮处理，得到多种FeNi球状粒子C。氮化脱氮处理是用于将FeNi球状粒子制成L10结构的处理。
氮化脱氮处理：将FeNi球状粒子B的纳米粒子放入试样皿中。将该试样皿设置于管状炉中。管状炉能够导入氨气及氢气。将管状炉的气氛设定为氨气，在350℃下进行50小时氮化处理。
接着，将管状炉的气氛置换成氢气，在300℃下进行2小时脱氮处理。接着，将管状炉冷却后，将试样皿从管状炉中取出。其结果是，得到由L10结构的FeNi球状粒子形成的磁粉C。
对于多种磁粉C中的磁粉C1、C2，测定Pavg、Davg、Ms及Hc。将其结果示于表1中。需要说明的是，就磁粉C1和C2而言，由于激光照射法中的YAG激光的照射时间不同，因而Pavg、Davg不同。
表1中Ms为通过VSM法测定的磁化。表1中Ms为外部磁场3T时的值。Hc为使将磁粉的比例设定为10质量％的混合物进行磁场取向、使用VSM测定的保持力。
表1
Figure BDA0002272495940000061
(4-2)磁粉D1～3的制造
准备粒径不同的3种FeNi球状粒子A。对3种FeNi球状粒子A分别进行氮化脱氮处理。该氮化脱氮处理与磁粉C的制造中使用的处理同样。其结果是，得到由L10结构的FeNi球状粒子形成的磁粉D1～D3。测定磁粉D1～D3的Pavg、Davg、Ms及Hc。将其结果示于上述表1中。
(4-3)磁粉F1、F2的制造
作为原料，准备粒径不同的2种FeNi球状粒子E。FeNi球状粒子E为NisshinEngineering株式会社制的定制品。FeNi球状粒子E是通过公知的气体雾化法而制造的粒子。FeNi球状粒子E中的组成比为Fe：Ni＝50：50。组成比的单位为at.％。
对2种FeNi球状粒子E分别进行氮化脱氮处理。该氮化脱氮处理与磁粉C的制造中使用的处理同样。其结果是，得到由L10结构的FeNi球状粒子形成的磁粉F1、F2。测定磁粉F1、F2的Pavg、Davg、Ms及Hc。将其结果示于上述表1中。
(4-4)磁粉G的制造
通过将NdFeB烧结磁铁使用气流磨进行粉碎，制造了由NdFeB形成的磁粉G。测定磁粉G的Pavg、Davg、Ms及Hc。将其结果示于上述表1中。
(4-5)大径磁粉L的制造
准备大径磁粉L。大径磁粉L为包含SmFeN的磁粉，为市售品。测定大径磁粉L的Pavg、Davg、Ms及Hc。将其结果示于上述表1中。
(4-6)粘结磁铁M1～M8的制造
如以下那样操作而制造了粘结磁铁M1～M8。将小径磁粉与树脂以规定的质量比混合，在140℃下进行10小时真空混炼，制作了预混合物。小径磁粉为磁粉C1、C2、D1～D3、F1、F2、G中的任一者。粘结磁铁与其所含有的小径磁粉的对应关系如以下的表2中所示的那样。另外，表2中示出粘结磁铁M1～M8中包含的小径磁粉的内容。在粘结磁铁M1～M8各自中，树脂为聚酰胺。
表2
Figure BDA0002272495940000071
接着，使用破碎机，将预混合物破碎成1mm以下的大小。接着，将破碎的预混合物与大径磁粉L使用掺合机混合，在140℃下进行10小时真空混炼而制作了复合混合物。
接着，通过注射成形，将复合混合物成型为直径为3mm、高度为3mm的圆柱状。接着，一边对圆柱的轴方向施加1.0T的磁场，一边在180℃下进行4小时的热处理，完成粘结磁铁M1～M8。
在粘结磁铁M1～M8中的任一者中，小径磁粉、大径磁粉L及树脂的配合比均设定为全部磁粉的填充率成为93质量％的配合比。在粘结磁铁M1～M8各自中，有全部磁粉中的小径磁粉所占的质量比(以下记为小径磁粉比)为10质量％的粘结磁铁、和20质量％的粘结磁铁这2种。
另外，基本上和与粘结磁铁M1～M8同样的制造方法同样，但作为磁粉仅使用大径磁粉L，制造了粘结磁铁M9。在粘结磁铁M9中，磁粉的填充率也设定为93质量％。
(4-7)粘结磁铁M1～M9的评价
对粘结磁铁M1～M9各自测定Ms、Mr。另外，算出Mr/Ms。将它们示于上述表2中。Mr为使用VSM测定的剩余磁化。将施加3T的外部磁场后将外部磁场设定为0时的磁化的值作为Mr。就粘结磁铁M1～M4而言，Ms、Mr、Mr/Ms的值特别大。
<其他实施方式>
以上，对本公开的实施方式进行了说明，但本公开并不限定于上述的实施方式，可以进行各种变形而实施。
(1)小径磁粉的合成方法也可以是除上述方法以外的方法。
(2)也可以通过多个构成要素来实现上述实施方式中的1个构成要素所具有的多个功能，或者通过多个构成要素来实现1个构成要素所具有的1个功能。另外，还可以通过1个构成要素来实现多个构成要素所具有的多个功能，或者通过1个构成要素来实现通过多个构成要素而实现的1个功能。另外，也可以将上述实施方式的构成的一部分省略。另外，也可以将上述实施方式的构成中的至少一部分相对于其他上述实施方式的构成进行附加或置换。需要说明的是，由权利要求书中记载的文字所规定的技术思想中包含的所有方案为本公开的实施方式。
(3)除了上述的L10-FeNi磁粉、粘结磁铁以外，还可以通过以该L10-FeNi磁粉或粘结磁铁作为构成要素的系统、L10-FeNi磁粉的制造方法、粘结磁铁的制造方法等各种方式来实现本公开。

Claims (4)

1.一种L10-FeNi磁粉(11)，其平均粒径为400nm～1μm，通过以下的式(1)定义的球状度P的平均值为0.9以上，
式(1)P＝Ls/Lr
在所述式(1)中，Lr为显微镜的图像中的所述L10-FeNi磁粉的周长；在所述式(1)中，Ls为具有与算出所述Lr的所述L10-FeNi磁粉的所述图像中的面积相同面积的正圆的周长。
2.一种粘结磁铁，其具备：
母材(7)、和
分散于所述母材中的磁粉(9)，
所述磁粉包含平均粒径为50nm～1μm、且通过以下的式(1)定义的球状度P的平均值为0.9以上的L10-FeNi磁粉(11)、和平均粒径为1～500μm的大径磁粉(13)，
所述磁粉中的5质量％以上为所述L10-FeNi磁粉，
式(1)P＝Ls/Lr
在所述式(1)中，Lr为显微镜的图像中的所述L10-FeNi磁粉的周长；在所述式(1)中，Ls为具有与算出所述Lr的所述L10-FeNi磁粉的所述图像中的面积相同面积的正圆的周长。
3.根据权利要求2所述的粘结磁铁，其中，
所述磁粉的填充率为80质量％以上。
4.根据权利要求2或3所述的粘结磁铁，其中，
所述磁粉中的10质量％以上为所述L10-FeNi磁粉。
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