CN1221513A - 低损失及易饱和的粘结磁铁 - Google Patents

低损失及易饱和的粘结磁铁 Download PDF

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CN1221513A
CN1221513A CN97195308A CN97195308A CN1221513A CN 1221513 A CN1221513 A CN 1221513A CN 97195308 A CN97195308 A CN 97195308A CN 97195308 A CN97195308 A CN 97195308A CN 1221513 A CN1221513 A CN 1221513A
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V·潘查纳坦
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Abstract

本发明提供了一种粘结的各向同性磁铁,它含有包含如下成分的组合物:约5～约25%的稀土金属,约0.5～约4.5%的硼,约0.3～约3.0%的铌,其余主要为铁。这种磁铁显示出低的矫顽力及低的时效损失。

Description

低损失及易饱和的粘结磁铁
背景技术
对于由稀土含量低组合物制成的粘结磁铁有着很大的需求。它们可用于办公自动化、计算机辅助设备及消费者的电子方面的用途。制造这类磁铁的工艺可用熔融-旋压法进行，该法用熔体产生了具有合乎要求的微观组织的粉末。
磁铁在特定的温度下时效后承受了不可逆的损失。这种磁铁损失随时间的延长及温度的升高而增大。过去通常认为：室温下的磁铁初始的矫顽力决定该磁铁的损失行为。一般认为，矫顽力越低则这种损失越高，反之亦然。因而磁铁应有高的矫顽力以减少这类损失；但是这又导致在饱和方面产生困难。已在探索将产生与易饱和行为明显矛盾的性能，低矫顽力和低时效损失的磁铁的精确合金成份上已化费了大量劳动。这类磁铁将在难以饱和的多极磁铁的场合找到用途。
发明简述
本发明提供含低稀土含量组合物的粘结磁铁，它们具有易饱和的行为，低的矫顽力(＜10kOe，更好是＜8kOe)及低的时效损失。本发明通过添加铌来克服与低矫顽力相关的高时效损失，铌是能降低时效损失的。在退火、与环氧树脂混合后及固化后产生的这类粘结磁铁，在于80℃下加热2000小时后的时效损失小于4％，而在100℃下加热2000小时后的时效损失小于6％。
这类磁铁用成份如下的合金制成(％重量)：约5％～约25％的总稀土金属(“TRE”)，该成份中至少95％是钕，而其余主要是镨，约0.5％～约4.5％的硼，其中所述稀土金属和硼的总量为约9％～约26％，约0.5％～3.0％的铌，及其余主要为铁。较佳范围是TRE约10～约20％,B约0.8-4.0％,Nb约1％～约2.5％，余量主要是Fe。稀土金属和硼总量的较佳范围是约12％～约22％。更大量的TRE是不适宜的，因为Hci将很高，而且将难于饱和。更低量的TRE也不好，因为Hci值将很低因而将失去工业意义。正确的B及TRE值有助于得到正确的、硬磁2-14-1相及α-Fe和/或Fe3B软相的微观组织。钴降低Br和Hci值；但在希望Br的低温矫顽力的应用场合，推荐用钴。该合金成份可含最多为16％的钴。
其它的金属也可以最多为2％(重量)的小量，单独地或混合地存在。这些金属包括W、Cr、Ni、Al、Cu、Mg、Mn、Ga、V、Mo、Ti、Ta、Sn、Zr、C和Ca。Si和O和N一样也可以小量存在。
一般来说，这类优选成份的永磁体是这样形成的：开始通过在干燥的，基本上无氧的Ar气、惰性或真空的气氛下进行感应加热，形成熔融的均匀组合物而制成合金锭。最好使此熔融组合物在惰性气氛下或真空中快速凝固，产生一种非晶态的材料或细晶的材料，其中，以其最大尺寸计，晶粒尺寸不大于约500nm，最好是小于约400nm。最好是，这种快速凝固的材料的晶粒尺寸小于约20nm。这类材料，比如，可用常规的熔融-旋压作业生产。这种优选成份的合金以22m/秒的速度被熔融-旋压，该步骤形成了一种带材，在其整个厚度上是非晶态或是微晶态的组织。
用辊式破碎机将此带材粉碎成细粉，其平均颗粒最好为200μm。
最好将所得的粉末于700℃，在Ar中退火约4分钟。退火后，晶粒尺寸在约20～约500nm的范围内，更好是在20-100nm之间。
将此退火后的粉末与粘结剂混合，此粘结剂随后可经硬化而形成自支撑的未磁化的，但是可磁化的原料压块。该粘结剂可以是可硬化的树脂类物质，如用于压力成形的2％(重量)的环氧树脂。由于此粉末是各向同性的，所以在粘结过程中无需校正磁场，这使作业周期的时间得以加快。可沿任何方向使成品磁铁磁化，这使得设计具较大的灵活性。
最好以170℃的温度，30分钟的时间使此原料压块固化。使环氧树脂固化，然后将这样形成的粘结磁铁用于进一步的用途。该原料压块可压制成形。
还可用压制成形之外的其它工艺制造粘结磁铁。它们包括喷塑、压延、挤压等。虽然本发明涉及了用压制成形法制成的粘结磁铁，但可以预料用其它方法制成的粘结磁铁有类似的或更好的结果，在这类磁铁含较大量粘结剂时尤为如此。
为测试所得磁铁的损失性能，最好在80℃的温度下使其时效2小时。
详细描述及实施例：实施例1
以22m/秒的速度熔融旋压具有下列成份的合金。该合金由稀土、硼及余量的铁构成。至少总稀土组份中的95％是钕，而其余的主要是镨。将带材粉碎成平均颗粒尺寸为200μm的粉末。于700℃将此粉末退火4分钟。将此粉末与环氧树脂(2％重量)混合，再用压制成形法制成原料压块。将其于170℃固化30分钟。将这样制成的粘结磁铁在80℃时效2小时。测量试样A-G的损失，结果示于下表中。
    TRE％  B％  Hci,kOe 损失，％
A    15    1.5    1.3    ＞10
B    16    1.4    1.4    ＞10
C    17    1.3    1.7    ＞10
D    18    1.2    3.6      8
E    19    1.1    4.0      8
F    18.5  1.2    3.8      8
G    19.5  1.2    4.2      8
实施例2：
将下列成份的合金进行熔融旋压，再以与相同的方式制成粘结磁铁。该合金由稀土、硼和余量的铁组成，任选地含有Co或Nb。稀土组份中至少95％是钕，其余基本上是镨。试样H-N的性能如下。
     TRE％   B％    其它  Br,KG  Hci,kOe
H    18.0    0.99    -     10.1    4.3
I    19.0    1.0     -     9.94    4.3
J    21.3    1.6     -     8.43    4.93
K    21.9    1.9     -     8.06    4.64
L    18.0    1.03   Co2.5  9.93    3.53
M    18.0    .85    Co10.7 9.24    2.99
N    18.0    1.07   Nb1.8  8.68    5.02
可见，加Co使Br和Hci下降。但加Nb使Br下降，使Hci上升。
实施例3
按实施例用试样H和N制成粘结磁铁。使它们在80℃和100℃时时效最高达1000小时。测量损失。
           损失％
       试样H    试样N
80℃     10      3.7
100℃    15      5.2
试样N在80℃和100℃时时效2小时后的损失分别为0.5％和1％试样H分别在80℃和100℃时效后的类似的数值为5％和8％。因而含Nb的磁铁不仅在2小时的短期时效后，而且在高达2000小时的时效后都显示出很低的损失。
实施例4
以不同的磁场使实施例3中的试样H和N的粘接磁铁饱和。下表列出了两磁铁的饱和行为：
                 Bv饱和％
磁场，kOe    试样H    试样N
10            60       67
15            83       90
20            91       96
注意Hci较高的含Nb磁铁比Hci较低但不含Nb的磁铁更易被饱和。
因此，本发明所涉及的是用组成为TRE5～25％、B0.05～4.5％，TRE+B为9-26％,Nb0.5～3.0，余量的Fe，制成的磁铁，它具有较低的损失及较好的饱和行为。
下图描绘了各实施例中用于测量该粘结磁铁的时效损失和饱和程度的方法。时效研究
该磁铁在40kOe时被脉冲磁化。得到退磁曲线。确定与该磁铁的饱和线相对应的起始磁通量值。将其在40kOe时磁化，然后于适宜温度的烘炉内保持一段时间。此后，从炉中取出磁铁，将其冷至室温，绘制退磁曲线。确定磁通量值。其损失以原值的百分比表示。
％损失=(B1-B2)/B1％
Figure A9719530800091
磁性测量
将此磁铁在10kOe-40kOe的变化的磁场中磁化。制取各种磁场时的退磁曲线。超过35kOe时磁性无进一步提高。B3/B1之比为15kOe时的饱和程度，而B2/B1之比为20kOe时的饱和程度等。

Claims (19)

1．一种粘结的各向同性的磁铁，它包含粘结剂及经熔融旋压的结晶颗粒，该颗粒的成份包括(％重量)，约5～25％的稀土金属，约0.5～约4.5％的硼，其中所述稀土金属与所述硼之和为约9～约26％，约0.5～3.0％的铌，其余主要是铁。
2．权利要求1的磁铁，其矫顽力小于10kOe。
3．权利要求1的磁铁，其中该成份含最多达16％的Co。
4．权利要求1的磁铁，其中该成份中含(％重量)约10～约20％的稀土金属，约0.8～约4.0％的硼，约1.0～约2.5％的铌，其余主要是铁。
5．权利要求1的磁铁，其中所述稀土金属主要是钕和/或镨。
6．权利要求1的磁铁，其中所述的各向同性颗粒的平均颗粒尺寸为200μm。
7．形成粘结的各向同性磁铁的方法，它包括如下步骤：
熔炼包含如下成份的组合物(％重量)：约5％～约25％的稀土金属，约0.5％～约4.5％的硼，其中所述稀土金属和所述硼的总和为约0.9％～约26％，约0.5％～约3.0％的铌，其余主要是铁；
将所述组合物熔融旋压，心形成带；
将所述的带磨成粉末；
将所述粉末退火；
将退过火的所述粉末与粘结剂混合而形成压块；
使所述压块固化以形成最终的粘结磁铁。
8．权利要求1的方法，其中以约700℃的温度，约4分钟的时间进行该退火工艺。
9．权利要求7的方法，其中所述的各向同性的颗粒用约2％的环氧树脂粘结剂粘结。
10．权利要求7的方法，其中的与粘结剂混合的所述各向同性颗粒在约170℃的温度下固化约30分钟。
11．一种粘结的各向同性的磁铁，它包含环氧树脂粘结剂和经熔融旋压的结晶颗粒，该颗粒是由包含如下成份(％重量)的组份物形成的：约5％～约25％的稀土金属，约0.5％～约4.5％的硼，其中该稀土金属与所述硼的总和为约9％～约26％，约0.5％～约3.0％的铌，其余主要是铁，所述的熔融旋压的结晶颗粒的微观组织为2-14-1及α-Fe和/或Fe3B软相。
12．权利要求11的磁铁，其中该组合物含(％重量)：约10～约20％的稀土金属，约0.8～约4.0％的硼，约1.0～约2.5％的铌，其余主要是铁。
13．一种粘结的各向同性的磁铁，它包含环氧树脂粘结剂及经熔融旋压的结晶颗粒，该颗粒是由包含成份如下(％重量)的组合物构成的：约5～约25％的稀土金属，约0.5～约4.5％的硼，其中所述稀土金属和所述硼的总和为约9～约26％，约0.5～约3％的铌，其余主要是铁；
所述磁铁在10kOe的磁场中的饱和程度大于60％。
14．权利要求13的磁铁，它显示出在将所述磁铁于80℃的温度下加热2000小时后的时效损失小于4％。
15．权利要求13的磁铁，它显示出在将所述磁铁于100℃的温度下加热2000小时后的时效损失小于6％。
16．权利要求13的磁铁，其中该组合物含(％重量)：约10～约20％的稀土金属，约0.8～约4.0％的硼，约1.0～约2.5％的铌，其余主要是铁。
17．一种形成粘结的铁-稀土金属永磁铁的方法，其包括的步骤为：
提供一定量的晶粒尺寸不大于约500nm的各向同性的铁-稀土金属颗粒，其中所述的各向同性的铁-稀土金属颗粒由含如下成份的组合物构成(％重量)：约5～约25％的稀土金属，所述的稀土金属组份中主要是钕，及约0.5～约4.5％的硼，约0.5～约3.0％的铌，其中所述稀土金属和所述硼之总和为约9～约26％；其余主要是铁；
将所述量的各向同性的铁-稀土金属颗粒与粘结剂混合，从而形成压块；
使所述压块在一定温度下，以足够的时间固化，以形成特征为均匀地存有硬磁性Nb2Fe14B相和软相Fe3B和/或α铁的粘结的，各向同性的铁-稀土金属永磁铁。
18．权利要求17的形成粘结的铁-稀土金属永磁铁的方法，它还含最多为约16％的钴。
19．权利要求17的形成粘结的铁-稀土金属永磁铁的方法，其中所述的稀土的范围为约10～约20％的稀土金属，所述的硼的范围为约0.8～约4.0％的硼，其中所述稀土金属和所述硼的总和的范围为约12～约22％。
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