CN1215493C - 氧化物磁性材料系永磁铁的制造方法 - Google Patents

氧化物磁性材料系永磁铁的制造方法 Download PDF

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CN1215493C
CN1215493C CNB028032799A CN02803279A CN1215493C CN 1215493 C CN1215493 C CN 1215493C CN B028032799 A CNB028032799 A CN B028032799A CN 02803279 A CN02803279 A CN 02803279A CN 1215493 C CN1215493 C CN 1215493C
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moisture
moulding
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mixture
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CN1479928A (zh
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坪仓多惠子
铃木常雄
森宜宽
村濑琢
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TDK Corp
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Abstract

本发明是氧化物磁性材料系永磁铁的制造方法，它包括：在包含氧化物磁性材料的原料粉末中加入粘合剂并混合的粘合剂添加工序；调节包含上述原料粉末与粘合剂的成型用混合物中水分的水分调节工序；将水分调节好的上述成型用混合物加入模具中，施加磁场，使氧化物磁性粉料全部沿容易磁化方向排列同时加压的磁场中干式成型工序；以及在1200～1260℃的温度下对已成型的成型体进行烧制的烧制工序，其特征在于：上述粘合剂添加工序中的粘合剂是分子量为400～600的脂肪酸酯系的蜡，成型用混合物中粘合剂的含量为0.2～1.5wt%，上述水分调节工序的混合物中的水分含量为0.20～0.80wt%，而上述磁场中干式成型工序中加入模具内的成型用混合物内所存在的粒度在500μm以上的聚集体的存在比例为0.01～0.80wt%，由此可以制得能够低成本化且具有优越磁性质的氧化物磁性材料系的永磁铁。

Description

氧化物磁性材料系永磁铁的制造方法
技术领域
本发明涉及氧化物磁性材料系永磁铁的制造方法。特别涉及用于所谓干式成型法成型的氧化物磁性材料系永磁铁的制造方法。
背景技术
Sr铁氧体与Ba铁氧体等磁铁铅矿各向异性的氧化物永磁铁，是在磁场中成型后经烧结制成。磁场中的成型根据所用方法大致分为干式成型法与湿式成型法。湿式成型法由于永磁铁粒料能在分散介质中容易转动，可以使磁性材料获得良好的取向性，从而能取得良好的磁性。但由于在加压成型中必须将分散介质排出到成型空间之外(模具模腔之外)，会降低生产率。此外需用大型模具结构，加大了设备费用。
另一方面，干式成型法是把干燥状态的永磁铁材料粉末充填到成型空间(模腔)内、于磁场中成型的方法，这同湿式成型法相比，虽然磁性材料的取向性差，但有生产率高，设备费用低廉的特别有利的优点。
干式成型法中，充填到模具中永磁材料内含有粘合剂。这种粘合剂所要求的理想特性例如要求对永磁粒料有良好的粘合作用，不妨碍磁性粒料在磁性上沿容易磁化的轴向排列等。作为取向性不良的理由例如有：(1)永磁粒料的磁性受到抑制，也就是永磁粒料与粘合剂的粘合作用太强而妨碍了粒料在磁性上沿容易磁化的轴向排列；(2)成型时的摩擦，即由于粒料相互的接触摩擦，以及由于粒料与模具间产生的摩擦导致通过加压来压实的作用不充分，而降低了成型性。为了改进这种取向性的恶化趋势，已尝试在干式成型法中选择低摩擦的不妨碍磁性的粘合剂添加到永磁材料中。
具体地说，是在由干式成型法成型时，将固体石蜡、硬脂酸、樟脑等用作磁铁材料中所含有的粘合剂。
固体石蜡与硬脂酸虽有优越的粘合作用，但由于粘合作用太强，存在妨碍磁性粒料在磁性上沿容易磁化的轴向排列的倾向。樟脑虽可有效地用作在附加有磁场成型时的粘合剂，但由于它会升华，它与铁氧体粉末的混合比会随时间的经过而变化，因而会产生妨碍成型作业或使已成型的成型体的强度降低等缺点。
为了解决上述问题，作为干式磁场成型用铁氧体磁铁粉末的粘合剂，已提出有采用硬脂酸金属盐(金属M为Ca、Ba、Sr、Pb)的(特公昭47-21197号公报)，以及采用硬脂酸镁(特公昭62-176102号公报)的，等等。但是这种硬脂酸金属盐的粘合剂难以均匀涂布到各粒子的表面上。故不得不增多粘合剂的添加量。结果，烧结后磁铁中的碳量增多，导致磁性变差以及使烧成后的烧制体中易产生裂纹。
此外，作为粘合剂的混合方法，例如有通过加热或减压来涂布气相粘合剂的方法，但这种方法存在设备大、工序多、未能低成本化等问题。
本发明正是根据这种实际状况而提出的，目的在于在利用干式成型制造氧化物磁性材料系永磁铁时，能获得低成本、改进了取向性与提高了烧结体密度且具有优越磁性质的氧化物磁性材料系的永磁铁。
发明内容
为了解决上述问题，本发明提供氧化物磁性材料系永磁铁的制造方法，它包括：在包含氧化物磁性材料的原料粉末中加入粘合剂并混合的粘合剂添加工序；调节包含上述原料粉末与粘合剂的成型用混合物中水分的水分调节工序；将水分调节好的上述成型用混合物加入模具中，施加磁场，使氧化物磁性粉料全部沿容易磁化方向排列同时加压的磁场中干式成型工序；以及在1200～1260℃的温度下对已成型的成型体进行烧制的烧制工序，其特征在于：上述粘合剂添加工序中的粘合剂是分子量为400～600的脂肪酸酯系的蜡，成型用混合物中粘合剂的含量为0.2～1.5wt％，上述水分调节工序的混合物中的水分含量为0.20～0.80wt％，而上述磁场中干式成型工序中加入模具内的成型用混合物内所存在的粒度在500μm以上的聚集体的存在比例为0.01～0.80wt％。
作为本发明的最佳形式，上述脂肪酸酯系蜡是植物蜡。
作为本发明的最佳形式，上述氧化物磁性材料的原料粉末是在配合上氧化物原料并混合后，经焙烧后再粉碎成的原料粉末。
作为本发明的最佳形式，上述水分调节工序是于恒温槽中或置于室温下作湿度调节而调节混合物中的水分。
作为本发明的最佳实施形式，在上述水分调节工序之后再添加粉碎成型用混合物中聚集体的破碎工序。
作为本发明的最佳实施形式，使上述破碎工序结束时混合物中的水分含量为0.20～0.80wt％。
具体实施方式
下面详述本发明的氧化物永磁铁的制造方法。
本发明的氧化物磁性材料系永磁铁的制造方法的主要工序包括：将粘合剂加到包含氧化物磁性材料的原料粉末中再混合的粘合剂添加工序；给上述包含原料粉末与粘合剂的成型用混合物中加水，调节混合物的水分的水分调节工序；将已调节过水分的上述成型用混合物加入模具中，在施加磁场作用下使氧化物磁性材料粉末粒子全排列到容易磁化方向，然后加压的磁场中干式成型工序；以及将已成型的成型体进行烧制的烧制工序。
上述粘合剂添加工序之前应准备的氧化物磁性材料的原料粉末通常按以下步骤制备。
[原料粉末的制备]
在钡铁氧体的情形中，例如一般以氧化铁(Fe2O3)和碳酸钡(BaCO3)的粉末为主要原料；而对于锶铁氧体，一般是以氧化铁(Fe2O3)和碳酸锶(SrCO3)的粉末为主要原料，将这些原料称量以获得预定组成，再在加入预定的添加剂后用球磨机等混合。作为添加剂例如可用Bi、As、B、Si、Ge、Na、Al、Cr、Ti、W、Mo等的氧化物、氯化物等。这类添加物用来促进烧结、防止生成过大的晶粒。这样的混合物于约1000℃温度下焙烧。通过这种焙烧，使二氧化碳气体成分分解、发散，使氧化钡与氧化铁或氧化锶与氧化铁进行化合。
这样焙烧过的材料用球磨机等充分粉碎。粉碎后可根据需要再加入添加物。
[粘合剂添加工序]
将粘合剂加入包含有按上述步骤准备的氧化物磁性材料的原料粉末中并混合。作为所添加的粘合剂，最好采用脂肪酸酯系蜡，特别是经乳化的分子量为300～800的脂肪酸酯系蜡。本发明中，在采用脂肪酸酯系蜡的同时，特别是通过将后述成型用混合物中存在的粒度在500μm以上的聚集体的存在比例按预定范围设定后，能获得已有技术未曾有的格外优异的效果，亦即发现了可以获得不妨碍材料粒子在磁性上沿容易磁化方向排列的材料的极为优异的效果。
在脂肪酸酯系蜡中，尤以植物蜡(例如巴西棕榈蜡、小烛树蜡、漆蜡、小冠巴西棕蜡等)为最好。
粘合剂的添加量为0.2～1.5wt％、更好是0.25～1.2wt％，最好是0.3～0.9wt％。添加量过少，粘合剂不能发挥效果，成型性变差。添加量过多，由于烧结时有机物的碳化而使烧结体的密度下降，使Br等磁性变差。
在此粘合剂添加工序中还可添加成型辅助剂。
适用作成型辅助剂的例如有硬脂酸与硬脂酸酯(硬脂酸钙、硬脂酸锌、硬脂酸镁、硬脂酸铝等等)。通过添加成型辅助剂能有效地改进成型性、提高流动性和减少摩擦力，结果能进一步改进磁性质。添加量最好为0.04～4wt％。添加量过少，不能看到成型辅助剂增加的效果，相反，当添加量过多，会因烧结时有机物质的碳化而使密度下降，以及令Br磁性变差。
在把包含磁性粉末的原料粉末与粘合剂混合时，可采取液体状或固体状的混合方法。采用液体状粘合剂时易产生凝聚而有可能降低磁性粉末的取向性的倾向。采用固体状粘合剂时则有难以均匀混合的问题。混合中采用Henschel混合机、搅拌机等混料装置将粘合剂充分搅拌。混合时最好在粘合剂熔点以下的温度范围进行。若在粘合剂熔点以上混合，粘合剂熔融而产生难以均匀涂布到磁性粉末粒子上的不良情形。
[水分调节工序]
水分调节工序中是对包含上述原料粉末与粘合剂的成型用混合物中进行水分的加或减来调节此混合物的水分。
混合后的成型用混合物的水分对成型性与磁性有很大影响。此种水分含量宜为0.20～0.80wt％，而最好是0.25～0.35wt％。水分不到0.20wt％，在下道工序成型时就难保持所希望的形态。水分含量超过0.80wt％，磁性粉末会发生凝聚，妨碍磁性粉末粒子在磁性上易于沿磁化的轴向排列而降低磁性(Br)。此外还有可能降低烧结密度、出现裂纹与针孔等。
在水分的调节中，通过控制温度与湿度就可实现任意所需的水分量。最好是通过将这种混合物置于室温之下来调节水分，或通过恒温恒湿槽或是喷雾器等添加细微的水蒸汽(水粒径度约为数微米至数十微米)来添加水分。例如若采用喷吹等形式而形成大的水粒时，则有可能易发生凝聚而干扰成型时的取向性。
在此水分调节工序之后，最好设有用以粉碎成型用混合物中聚集物的粉碎工序。通过设置粉碎工序，例如能除去因干燥而形成的聚集物(粉碎成细微粒子)。由于存在聚集物，于后述的磁场中干式成型工序中施加磁场时难以实现所需取向，导致磁性劣化。此外，在上述水分调节工序之后附加破碎工序时，希望在破碎工序结束时混合物中的水分含量为0.20～0.80wt％，其理由与上述水分调节工序中所述的相同。
[磁场中干式成型工序]
水分经调节后的上述成型有混合物加入模具中，施加磁场，进行压制。由此可使原料粉末(磁性粉末粒子)取容易磁化方向，而能提高磁性。
本发明中，加入磁场中干式成型工序的模具中的成型用混合物(投入原料)，其中500μm以上粒度的聚集物的存在比例宜为0.01～0.80wt％，最好为0.01～0.78wt％。当此值超过0.80wt％，在对磁场中干式成型工序中施加磁场时，难以实现所需的取向，这样就会降低磁性。下限值虽可以为零，但在目前的技术水平下，看来以0.01wt％为适宜。
粒度在500μm以上的聚集物的存在比例按以下步骤求出。具体地说，将成型用混合物置于自动筛分机中，经3分钟振动后，测定粒度500μm以上的聚集物的比例，根据此测定值，计算出粒度500μm以上的聚集物的存在比例。
在磁场中干式成型工序中，定向磁场强度约为3～12Koe(239～955KA/m)，成型压力约为1～5吨/cm2。
这样形成的成型物通常由后续工序的烧制工序烧制。
[烧制工序]
上述磁场中干式成型工序中形成的成型物用这里的烧制工序进行烧制。烧制温度最好为1200～1260℃的范围。当烧制温度不到1200℃时，难以获得充分的烧结密度。另一方面，当烧制温度超过1260℃，就易产生异常晶粒的迅速生长。而有可能降低iHc值。烧制的稳定时间约为0.5～4.0小时。烧制气氛可以是空气，但若通过控制氧的分压进行烧制，则能获得高密度的有优良磁性的磁铁。
下面以具体实施形式进一步详细说明本发明。
按重量计，将100份的Sr铁氧体的焙烧粉末、0.5份的SiO2与1份的CaCO3，用水进行湿式微粉碎，使焙烧粉末的比表面积成为7.0m2/g。然后将这种泥浆干燥，用作试验用原料粉末。
在对这样制得的原料粉末中添加下述表1中所示的种种粘合剂之后，用搅拌机于75℃下进行10分钟混合。混合后添加表1所示预定量的成型辅助剂(硬脂酸钙)。
随即用恒温恒湿槽按表1所示调节此混合粉末中的水分。
再如下述表1所示，必要时用粉碎机将此混合粉末破碎，作为永磁材料。
然后将此永磁材料于约7.5Koe的磁场中干式成型。成型压力设为1吨/cm2。获得的成型体置于大气中于1240℃下经1小时烧制，制得直径约26mm、高10mm的磁铁样品。
对于这样的制得的磁铁样品，用B-H跟踪器[东英工业(株)的直流磁化特性测定装置TRF-5BH]评价了Br、iHc等磁性质。
按以下步骤测定了成形体的密度(dp)与烧制体的密度(df)。
成型体的密度(dp)
根据成型体的实际尺寸，求出体积V同时实测其重量W，以此体积V除重量W，得出dp＝w/v。
烧制体(df)的密度
烧制体的密度(df)根据由阿基米德法求得的值算出。
此外，根据以下准则评价了成型体与针孔。
成型性
观察实际成型体进行判断。
(判断准则)
○：制得完善的成型品
△：部分产生开裂
×：不能作为成型品
针孔
对烧结后的样品剖面进行镜面加工，用光学显微镜观察放大50倍后的组成。结果，对于能明显看到针孔而不能提供实用的于表1中以“×”表示，未能发现针孔的于表1中的“○”表示，以“-”标明的则是不能成型的样品。
表1中对于成型用混合物来所存在的粒度为500μm以上的聚集物存在比例的测定方法与以上所述的相同。
结果示于下面的表1中。
表1
样品No.                  粘合剂 成型辅助剂(wt％) 有无破碎工序  烧制温度(℃) 水分(wt％)  粒度在500μm以上的聚集物(wt％)
      种类   分子量    含量(wt％)
实施例1   脂肪酸酯系蜡   400～600     0.24     -     有     1240     0.30     0.20
实施例2   脂肪酸酯系蜡   400～600     0.36     -     有     1240     0.30     0.05
实施例3   脂肪酸酯系蜡   400～600     0.60     -     有     1240     0.30     0.20
实施例4   脂肪酸酯系蜡   400～600     0.90     -     有     1240     0.30     0.30
实施例5   脂肪酸酯系蜡   400～600     0.36     0.15     无     1240     0.25     0.78
实施例6   脂肪酸酯系蜡   400～600     0.36     0.06     有     1240     0.30     0.22
实施例7   脂肪酸酯系蜡   400～600     0.36     0.10     有     1240     0.30     0.20
实施例8   脂肪酸酯系蜡   400～600     0.36     0.15     有     1240     0.30     0.18
实施例9   脂肪酸酯系蜡   400～600     0.36     0.20     有     1240     0.30     0.28
实施例10   脂肪酸酯系蜡   400～600     0.36     0.35     有     1240     0.30     0.25
实施例11   脂肪酸酯系蜡   400～600     0.36     0.15     有     1240     0.60     0.56
实施例12   脂肪酸酯系蜡   400～600     0.36     0.15     有     1240     0.80     0.78
比较例1   脂肪酸酯系蜡   400～600     0.36     0.15     有     1240     0.07     0.15
比较例2   脂肪酸酯系蜡   400～600     0.36     0.15     有     1240     0.90     1.40
比较例3   脂肪酸酯系蜡   400～600     0.36     0.15     无     1240     0.55     1.10
比较例4   樟脑   152     1.2     -     有     1240     0.94     0.58
比较例5*   樟脑*   152     1.2     -     有     1240     0.30     0.58
比较例6   microstacline蜡   800     0.60     -     有     1240     0.35     1.45
比较例7   石蜡   300～500     0.60     -     有     1240     0.35     1.80
比较例8   石蜡   400～600     0.60     -     有     1240     0.35     1.58
比较例9   聚乙烯蜡   2000     0.60     -     有     1240     0.35     1.38
比较例10   硬脂酸   284     0.60     -     有     1240     0.35     0.45
比较例11   硬脂酸钙   607     0.60     -     有     1240     0.35     0.48
比较例12   石蜡   300～500     0.60     -     有     1240     0.35     0.55
比较例13   聚乙烯蜡   2000     0.60     -     有     1240     0.35     0.55
比较例14   microstacline蜡   800     0.60     -     有     1240     0.35     0.55
比较例5*的样品是在混合了粘合剂后，将该原料放置一周后进行成型的样品
表1(续页)
样品No. 成型体密度dp(Mg/m3) 烧制体密度df(Mg/m3) Br(G) IHc(Oc) 成型性 针孔
实施例1     2.92     4.95     3767     3143     ○     ○
实施例2     2.93     4.94     3814     3114     ○     ○
实施例3     2.93     4.95     3800     3111     ○     ○
实施例4     2.93     4.94     3756     3088     ○     ○
实施例5     2.92     4.93     3785     3129     ○     ○
实施例6     2.91     4.95     3899     3096     ○     ○
实施例7     2.90     4.94     3908     3098     ○     ○
实施例8     2.91     4.94     3912     3091     ○     ○
实施例9     2.91     4.94     3878     3093     ○     ○
实施例10     2.91     4.93     3762     3140     ○     ○
实施例11     2.90     4.94     3828     3155     ○     ○
实施例12     2.91     4.93     3738     3203     ○     ○
比较例1     -     -     -     -     ×     -
比较例2     2.94     4.94     3648     3238     ○     ×
比较例3     2.93     4.93     3639     3198     ○     ×
比较例4     2.90     4.90     3700     3188     ○     ○
比较例5*     -     -     -     -     ×     -
比较例6     2.89     4.91     3365     3195     △     ○
比较例7     2.88     4.90     3308     3245     △     ○
比较例8     2.89     4.89     3491     3226     △     ○
比较例9     2.90     4.90     3376     3203     ○     ○
比较例10     -     -     -     -     ×     -
比较例11     -     -     -     -     ×     -
比较例12     2.88     4.90     3428     3190     △     ○
比较例13     2.88     4.89     3608     3178     △     ○
比较例14     2.89     4.90     3495     3159     △     ○
比较例4的结果虽然良好，但若在混合粘合剂后立即成型，则会成为比较例5*的不良结果。
因此，比较例4的样品缺乏粘合剂混合后的长时期稳定性，极不利于处理。
从以上结果可以了解到本发明的效果。具体地说，本发明是氧化物磁性材料系永磁铁的制造方法，它包括：在包含氧化物磁性材料的原料粉末中加入粘合剂并混合的粘合剂添加工序；调节包含上述原料粉末与粘合剂的成型用混合物中水分的水分调节工序；将水分调节好的上述成型用混合物加入模具中，施加磁场，使氧化物磁性粉料全部沿容易磁化方向排列同时加压的磁场干式成型工序；以及将已成型的成型体进行烧制的烧制工序，其中上述粘合剂添加工序中的粘合剂是脂肪酸酯系的蜡，而上述磁场中干式成型工序中加入模具内的成型用混合物内所存在的粒度在500μm以上的聚集体的存在比例为0.01～0.80wt％，由此可以制得低成本且具有优越磁性质的氧化物磁性材料系的永磁铁。
产业上可利用的领域
本发明可以用于制造氧化物磁性材料系永磁铁。

Claims (4)

1.氧化物磁性材料系永磁铁的制造方法，它包括：在包含氧化物磁性材料的原料粉末中加入粘合剂并混合的粘合剂添加工序；调节包含上述原料粉末与粘合剂的成型用混合物中水分的水分调节工序；将水分调节好的上述成型用混合物加入模具中，施加磁场，使氧化物磁性粉料全部沿容易磁化方向排列同时加压的磁场中干式成型工序；以及在1200～1260℃的温度下对已成型的成型体进行烧制的烧制工序，其特征在于：上述粘合剂添加工序中的粘合剂是分子量为400～600的脂肪酸酯系的蜡，成型用混合物中粘合剂的含量为0.2～1.5wt％，上述水分调节工序的混合物中的水分含量为0.20～0.80wt％，而上述磁场中干式成型工序中加入模具内的成型用混合物内所存在的粒度在500μm以上的聚集体的存在比例为0.01～0.80wt％。
2.如权利要求1所述的氧化物磁性材料系永磁铁的制造方法，其中，上述脂肪酸酯系蜡是植物蜡。
3.如权利要求1所述的氧化物磁性材料系永磁铁的制造方法，其中，上述氧化物磁性材料的原料粉末是在配合上氧化物原料并混合后，经焙烧之后再粉碎成的原料粉末。
4.如权利要求1所述的氧化物磁性材料系永磁铁的制造方法，其中，在上述水分调节工序之后，再添加粉碎成型用混合物中聚集体的破碎工序。
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