CN1211943A - 经过磷化处理的铁粉及其制造方法 - Google Patents
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Abstract
本发明涉及一种新颖的低氧粉末,它包括主要由具有绝缘的含氧和含磷隔离层的纯铁构成的基体粉末的颗粒。新粉末的含氧量按重量计至多比基体粉末的含氧量高0.2%,并且在用ESCA方法测量时,O:P比为30~1,最好为15~12,更好为10~3。本发明还涉及一种制备铁基粉末的新方法,它包括下列步骤:制备由水粉碎铁粉或海绵铁粉构成的基体粉末;用磷酸在有机溶剂中的溶液处理混合物并干燥得到的混合物,由此在混合的同时将磷酸溶液喷射到基体粉末上。
Description
本发明涉及一种新的铁基粉末。更具体一些,本发明涉及一种用于制备软磁材料的新的铁基粉末,该软磁材料在高频和低频下使用时都具有改进的性能。本发明还涉及一种用于制造新的铁基粉末的新方法。
在用粉末冶金方法制造结构元件时,铁基颗粒曾长期被用作基体材料。铁基颗粒首先在高压下在模具中被模制,以便得到所要求的形状。在模制步骤之后,结构元件通常要经过烧结步骤,从而赋予零件以必要的强度。
磁芯元件也曾经用这种粉末冶金方法制造,但是,在这些方法中所用的铁基颗粒通常都涂覆以环绕的绝缘材料层。
铁芯元件的两个主要特性是其磁导率和铁芯损耗特性。材料的磁导率是其被磁化的能力或其传播磁通量的能力的指标。磁导率被定义为感应的磁通量与磁化力或磁场强度之比。当磁性材料受到快速变化的磁场的作用时,芯部的总能量由于产生滞后回线损失和/或涡流损耗而减少。滞后回线损失是由于必须消耗能量,以在铁芯元件中克服剩余磁力而产生的。涡流损耗的产生是因为由于交流(AC)条件所引起的磁通变化而在铁芯元件中产生电流。
磁芯元件通常用层压的薄钢板制造,但是这些元件难于制造成得到小的复杂零件的网状,并且在高频时遭受大的铁芯损耗。这些叠片基芯子的应用还受到这样的限制,即必须只在薄板的平面中传播磁通量,以免有过大的涡流损耗。作为用于磁芯元件的材料,曾经用烧结的金属粉末代替层压的薄钢板,但是这些烧结的零件也有高的铁芯损失并且主要限于直流(DC)工作。
采用包覆铁基粉末通过粉末冶金制造磁芯元件的研究曾经针对铁粉成分的研制,这种铁粉成分能加强某些物理性能和磁性能,而且不会不利地影响其它性能。所要求的性能包括经过宽广的频率范围的高磁导率,高的压缩强度,低的铁芯损耗和用于压缩模制技术的适合性。
当模制一用于AC动力场合的芯部元件时,通常要求铁颗粒有电绝缘涂层,以减少铁芯损耗。
在文献中公开了各种类型的用于铁颗粒的绝缘涂层。
按照DE 129 1028,用磷酸溶液处理铁粉,接着经过洗涤和干燥。这一工艺的特征为,铁粉的颗粒尺寸最大为10μm,并且除了磷酸以外还用铬酸处理铁粉。该公报没有公开由铁粉制备的材料的磁性能。
此领域中的另一公开文献为DE2825235,它公开了一种由被涂覆以氧化物层的颗粒组成的铁粉。颗粒尺寸在0.05mm至0.15mm之间,并且颗粒具有氧化物涂层,该涂层按颗粒重量计算包括0.3%-0.8wt%的氧。氧化物涂层可以通过在空气中加热或通过化学氧化得到,但是没有公开任何工艺参数和包覆粉粒的分析。根据一些例子可以计算出,所得到的磁导率的范围为30-35。
欧洲专利申请434669涉及一种磁粉,其中,电绝缘涂层将磁粉颗粒分开。颗粒具有10-300μm的平均颗粒尺寸,并且包覆磁粉的每个颗粒的绝缘材料包括厚度为10μm或更小的连续绝缘膜,而且此膜包括一金属酚盐或其分解产物。
WO 95/29490公开了通过采用一种以水中的磷酸为基础的方法得到的绝缘层。
最后,DE专利3439397公开了由磷酸盐涂层电绝缘的铁颗粒。这种涂层可以例如是磷酸镁或磷酸锌。绝缘的磷酸盐涂层应当为铁颗粒的重量的0.1%-1.5%。此公开文献的例1较详细地披露了这种电绝缘的涂层是通过在浓度为89%的磷酸在丙酮中的溶液中搅拌铁粉而得到的。按照WO专利申请的粉末和按照DE专利的粉末之间的比较性研究表明,按照DE专利的绝缘层包括比按照WO申请的粉末多得多的氧和磷。
现在已经非常意外地发现,通过采用按照本发明的新的低氧粉末可以得到显著改进的性能。这些性能包括强度、密度、磁感和磁导率,同时有较低的损耗。
新的粉末以一种基体粉末为基础,它主要由纯铁组成并且可以例如是可从市场上得到的水粉碎铁粉或具有圆的,不规则的或扁平的颗粒的海绵铁粉。可以使用的不规则的、水粉碎的铁粉的典型例子为可以从瑞典Hgans公司得到的ABC 100和ASC100系列的粉末。基体粉末的颗粒尺寸取决于粉末的预定最终用途并且通常小于200μm,而且最好小于150μm。对于较高的频率,优选小于45μm的颗粒尺寸。更为优选的是,多数铁基粉末的颗粒应有大于10μm的颗粒尺寸。
按照本发明,此基体粉末设有一氧涂层或隔离层,其与众不同的新特征在于,新粉末的氧气量只比基体粉末的略高一些。更具体一些,新粉末中的氧气量按重量百分比计比基体粉末中的至多多0.2%,最好至多多0.15%。
可以认为,对于新粉末的性能来说,颗粒的表面结构和成分是重要的,为此,曾经用FSCA法研究了新粉末(参看:“第六届国际X射线光学和微量分析会议会刊”东京大学出版社,1972,385~392页和393~398页;或Anthony R.west著的“固体化学及其应用”,由John willey and sons出版社出版1984,第86页和第92~96页)。按照此方法,O∶P比此应当小于30并大于1。此比例最好应小于15,且大于2,小于10并大于3更好。
新粉末的颗粒的表面膈离层的另一重要特征为厚度,而且通过使用AES方法(参看上面所引用的出版物“固体化学及其应用”)已发现,绝缘膈离层或涂层应当小于100nm,最好小于70nm,更好的是小于50nm。
按照本发明的绝缘涂层是通过以一段足以得到所要求的量的时间用有机溶剂中的磷酸处理基体粉末而施加在基体粉末上的。磷酸在有机溶剂中的浓度应当大大地低于在DE专利中公开的浓度并在0.5%~50%之间变化,最好在0.5%~20%之间变化,更好一些在1%~5%之间变化。新粉末可以通过在一段足以达到上述水平的时间内将磷酸溶液喷射在基体粉末上而得到。磷酸的浓度最好应当小于按重量计的l0%,更好一些小于5%。
按照本发明的新的铁基粉末在压实步骤之前可以与按重量计为0.1%~1.0%的润滑剂和任选的一种有机热固性或热塑性树脂结合。润滑剂的代表性例子为Kenolube、H蜡、EBS和像硬脂酸锌这样的硬脂酸盐。有机树脂可以从由Peracit、Ultem组成的组中选取。
压实可以在最高达1000Mpa的传统压力下进行,而且压实可在环境温度或高温下进行。
本发明进一步地由下列试验说明。
使1kg在市场上可从瑞典Hgans公司得到的粉末ABC100。30的试样分别通过使用在水和乙醇中的正磷酸而受到涂层处理。在一段足以得到氧和磷的涂层或膈离层的时间内,将其量在2.5~120ml/kg间变化的溶液喷射在铁基粉末上随后干燥所有的试样,以便去掉溶剂。所得到的粉末的ESCA分析显示,通过使用水溶液得到的粉末的O∶P比(原子%O∶原子%P)约为30,而且通过采用按照本发明的方法得到的同样比例在5~10之间变化。
对试样的化学分析表明,通过使用水溶液得到的粉末的氧含量要比基体粉末中的高0.2%以上,而通过采用按照本发明的方法得到的粉末的氧含量要比基体粉末中的高0.2%以下。试样的AES分析表明,所有试样的氧化物厚度均小于100nm。
下表综合了用由A指代的新粉末得到的数据,以与本发明范围以外的粉末比较。
表1
试样 | O/P | 原子%P | 原子%O | O总量 | O增加 | P总量 | P增加 |
基体粉末(1) | 0.00 | 53.98 | 0.067 | 0 | 0.003 | 0 | |
A4 | 9.3 | 5.83 | 53.98 | 0.070 | 0.003 | 0.004 | 0.001 |
A3 | 6.95 | 5.91 | 41.13 | 0.093 | 0.026 | 0.014 | 0.011 |
A2 | 4.6 | 13.49 | 61.92 | 0.171 | 0.104 | 0.048 | 0.045 |
参考B | 29.7 | 1.92 | 57.01 | 0.214 | 0.147 | 0.013 | 0.010 |
采用以单色Al作为X射线源的KRATOS AXIS HS光谱仪的ESCA测量O/P比,Kα=1486.6eV;-39.5nm。
O和P的量用化学分析测量。
参考B是根据在WO 95/29490中公开的方法用水溶液制备的试样。
表2公开了与本发明范围以外的粉末相比,用从新型粉末制备的材料得到的湿强度和密度。粉末在800Mpa下压实并加入0.6%的Kenolube作为润滑剂。
表2
材料 | 湿强度(N/mm2) | 密度(g/cm3) |
参考B | 26.71 | 7.25 |
A | 39.55 | 7.31 |
参考C | 19.24 | 7.14 |
参考C是按照DE专利3439397制备的试样。
图1示出了按照本发明的低氧粉末在用低氧粉末制备的试样的磁性能方面的改进效果。粉末曾经用其由ESCA方法测量的O/P比定义。试样通过在800MP下压实粉末并在500℃加热压实的试样30min而制备。“参考B”代表通过对同样的铁基粉末采用水处理而得到的结果。可以看出,采用按照本发明的新的低氧铁可以得到惊人的改进。
图2公开了作为图1中示出的试样的总含氧量的函数的改进效果。
Claims (8)
1.一种低氧粉末,包括主要由具有绝缘的含氧和含磷膈离层的纯铁构成的基体粉末的颗粒,其特征为,粉末的含氧量按重量计至多比基体粉末的含氧量高0.2%,并且用ESCA方法测量,O∶P比在30和1之间,较好地是在15和2之间,最好在10和3之间。
2.如权利要求1所述的低氧粉末,其特征为,基体粉末为海绵铁粉或水粉碎的铁粉。
3.如权利要求1或2所述的低氧粉末,其特征为,用AES方法测量,氧膈离层的厚度至多为100nm。
4.一种用于制备铁基粉末的方法,它包括下列步骤:制备由水粉碎铁粉或海绵铁粉构成的基体粉末,用磷酸在有机溶剂中的溶液处理混合物并干燥所得到的混合物,其特征为,在混合的同时将磷酸溶液喷射到基体粉末上。
5.如权利要求4所述的方法,其特征为,磷酸在有机溶剂中的浓度在按重量计为0.5%~20.0%之间变化,最好在按重量计为0.5%~5%之间变化。
6.如权利要求4或5所述的方法,其特征为,有机溶剂是从包括乙醇和丙酮的组中选取的。
7.如权利要求4至6中的任一项所述的方法,其特征为,在一段足以提供一按AES方法测量至多为100nm的绝缘涂层的时间里将磷酸溶液喷射到铁基粉末上。
8.如权利要求4至7中的任一项所述的方法,其特征为,在一段足以提供按重量计最多比基体粉末的含氧量高0.2%的粉末的含氧量的时间里,将磷酸溶液喷射到铁基粉末上。
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SE9600724A SE9600724D0 (sv) | 1996-02-23 | 1996-02-23 | Iron based powder |
SE96007240 | 1996-02-23 | ||
SE96007257 | 1996-02-23 | ||
SE9600725A SE9600725D0 (sv) | 1996-02-23 | 1996-02-23 | Manufacturing method |
Publications (2)
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CN1211943A true CN1211943A (zh) | 1999-03-24 |
CN1223422C CN1223422C (zh) | 2005-10-19 |
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CNB97192452XA Expired - Lifetime CN1223422C (zh) | 1996-02-23 | 1997-02-19 | 经过磷化处理的铁粉及其制造方法 |
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US (1) | US6348265B1 (zh) |
EP (1) | EP0881959B1 (zh) |
JP (1) | JP4187266B2 (zh) |
KR (1) | KR100454855B1 (zh) |
CN (1) | CN1223422C (zh) |
AT (1) | ATE248674T1 (zh) |
AU (1) | AU714473B2 (zh) |
BR (1) | BR9707648A (zh) |
DE (1) | DE69724589T2 (zh) |
ES (1) | ES2203784T3 (zh) |
MX (1) | MX220648B (zh) |
PL (1) | PL183359B1 (zh) |
RU (1) | RU2176577C2 (zh) |
WO (1) | WO1997030810A1 (zh) |
Cited By (6)
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1997
- 1997-02-19 BR BR9707648A patent/BR9707648A/pt not_active IP Right Cessation
- 1997-02-19 RU RU98117805/02A patent/RU2176577C2/ru active
- 1997-02-19 CN CNB97192452XA patent/CN1223422C/zh not_active Expired - Lifetime
- 1997-02-19 KR KR19980706508A patent/KR100454855B1/ko not_active IP Right Cessation
- 1997-02-19 WO PCT/SE1997/000283 patent/WO1997030810A1/en active IP Right Grant
- 1997-02-19 EP EP97905537A patent/EP0881959B1/en not_active Expired - Lifetime
- 1997-02-19 PL PL97328509A patent/PL183359B1/pl unknown
- 1997-02-19 AT AT97905537T patent/ATE248674T1/de active
- 1997-02-19 DE DE69724589T patent/DE69724589T2/de not_active Expired - Lifetime
- 1997-02-19 AU AU22382/97A patent/AU714473B2/en not_active Expired
- 1997-02-19 JP JP53006797A patent/JP4187266B2/ja not_active Expired - Lifetime
- 1997-02-19 ES ES97905537T patent/ES2203784T3/es not_active Expired - Lifetime
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1998
- 1998-08-21 US US09/137,311 patent/US6348265B1/en not_active Expired - Lifetime
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100439012C (zh) * | 2003-09-09 | 2008-12-03 | 霍加纳斯股份有限公司 | 铁基软磁粉末 |
CN101142044B (zh) * | 2005-01-25 | 2010-12-01 | 大冶美有限公司 | 含Mg氧化膜包覆的铁粉末 |
US8075710B2 (en) | 2005-06-15 | 2011-12-13 | Höganäs Ab | Soft magnetic composite materials |
CN102917819A (zh) * | 2010-05-07 | 2013-02-06 | 赫格纳斯公司 | 改进的压实方法 |
CN102917819B (zh) * | 2010-05-07 | 2015-04-01 | 赫格纳斯公司 | 改进的压实方法 |
CN107745120A (zh) * | 2014-06-20 | 2018-03-02 | 昭荣化学工业株式会社 | 碳被覆金属粉末、导电性糊剂及层叠电子部件、以及碳被覆金属粉末的制造方法 |
CN107745120B (zh) * | 2014-06-20 | 2019-08-20 | 昭荣化学工业株式会社 | 碳被覆金属粉末、导电性糊剂及层叠电子部件、以及碳被覆金属粉末的制造方法 |
CN105742049A (zh) * | 2016-04-29 | 2016-07-06 | 成都锦粼科技有限公司 | 一种铁芯及其制作方法 |
Also Published As
Publication number | Publication date |
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EP0881959A1 (en) | 1998-12-09 |
JP4187266B2 (ja) | 2008-11-26 |
MX9806871A (en) | 1999-01-31 |
PL328509A1 (en) | 1999-02-01 |
EP0881959B1 (en) | 2003-09-03 |
KR100454855B1 (ko) | 2004-12-16 |
WO1997030810A1 (en) | 1997-08-28 |
DE69724589T2 (de) | 2004-08-05 |
CN1223422C (zh) | 2005-10-19 |
RU2176577C2 (ru) | 2001-12-10 |
KR19990087118A (ko) | 1999-12-15 |
ATE248674T1 (de) | 2003-09-15 |
MX220648B (en) | 2004-05-28 |
ES2203784T3 (es) | 2004-04-16 |
AU714473B2 (en) | 2000-01-06 |
JP2000504785A (ja) | 2000-04-18 |
BR9707648A (pt) | 1999-07-27 |
DE69724589D1 (de) | 2003-10-09 |
PL183359B1 (pl) | 2002-06-28 |
AU2238297A (en) | 1997-09-10 |
US6348265B1 (en) | 2002-02-19 |
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