CN1068265C - 制备有高拉伸强度和改进的软磁性能的产品的方法 - Google Patents

制备有高拉伸强度和改进的软磁性能的产品的方法 Download PDF

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CN1068265C
CN1068265C CN95194240A CN95194240A CN1068265C CN 1068265 C CN1068265 C CN 1068265C CN 95194240 A CN95194240 A CN 95194240A CN 95194240 A CN95194240 A CN 95194240A CN 1068265 C CN1068265 C CN 1068265C
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Abstract

本发明涉及一种方法，其中铁基颗粒粉末组合物与一种热塑性物质和润滑剂混合。在低于所述热塑性树脂的玻璃化转变温度或熔点的温度下压实所获得的混合物，并加热压实产品至高于其软化点温度。随后，得到的压实元件任选地加热到高于固化温度的温度。

Description

制备有高拉伸强度和改进的软磁性能的产品的方法
本发明涉及一种热处理压实的铁基粉末组合物的方法。更具体讲，本发明涉及的方法包括将铁粉组合物与热塑性树脂混合，压实和加热处理。该方法特别适合用于制造具有好的软磁性能和高强度的磁芯元件。
美国专利5268140公开了一种通过粉末冶金技术制造高强度铁基元件的方法。根据该方法，将在有机溶剂存在下用热塑性物质涂布或混合后的铁基颗粒粉末组合物在模具中、在高于热塑性物质的玻璃化转变温度的温度下压实，并将得到的元件在不低于压实温度并不超过约800°F(427℃)的温度下单独加热。所得元件强度有所改善，能用作结构元件或作为磁芯元件。此外，根据其最优选的实施方案，该发明公开的热塑性物质以涂层存在于各个铁颗粒的表面。在该实施方案的各种变化形式中，铁颗粒可以双层涂布，例如除了外层热塑性物质以外，颗粒还可以有一层绝缘物质例如磷酸铁的第一内涂层。
简言之，本发明涉及一种方法，其中铁基颗粒粉末组合物与一种热塑性物质混合。所得混合物在低于热塑性物质的玻璃化转变温度或其熔点的温度下压实，并加热压实的产物以固化热塑性树脂。随后，所得的压实的元件任选地退火到高于固化温度的温度。
具体地讲，本发明涉及一种制备具有高强度和改进的软磁性质的产品的粉末冶金方法，它包括以下步骤：
a)在足以形成一层磷酸铁物质的温度和时间下，用磷酸处理雾化的或海绵铁粉末颗粒，
b)干燥所得粉末，
c)用选自聚苯醚、聚醚酰亚胺和酰胺类低聚物的热塑性树脂干粉末，和低熔点润滑剂与上述干粉末混合，得到基本均匀的颗粒混合物，
d)在低于上述热塑性树脂的玻璃化转变温度或熔点的温度下在模具中压实上述所得粉末混合物，
e)将压实的产品加热到高于热塑性树脂的软化点温度，和
f)任选地，将所得元件退火到高于所述热塑性树脂的固化温度的温度。
在该方法的步骤a)中，优选用磷酸水溶液处理雾化的或海绵铁粉末颗粒，以在铁颗粒表面形成一层磷酸铁。磷酸处理在室温下进行0.5至约2小时。然后，在约90-约100℃的温度下蒸发水分，以形成干粉末。根据本发明的另一实施方案，铁粉是用溶于有机溶剂的磷酸处理。
亚磷层应尽可能薄，而同时又尽可能地完全涂布各个颗粒。因此，具有较大比表面积的粉末的磷含量较高。因为海绵铁粉末的比表面积比雾化铁粉末的大，因此海绵铁粉末的P含量一般高于雾化铁粉末。前一种情况P含量可为约0.02-0.06，优选0.03-0.05％，而后一种情况P含量可为约0.005-0.04，优选0.008-0.03％，以粉末的重量为基准。
本发明方法中使用的热塑性物质可以是重均分子量在约10000-50000范围内的聚合物，其结晶度应使其能溶于有机溶剂。更具体地说，聚合物是美国专利5268140中提到过的聚苯醚和聚醚酰亚胺或其它聚合物，该专利引入本文作为参考。一种可市购的聚醚酰亚胺是以商品名ULTEM出售的树脂。最优选的ULTEM树脂是ULTEM1000级的。另一种根据本发明可使用的热塑性物质是重均分子量小于30000的酰胺类低聚物。该类型的低聚物在PCT/SE95/00636中公开过，该文引入此作为参考。低聚物的特殊实例是有机溶胶，如可从ELF Atochem,France获得的Orgasol3501和Orgasol2001。这类聚合物比美国专利5268140中的聚合物更少无定形态，即结晶度更高，因此它们不用玻璃化转变温度而用熔点来表征。
热塑性物质的粒径不是很关键的。但优选的粒径低于约100μm。热塑性物质的含量为铁粉重量的0.1-1％，优选0.2-0.6％。
与美国专利5268140中所述方法不同，在本发明中使用润滑剂是强制性的。
可使用各种润滑剂与铁和热塑性颗粒混合。优选的润滑剂是低熔点的，可选自金属硬脂酸盐，蜡，链烷烃，天然或合成脂肪衍生物以及上面讨论过的酰胺类低聚物。可用于本发明方法中的可市购的润滑剂有Hoganas AB Sweden的Kenolube,Hoechst AG,Germany的H-wax,以及Morton International of Cincinatti,Ihio的Promold。应该指出，在本文中，酰胺类低聚物可用作热塑性树脂或润滑剂，或二者兼用。因此，根据本发明的一个实施方案，绝缘铁粉仅与所研究的低聚物混合，并在低于低聚物熔点的温度下压实，加热以固化低聚物以及任选地退火。
润滑剂以铁粉重量的0.1-1％，优选0.2-0.8％的量使用。
铁、热塑性树脂和润滑剂的粉末组合物可通过适合的成形技术，用不带任何附加加热设备的常规模具成形为成形元件，如同在上述美国专利中的方法一样。但是，铁粉、热塑性物质和润滑剂的混合物也可以在装入模具中之前，先预热到低于热塑性物质的玻璃化转变温度或熔点的温度，而所述模具本身也预热到低于玻璃转变温度/熔点的温度。根据一个优选实施方案，粉末组合物可用冷压实方法(即在室温下进行压实步骤)成形为成形元件。压实步骤可在约400-1800Mpa的压力下进行。
最后在任选的热处理或退火步骤中，压实并固化的混合物经历一个远高于热塑性物质的固化温度的温度。对于本发明优选的热塑性物质而言，该步骤包括加热到约100-600℃的温度。优选地该温度为200-500℃，最优选在300-400℃。该热处理优选在一个单独的步骤进行。
本发明方法与现有已知方法的主要区别在于，本发明方法的压实步骤在低于热塑性树脂的玻璃化转变温度或熔点的温度下进行。由此，本发明方法的能耗较少因此更加经济，而同时又出乎意料地获得了基本相同的软磁性能。此外，在粉末混合物中使用润滑剂就可省去在前述美国专利方法中所需的模具的润滑。相对于已知方法的另一个优点是，本发明方法可在不使用有害环境的有机溶剂的条件下在常规模具中进行。
根据本发明所使用的特定热塑性物质与德国专利3439397中所述情况不同，它无需使用变动的温度和压力以获得最好的结果。这一点使本发明与上述德国专利相比，在工业意义上更具吸引力。
至于软磁性能，已发现根据本发明方法制得的产品与根据已有方法制得的产品在高频条件下，磁导率与频率关系的曲线是基本相同的。并且材料强度也类似。
图1是热压实Ultem产品(◆表示)，冷压实的分别含有0.5％Ultem+0.5％Promold(用△表示)和0.6％Orgasol+0.1％硬脂酸锌(用■表示)的产品的频率和磁导率的关系曲线。
图2是冷压实的分别含0.5％Ultem+0.5％Kenolube(用△表示)，0.5％Ultem+0.5Orgasol(用●表示)和0.6％Orgasol(用○表示)的产品的频率和磁导率的关系曲线。
图3是比较冷压实和热压实的分别含0.5％Ultem+0.5％Orgasol(冷压实用□，热压实用■表示)和0.6％Orgasol(冷压实用○，热压实用●表示)的产品的频率和磁导率的关系曲线。
图4是比较分别含0.5％Ultem+0.5％Orgasol(冷压实用□表示，热压实用■表示)和0.6％Orgasol(热压实用表示▲表示)的冷压实产品和热压实产品与含0.5％Kenolube的对比试样(热压实用△表示)在不同频率下的总损失的比较曲线图。
通过以下实施例进一步说明本发明。
实施例1
用磷酸水溶液处理基于SCM 100.28(一种可从HgansAB,Sweden处购得的铁粉)的混合物，并干燥以在铁颗粒上提供一个亚磷涂层。由0.5％Ultem(粒径小于70μm)和0.5％Promold润滑剂组成的总量1％的有机物与上述混合物干混，得到均匀材料的试样。
一种基于ABM 100.32(一种可从Hgans AB,Sweden处购得的铁粉)的混合物，已经用磷酸处理，并干燥以便在铁颗粒表面提供一个亚磷涂层，由0.6％Orgasol和0.1％硬脂酸锌润滑剂组成的0.7％有机物与上述混合物干混，得到均匀材料的试样。
一种根据美国专利5268140制备并由Hoegans Corporation,Riverton N.J.按TC粉投放市场的TC铁粉用作参比试样，该试样是以有亚磷涂层的铁粉为基的。而且在磷酸盐绝缘的铁颗粒上已经提供了一层Ultem1000附加涂层。(1％的Ultem聚合物溶于一种有机溶剂中并与磷酸盐绝缘的铁颗粒混合。然后蒸发溶剂)。
所有试样在600MPa下压实。根据本发明的产品，即分别含有Ultem和Promold，Orgasol和硬脂酸锌的产品在室温下用常规的压机压实。根据已知方法的两涂层或双涂层粉末先预热到150℃的温度，并在加热到218℃的模具中压实，该温度正好高于Ultem1000的玻璃化转变温度。所有三个试样均接着在300℃下退火。根据本发明的包括Ultem和Promold的冷压实产品与基于两或双涂层产品的热压实已知产品的磁性能基本相同。基于Orgasol和硬脂酸锌的产品具有稍微不同的曲线，它在低频率下有较高磁导率，在高频率下有较低磁导率，如图1中磁导率与频率的关系所示。
实施例2
混合物基于ABM 100.32(一种可从Hgans AB,Sweden处购得的铁粉)，已经用磷酸处理，并干燥，以在铁颗粒上提供一层亚磷涂层。由0.5％Ultem和0.5％Orgasol组成的总量1％的有机物质与上述混合物干混得到均匀材料的试样。
一种如上所述用磷酸处理的基于ABM 100.32的混合物与0.5％Ultem和0.5％Kenolube润滑剂干混，得到均匀材料的试样。
一种如上所述用磷酸处理的基于ABM 100.32的混合物与既作润滑剂又作热塑性树脂的0.6％Orgasol干混，得到均匀材料的试样。
各试样在600MPa和室温下压实以后，再在空气中于300℃下热处理60分钟。强度比较列于表1。
表1
    材料300℃,60分钟，空气     密度600MPa     生坯强度600MPa
ABM 100.32+0.5％Ultem(D.M.)+0.5％Kenolube 6.83g/cm3 80N/mm2
ABM 100.32+0.5％Ultem(D.M.)+0.5％Orgasol     6.89g/cm3 108N/mm2
ABM100.32+0.6％Orgasol     7.15g/cm3     107N/mm2
在室温下，于800MPa压实之后，再在空气中于300℃下热处理60分钟，然后对各试样进行比较。磁导率和频率的关系公开于图2。
实施例3
混合物基于ABM 100.32(一种可购自Hoganas AB,Sweden的铁粉)，它已经用磷酸处理过，并干燥以在铁颗粒上提供亚磷涂层。由0.5％ Ultem和0.5％ Orgasol组成的总量1％的有机物质与上述混合物干混，得到均匀材料的试样。
一种基于ABM 100.32，并含既作润滑剂又作热塑性物质的0.6％ Orgasol的混合物干混后，得到均匀材料的试样。
在约600MPa下热压实的效果，和在800MPa下室温压实的效果比较于图3和图4。热压实的温度是：对两试样而言，粉末温度110℃-115℃，模具温度温度130℃，此温度低于Ultem的玻璃化转变温度(Tg)。在Orgasol情况下，该温度低于其熔点(Tm)。

Claims (9)

1．一种制备有高拉伸强度和改进的软磁性能的产品的粉末冶金方法，包括以下步骤：
a)在足以形成一层磷酸铁物质的温度和时间下，用磷酸处理雾化的或海绵铁粉末颗粒，
b)干燥所得粉末，
c)用选自聚苯醚、聚醚酰亚胺和酰胺类低聚物的热塑性树脂干粉末，和低熔点润滑剂与上述干粉末混合，得到基本均匀的颗粒混合物，
d)在低于上述热塑性树脂的玻璃化转变温度或熔点的温度下在模具中压实上述所得粉末混合物，
e)将压实的产品加热至高于所述热塑性树脂的软化点的温度。
2．根据权利要求1的方法，其特征在于，它还包括步骤e)之后的步骤f)将所得元件退火到100℃和600℃之间的温度。
3．根据权利要求1的方法，其特征在于，所述润滑剂选自硬脂酸盐，蜡，链烷烃，天然和合成脂肪衍生物以及酰胺类低聚物。
4．根据权利要求1或2的方法，其特征在于，雾化的或海绵铁粉末颗粒用磷酸水溶液处理。
5．根据权利要求1的方法，其特征在于，所述树脂的添加量为铁粉重量的0.1-2％。
6．根据权利要求1的方法，其特征在于，热塑性树脂的粒径小于200μm。
7．根据权利要求2的方法，其特征在于所述退火温度在200℃和500℃之间。
8．根据权利要求1的方法，其特征在于，压实是在室温下进行的。
9．根据权利要求1的方法，其特征在于，所述热塑性树脂和低熔点润滑剂是一种酰胺类低聚物。
CN95194240A 1994-07-18 1995-07-17 制备有高拉伸强度和改进的软磁性能的产品的方法 Expired - Fee Related CN1068265C (zh)

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