CN108285348B - 一种干压异性永磁铁氧体用磁粉的制造方法 - Google Patents

一种干压异性永磁铁氧体用磁粉的制造方法 Download PDF

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CN108285348B
CN108285348B CN201810130155.5A CN201810130155A CN108285348B CN 108285348 B CN108285348 B CN 108285348B CN 201810130155 A CN201810130155 A CN 201810130155A CN 108285348 B CN108285348 B CN 108285348B
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周小霞
吕宝顺
齐勉达
晁向
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Anhui Shengmeige New Material Co ltd
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Abstract

本发明公开了一种干压异性永磁铁氧体用磁粉的制造方法，包括：采用小粒径的铁红和碳酸锶，混合后低温预烧，得到平均晶粒尺寸为1.2μm以下的铁氧体预烧料，向该铁氧体预烧料中加入碳酸钙和二氧化硅后，通过干式磨机干磨后制成平均粒度为1.0～1.7μm的细粉，向所述细粉中加入樟脑粉和硬脂酸钙后，经过高粉机分散制得的用于干压异性永磁体用磁粉。本发明改变了目前制粉常用方法，即细磨的方式从常用的湿式细磨，改为干式细磨，省去了湿法磨料、脱水和烘干工序，减少工艺流程，减少了生产中耗水量和能量消耗，更加环保低碳。

Description

一种干压异性永磁铁氧体用磁粉的制造方法
技术领域
本发明涉及永磁材料制备领域，尤其涉及一种干压异性永磁铁氧体用磁粉的制造方法。
背景技术
铁氧体永磁是一类具有磁铅石型(M型)晶体结构的材料，由于价格低廉、具有良好的磁特性和温度特性，广泛用于家电、办公设备及汽车上的电气设备中的电机磁瓦和转子等。
铁氧体磁体制造，一般通过原料混合后，预烧，然后粉碎成合适的粒度成为预烧料粗粉，然后细磨成细粉，成型成为所需要的形状进行烧结而制成磁体。为了制造各向异性烧结磁体，在磁场中进行成型。
铁氧体磁体按照成型工艺可分为湿压和干压。湿压成型是将细磨后的料浆脱水达到一定浓度后，加入模腔中，施加外磁场取向压制成磁体。由于磁性颗粒分散在有水或其它有机液体作为溶剂的料浆中，磁性颗粒本身不发生粘连，施加磁场时，磁性颗粒易于转动，它的易磁化轴与磁场方向一致，所以性能高；但成型设备复杂，需要吸水系统，而且不易加工成小产品，需要磨削，加工成本高。干压成型是把细磨后的料浆经脱水、干燥、分散后，加入硬脂酸钙作为润滑剂、樟脑作为粘接剂，得到干压粉末；将干压粉末填充到成型模腔内，外加取向磁场成型；由于压制时不需要脱水，生产效率高，设备费用低，尤其适用于难于用湿法生产的异型器件和小器件，较湿法成型的产品，取向度略低，磁性能略差。最高剩磁的磁体一般采用湿式成型法。因为在本领域中，磁体的性能主要包括剩磁Br和内禀矫顽力iHc，其中剩磁Br由材料的饱和磁感应强度、密度和取向度决定，表达式如下：Br＝4πσs×η×ρ；其中的比饱和磁化强度σs由材料的本征特性决定，取向度η和密度ρ主要由工艺条件决定的。为了保证得到高的取向度η，异性干压磁粉一般采用湿法球磨或砂磨制粉，保证磁粉颗粒尽可能的成为单晶体，提高取向的可能性，进而提高磁体的剩磁Br。同时细粉的粒度需要足够的小，使其小于单畴尺寸颗粒尽可能的多，提高磁体的內禀矫顽力iHc。按现有通常生产工艺，预烧温度一般1250～1300℃，要想在生产中得到性能满意的干压异性磁体，必须采用湿法磨料(砂磨和球磨机)的方式，将磁粉平均粒度控制在1μm以下，可以保证在iHc一定的前提下，Br尽可能高。但湿法磨料，存在脱水和烘干等工序，不仅工艺流程复杂，用水量量大，且能耗高。
发明内容
基于现有技术所存在的问题，本发明的目的是提供一种干压异性永磁铁氧体用磁粉的制造方法，省去了湿法磨料、脱水和烘干工序，减少工艺流程，减少了用水量，降低了能耗，更加环保和低碳。
本发明的目的是通过以下技术方案实现的：
本发明实施方式提供一种用于干压异性永磁体用磁粉的制造方法，包括：
将平均晶粒尺寸为1.2μm以下的铁氧体预烧料，加入碳酸钙和二氧化硅后，通过干式磨机干磨后制成平均粒度为1.0～1.7μm的细粉，向所述细粉中加入樟脑粉和硬脂酸钙后，经过高粉机分散制得的用于干压异性永磁体用磁粉。
由上述本发明提供的技术方案可以看出，本发明实施例提供的干压异性永磁铁氧体用磁粉的制造方法，有益效果为：
将平均晶粒尺寸为1.2μm以下的铁氧体预烧料，加入碳酸钙和二氧化硅后，通过干式磨机干磨后制成平均粒度为1.0～1.7μm的细粉，向所述细粉中加入樟脑粉和硬脂酸钙后，经过高粉机分散制得的用于干压异性永磁体用磁粉。该方法仅采用干磨的方式制粉，省去了常规工艺中湿法磨料、脱水和烘干工序，减少工艺流程，减少了用水量，降低了能耗，更加环保和低碳，且能保证制备干压异性永磁铁氧体性能。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域的普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他附图。
图1为本发明实施例1提供的铁氧体预烧料晶体形貌图；
图2为本发明实施例2提供的铁氧体预烧料晶体形貌图；
图3为本发明实施例3提供的铁氧体预烧料晶体形貌图；
图4为本发明实施例3提供的干压磁粉粒度分布图。
具体实施方式
下面结合本发明的具体内容，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明的保护范围。本发明实施例中未作详细描述的内容属于本领域专业技术人员公知的现有技术。
本发明实施例提供一种用于干压异性永磁体用磁粉的制造方法，是一种仅用干磨制备符合性能的干压异性永磁体用磁粉的方法，包括：
将平均晶粒尺寸为1.2μm以下的铁氧体预烧料，使用时将该铁氧体预烧料粗破碎为平均粒度为2.0μm的粗粉，加入碳酸钙和二氧化硅后，通过干式磨机干磨后制成平均粒度为1.0～1.7μm的细粉，向细粉中加入樟脑粉和硬脂酸钙后，经过高粉机分散制得的用于干压异性永磁体用磁粉。
上述方法中，平均晶粒尺寸为1.2μm以下的铁氧体预烧料采用以下方式制得：
以平均粒度小于0.8μm的氧化铁和平均粒径小于2.0μm的碳酸锶为原料，将所述氧化铁和碳酸锶按摩尔比5.0～6.0混合后，在1050～1180℃预烧后，制得的平均晶粒尺寸为1.2μm以下的铁氧体预烧料，该铁氧体预烧料使用时经粗破碎为平均粒度为2.0μm左右的粗粉。
上述制备预烧料还包括：在氧化铁和碳酸锶混合后的原料中可加入低熔点盐类作为助溶剂；优选的，低熔点盐类采用钠盐、钾盐、锶盐、钡盐、Bi2O3中的任一种。
上述制备预烧料中，氧化铁优选采用纯度大于98.5％的氧化铁；碳酸锶优选采用纯度大于97％的碳酸锶；低温预烧时间为2～4小时。
上述方法中，向预烧料粗碎后的粗粉中加入碳酸钙和二氧化硅，
碳酸钙的加入量占粗粉的重量为：0.3％～1.2％；
二氧化硅的加入量占粗粉的重量为：0.1～0.6％；
向细粉中加入樟脑粉和硬脂酸钙，
樟脑粉的加入量占细粉的重量为：0.3％～1.2％；
硬脂酸钙的加入量占细粉的重量为：0.1％～0.8％。
上述方法中，干式磨机采用球磨机、振磨机、干式砂磨机中的任一种。
上述方法中，在干式磨机干磨中，若采用干式振磨，在干式振磨中加入占磁粉总重量0.1～0.5％的助磨剂。
本发明通过采用特定的小粒径的氧化铁和碳酸锶为原料，或加入一定量的低熔点盐类作为助溶剂后，降低反应温度，达到降低晶粒的大小和晶粒间粘结的强度，解决了高温预烧带来的预烧料的晶粒粘结强度大，紧实、密度大和本身硬度也大的问题(该问题会造成了后续的干式磨料达不到粒度要求，或造成磁粉颗粒中单晶颗粒比例减少，取向度η降低，使磁体Br达不到要求)，再进行低温预烧制成预烧料，仅采用干法磨料工艺就能达到采用原来湿法制粉的磁体性能(即保证磁粉颗粒尽可能多为单晶体，保证取向度，从而不至于降低磁体的Br)，实现了省却湿法磨料这一环节，该方法改变了目前制粉常用方法，细磨的方式采用干式细磨，而非常用的湿式细磨，省去了湿法磨料、脱水和烘干工序，减少工艺流程，减少了用水量，降低了能耗，更加环保和低碳，达到使用要求，很好的解决了迄今为止制备异性干压粉环节都不能缺少湿式细磨制粉这一工序的难题。
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
本实施例提供一种干压异性永磁铁氧体用磁粉的制造方法，包括：
选择小粒径的氧化铁和碳酸锶原料，或加入部分助溶剂，混合后，通过低温预烧制成铁氧体预烧料，进行粗破碎后制成平均粒径为2.0μm左右粗粉，将该粗粉加入一定量的二次添加剂(碳酸钙、二氧化硅)在干式磨机(如球磨机、振磨机和干式砂磨机等中的任一种)内进行干式磨料制成平均粒度为1.0～1.7μm的细粉，即为干压异性永磁铁氧体用磁粉。用该磁粉制备干压异性永磁铁氧体时，向该细粉中加入分散剂和粘结剂高速分散，在磁场中压制，烧结，即制得干压异性永磁铁氧体。
具体的，本发明制造细粉及制备永磁铁氧体的步骤如下：
(1)本发明的永磁铁氧体成分没有特别限定，只要是磁铅石型铁氧体即可，主相为MFe12O19，M可以是Sr、Ba或Ca中的一种或多种。另外，也可以含有La、Nd、Pr、Co、Zn等不同种元素，取代M或Fe。
(2)利用粒度小于0.8μm、纯度为大于98.5％的Fe2O3，粒度小于2μm纯度大于97％的SrCO3或加入一定量低熔点的助溶剂按一定比例混合，制粒，在温度为1050～1180℃预烧，制成铁氧体预烧料；
(3)将铁氧体预烧料破碎成平均粒度为2.0μm左右的粗粉，并在该粗粉中添加由碳酸钙、二氧化硅等其他物质组成的二次配方后进行干式振磨，制成平均粒度为1.0～1.7μm的细粉；在所述干式振磨粉料中加入一定量的樟脑粉和硬脂酸钙后，经过高粉机分散制得干压磁粉；
(4)按正常干压异性磁体的制作方法制成磁体；将上述干压磁粉在磁场中干法压制，成型磁场大于6000Gs；然后在空气气氛下烧结，烧结温度1050～1180℃，保温2小时，获得烧结磁体，测量磁特性。
实施例1
本实施例提供一种干压异性永磁铁氧体用磁粉的制造方法，包括以下步骤：
铁氧体预烧料采用以下原料：
氧化铁(即铁红)：1200克(粒度为0.70μm、纯度大于98.5％)；
碳酸锶：190克(粒度为1.8μm、纯度为大于97.5％)；
用振磨机混料(将上述氧化铁和碳酸锶混合)，制粒，在1100℃保温2小时进行预烧制成铁氧体预烧料，将铁氧体预烧料粗碎成平均粒度为2μm左右的粗粉，在粗粉中加入占粗粉重量为1.0％的CaCO3和0.35％的SiO2，振磨2小时，磁粉平均粒度1.40μm，再在细粉中加入占细粉重量为1.0％樟脑粉和0.3％硬脂酸钙，过高速分散机，制得可供干压成型的干压磁粉；对上述干压磁粉进行磁场压制，成型磁场大于6000Gs。然后在空气气氛下烧结，烧结温度1220℃，保温2小时，获得烧结磁体。
实施例2、实施例3：
按上述实施例1的工艺，仅改变低温预烧温度为1150℃和1180℃，分别得到制备干压磁粉的实施例2和实施例3。
实施例4～6：
按上述实施例1、2和3中的工艺，但改变二次配料中的CaCO3和SiO2，从原来的在粗粉中加入占粗粉重量为1.0％的CaCO3和0.35％的SiO2，改为加入占粗粉重量为0.75％的CaCO3和0.3％的SiO2，分别得到制备干压磁粉的实施例4、实施5和实施6。
实施例7、实施例8：
将上述实施例1、实施例2的工艺，将振磨时间从2小时增加到4小时，分别得到制备干压磁粉的实施例7和实施例8。
比较例：
采用目前市场上的、用湿法细磨的干压异性磁粉，加入重量为1.0％樟脑粉和0.3％硬脂酸钙，过高速分散机，在6000Gs取向磁场下压制成型，然后在空气气氛下烧结，烧结温度1225℃，保温2小时，获得烧结磁体。
上述各实施例和比较例制成的磁粉的性能见表1。
表1
Figure BDA0001574627290000061
通过上述表1可以看出，本发明方法制得的磁粉，仅采用干磨制粉方式，就制得性能符合要求的干压异性永磁铁氧体用磁，且省去了湿法磨料、脱水和烘干工序，减少工艺流程，减少了用水量，降低了能耗，更加环保和低碳。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。

Claims (7)

1.一种用于干压异性永磁体用磁粉的制造方法，其特征在于，包括：
将平均晶粒尺寸为1.2μm以下的铁氧体预烧料，加入碳酸钙和二氧化硅后，通过干式磨机干磨后制成平均粒度为1.0～1.7μm的细粉，向所述细粉中加入樟脑粉和硬脂酸钙后，经过高粉机分散制得的用于干压异性永磁体用磁粉；
所述平均晶粒尺寸为1.2μm以下的铁氧体预烧料采用以下方式制得：以平均粒度小于0.8μm的氧化铁和平均粒径小于2.0μm的碳酸锶为原料，将所述氧化铁和碳酸锶按摩尔比5.0～6.0混合后，在1050～1180℃预烧后，制得的平均晶粒尺寸为1.2μm以下的铁氧体预烧料；
所述方法中，在1050～1180℃预烧的预烧时间为2～4小时。
2.根据权利要求1所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，制备所述预烧料还包括：在所述氧化铁和碳酸锶混合后的原料中加入低熔点盐类作为助溶剂。
3.根据权利要求2所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，所述低熔点盐类采用钠盐、钾盐、锶盐、钡盐、Bi2O3中的任一种。
4.根据权利要求1至3任一项所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，所述方法中，向预烧料粗碎后的粗粉中加入碳酸钙和二氧化硅，
碳酸钙的加入量占所述粗粉的重量为：0.3％～1.2％；
二氧化硅的加入量占所述粗粉的重量为：0.1～0.6％；
向细粉中加入樟脑粉和硬脂酸钙中，
樟脑粉的加入量占所述细粉的重量为：0.3％～1.2％；
硬脂酸钙的加入量占所述细粉的重量为：0.1％～0.8％。
5.根据权利要求1至3任一项所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，所述方法中，加入碳酸钙和二氧化硅之前，将所述铁氧体预烧料粗破碎为平均粒度为2.0μm的粗粉。
6.根据权利要求1所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，所述方法中，干式磨机采用球磨机、振磨机、干式砂磨机中的任一种。
7.根据权利要求1或6所述的一种用于干压异性永磁体用磁粉的制造方法，其特征在于，所述方法中，在干式磨机干磨中，若采用干式振磨，在干式振磨中加入占磁粉总重量为0.1～0.5％的助磨剂。
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PE01 Entry into force of the registration of the contract for pledge of patent right
CP03 Change of name, title or address
CP03 Change of name, title or address

Address after: 245700 Industrial Zone, Mount Huangshan District, Anhui, Huangshan City

Patentee after: Anhui Shengmeige New Material Co.,Ltd.

Address before: 245000 Huangshan Industrial Park, Huangshan City, Anhui Province

Patentee before: ANHUI SHENGMEIGE NEW MATERIAL CO.,LTD.

PC01 Cancellation of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Granted publication date: 20200626

Pledgee: Postal Savings Bank of China Limited Huangshan District Sub-branch

Pledgor: ANHUI SHENGMEIGE NEW MATERIAL CO.,LTD.

Registration number: Y2023980032470

PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A manufacturing method of magnetic powder for dry pressed anisotropic permanent magnet ferrite

Granted publication date: 20200626

Pledgee: Postal Savings Bank of China Limited Huangshan District Sub-branch

Pledgor: Anhui Shengmeige New Material Co.,Ltd.

Registration number: Y2024980004942