CN103553585A - 铁氧体陶瓷的制备方法 - Google Patents

铁氧体陶瓷的制备方法 Download PDF

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CN103553585A
CN103553585A CN201310497364.0A CN201310497364A CN103553585A CN 103553585 A CN103553585 A CN 103553585A CN 201310497364 A CN201310497364 A CN 201310497364A CN 103553585 A CN103553585 A CN 103553585A
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苏绍华
余金辉
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AAC Technologies Holdings Shenzhen Co Ltd
AAC Precision Manufacturing Technology Changzhou Co Ltd
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AAC Acoustic Technologies Shenzhen Co Ltd
AAC Precision Manufacturing Technology Changzhou Co Ltd
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Abstract

本发明提供了一种铁氧体陶瓷的制备方法，其通过对铁氧体粉末进行制浆和流延成型，然后进行烧结而成。本发明提供的铁氧体陶瓷的制备方法，可制备单向或复相陶瓷薄片材料，缺陷尺寸小，产品成分起伏小，性能稳定，生产效率高，可连续操作，可大批量生产，适合工业生产，适于成型大型薄片，厚度控制精度高，浆料配比可调等优点，满足了铁氧体基片小型化、高性能化、多功能化的发展趋势。

Description

铁氧体陶瓷的制备方法
技术领域
本发明涉及一种铁氧体陶瓷的制备方法。
背景技术
烧结铁氧体磁铁可以用于各种电动机、发电机、扬声器等各种用途中。作为代表性的烧结铁氧体磁铁，已知有具有六方晶系的M型磁铁铅矿(magneto plumbite)结构的Sr铁氧体(SrFe12O19)、Ba铁氧体(BaFe12O19)。这些烧结铁氧体磁铁例如以氧化铁和锶(Sr)或钡(Ba)等的碳酸盐为原料，利用粉末冶金法比较廉价地制造。
近年来，从对环境的顾虑等出发，在汽车用电装部件、电气设备用部件等中，以部件的小型、轻量化和高效化作为目的，要求烧结铁氧体磁铁的高性能化。尤其在用于汽车用电装部件的电动机中，要求保持高剩磁通密度Br(以下简称为“Br”)且具有难以引起由薄型化时的退磁场所致的去磁的高保磁力HcJ(以下简称为“HcJ”)的烧结铁氧体磁铁。
但是目前铁氧体的成型多采用干压法：将铁氧体粉末与一定的粘结剂等有机物按照一定的配比混合均匀，经过初步的过筛造粒后，在模具中施加一定压力干压成所需形状，然后再进行排胶烧结，进而测试磁性能。
干压方法的压制过程经常会出现层裂、变形等现象。如果模具设计和压型方式不合理，将造成烧结产品超出公差，严重影响产品的成品率和生产效率。除此之外，干压成型还具有结构单一、尺寸不易控制、产品成分起伏大、生产效率低、不适于批量生产、不能生产大型薄板等缺点，不能满足现代化生产中各种尺寸和形状胚体制作的需要，且质量不能保证。
因此，需要寻找一种新的铁氧体磁铁的制备方法来克服上述缺陷。
发明内容
本发明提供了一种铁氧体陶瓷的制备方法，其解决了现有干压法制备铁氧体的压制过程中经常会出现的层裂、变形等现象，容易造成烧结出的产品超出公差，从而严重影响产品的成品率和生产效率的技术问题，以及干压成型还具有结构单一、尺寸不易控制、产品成分起伏大、生产效率低、不适于批量生产、不能生产大型薄板等缺点，不能满足现代化生产中各种尺寸和形状胚体制作的需要，且质量不能保证。
本发明提供一种铁氧体陶瓷的制备方法，该方法包括如下步骤：配料：提供铁氧体粉末；烘干：将上述铁氧体粉末烘干；制浆：向上述烘干后的铁氧体粉末中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成浆料；除泡：除去浆料中的气泡；流延：将除气泡后的浆料在流延机上流延以产生陶瓷膜带；裁切：将上述陶瓷膜带裁切成所需尺寸的生坯；排胶：在300-500℃保温5h以上以去除上述生坯中的有机物；烧结：在900-1000℃保温2-5h烧制上述排胶后的生坯以产生致密的铁氧体陶瓷。
优选的，在配料步骤中，通过原料控制使得所述铁氧体粉末的中心粒径在0.5-3.5μm。
优选的，在烘干步骤中，所述铁氧体粉末烘干至含水率在0.1%以下。
优选的，所述除泡步骤中，通过抽真空并加热的方式去除浆料中的气泡。
相较于相关技术，本发明提供的铁氧体陶瓷的制备方法，可制备单向或复相陶瓷薄片材料，缺陷尺寸小，产品成分起伏小，性能稳定，生产效率高，可连续操作，可大批量生产，适合工业生产，适于成型大型薄片，厚度控制精度高，浆料配比可调等优点，满足了铁氧体基片小型化、高性能化、多功能化的发展趋势。
附图说明
为了更清楚地说明本发明实施例中的技术方案，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它的附图，其中：
图1是本发明流延后的生坯的表面显微形貌；
图2是流延后的生坯的热重和差热谱图；
图3是铁氧体陶瓷的表面显微形貌；
图4是铁氧体陶瓷的磁导率频谱。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，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它实施例，都属于本发明保护的范围。
本发明为了克服背景技术中关于目前铁氧体采用的干压法所存在的技术缺陷，而提供了一种铁氧体陶瓷的制备方法，该方法包括如下步骤：
S1，配料：提供铁氧体粉末，该铁氧体粉末需要通过原料控制使得中心粒径在0.5-3.5μm，并且具有较为集中的粒度分布。
S2，烘干：将上述铁氧体粉末烘干，从而使得所述铁氧体粉末的含水率在0.1%以下。
S3，制浆：向上述烘干后的铁氧体粉末中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成浆料；
其中，所述制浆所加入的粘结剂、增塑剂、分散剂、溶剂如下表1所示。
表1
Figure BDA0000399432770000031
其中，所述分散剂用于控制浆料的PH和颗粒表面电荷，提供颗粒之间的位阻，分散凝聚的颗粒。主要通过以下两种方式起作用：1.离子分散剂在颗粒表面形成扩散双电层，增加颗粒间的静电排斥作用；2.非离子分散剂通过氢键或范德华力吸附在粉料表面，其亲油链溶解在有机溶剂中，形成空间位阻作用，阻止粉料颗粒间的聚沉。
所述增塑剂用于使浆料具有流变性，赋予坯件一定的可塑性和柔软性，并降低粘结剂在室温和较低温度时的玻璃化转变温度。增塑剂的质量要求包括：与树脂粘结剂有良好的兼容性；高的可塑效率；沸点高，蒸气压低；对热、光和化学物质的稳定性；在低温下有极好的柔软性；与其他物质接触时不易迁移。
所述粘结剂用于增加成型性并赋予坯件一定的强度。其中PVB1的分子量为5-7万，PVB2的分子量为10-12万。粘结剂的分子量越大，则粘结强度就越大，与此同时溶解度越小。
S4，除泡：除去浆料中的气泡，在本发明优选的实施方式中，采用抽真空并加热的方式去除浆料中的气泡，从而使粘度控制在规定的范围内。
S5，流延：将除气泡后的浆料在流延机上流延以产生陶瓷膜带。通过控制浆料粘度、流延刀锋间隙、载送带运行速度和浆罐中的液面高度等来控制陶瓷膜带的厚度。在流延过程中，溶剂不断挥发，粘结剂则自身固化成三维网络结构防止陶瓷膜带中的颗粒沉降，并赋予陶瓷膜带一定的强度。
S6，裁切：将上述陶瓷膜带裁切成所需尺寸的生坯。
S7，排胶：在300-500℃保温5h以上以去除上述生坯中的有机物，在空气中加热时，由于空气中氧的存在，部分聚合物先氧化，生成过氧化氢基团和羰基基团等氧化物，分子量降低。接着，当温度接近所产生的氧化物的沸点时，它们就会挥发，质量减小。在排胶时一定要保证氧气的充足，否则有机物分解不彻底，在烧结后依然会有残留，进而影响性能。
S8，烧结：在900-1000℃保温2-5h烧制上述排胶后的生坯以产生致密的铁氧体陶瓷。
之后，对烧结得到的铁氧体陶瓷按照国标进行测量以得到该铁氧体陶瓷的磁性能。
如表2所示，为了详细的用实验数据对本发明进行说明，本发明提供了配方举例，以便进行性能对比。
表2
Figure BDA0000399432770000051
由图1所示，由上述举例配比制成的流延后的生坯的表面显微形貌可以看出，与浆料配方a相比，b的陶瓷颗粒与有机物分散更均匀，且无团聚。
由图2所示的流延后的生坯的热重和差热图谱，描述了生坯样品的质量和热流随温度的变化。在热重曲线上，当加热温度处于150-400℃时，流延膜片的质量一直在减少，这是由于样品内部有机物的挥发或分解所致，当温度超过400℃，流延膜片的质量变化较小。在150-200℃左右有一个较大幅度的失重，这是对应的增塑剂的挥发和热分解；在250-300℃对应的较大幅度的失重对应于粘结剂的挥发分解，350-400℃的失重则主要是分散剂所致。
由图3所示的烧结后的铁氧体陶瓷的表面显微形貌可以看出，在同样的排胶和烧结条件下，与浆料配方a相比，b的陶瓷由于两种粘接剂的分段挥发，气孔更小，致密性更好。
最后，由图4所示的烧结后的铁氧体陶瓷的磁导率频谱可以看出，与浆料配方a相比，b拥有更高的μ’和更低的μ”，即拥有更好的磁性能。
相较于相关技术，本发明提供的铁氧体陶瓷的制备方法，可制备单向或复相陶瓷薄片材料，缺陷尺寸小，产品成分起伏小，性能稳定，生产效率高，可连续操作，可大批量生产，适合工业生产，适于成型大型薄片，厚度控制精度高，浆料配比可调等优点，满足了铁氧体基片小型化、高性能化、多功能化的发展趋势。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换，或直接或间接运用在其它相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (4)

1.一种铁氧体陶瓷的制备方法，其特征在于，该方法包括如下步骤：
配料：提供铁氧体粉末；
烘干：将上述铁氧体粉末烘干；
制浆：向上述烘干后的铁氧体粉末中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成浆料；
除泡：除去浆料中的气泡；
流延：将除气泡后的浆料在流延机上流延以产生陶瓷膜带；
裁切：将上述陶瓷膜带裁切成所需尺寸的生坯；
排胶：在300-500℃保温5h以上以去除上述生坯中的有机物；
烧结：在900-1000℃保温2-5h烧制上述排胶后的生坯以产生致密的铁氧体陶瓷。
2.根据权利要求1所述的铁氧体陶瓷的制备方法，其特征在于，在配料步骤中，通过原料控制使得所述铁氧体粉末的中心粒径在0.5-3.5μm。
3.根据权利要求1所述的铁氧体陶瓷的制备方法，其特征在于，在烘干步骤中，所述铁氧体粉末烘干至含水率在0.1%以下。
4.根据权利要求1所述的铁氧体陶瓷的制备方法，其特征在于，所述除泡步骤中，通过抽真空并加热的方式去除浆料中的气泡。
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