CN112430102A - 一种铁氧体颗粒料及其制备方法 - Google Patents

一种铁氧体颗粒料及其制备方法 Download PDF

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CN112430102A
CN112430102A CN202011423481.9A CN202011423481A CN112430102A CN 112430102 A CN112430102 A CN 112430102A CN 202011423481 A CN202011423481 A CN 202011423481A CN 112430102 A CN112430102 A CN 112430102A
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plasticizer
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黄爱萍
陈健光
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A-CORE JIANGMEN ELECTRONICS CO LTD
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Abstract

本发明涉及一种铁氧体颗粒料及其制备方法，所述颗粒料由主成分、辅助成分、粘结剂、增塑剂和水制备而成，其中主成分包括Fe2O3以及Mn3O4、ZnO、NiO、CuO的一种或多种，辅助成分包括SiO2、CaCO3、V2O5、Nb2O5、ZrO2、TiO2、SnO2、Co2O3、NiO、Bi2O3、MoO3、Fe2O3、Mn3O4的一种或多种，粘结剂为聚乙烯醇，增塑剂选自甘油或聚乙二醇的一种；其中，粘结剂占主成分的1.0‑2.0wt％；增塑剂占主成分的0.5‑1.0wt％。本发明所述的铁氧体颗粒料及其制备方法对颗粒料的压缩性和成形性具有显著的改善和优化效果。

Description

一种铁氧体颗粒料及其制备方法
技术领域
本发明涉及铁氧颗粒材料领域，具体地涉及一种铁氧体颗粒料及其制备方法。
背景技术
磁性材料作为电子领域中不可缺少的功能材料，其产量和生产技术水平已成为衡量一个国家信息产业发展的标志之一。其中软磁铁氧体是品种最多、应用最广、用量最大的一种磁性材料，在软磁铁氧体生产和使用中占主导地位的是MnZn铁氧体，MnZn铁氧体的产量约占软磁铁氧体总产量的70％，是目前软磁材料中最受关注和最为活跃的领域。
随着电子产品整机向轻、薄、小型化方向发展，对电子元器件也同样提出了小型化的要求。锰锌软磁铁氧体磁芯产品的形状也向体积小型化、结构扁平化和形状复杂化的方向转变发展，以适应电子整机产品的小、薄化要求，且此类产品的需求量越来越大，已成为市场的主流需求产品。传统方法生产的软磁铁氧体粉料在用作压制这些小型化、扁平化和复杂化磁芯产品的过程中，会出现成型坯体分层、开裂和破损等问题，导致压制困难、合格率低。因此必须对粉料进行改性，提高粉料的可压制性，进而提高这类新磁芯产品的合格率。锰锌软磁粉料在压制过程中成型的难易程度，通常与粉体的粘结剂含量、含水量、颗粒分布、松装密度、流动角以及颗粒形状等指标密切相关。
目前市场上的产品中，几种常见的颗粒料加胶量在0.75-0.90wt％之间，喷雾造粒塔进风温度为300-380℃。这几种颗粒料的缺陷在于：用于复杂形状成型时都出现了疏松、粘模、起层、开裂等不良，压制产品良率低的情况。这是因为，这几种颗粒料的加胶量偏低、未添加增塑剂、进风温度为300-380℃，明显高于粘结剂PVA胶粒开始大量分解的温度(约260℃左右)，由于热风温度过高，料浆雾滴与高温热风接触时表面迅速生成一层硬壳，表面粘结剂部分分解，实际粘结剂存留量更少，粉料之间的粘结性减弱，颗粒料的压缩性和成形性变差。
因此，亟需找到一种新型颗粒材料及其制备方法，来克服现有技术中存在的问题。
发明内容
本发明依据粘结剂的热分解温度，设置喷雾造粒的进风温度(230-250℃)，从而避免进风温度过高，导致粘结剂分解和表面硬壳的产生；同时适当增加粘结剂添加比例，并添加合适比例的增塑剂，改善了颗粒料的压缩性和成形性。
本发明的一个目的在于提供一种铁氧体颗粒料，其由主成分、辅助成分、粘结剂、增塑剂和水制备而成；
其中，所述主成分包括Fe2O3；
还包括Mn3O4、ZnO、NiO、CuO的一种或多种；
所述辅助成分包括SiO2、CaCO3、V2O5、Nb2O5、ZrO2、TiO2、SnO2、Co2O3、NiO、Bi2O3、MoO3、Fe2O3、Mn3O4的一种或多种；
其中，粘结剂占主成分的1.0-2.0wt％；
增塑剂占主成分的0.5-1.0wt％。
进一步地，所述粘结剂为聚乙烯醇。
进一步地，所述增塑剂选自甘油或聚乙二醇的一种。
本发明的另一个目的，在于提供上述铁氧体颗粒料的制备方法，包括如下步骤：
S1.将主成分和水混合得到料浆；
S2.将上述料浆喷雾干燥，得到颗粒；
S3.将上述颗粒煅烧，得到预烧料；
S4.将预烧料和辅助成分与水共混并研磨，得到粉体料浆；
S5.将粉体料浆、粘结剂和增塑剂混合，喷雾造粒，得到颗粒料；其中所述喷雾造粒的进风温度为230-250℃。
进一步地，步骤S4中，所述粉体的粒径为1-2μm。
进一步地，步骤S5中，所述粘结剂的浓度为8-10wt％。
本发明的有益效果在于：
现有市面上的颗粒料未添加增塑剂，粘结剂添加比例低，并且进风温度为300-380℃，明显高于粘结剂开始大量分解的温度约260℃左右，由于热风温度过高，料浆雾滴与高温热风接触时表面迅速生成一层硬壳，表面粘结剂部分分解，实际粘结剂存留量更少，粉料之间的粘结性减弱，颗粒料的压缩性和成形性变差；本发明依据粘结剂的热分解温度，设置喷雾造粒的进风温度(230-250℃)，从而避免进风温度过高，导致粘结剂分解和表面硬壳的产生；同时适当地增加了增塑剂，改善了颗粒料的压缩性和成形性。
附图说明
图1分别是实施例1-3中，粘结剂117、粘结剂1799和粘结剂217SB的热失重曲线。
具体实施方式
为更好地理解本发明，下面结合实施例对本发明作进一步的说明。但本发明所要求的保护范围并不局限于本发明实施例所涉及的范围。除非特别提及，否则本专利公开的实施例中所提及的成分和测试方法均为本领域技术人员所知的常规方法。
实施例1
一种铁氧体颗粒料，由主成分、辅助成分、粘结剂聚乙烯醇(采购自可乐丽；型号为：117)、增塑剂甘油和水制备而成。
其中，按质量份数计，主成分包括：
Fe2O3 70份
Mn3O4 23份
ZnO 7份；
按质量份数计，辅助成分包括：
Figure BDA0002823609750000031
其中，粘结剂聚乙烯醇的质量为主成分的1.0wt％；
增塑剂甘油的质量为主成分的0.5wt％。
上述铁氧体颗粒料的制备方法包括如下步骤：
S1.将主成分和水(主成分：水的质量比为1：1)混合得到料浆；
S2.将上述料浆喷雾干燥，得到干燥颗粒，其中喷雾干燥的进风温度为300℃；
S3.将上述干燥颗粒在900℃的回转窑中煅烧，并保温0.5h，然后自然降温得到预烧料；
S4.将预烧料和按上述质量份数的辅助成分，与水共混(预烧料：水的质量比：2:1)并通过球磨机研磨，得到粒径为1.2μm的粉体料浆；
S5.将粉体料浆、粘结剂聚乙烯醇(浓度为8wt％)和增塑剂甘油混合，喷雾造粒，得到颗粒料；其中所述喷雾造粒的进风温度为250℃。
实施例2
一种铁氧体颗粒料，由主成分、辅助成分、粘结剂聚乙烯醇(采购自皖维；型号为：1799)、增塑剂聚乙二醇和水制备而成。
其中，按质量份数计，主成分包括：
Fe2O3 68份
Mn3O4 17份
ZnO 15份；
按质量份数计，辅助成分包括：
Figure BDA0002823609750000041
其中，粘结剂聚乙烯醇的质量为主成分的2.0wt％；
增塑剂甘油的质量为主成分的1.0wt％。
上述铁氧体颗粒料的制备方法包括如下步骤：
S1.将主成分和水(主成分：水的质量比为1：1)混合得到料浆；
S2.将上述料浆喷雾干燥，得到干燥颗粒，其中喷雾干燥的进风温度为400℃；
S3.将上述干燥颗粒在700℃的回转窑中煅烧，并保温1h，然后自然降温得到预烧料；
S4.将预烧料和按上述质量份数的辅助成分，与水共混(预烧料：水的质量比：2:1)并通过球磨机研磨，得到粒径为1.0μm的粉体料浆；
S5.将粉体料浆、粘结剂聚乙烯醇(浓度为10wt％)和增塑剂聚乙二醇混合，喷雾造粒，得到颗粒料；其中所述喷雾造粒的进风温度为240℃。
实施例3
一种铁氧体颗粒料，由主成分、辅助成分、粘结剂聚乙烯醇(采购自可乐丽；型号为：217SB)、增塑剂甘油和水制备而成。
其中，按质量份数计，主成分包括：
Figure BDA0002823609750000051
按质量份数计，辅助成分包括：
Figure BDA0002823609750000052
其中，粘结剂聚乙烯醇的质量为主成分的1.5wt％；
增塑剂甘油的质量为主成分的0.8wt％。
上述铁氧体颗粒料的制备方法包括如下步骤：
S1.将主成分和水(主成分：水的质量比为1：1)混合得到料浆；
S2.将上述料浆喷雾干燥，得到干燥颗粒，其中喷雾干燥的进风温度为350℃；
S3.将上述干燥颗粒在1000℃的回转窑中煅烧，并保温0.8h，然后自然降温得到预烧料；
S4.将预烧料和按上述质量份数的辅助成分，与水共混(预烧料：水的质量比：2:1)并通过球磨机研磨，得到粒径为2μm的粉体料浆；
S5.将粉体料浆、粘结剂聚乙烯醇(浓度为9wt％)和增塑剂甘油混合，喷雾造粒，得到颗粒料；其中所述喷雾造粒的进风温度为230℃。
实施例4
实施例4与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例4中粘结剂117以型号为217SB进行等质量的替换。
实施例5
实施例5与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例5中粘结剂117以117：217SB＝1：1进行等质量的替换。
实施例6
实施例6与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例6中增塑剂甘油以等质量的聚乙二醇替换。
对比例1
实施例4与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例4中粘结剂的质量为主成分的0.8wt％。
对比例2
实施例5与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例5中粘结剂的质量为主成分的2.5wt％。
对比例3
实施例6与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例6中增塑剂的质量为主成分的0.2wt％。
对比例4
实施例7与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于实施例7中增塑剂的质量为主成分的1.5wt％。
对比例5
对比例1与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于对比例5中不含增塑剂。
对比例6
对比例2与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于对比例6中，步骤S5中，进风温度为210℃。
对比例7
对比例3与实施例1的原料成分、原料质量份数和制备方法均相同，唯一不同在于对比例7中，步骤S5中，进风温度为280℃。
测试例
图1分别是实施例1-3中，所述粘结剂117、粘结剂1799和粘结剂217SB的热失重曲线，可以看出，三种粘结剂开始大量热分解的温度都在260℃左右。
对上述实施例1-6和对比例1-7所制得的铁氧体颗粒料，进行压缩性和成形性的评价。
参照粉末压制曲线的公式：r＝bpa：
其中，r为压坯密度(g/cm3)；p为压制压力(MPa)；a为常数；b是压缩常数，表示粉末压缩性能好坏的参数之一。
采用压缩常数b，来判定铁氧体颗粒料的压缩性；采用压坯强度来判定铁氧体颗粒料的成形性。
压缩常数b和压坯强度的测试方法如下：
S1.检验员在粉料上机前抽取500g待用粉料，核对并记录粉料信息：批次、松比、水分、流动性、润滑剂、粒度分布；
S2.检验员启动试验压机，调整压制参数：
S2.1进入主页输入成型力设置数值aT，其余保持不变；
S2.2进入参数设定(一)界面，主缸慢下设定a+1，主缸慢压设定a+b，浮动压制设定a+b，其余保持不变，返回主页(主缸慢下设定要比成型力设置大于1即可，主缸慢压和浮动压制要设定一致，否则故障，根据成型力大小调整b值，b值设定范围在0-2)；
S3.参数设置后，运行方式选择单次，把模具复位后(运行指示灯和允许自动灯同时亮起)，同时按下自动启动1和自动启动2即可压制；
S4.主页显示成型力数值为实际压力输出值a+cT,单位换算为1MPa＝0.8T(c值范围一般在0-1，通过调整b值可以实际获得目标压力：成型力a+c值)；
S5.用8MPa、10MPa、12MPa三种压力分别成形方块各10pcs，要求粉重8.5±0.3g，高度为17±1mm；
S6.分别测量三组不同压力压制的产品尺寸、质量，计算压坯密度，最后计算压缩常数b，试验误差超过±1％，须重新试验；
S7.压缩常数合格后，将压坯送到检测室沿高度方向测试压坯I强度，采用一字压头、跨度27mm、下压速度：20mm/min。
最后将所得颗粒料用于压制复杂形状产品，评价成型效果，不良率低于0.5％为良好，单项不良率超过1％记录不良项目。
所得结果如表1所示。
表1实施例1-6与对比例1-7的压缩常数b和压坯强度的值
Figure BDA0002823609750000071
Figure BDA0002823609750000081
表1的实施例1-6，压缩常数b大于2.30，压坯强度大于3.5MPa，铁氧体颗粒料的成型效果良好。
在对比例1-2中的粘结剂用量的设定可以看出，其中对比例1的粘结剂用量过低，导致粉末之间的粘结性不足，压制生产过程中易出现起层开裂不良；对比例2的粘结剂用量过高，导致压制生产过程中粘模现象频发，且进一步烧结时还易出现因排胶不充分导致的排胶开裂。
在对比例3-5中的增塑剂用量的设定可以看出，其中对比例3、5的增塑剂用量过低，使得粘结剂的塑性不足，压制生产过程中易出现起层开裂不良；对比例4的增塑剂用量过高，使得压制生产过程中粘模现象频发。
在对比例6-7中，进风温度的设定可以看出，其中对比例6的进风温度过低，导致干燥效率低颗粒料水分高粘结剂的塑性不足，压制生产过程中粘模现象频发；对比例7的进风温度过高，会导致粘结剂分解和表面硬壳的产生，压制生产过程中易出现起层开裂不良。
上述数据表明了本发明技术方案相对于对比例的先进性。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。

Claims (6)

1.一种铁氧体颗粒料，其特征在于，由主成分、辅助成分、粘结剂、增塑剂和水制备而成；
其中，所述主成分包括Fe2O3；
还包括Mn3O4、ZnO、NiO、CuO的一种或多种；
所述辅助成分包括SiO2、CaCO3、V2O5、Nb2O5、ZrO2、TiO2、SnO2、Co2O3、NiO、Bi2O3、MoO3、Fe2O3、Mn3O4的一种或多种；
其中，粘结剂占主成分的1.0-2.0wt％；
增塑剂占主成分的0.5-1.0wt％。
2.根据权利要求1所述铁氧体颗粒料，其特征在于，所述粘结剂为聚乙烯醇。
3.根据权利要求1所述铁氧体颗粒料，其特征在于，所述增塑剂选自甘油或聚乙二醇的一种。
4.根据权利要求1-3任一项所述铁氧体颗粒料的制备方法，其特征在于，包括如下步骤：
S1.将主成分和水混合得到料浆；
S2.将上述料浆喷雾干燥，得到颗粒；
S3.将上述颗粒煅烧，得到预烧料；
S4.将预烧料和辅助成分与水共混并研磨，得到粉体料浆；
S5.将粉体料浆、粘结剂和增塑剂混合，喷雾造粒，得到颗粒料；其中所述喷雾造粒的进风温度为230-250℃。
5.根据权利要求4所述铁氧体颗粒料的制备方法，其特征在于，步骤S4中，所述粉体的粒径为1-2μm。
6.根据权利要求4所述铁氧体颗粒料的制备方法，其特征在于，步骤S5中，所述粘结剂的浓度为8-10wt％。
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