CN107324791B - 一种提高磁瓦机械强度的加工方法 - Google Patents

一种提高磁瓦机械强度的加工方法 Download PDF

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CN107324791B
CN107324791B CN201710349502.9A CN201710349502A CN107324791B CN 107324791 B CN107324791 B CN 107324791B CN 201710349502 A CN201710349502 A CN 201710349502A CN 107324791 B CN107324791 B CN 107324791B
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CN107324791A (zh
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周国胜
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Maanshan Qijin Magnet Co ltd
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Abstract

本发明属于永磁铁氧体磁瓦加工技术领域，具体涉及一种提高磁瓦机械强度的加工方法，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品。本发明相比现有技术具有以下优点：本发明中通过对不同性质的原料分别混合后预烧结，控制相应的球磨工艺和烧结参数，形成相应的晶体微结构，有助于形成活性络合物，使激活能降低，烧结后所得磁瓦密度达到5.4g/cm³以上，机械强度和抗拉强度都达到较高水平，磁瓦的取向度达到98.6%以上，磁瓦在具有高剩余磁感应强度的同时，又具有较高的内禀矫顽力，综合机械性能明显提高。

Description

一种提高磁瓦机械强度的加工方法
技术领域
本发明属于永磁铁氧体磁瓦加工技术领域，具体涉及一种提高磁瓦机械强度的加工方法。
背景技术
磁瓦作为铁氧体烧结磁体的一个重要组成部分，由于其广泛应用于电机领域，有着优越的市场前景，加上近几年国内外在扬声器磁环和磁块上的过度恶性竞争，使得铁氧体烧结磁环和磁块的生存越来越困难，所以磁瓦被国内铁氧体磁性材料行业一直看好，单由于其生产技术上明显高于磁环和磁块，对生产设备和模具的要求也相对较高，因而原来许多生产磁环的厂家对生产磁瓦力不从心，在磨加工时，材料的机械强度、收缩率通常受到原料、添加剂、生产工艺条件变化的影响，导致磁瓦烧结后应力集中，容易出现破损现象，造成材料浪费，延长生产周期，因此，需要对如何制备机械强度良好的磁瓦进行进一步研究和改进。
发明内容
本发明的目的是针对现有的问题，提供了一种提高磁瓦机械强度的加工方法。
本发明是通过以下技术方案实现的：一种提高磁瓦机械强度的加工方法，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品，具体包括以下内容：
（1）制备预烧料A：将Fe2O3、Sr2O3、ZrO2、WO3、V2O5按重量比147-150:14-15:1-2:1-2:0.5-1混合，用球磨机混合，料：球：水的重量比为1:10:2混合，球径为6mm，转速为380转/分钟，球磨4-6小时，然后在空气中进行预烧，预烧温度为1300-1400℃，保温时间为1.5-2.5小时，粗磨后再细磨，得到粒径为60-300nm的粉末，即为预烧料A；
（2）制备预烧料B：将Fe2O3、Sr2O3、GeO2、In2O3、β-Ga2O3按重量比165-168:16-17:2-3:1-2:1-2混合，用球磨机混合，料：球：丙酮的重量比为1:8:0.8混合，球径为10mm，转速为240转/分钟，球磨22-25小时，然后在空气中进行预烧，预烧温度为950-1050℃，保温时间为3.5-4小时，粗磨后再细磨，得到粒径为200-800nm的粉末，即为预烧料B；
（3）与配料混合及球磨：将预烧料A和预烧料B混合后加入相当于其总重量4-6%芳纶微米短纤维、1-3%的纤维状羟基磷灰石，装入振磨机中，粉碎1.5-2小时出料；
（4）压制生坯：使用全径向充磁干压成型方式压制，其中上、下模冲、阴模为无磁钢，芯杆及垫铁为导磁材料的45#钢，在阴模内壁中部区域的磁场强度达到0.08T、在芯杆中部区域的磁场强度达到0.1T；
（5）烧结：生坯在1220-1260℃的温度下烧结，烧结时间为2.5-3小时，推进速度为13-17min/板，保温时间为1.5小时。
作为对上述方案的进一步改进，所述纤维状羟基磷灰石的纤维状晶体的长度为80-120μm、线宽度为22-26μm。
作为对上述方案的进一步改进，所述步骤（3）中球磨后出料粒径小于1μm。
作为对上述方案的进一步改进，所述生坯密度为3.4-3.6g/cm³。
作为对上述方案的进一步改进，所述铁红理化指标为Fe2O3≥99.0%、SiO2＜0.1%、氯离子小于0.4%，粒径＜800nm；所述碳酸锶理化指标为Sr2O3≥98%、BaCO3＜0.8%、CaCO3＜0.6%、盐酸不溶物＜0.1%，粒径＜1μm。
本发明相比现有技术具有以下优点：本发明中通过对不同性质的原料分别混合后预烧结，控制相应的球磨工艺和烧结参数，形成相应的晶体微结构，提高饱和的磁化强度和磁晶各项异性常数，有助于磁瓦内部组织更加致密化，在与配料混合及球磨过程中不加弥散剂，而加入芳纶微米短纤维和纤维状羟基磷灰石，有助于形成活性络合物，使激活能降低，部分晶格点阵畸变、熔点降低，成为反应中心，在适当的温度下形成新的结晶中心，有助于晶粒成长，使预烧料A和预烧料B的固相反应加速进行，再次烧结时可以省去湿混需要烘干、磨细的操作步骤，烧结后所得磁瓦密度达到5.4g/cm³以上，机械强度和抗拉强度都达到较高水平，磁瓦的取向度达到98.6%以上，磁瓦在具有高剩余磁感应强度的同时，又具有较高的内禀矫顽力，综合机械性能明显提高。
具体实施方式
实施例1
一种提高磁瓦机械强度的加工方法，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品，具体包括以下内容：
（1）制备预烧料A：将Fe2O3、Sr2O3、ZrO2、WO3、V2O5按重量比148:15:1.6:1.4:0.8混合，用球磨机混合，料：球：水的重量比为1:10:2混合，球径为6mm，转速为380转/分钟，球磨4-6小时，然后在空气中进行预烧，预烧温度为1300-1400℃，保温时间为1.5-2.5小时，粗磨后再细磨，得到粒径为60-300nm的粉末，即为预烧料A；
所述铁红理化指标为Fe2O3≥99.0%、SiO2＜0.1%、氯离子小于0.4%，粒径＜800nm；所述碳酸锶理化指标为Sr2O3≥98%、BaCO3＜0.8%、CaCO3＜0.6%、盐酸不溶物＜0.1%，粒径＜1μm；
（2）制备预烧料B：将Fe2O3、Sr2O3、GeO2、In2O3、β-Ga2O3按重量比165:17:2.5:1.5:1.5混合，用球磨机混合，料：球：丙酮的重量比为1:8:0.8混合，球径为10mm，转速为240转/分钟，球磨22-25小时，然后在空气中进行预烧，预烧温度为950-1050℃，保温时间为3.5-4小时，粗磨后再细磨，得到粒径为200-800nm的粉末，即为预烧料B；
（3）与配料混合及球磨：将预烧料A和预烧料B混合后加入相当于其总重量5%芳纶微米短纤维、2%的纤维状羟基磷灰石，装入振磨机中，粉碎1.5-2小时出料，出料粒径小于1μm；
（4）压制生坯：使用全径向充磁干压成型方式压制，其中上、下模冲、阴模为无磁钢，芯杆及垫铁为导磁材料的45#钢，在阴模内壁中部区域的磁场强度达到0.08T、在芯杆中部区域的磁场强度达到0.1T；
（5）烧结：生坯在1220-1260℃的温度下烧结，烧结时间为2.5小时，推进速度为13min/板，保温时间为1.5小时。
其中，所述纤维状羟基磷灰石的纤维状晶体的长度为80-120μm、线宽度为22-26μm。
经检测，所述生坯密度为3.52g/cm³，烧结后磁瓦密度达到5.47g/cm³。
实施例2
一种提高磁瓦机械强度的加工方法，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品，具体包括以下内容：
（1）制备预烧料A：将Fe2O3、Sr2O3、ZrO2、WO3、V2O5按重量比147:15:2:1:1混合，用球磨机混合，料：球：水的重量比为1:10:2混合，球径为6mm，转速为380转/分钟，球磨4-6小时，然后在空气中进行预烧，预烧温度为1300-1400℃，保温时间为1.5-2.5小时，粗磨后再细磨，得到粒径为60-300nm的粉末，即为预烧料A；
所述铁红理化指标为Fe2O3≥99.0%、SiO2＜0.1%、氯离子小于0.4%，粒径＜800nm；所述碳酸锶理化指标为Sr2O3≥98%、BaCO3＜0.8%、CaCO3＜0.6%、盐酸不溶物＜0.1%，粒径＜1μm；
（2）制备预烧料B：将Fe2O3、Sr2O3、GeO2、In2O3、β-Ga2O3按重量比168:16:3:1:1混合，用球磨机混合，料：球：丙酮的重量比为1:8:0.8混合，球径为10mm，转速为240转/分钟，球磨22-25小时，然后在空气中进行预烧，预烧温度为950-1050℃，保温时间为3.5-4小时，粗磨后再细磨，得到粒径为200-800nm的粉末，即为预烧料B；
（3）与配料混合及球磨：将预烧料A和预烧料B混合后加入相当于其总重量6%芳纶微米短纤维、1%的纤维状羟基磷灰石，装入振磨机中，粉碎1.5-2小时出料，出料粒径小于1μm；
（4）压制生坯：使用全径向充磁干压成型方式压制，其中上、下模冲、阴模为无磁钢，芯杆及垫铁为导磁材料的45#钢，在阴模内壁中部区域的磁场强度达到0.08T、在芯杆中部区域的磁场强度达到0.1T；
（5）烧结：生坯在1220-1260℃的温度下烧结，烧结时间为3小时，推进速度为17min/板，保温时间为1.5小时。
其中，所述纤维状羟基磷灰石的纤维状晶体的长度为80-120μm、线宽度为22-26μm。
经检测，所述生坯密度为3.53g/cm³，烧结后磁瓦密度达到5.46g/cm³。
实施例3
一种提高磁瓦机械强度的加工方法，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品，具体包括以下内容：
（1）制备预烧料A：将Fe2O3、Sr2O3、ZrO2、WO3、V2O5按重量比150:14:2:2:0.5混合，用球磨机混合，料：球：水的重量比为1:10:2混合，球径为6mm，转速为380转/分钟，球磨4-6小时，然后在空气中进行预烧，预烧温度为1300-1400℃，保温时间为1.5-2.5小时，粗磨后再细磨，得到粒径为60-300nm的粉末，即为预烧料A；
所述铁红理化指标为Fe2O3≥99.0%、SiO2＜0.1%、氯离子小于0.4%，粒径＜800nm；所述碳酸锶理化指标为Sr2O3≥98%、BaCO3＜0.8%、CaCO3＜0.6%、盐酸不溶物＜0.1%，粒径＜1μm；
（2）制备预烧料B：将Fe2O3、Sr2O3、GeO2、In2O3、β-Ga2O3按重量比165:17:2:1:2混合，用球磨机混合，料：球：丙酮的重量比为1:8:0.8混合，球径为10mm，转速为240转/分钟，球磨22-25小时，然后在空气中进行预烧，预烧温度为950-1050℃，保温时间为3.5-4小时，粗磨后再细磨，得到粒径为200-800nm的粉末，即为预烧料B；
（3）与配料混合及球磨：将预烧料A和预烧料B混合后加入相当于其总重量4%芳纶微米短纤维、3%的纤维状羟基磷灰石，装入振磨机中，粉碎2小时出料，出料粒径小于1μm；
（4）压制生坯：使用全径向充磁干压成型方式压制，其中上、下模冲、阴模为无磁钢，芯杆及垫铁为导磁材料的45#钢，在阴模内壁中部区域的磁场强度达到0.08T、在芯杆中部区域的磁场强度达到0.1T；
（5）烧结：生坯在1220-1260℃的温度下烧结，烧结时间为2.5小时，推进速度为15min/板，保温时间为1.5小时。
其中，所述纤维状羟基磷灰石的纤维状晶体的长度为80-120μm、线宽度为22-26μm。
经检测，所述生坯密度为3.56g/cm³，烧结后磁瓦密度达到5.51g/cm³。
设置对照组1，将预烧料A按照预烧料B的方法制备，步骤（2）-（5）与实施例1中相同；设置对照组2，将预烧料倍B按照预烧料A的方法制备，步骤（2）-（5）与实施例1中相同；设置对照组3，将实施例1中所述步骤（3）替换为常规的湿混方式，以适量水为弥散剂，相应的压制生坯按照现有技术进行相应改变，其余内容不变；
对上述各组制得的磁瓦成品进行检测，由信息产业部磁性产品质量监督检验中心检验，所得检测结果如下：
表1
检测项目 实施例1 实施例2 实施例3 对照组1 对照组2 对照组3
Br（mT） 436 439 437 428 435 432
Hcb（kA/m） 317 315 317 312 316 318
Hcj（kA/m） 401 399 400 394 393 392
（BH）max（kJ/m³） 32.9 32.6 32.8 32.3 32 31.8
H（kA/m） 399 398 399 394 392 396
抗拉强度（MPa） 31.6 31.2 31.5 30.2 30.1 30.5
通过表1中数据可以看出，各个过程中配料的适当添加以及加工条件决定了生产产品的机械性能，本发明中生产的磁瓦机械强度较好，能适用于对磁瓦强度要求较高的领域。

Claims (4)

1.一种提高磁瓦机械强度的加工方法，其特征在于，制备预烧料A、预烧料B后与配料混合后球磨，在磁场中压制生坯，将生坯烧结成烧结磁体后，经磨加工、清洗、检测得到成品，具体包括以下内容：
（1）制备预烧料A：将Fe2O3、Sr2O3、ZrO2、WO3、V2O5按重量比147-150:14-15:1-2:1-2:0.5-1混合，用球磨机混合，料：球：水的重量比为1:10:2混合，球径为6mm，转速为380转/分钟，球磨4-6小时，然后在空气中进行预烧，预烧温度为1300-1400℃，保温时间为1.5-2.5小时，粗磨后再细磨，得到粒径为60-300nm的粉末，即为预烧料A；
（2）制备预烧料B：将Fe2O3、Sr2O3、GeO2、In2O3、β-Ga2O3按重量比165-168:16-17:2-3:1-2:1-2混合，用球磨机混合，料：球：丙酮的重量比为1:8:0.8混合，球径为10mm，转速为240转/分钟，球磨22-25小时，然后在空气中进行预烧，预烧温度为950-1050℃，保温时间为3.5-4小时，粗磨后再细磨，得到粒径为200-800nm的粉末，即为预烧料B；
（3）与配料混合及球磨：将预烧料A和预烧料B混合后加入相当于其总重量4-6%芳纶微米短纤维、1-3%的纤维状羟基磷灰石，装入振磨机中，粉碎1.5-2小时出料；
（4）压制生坯：使用全径向充磁干压成型方式压制，其中上、下模冲、阴模为无磁钢，芯杆及垫铁为导磁材料的45#钢，在阴模内壁中部区域的磁场强度达到0.08T、在芯杆中部区域的磁场强度达到0.1T；
（5）烧结：生坯在1220-1260℃的温度下烧结，烧结时间为2.5-3小时，推进速度为13-17min/板，保温时间为1.5小时。
2.如权利要求1所述一种提高磁瓦机械强度的加工方法，其特征在于，所述纤维状羟基磷灰石的纤维状晶体的长度为80-120μm、线宽度为22-26μm。
3.如权利要求1所述一种提高磁瓦机械强度的加工方法，其特征在于，所述步骤（3）中球磨后出料粒径小于1μm。
4.如权利要求1所述一种提高磁瓦机械强度的加工方法，其特征在于，所述生坯密度为3.4-3.6g/cm³。
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