CN109678485A - 一种具有较高强度的锰锌软磁铁氧体材料的制备方法 - Google Patents

一种具有较高强度的锰锌软磁铁氧体材料的制备方法 Download PDF

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CN109678485A
CN109678485A CN201811559264.5A CN201811559264A CN109678485A CN 109678485 A CN109678485 A CN 109678485A CN 201811559264 A CN201811559264 A CN 201811559264A CN 109678485 A CN109678485 A CN 109678485A
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strength
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周海波
张泂
沈军刚
刘浩松
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NANJING ZHONGDIAN PANDA MAGNET TECHNOLOGY Co Ltd
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Abstract

本发明涉及一种具有较高强度的锰锌软磁铁氧体材料的制备方法，包括以下步骤：按Fe2O3：MnO：ZnO摩尔比为(52.0‑55.0)：(34.5‑37.5)：(11.0‑13.0)配主料；取相当于主料0.004‑0.008wt％的ZrO2、0.015‑0.020wt％的CaCO3、0.003‑0.005wt％的SiO2、0.15‑0.20wt％的V2O5；主料混合一次球磨粉碎：将配好的主料加去离子水、胶合剂和分散剂充分进行球磨；主料预烧；主料、辅料混合与二次粉碎球磨；成型；烧结。本发明制造的磁心在同等条件下比普通材料制造的同种磁心的机械强度有较大提高，从而同时满足电气性能和机械强度的高要求。

Description

一种具有较高强度的锰锌软磁铁氧体材料的制备方法
技术领域
本发明涉及软磁铁氧体领域，具体涉及一种具有较高强度的锰锌软磁铁氧体材料的制备方法。
背景技术
锰锌软磁铁氧体属于软磁铁氧体中的一大类，目前被广泛用于滤波器、电感器、变压器、功率转换器等电子领域。在现今复杂的国际环境中，为了自主可控，国产电子元器件领域有着极大的国产化替代空间，由于航空、航天及高新电子的特殊、苛刻的应用环境，对于国产电子元器件要求具有高度稳定性的情况下，同时应具备较高的强度，作为基础元件的铁氧体磁心，较高强度也是不可忽视的基本特性，通过测试我们发现国产磁心普遍存在强度较低的现象，本发明就是在保证材料的电气性能较为稳定的基础上，使得用该种材料制造的磁心在同等条件下比普通材料制造的同种磁心的机械强度有较大的提高，从而同时满足特殊客户对于电气性能和机械强度的高要求。
发明内容
本发明的目的是针对现有技术的不足，提供一种具有较高强度的锰锌软磁铁氧体材料的制备方法，能够有效增加软磁铁氧体材料的强度，以满足特殊客户的需求。
为实现上述目的，本发明提供的技术方案是：
一种具有较高强度的锰锌软磁铁氧体材料的制备方法，包括以下步骤：
1)配主料：按Fe2O3：MnO：ZnO摩尔比为(52.0-55.0)：(34.5-37.5)：(11.0-13.0)配主料；
2)配辅料：取相当于主料0.004-0.008wt％的ZrO2、0.015-0.020wt％的CaCO3、0.003-0.005wt％的SiO2、0.15-0.20wt％的V2O5；
3)主料混合一次球磨粉碎：将步骤1)配好的主料加去离子水、胶合剂和分散剂充分进行球磨；
4)主料预烧：将步骤3)喷雾造粒的颗粒料进行预烧；
5)主料、辅料混合与二次粉碎球磨：将步骤4)预烧好的主料加入去离子水、胶合剂和分散剂进行球磨2-2.5小时，在球磨至1.5小时时加入步骤2)配好的辅料共同球磨至结束，喷雾造粒；
6)成型：将喷雾造粒颗粒料加入0.015％的硬脂酸锌后用混料机充分混合，然后压制毛坯；
7)烧结：将步骤6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以80-120℃/小时速率升温至800-850℃，保温1-1.5小时；在6.0-9.5％氧含量的氮气氛围中，以80-100℃/小时速率升温至1280-1320℃，烧结时间为3.5-4.0小时；烧结后在0.001-0.003％氧含量的氮气氛围中，按照100-130℃/小时降温即可得到具有较高强度的锰锌铁氧体磁心。
步骤3)球磨1-1.5小时，喷雾造粒制成40-180目的颗粒料。
步骤4)预烧温度为850-900℃，预烧时间为1-2小时。
步骤5)检测球磨粒度控制在0.95-1.10μm之间，喷雾造粒制成40-180目的颗粒料。
与现有技术相比，本发明的有益效果是：
本发明通过合理调配配方中的微量添加剂，改变材料的制备工艺，同时通过优化烧结气氛的控制，在保证材料的电气性能较为稳定的基础上，使得用该种材料制造的磁心在同等条件下比普通材料制造的同种磁心的机械强度有较大的提高，从而同时满足电气性能和机械强度的高要求。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1：较高强度锰锌软磁铁氧体材料的制备方法，包括以下步骤：
(1)配主料：按摩尔比为Fe2O3 53.0mol、MnO 35.5mol、ZnO 12.0mol配主料；
(2)配辅料：相当于主料0.006wt％的ZrO2、0.018wt％的CaCO3、0.004wt％的SiO2、0.17wt％的V2O5；
(3)主料混合一次球磨粉碎：将步骤(1)配好的主料加去离子水、胶合剂和分散剂充分进行球磨1.5小时，喷雾造粒制成40-180目的颗粒料；
(4)主料预烧：将步骤(3)喷雾造粒的颗粒料进行预烧，预烧温度为860℃，预烧时间为1.5小时；
(5)主料、辅料混合与二次粉碎球磨：将步骤(4)预烧好的主料加入去离子水、胶合剂和分散剂进行球磨2小时，在砂磨至1.5小时时加入步骤(2)配好的辅料共同球磨至结束，检测球磨粒度控制在0.95-1.10μm之间，喷雾造粒制成40-180目的颗粒料；
(6)成型：将喷雾造粒颗粒料加入0.015％的硬脂酸锌后用混料机充分混合10分钟，然后压制毛坯；
(7)烧结：将步骤(6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以90℃/小时速率升温至800-850℃，保温1-1.5小时；在6.0-9.5％氧含量的氮气氛围中，以90℃/小时速率升温至1280-1320℃，烧结时间为3.5小时；烧结后在0.001-0.003％氧含量的氮气氛围中，按照120℃/小时降温即可得到具有较高强度的锰锌铁氧体磁心。
实施例2：较高强度锰锌软磁铁氧体材料的制备方法，包括以下步骤：
(1)配主料：按摩尔比为Fe2O3 52.0mol、MnO 34.5mol、ZnO 11.0mol配主料；
(2)配辅料：相当于主料0.004wt％的ZrO2、0.015wt％的CaCO3、0.003wt％的SiO2、0.15wt％的V2O5；
(3)主料混合一次球磨粉碎：将步骤(1)配好的主料加去离子水、胶合剂和分散剂充分进行球磨1小时，喷雾造粒制成40-180目的颗粒料；
(4)主料预烧：将步骤(3)喷雾造粒的颗粒料进行预烧，预烧温度为850℃，预烧时间为2小时；
(5)主料、辅料混合与二次粉碎球磨：将步骤(4)预烧好的主料加入去离子水、胶合剂和分散剂进行球磨2.5小时，在砂磨至1.5小时时加入步骤(2)配好的辅料共同球磨至结束，检测球磨粒度控制在0.95-1.10μm之间，喷雾造粒制成40-180目的颗粒料；
(6)成型：将喷雾造粒颗粒料加入0.015％的硬脂酸锌后用混料机充分混合10分钟，然后压制毛坯；
(7)烧结：将步骤(6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以80℃/小时速率升温至800-850℃，保温1-1.5小时；在6.0-9.5％氧含量的氮气氛围中，以80℃/小时速率升温至1280-1320℃，烧结时间为4.0小时；烧结后在0.001-0.003％氧含量的氮气氛围中，按照100℃/小时降温即可得到具有较高强度的锰锌铁氧体磁心。
实施例3：较高强度锰锌软磁铁氧体材料的制备方法，包括以下步骤：
(1)配主料：按摩尔比为Fe2O3 55.0mol、MnO 37.5mol、ZnO 13.0mol配主料；
(2)配辅料：相当于主料0.008wt％的ZrO2、0.020wt％的CaCO3、0.005wt％的SiO2、0.20wt％的V2O5；
(3)主料混合一次球磨粉碎：将步骤(1)配好的主料加去离子水、胶合剂和分散剂充分进行球磨1-1.5小时，喷雾造粒制成40-180目的颗粒料；
(4)主料预烧：将步骤(3)喷雾造粒的颗粒料进行预烧，预烧温度为850-900℃，预烧时间为1-2小时；
(5)主料、辅料混合与二次粉碎球磨：将步骤(4)预烧好的主料加入去离子水、胶合剂和分散剂进行球磨2小时，在砂磨至1.5小时时加入步骤(2)配好的辅料共同球磨至结束，检测球磨粒度控制在0.95-1.10μm之间，喷雾造粒制成40-180目的颗粒料；
(6)成型：将喷雾造粒颗粒料加入0.015％的硬脂酸锌后用混料机充分混合10分钟，然后压制毛坯；
(7)烧结：将步骤(6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以120℃/小时速率升温至800-850℃，保温1-1.5小时；在6.0-9.5％氧含量的氮气氛围中，以100℃/小时速率升温至1280-1320℃，烧结时间为3.5小时；烧结后在0.001-0.003％氧含量的氮气氛围中，按照130℃/小时降温即可得到具有较高强度的锰锌铁氧体磁心。
通过对实施例1制得的软磁铁氧体磁心的电气性能数据：
通过对实施例1制得的软磁铁氧体磁心的抗压强度数据：(以磁心在断裂前能承受最大的抗压强度为准，单位：N)
以上所述，仅是本发明的较佳实施例，并非对本发明作任何形式上的限制，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，依据本发明的技术实质，对以上实施例所作的任何简单的修改、等同替换与改进等，均仍属于本发明技术方案的保护范围之内。

Claims (4)

1.一种具有较高强度的锰锌软磁铁氧体材料的制备方法，其特征在于：包括以下步骤：
1)配主料：按Fe2O3：MnO：ZnO摩尔比为(52.0-55.0)：(34.5-37.5)：(11.0-13.0)配主料；
2)配辅料：取相当于主料0.004-0.008wt％的ZrO2、0.015-0.020wt％的CaCO3、0.003-0.005wt％的SiO2、0.15-0.20wt％的V2O5；
3)主料混合一次球磨粉碎：将步骤1)配好的主料加去离子水、胶合剂和分散剂充分进行球磨；
4)主料预烧：将步骤3)喷雾造粒的颗粒料进行预烧；
5)主料、辅料混合与二次粉碎球磨：将步骤4)预烧好的主料加入去离子水、胶合剂和分散剂进行球磨2-2.5小时，在球磨至1.5小时时加入步骤2)配好的辅料共同球磨至结束，喷雾造粒；
6)成型：将喷雾造粒颗粒料加入0.015％的硬脂酸锌后用混料机充分混合，然后压制毛坯；
7)烧结：将步骤6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以80-120℃/小时速率升温至800-850℃，保温1-1.5小时；在6.0-9.5％氧含量的氮气氛围中，以80-100℃/小时速率升温至1280-1320℃，烧结时间为3.5-4.0小时；烧结后在0.001-0.003％氧含量的氮气氛围中，按照100-130℃/小时降温即可得到具有较高强度的锰锌铁氧体磁心。
2.根据权利要求1所述的具有较高强度的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤3)球磨1-1.5小时，喷雾造粒制成40-180目的颗粒料。
3.根据权利要求1所述的具有较高强度的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤4)预烧温度为850-900℃，预烧时间为1-2小时。
4.根据权利要求1所述的具有较高强度的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤5)检测球磨粒度控制在0.95-1.10μm之间，喷雾造粒制成40-180目的颗粒料。
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