CN112321294A - 一种铁氧体永磁材料及其制备方法 - Google Patents
一种铁氧体永磁材料及其制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 32
- 239000000696 magnetic material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 9
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
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- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 229910052682 stishovite Inorganic materials 0.000 abstract description 3
- 229910052905 tridymite Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229940029329 intrinsic factor Drugs 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
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- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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Abstract
本发明提供了一种铁氧体永磁材料及其制备方法，属于永磁材料技术领域。所述永磁材料按重量份计，由以下成分组成：Fe2O3，SrCO3，La2O3，Co2O3，CaCO3，SiO2。其制备方法包括：配料，湿辊，沉淀，一次成型，预烧，一次破碎，二次球磨，二次成型和烧结。本发明的铁氧体永磁材料通过在预烧中增加组合离子在材料中的替换量，在充分的氧化气氛下预烧结，并设定合适的预烧结温度，能够充分生成永磁铁氧体M相，得到更好的磁性能；通过在二次球磨步骤中控制粒度，提高了成型的生产效率和合格率，产品烧结出来后具有剩磁高、矫顽力高、内禀高的特点性能能达到TDKFB12性能要求，具有推广应用价值。
Description
技术领域
本发明属于永磁材料技术领域，具体涉及一种铁氧体永磁材料及其制备方法。
背景技术
永磁材料是电子行业中不可或缺的材料，以其原料来源广、价格低廉和优异的磁性能在磁性材料的研究与发展中占有重要地位。广泛应用于家电、汽车、计算机、通讯、医疗、航天、军事等领域。随着永磁材料的广泛应用对永磁材料的性能要求也越来越高，为满足市场需求铁氧体行业的王牌企业——日本TDK公司推出了FB9、FB12系列高性能永磁铁氧体产品后，各厂家纷纷从原材料、二次添加、生产工艺等方面探索提高永磁铁氧体磁性能的途径。在永磁铁氧体中常用的添加剂有CaCO3、Al2O3、SiO2、H3BO3及部分稀土氧化物。这些添加剂的缺点是CaCO3及部分稀土氧化等添加剂在提高剩磁的同时，材料矫顽力和内禀矫顽力也随着下降；Al2O3、SiO2等添加剂在提高材料矫顽力和内禀矫顽力的同时，剩磁也随着急剧下降。
发明内容
有鉴于此，本发明的目的在于提供一种铁氧体永磁材料及其制备方法。
经研究，本发明采用以下技术方案：
1、一种铁氧体永磁材料，按重量份计，由以下成分组成：Fe2O3：100份；SrCO3：10-15份；La2O3：1.5-5份；Co2O3：0.5-3份；CaCO3：2-5份；SiO2：0.3-1份。
优选的，按重量份计，由以下成分组成：Fe2O3：100份；SrCO3：15份；La2O3：4.5份；Co2O3：2份；CaCO3：4份；SiO2：0.3份。
2、上述铁氧体永磁材料的方法，包括以下步骤：
湿混：将按配比得到的原料进行湿混1-3小时；
沉淀：对湿混得到的原料进行沉淀；
一次成型：对沉淀后的原料压制成型；
预烧：对压制成型的原料进行预烧结处理，预烧结温度为1200-1220℃，保温1-3.5小时后，自然冷却，得到预烧料；
一次破碎：对预烧料进行干式球磨破碎，并通过超声波分级过筛；
二次球磨：采用料：球：水之比为1-1.5:8-10:1.5-2.5的湿法磨料；
二次成型：对二次球磨得到的料浆压制成型；
烧结：对成型后的生坯进行烧结处理，烧结的温度为1180-1200℃，保温2-4小时后，冷却至常温。
优选的，所述沉淀后原料中的水分含量为32～35％。
优选的，所述二次球磨，磨料后的粒度为0.80～0.9μm。
优选的，所述二次球磨后，还进行脱水处理，脱水后的浆料含水率为32～35％。
优选的，所述二次成型后，成型得到的生胚密度为2.9～3.8g/cm2。
优选的，所述烧结采用双推板隧道电窑对成型后的生坯进行烧结处理，且进车速度为8-10分钟/板。
本发明的有益效果在于：
本发明的铁氧体永磁材料在一次预烧料中通过La-Co离子联合取代六角锶铁氧体中的锶/铁在材料中的替换量，在45米烧结窑炉进行烧结。并通过设定合适的预烧结温度，充分的保温时间使预烧料在烧结过程中能更好的氧化，能得到更好的磁性能；通过在二次球磨步骤中控制粒度，使得球磨后粒度一致性好，产品成型性好，从而提高了成型的生产效率和合格率；通过烧结处理，得到的铁氧体永磁材料通过磁性材料测试装置测试结果具有剩磁高、矫顽力高、内禀高等优点，能达到TDKFB12性能要求，具有推广应用价值。
附图说明
图1为本实施例1制得的铁氧体永磁材料的性能检测分析图；
图2为本实施例2制得的铁氧体永磁材料的性能检测分析图；
图3为本实施例3制得的铁氧体永磁材料的性能检测分析图；
图4为本实施例4制得的铁氧体永磁材料的性能检测分析图。
具体实施方式
下面结合本发明实施例，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他实施例，都属于本发明保护的范围。
实施例1
本实施例中铁氧体永磁材料的制备方法，包括以下步骤：
1)配料：按以下重量百分比配料：Fe2O3：100份；SrCO3：15份；La2O3：3份；Co2O3：1份；CaCo3：5份；SiO2：1份；
2)湿混：将配料得到的原料采用球磨机湿混2小时，保证混料均匀性；
3)沉淀：采用沉淀塔或木箱对湿混得到的原料进行沉淀，使沉淀后的原料中的水分含量为34％；
4)一次压制成型：采用150吨成型自动压机和150㎏/㎝2的压力对沉淀后的原料压制成型，保证密度的一致性，有利于预烧时的固相反应；
5)预烧：采用45米窑对压制成型的原料进行预烧结处理，预烧结温度为1210℃，保温2小时后，自然冷却，得到预烧料，通过采用该预烧温度，能够保证预烧料中生产高性能M相，稀土离子置换率更高；
6)一次破碎：对预烧料进行干式球磨破碎，并采用超声波振动筛将破碎的预烧料过筛分级，通过采用超声波分级筛选，保证二次磨料的进料颗粒的一致性，从而达到料浆颗粒的一致性；
7)二次球磨：采用料：球：水之比为1:10:1.8的湿法磨料，磨料后的粒度为0.80-0.90μm，然后进行脱水，使脱水后的料浆含水率33％；
8)二次成型：采用150吨自动液压机和硬质合金流道式模具对二次球磨得到的料浆压制成型，成型得到的生坯密度为2.9-3.8g/㎝2；
9)烧结：采用36米双推板隧道电窑对成型后的生坯进行烧结处理，且进车速度为8分钟/板，烧结的温度为1190℃，保温2.5小时后，随出窑速度冷却至常温。
实施例2
本实施例中铁氧体永磁材料的原料，按以下重量百分比配料：Fe2O3：100份；SrCO3：15份；La2O3：4份；Co2O3：1.5份；CaCO3：2份；SiO2：0.5份。其余制备步骤及条件与实施例1相同。
实施例3
本实施例中铁氧体永磁材料的原料，按以下重量百分比配料：Fe2O3：100份；SrCO3：15份；La2O3：4.5份；Co2O3：2份；CaCo3：4份；SiO2：0.3份。其余制备步骤及条件与实施例1相同。
实施例4
本实施例中铁氧体永磁材料的原料，按以下重量百分比配料：Fe2O3：100份；SrCO3：15份；La2O3：4.5份；Co2O3：1.5份；CaCo3：4.5份；SiO2：0.8份。其余制备步骤及条件与实施例1相同。
将实施例1～实施例4制得的磁性材料经磁性材料测试装置进行测试，测试结果如图1～图4所示：
从图3中分析可知，采用实施例3的添加配比所得到的永磁材料的性能达到:剩余磁通密度Br:≥445mT、矫顽力Hcb:≥330KA/m、内禀矫顽力Hcj:≥400KA/m、最大磁能量积(BH)max:≥38KJ/m3。此配比生产出来的材料性能接近日本TDKFB12的性能要求。
从图1～图4的测试数据综合分析可知，所制备的永磁铁氧体材料具有高剩磁：能确保电机有较高的转速，大的输出扭矩和大的功率；高矫顽力：确保电机输出所需的电动势，使电机工作点靠近最大磁能积，充分利用磁体的能力；高内禀：确保电机有较强的抗过载退磁及抗老化，抗高低温的能力；高磁能量积：电机中实际的运行的工作系数更好等特点。能满足各个不同的客户需求，增强了市场竞争力。
当然，以上仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种铁氧体永磁材料，其特征在于，按重量份计，由以下成分组成：Fe2O3：100份；SrCO3：10-15份；La2O3：1.5-5份；Co2O3：0.5-3份；CaCO3：2-5份；SiO2：0.3-1份。
2.根据权利要求1所述铁氧体永磁材料，其特征在于，按重量份计，由以下成分组成：Fe2O3：100份；SrCO3：15份；La2O3：4.5份；Co2O3：2份；CaCO3：4份；SiO2：0.3份。
3.如权利要求1或2所述铁氧体永磁材料的方法，其特征在于，包括以下步骤：
湿混：将按配比得到的原料进行湿混1-3小时；
沉淀：对湿混得到的原料进行沉淀；
一次成型：对沉淀后的原料压制成型；
预烧：对压制成型的原料进行预烧结处理，预烧结温度为1200-1220℃，保温1-3.5小时后，自然冷却，得到预烧料；
一次破碎：对预烧料进行干式球磨破碎，并通过超声波分级过筛；
二次球磨：采用料：球：水之比为1-1.5:8-10:1.5-2.5的湿法磨料；
二次成型：对二次球磨得到的料浆压制成型；
烧结：对成型后的生坯进行烧结处理，烧结的温度为1180-1200℃，保温2-4小时后，冷却至常温。
4.根据权利要求3所述铁氧体永磁材料的方法，其特征在于，所述沉淀后原料中的水分含量为32～35％。
5.根据权利要求3所述铁氧体永磁材料的方法，其特征在于，所述二次球磨，磨料后的粒度为0.8～0.9μm。
6.根据权利要求3所述铁氧体永磁材料的方法，其特征在于，所述二次球磨后，还进行脱水处理，脱水后的浆料含水率为32～35％。
7.根据权利要求3所述铁氧体永磁材料的方法，其特征在于，所述二次成型后，成型得到的生胚密度为2.9～3.8g/cm2。
8.根据权利要求3所述铁氧体永磁材料的方法，其特征在于，所述烧结采用双推板隧道电窑对成型后的生坯进行烧结处理，且进车速度为8-10分钟/板。
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