CN105439551A - 一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法 - Google Patents
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 24
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 17
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000006247 magnetic powder Substances 0.000 title abstract 4
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 230000005415 magnetization Effects 0.000 claims abstract description 14
- 239000002019 doping agent Substances 0.000 claims abstract description 12
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 31
- HHZHOPJRSHTPOP-UHFFFAOYSA-N [O--].[O--].[Fe++].[Sr++] Chemical compound [O--].[O--].[Fe++].[Sr++] HHZHOPJRSHTPOP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000696 magnetic material Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 8
- -1 compound ion Chemical class 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 2
- 235000010216 calcium carbonate Nutrition 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000004907 flux Effects 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 abstract 1
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 16
- 239000012071 phase Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920000831 ionic polymer Polymers 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明具体涉及一种高磁能积的La-Co共掺锶铁氧体及其制备方法，具体实施方案：以SrCO3和Fe2O3为原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，按摩尔比(0.5~0.9):(5.75~5.95):(0.05~0.25):(0.1~0.5)混合，添加适量CaCO3助熔剂，球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至950~1200℃，保温两小时，即得到La-Co共掺锶铁氧体磁性料粉。本发明工艺简单，适合工业生产，利用La-Co复合离子添加，实现本征磁性能可调，磁能积24.6~35.7kJ/m3，矫顽力267.4~345kA/m，剩余磁化强度367~430mT。
Description
技术领域
本发明属于永磁铁氧体材料领域，具体涉及一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备，特别是通过复合离子掺杂调控材料的本证磁性，获得最优掺杂配方的制备方法。
背景技术
锶铁氧体永磁材料因其较高的饱和磁化强度、高矫顽力以及高磁能积，广泛应用于磁记录仪、空调、音频变换器、分离器、吸持装置、电机转子中。尤其是近年来，直流变频电机开始采用永磁体取代感应线圈，减少了电机转子感应电流和磁场方面的损失，因此高饱和磁化强度、高磁能积的锶铁氧体材料具有更高的节能潜力而有望成为最具发展前景的焦点技术。
在永磁锶铁氧体材料领域，为了提高材料的本证磁性能，在材料改性方面，如单离子稀土离子或过渡金属离子取代掺杂，多离子稀土-过渡金属（La-Mn或La-Zn或La-Co等）共同掺杂,国内外进行了大量研究。研究表明，复合离子掺杂更容易实现调控铁氧体材料的本证磁性能。同时，通过碱土金属氧化物MgO、CaO等的添加能够进一步改善材料的电磁性能。如MuhammadJavedIqbal等研究了Ca2+离子掺杂SrFe12O19铁氧体的物理、介电性能。ZhangZeyang等研究了Nd-Co掺杂SrFe12O19铁氧体的电磁微波吸收性能，研究表明掺杂量x=0.2时，矫顽力和饱和磁化强度均出现极大值。Jean-MareLeBreton等详细研究了La-Co共同掺杂对锶铁氧体材料磁结构的影响，证实了稀土离子和过渡金属离子的晶格占位趋势。Takeyukikikuchi等对La-Co共掺对锶铁氧体材料磁性能的影响研究，结果表明复合掺杂明显提高矫顽力，出现极大值，但饱和磁化强度随掺杂量的增加而降低。
本发明通过工业上成熟的固相反应方法，具体利用La-Co复合离子添加技术，实现材料本征磁性能可控调节，本发明创新性在于通过简单易行的制备方法，获得了剩余磁化强度达430mT，并提高了矫顽力和磁能积等综合磁性能。
发明内容
本发明的目的在于针对Sr铁氧体材料粉体磁性能较低的缺陷，以及大离子半径稀土离子较难固溶于母体铁氧体的难点，通过复合离子添加，较大提高了铁氧体材料的剩余磁化强度，尤其是实现综合磁性能的提高。
为了实现上述目的，具体实施方案是：以SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料和掺杂剂按摩尔比(0.5~0.9):(5.75~5.95):(0.05~0.25):(0.1~0.5)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至950~1200℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
由于采用上述方案，本发明采用购自于北矿的高质量Sr铁氧体预烧料，通过控制预烧料和掺杂剂的配比，外加适量添加剂，经球磨混合均匀后煅烧制得La-Co共掺锶铁氧体磁性料粉，制备工艺简单，有利于大规模工业生产。
本发明方案科学合理，工艺参数选择简单易行，所制备的La-Co共掺锶铁氧体磁性料粉经表征为单一物相的Sr铁氧体，颗粒大小均匀，比例符合La-Co共掺锶铁氧体组成的成分范围，其料粉的磁能积24.6~35.7kJ/m3，内禀矫顽力267.4~345kA/m，剩余磁化强度367~430mT。
因此本发明具有工艺简单易实现，综合成本低，所制备La-Co共掺锶铁氧体磁性料粉综合磁性能优良，粉料质量易控制，有利于工业生产。
附图说明
图1为实施案例6中Sr1-xLaxFe12-yCoyO19，x=y=0无掺杂的的X射线衍射图。
图2为实施案例2中Sr1-xLaxFe12-yCoyO19掺杂量x=y=0.2的X射线衍射图。
图3为实施案例2中Sr1-xLaxFe12-yCoyO19掺杂量x=y=0.2的扫描电镜图。
图4为实施案例2中Sr1-xLaxFe12-yCoyO19掺杂量x=y=0.2的能谱图。
图5为实施案例中Sr1-xLaxFe12-yCoyO19不同掺杂量磁性能参数图。
实施案例
实施案例1
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.89~0.9):(5.94~5.95):(0.05~0.06):(0.1~0.11)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至1000~1050℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
本实施案例制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：剩余磁化强度高达410mT，磁能积31.8kJ/m3，内禀矫顽力326kA/m。
实施案例2
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.78~0.8):(5.88~5.9):(0.1~0.11):(0.18~0.2)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至1000~1050℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
本实施案例制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：剩余磁化强度高达430mT，磁能积35.7kJ/m3，结构表征表明为单一物相的Sr铁氧体。
实施案例3
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.7~0.75):(5.84~5.85):(0.15~0.16):(0.3~0.31)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至950~1000℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
本实施案例制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：剩余磁化强度达419mT，磁能积28.3kJ/m3，内禀矫顽力321kA/m。
实施案例4
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.6~0.62):(5.8~5.81):(0.19~0.21):(0.38~0.4)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，15℃/分钟升温速率升至1000~1150℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
本实施案例制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：剩余磁化强度达395mT，磁能积28.3kJ/m3，内禀矫顽力325.7kA/m。
实施案例5
一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.48~0.5):(5.75~5.76):(0.25~0.26):(0.49~0.51)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至1150~1200℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
本实施案例制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：剩余磁化强度367mT，磁能积24.6kJ/m3，内禀矫顽力270kA/m。
实施案例6
一种高磁能积La-Co共掺锶铁氧体磁性料粉及其制备方法。以购自北矿的SrCO3和Fe2O3为锶铁氧体原料，将所述原料按（SrCO3:Fe2O3:La2O3:CoO）的摩尔比(0.95~0.99):(5.96~5.98)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至1000~1050℃，保温两小时，随炉降温，即得到无La-Co共掺的锶铁氧体磁性料粉。
本实施案例制备了无La-Co共掺的锶铁氧体磁性料粉，作为对比案例，其磁性能参数：剩余磁化强度405mT，磁能积31.9kJ/m3，内禀矫顽力267.4kA/m。结构表征显示本发明能够以较为简单的工艺制备单一物相的Sr铁氧体。
Claims (2)
1.一种高磁能积的La-Co共掺锶铁氧体磁性料粉及其制备方法，其特征在于以SrCO3和Fe2O3为锶铁氧体原料，以氧化镧La2O3和氧化钴CoO为掺杂剂，将所述原料和掺杂剂按摩尔比(0.5~0.9):(5.75~5.95):(0.05~0.25):(0.1~0.5)混合，添加适量的CaCO3助熔剂，配成混合料后球磨,干燥，解碎，置于马弗炉中煅烧，10~20℃/分钟升温速率升至950~1200℃，保温两小时，随炉降温，即得到La-Co共掺锶铁氧体磁性料粉。
2.如权利要求1所述一种高磁能积的La-Co共掺锶铁氧体磁性料粉制备方法，其特征在于所制备的La-Co共掺锶铁氧体磁性料粉磁性能参数：磁能积(BH)max为24.6~35.7kJ/m3，内禀矫顽力Hcj为267.4~345kA/m，剩余磁化强度Br为367~430mT。
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