CN113956032B - 一种宽温低损耗高强度MnZn功率铁氧体及其制备方法与应用 - Google Patents
一种宽温低损耗高强度MnZn功率铁氧体及其制备方法与应用 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 claims description 63
- 239000000463 material Substances 0.000 claims description 50
- 238000005245 sintering Methods 0.000 claims description 47
- 230000008569 process Effects 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 24
- 229910052760 oxygen Inorganic materials 0.000 claims description 24
- 238000005469 granulation Methods 0.000 claims description 20
- 230000003179 granulation Effects 0.000 claims description 20
- 239000007921 spray Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000004576 sand Substances 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000000280 densification Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 6
- 230000004907 flux Effects 0.000 abstract description 6
- 229910000484 niobium oxide Inorganic materials 0.000 abstract description 6
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011787 zinc oxide Substances 0.000 abstract description 6
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract description 4
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract description 4
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 abstract 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical group [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 16
- 229910052720 vanadium Inorganic materials 0.000 description 7
- 238000005507 spraying Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000009817 primary granulation Methods 0.000 description 1
- 238000009818 secondary granulation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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Abstract
本发明涉及一种宽温低损耗高强度MnZn功率铁氧体及其制备方法与应用,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成;辅助成分的质量为所述主成分的0.165‑0.61wt%;主成分包括氧化铁、氧化锰与氧化锌;辅助成分包括第一辅助成分与第二辅助成分,第一辅助成分为氧化钴;第二辅助成分包括碳酸钙、氧化铌、氧化钒或氧化钼中的至少三种。本发明通过辅助成分的添加,尤其是特定质量氧化钴的添加,实现对Fe2+与Co2+特定比例的协同调节,保证在不受温度变化影响下功耗有效降低,从而使制备得到的宽温低损耗高强度MnZn功率铁氧体能够在25‑120℃下具有低损耗、高磁通密度且强度提升10%以上的特点。
Description
技术领域
本发明属于软磁领域,涉及一种铁氧体及其制备方法与应用,尤其涉及一种宽温低损耗高强度MnZn功率铁氧体及其制备方法与应用。
背景技术
随着通讯、计算机和网络等电子信息产业的高速发展,高性能软磁铁氧体的需求量与日俱增。目前,MnZn铁氧体的产量在工业化生产的软磁铁氧体材料中当居首位,占60%以上。作为广泛应用于各通讯及电子领域的MnZn铁氧体,其传统功率材料的宽温低损耗已经不能完全满足电子产品的要求,尤其在汽车电子领域,对强度有很高的要求。因此,如何在MnZn功率铁氧体保持宽温低损耗的同时,提高强度性能以满足对材料的综合性能要求,成为目前亟待解决的问题。
目前通过优化材料的成分配方并采用合适的制备方法可以在一定程度上提高材料的使用温度范围与强度,并降低损耗,然而对综合性能的控制和提升仍需要进行大量的实验和改进。
CN 107129291A公开了一种具有高频低温度系数低损耗MnZn软磁铁氧体材料的制备方法。该材料以Fe2O3:68-72wt%、ZnO:5-9wt%、MnO:余量为主成分,通过一次球磨、一次烧结、二次配料、二次球磨、造粒、压制成型、二次烧结等步骤制备而成。所得具有高频低温度系数低损耗MnZn软磁铁氧体材料最高可以在5Mz的频率下工作,且具有较高的温度稳定性和较低功率损耗。
CN 103496963A公开了一种不含Ni的兼具高温高Bs和宽温低损耗双重特性的MnZn功率铁氧体磁心及其制造方法。所述铁氧体磁心包括主成分和辅助成分,所述主料为以Fe2O3计53-54mol%的氧化铁、以MnO计39-42mol%的氧化锰、以ZnO计4-7mol%的氧化锌;所述辅助成分包括以Co2O3或CoO或Co3O4作为第一辅助成分,以SiO2、CaCO3作为第二辅助成分,选自MoO3、TiO2、SnO2、Nb2O5、V2O5、Sm2O3、ZrO2中任一种或几种作为第三辅助成分。所得兼具双重特性的MnZn功率铁氧体磁心从25-120℃的单位体积损耗Pcv(100kHz,200mT)都小于350kW/m3,在90℃附近最低损耗低于300kW/m3。
CN 107573051A公开了一种不提高损耗改善MnZn功率铁氧体磁芯强度的方法,在制备MnZn功率铁氧体时添加200-400ppm的CaCO3,240-410ppm的V2O5,和100-200ppm的ZrO2,能够在不提高损耗的前提下,有效提高铁氧体的磁芯强度。
上述技术方案均在传统的功率材料上进行了性能的改进,然而无法综合性地改善与提升相关性能。例如,CN 107129291A其材料存在对损耗以及使用温度范围的控制不足的缺陷;CN 107573051A其材料存在强度不足的缺陷;CN107573051A没有涉及同时提高材料的使用温度范围并降低损耗的方法。
因此,需要提供一种MnZn功率铁氧体的制备方法,使该制备方法得到的MnZn功率铁氧体具有较高温度稳定性与较低功率损耗的同时,还能够在较高的强度下进行工作。
发明内容
鉴于现有技术中存在的问题,本发明提供了一种宽温低损耗高强度MnZn功率铁氧体及其制备方法与应用,通过特定质量辅助成分的添加,使制备得到所述宽温低损耗高强度MnZn功率铁氧体保证在较宽的温度范围内不仅具备较低的功率损耗,而且具有较高的强度性能。
第一方面,本发明提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成;所述辅助成分的质量为所述主成分的0.165-0.61wt%;
以摩尔百分数计,所述主成分包括:Fe2O3:51-54mol%,MnO:35-38mol%以及ZnO:8-14mol%;
所述辅助成分包括第一辅助成分与第二辅助成分;以所述主成分的总质量为基准,所述第一辅助成分为Co2O3:0.1-0.4wt%;所述第二辅助成分包括CaCO3、Nb2O5、V2O5及MoO3中至少三种。
本发明通过调整MnZn功率铁氧体的组成,制备得到在25-120℃的温度条件下满足低损耗和高强度器件要求的MnZn功率铁氧体。
具体的,所述辅助成分的质量为所述主成分的0.165-0.61wt%,例如可以是0.165wt%、0.17wt%、0.2wt%、0.25wt%、0.3wt%、0.35wt%、0.4wt%、0.45wt%、0.5wt%、0.55wt%、0.6wt%或0.61wt%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
以摩尔百分数计,所述主成分中Fe2O3的摩尔百分数为51-54mol%,例如可以是51mol%、51.5mol%、52mol%、52.5mol%、53mol%、53.5mol%或54mol%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为52-53mol%。
以摩尔百分数计,所述主成分中MnO的摩尔百分数为35-38mol%,例如可以是35mol%、35.5mol%、36mol%、36.5mol%、37mol%、37.5mol%或38mol%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为36-38mol%。
以摩尔百分数计,所述主成分中ZnO的摩尔百分数为8-14mol%,例如可以是8mol%、8.5mol%、9mol%、9.5mol%、10mol%、10.5mol%、11mol%、11.5mol%、12mol%、13mol%或14mol%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为9-12mol%。
本发明所述第一辅助成分为Co2O3,以主成分的总质量为基准,所述第一辅助成分Co2O3的含量为0.1-0.4wt%,例如可以是0.1wt%、0.15wt%、0.2wt%、0.25wt%、0.3wt%、0.35wt%或0.4wt%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.1-0.35wt%。
通过上述质量分数Co2O3的添加,实现了对所述MnZn功率铁氧体中Fe2+与Co2+的特定比例含量的协同调节,使最终所得MnZn功率铁氧体在不受温度变化的影响下有效降低磁滞损耗,保证了所述MnZn功率铁氧体在25-120℃的宽温条件下具有较低的损耗。
以主成分的总质量为基准,当Co2O3的含量超过本发明所述范围时,制备得到的MnZn铁氧体的功耗增加或者强度降低。
本发明所述第一辅助成分包括CaCO3、Nb2O5、V2O5及MoO3中至少三种,典型但非限制性的组合包括碳酸钙与氧化铌的组合,氧化铌与氧化钒的组合,氧化钒与氧化钼的组合,钛酸钙、氧化铌与氧化钒的组合,氧化铌、氧化法与氧化钼的组合,或碳酸钙、氧化铌、氧化钒与氧化钼的组合。
优选地,以所述主成分的总质量为基准,所述第二辅助成分包括CaCO3:0.03-0.07wt%,Nb2O5:0.01-0.04wt%,V2O5:0.02-0.07wt%与MoO3:0.005-0.03wt%。
以所述主成分的总质量为基准,所述第二辅助成分中CaCO3的含量为0.03-0.07wt%,例如可以是0.03wt%、0.035wt%、0.04wt%、0.045wt%、0.048wt%、0.05wt%、0.055wt%、0.06wt%、0.065wt%或0.07wt%但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.035-0.048wt%。
以所述主成分的总质量为基准,所述第二辅助成分中Nb2O5的含量为0.01-0.04wt%,例如可以是0.01wt%、0.015wt%、0.02wt%、0.025wt%、0.03wt%、0.035wt%或0.04wt%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.02-0.04wt%。
以所述主成分的总质量为基准,所述第二辅助成分中V2O5的含量为0.02-0.07wt%,例如可以是0.02wt%、0.025wt%、0.03wt%、0.04wt%、0.042wt%、0.045wt%、0.048wt%、0.05wt%、0.055wt%、0.06wt%、0.065wt%或0.07wt%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.042-0.07wt%。
以所述主成分的总质量为基准,所述第二辅助成分中MoO3的含量为0.005-0.03wt%,例如可以是0.005wt%、0.01wt%、0.015wt%、0.02wt%、0.025wt%或0.03wt%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.01-0.03wt%。
第二方面,本发明提供了一种如第一方面所述宽温低损耗高强度MnZn功率铁氧体的制备方法,所述制备方法包括:
(1)按配方量称取主成分制备原料,对主成分制备原料进行一次砂磨、一次喷雾造粒和预烧,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合后得到混合料,进行二次砂磨,得到二次砂磨料;
(3)步骤(2)所得二次砂磨料依次进行二次喷雾造粒、成型与烧结,得到所述宽温低损耗高强度MnZn功率铁氧体。
本发明提供的制备方法工艺简单、生产成本低且工艺稳定,能制备出具有宽温低损耗高强度特性的MnZn功率铁氧体。
优选地,步骤(1)中所述一次砂磨的时间为20-60min,例如可以是20min、25min、30min、35min、40min、45min、50min、55min或60min,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为40-60min。
优选地,步骤(1)所述一次砂磨时主成分制备原料与溶剂的质量比为(1.8-2.2):1,例如可以是1.8:1、1.9:1、2:1、2.1:1或2.2:1,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
优选地,所述溶剂包括去离子水。
优选地,步骤(1)所述一次砂磨后的粒度为0.6-1.5μm,例如可以是0.6μm、0.7μm、0.8μm、0.9μm、1.0μm、1.1μ1.2μm、1.3μm、1.4μm或1.5μm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
本发明所述粒度为0.6-1.5μm是指,最小粒度在0.6μm以上,最大粒度在1.5μm以下。
优选地,步骤(1)所述一次造粒制备成颗粒料。
优选地,步骤(1)所述预烧的温度为800-1030℃,例如可以是800℃、850℃、900℃、940℃、960℃、980℃、1000℃、1010℃、1020℃或1030℃,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为960-1020℃。
优选地,步骤(1)所述预烧的时间为3-9h,例如可以是3h、4h、5h、6h、7h、8h或9h,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为3-6h。
优选地,步骤(2)所述二次砂磨时混合料与溶剂的质量比为2:(0.9-1.1),例如可以是2:0.9、2:0.95、2:1、2:1.05或2:1.1,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
优选地,所述溶剂包括去离子水或蒸馏水。
优选地,步骤(2)所述二次砂磨的时间为1-3h,例如可以是1h、1.5h、2h、2.5h或3h,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为2-3h。
优选地,步骤(2)所述二次砂磨的平均粒径为1.05-1.30μm,例如可以是1.05μm、1.10μm、1.15μm、1.20μm、1.25μm或1.30μm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
优选地,步骤(3)所述二次喷雾造粒的粒径为50-200μm,例如可以是50μm、60μm、70μm、80μm、90μm、100μm、120μm、140μm、150μm、160μm、180μm或200μm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为80-150μm。
本发明二次造粒的粒径为50-200μm是指,最小粒度在50μm以上,最大粒度在200μm以下。
本发明步骤(3)所述成型为坯件,所述坯件的高为20-30mm,例如可以是20mm、21mm、22mm、23mm、24mm、25mm、26mm、27mm、28mm、29mm或30mm,长为12-18mm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,例如可以是12mm、13mm、14mm、15mm、16mm、17mm或18mm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,宽为5-10mm,例如可以是5mm、6mm、7mm、8mm、9mm或10mm,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
优选地,步骤(3)所述烧结的温度为1290-1360℃,例如可以是1290℃、1300℃、1310℃、1320℃、1330℃、1340℃、1350℃或1360℃,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为1300-1360℃。
当烧结温度超过本发明范围时,所制备得到的MnZn功率铁氧体的损耗增大或强度降低。
优选地,步骤(3)所述烧结的时间为28-32h,例如可以是28h、29h、30h、31h或32h,但不限于所列举的数值,数值范围内其它未列举的数值同样适用。
本发明所述烧结包括升温以及保温过程,所述烧结时间是指升温至1290-1360℃后的保温时间。
优选地,步骤(3)所述烧结过程混合气体环境下进行。
优选地,所述混合气体包括氧气和氮气。
优选地,所述混合气体中氧气的分压在致密化区域段为0.01-1.5%,例如可以是0.01%、0.05%、0.1%、0.2%、0.3%、0.4%、0.5%、0.6%、0.7%、0.8%、0.9%、1.0%、1.1%、1.2%、1.3%、1.4%或1.5%,但不限于所列举的数值,数值范围内其它未列举的数值同样适用,优选为0.05-1.5%。
本发明烧结升温过程中的950-1100℃温度区间为烧结过程中所述的致密化区域段,通过控制该致密化区域段的氧气分压为0.01-1.5%,使制备而得的MnZn铁氧体综合性能优异,当氧分压高于1.5%,所制备得到的MnZn功率铁氧体的损耗增大且强度降低。
作为本发明第二方面所述制备方法的优选技术方案,所述制备方法包括:
(1)按配方量称取主成分制备原料,一次砂磨20-60min使粒度为0.6-1.5μm,再一次喷雾造粒制备得到颗粒料,在800-1030℃预烧3-9h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨1-3h,得到平均粒径为1.05-1.3μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成粒径为50-200μm的颗粒,成型为坯件,然后于1290-1360℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为0.01-1.5%。
第三方面,本发明提供了一种如第一方面所述宽温低损耗高强度MnZn功率铁氧体的应用,所述宽温低损耗高强度MnZn功率铁氧体用于变压器。
本发明所述的数值范围不仅包括上述例举的点值,还包括没有例举出的上述数值范围之间的任意的点值,限于篇幅及出于简明的考虑,本发明不再穷尽列举所述范围包括的具体点值。
与现有技术相比,本发明的有益效果为:
本发明通过调节组成成分和改善制备方法得到一种宽温低损耗高强度MnZn功率铁氧体。该宽温低损耗高强度MnZn功率铁氧体在100kHz、200mT的条件下,25℃功耗≤350mW/cm3,120℃功耗≤350mW/cm3;在1194A/m、50Hz的条件下,25℃的饱和磁通密度≥535mT。本发明能很好的满足器件对MnZn功率铁氧体宽温低损耗高强度要求且生产工艺具有生产成本低、工艺稳定的优点。
具体实施方式
下面结合通过具体实施方式来进一步说明本发明的技术方案。但下述的实例仅仅是本发明的简易例子,并不代表或限制本发明的权利保护范围,本发明的保护范围以权利要求书为准。
实施例1
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成,所述辅助成分的质量为所述主成分的0.49wt%,所述主成分为Fe2O3:52.5mol%、MnO:37mol%、ZnO:10.5mol%;所述辅助成分分为第一辅助成分与第二辅助成分;以所述主成分的总质量为基准,所述第一辅助成分为Co2O3:0.35wt%,所述第二辅助成分为CaCO3:0.04wt%、Nb2O5:0.03wt%、V2O5:0.05wt%、MoO3:0.02wt%。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法包括如下步骤:
(1)按配方量称取主成分制备原料,一次砂磨50min使粒度为0.6-1.5μm,再一次喷雾造粒制备得到颗粒料,在990℃预烧5h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨2h,得到平均粒径为1.15μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成平均粒径为100μm的颗粒,成型为坯件(H25×15×8),然后于1320℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为0.5%。
实施例2
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成,所述辅助成分的质量为所述主成分的0.407wt%,所述主成分为Fe2O3:52mol%、MnO:36mol%、ZnO:12mol%;所述辅助成分分为第一辅助成分与第二辅助成分;以所述主成分的总质量为基准,所述第一辅助成分为Co2O3:0.3wt%,所述第二辅助成分为CaCO3:0.035wt%、Nb2O5:0.02wt%、V2O5:0.042wt%、MoO3:0.01wt%。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法包括如下步骤:
(1)按配方量称取主成分制备原料,一次砂磨40min使粒度为0.6-1.5μm,再一次喷雾造粒制备得到颗粒料,在960℃预烧6h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨1.5h,得到平均粒径为1.1μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成平均粒径为80μm的颗粒,成型为坯件(H25×15×8),然后于1300℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为0.05%。
实施例3
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成,所述辅助成分的质量为所述主成分的0.538wt%,所述主成分为Fe2O3:53mol%、MnO:37.5mol%、ZnO:9.5mol%;所述辅助成分分为第一辅助成分与第二辅助成分;以所述主成分的总质量为基准,所述第一辅助成分为Co2O3:0.37wt%,所述第二辅助成分为CaCO3:0.048wt%、Nb2O5:0.035wt%、V2O5:0.06wt%、MoO3:0.025wt%。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法包括如下步骤:
(1)按配方量称取主成分制备原料,一次砂磨55min使粒度为0.6-1.5μm,再一次喷雾造粒制备得到颗粒料,在1020℃预烧4h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨2.5h,得到平均粒径为1.2μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成平均粒径为150μm的颗粒,成型为坯件(H25×15×8),然后于1360℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为1%。
实施例4
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成,所述辅助成分的质量为所述主成分的0.61wt%,所述主成分为Fe2O3:54mol%、MnO:38mol%、ZnO:8mol%;所述辅助成分分为第一辅助成分与第二辅助成分;以所述主成分的总质量为基准,所述第一辅助成分为Co2O3:0.4wt%,所述第二辅助成分为CaCO3:0.07wt%、Nb2O5:0.04wt%、V2O5:0.07wt%、MoO3:0.03wt%。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法包括如下步骤:
(1)按配方量称取主成分制备原料,一次砂磨60min使粒度为0.6-1.5μm,再一次喷雾造粒制备得到颗粒料,在1030℃预烧3h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨3h,得到平均粒径为1.3μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成平均粒径为200μm的颗粒,成型为坯件(H30×18×10),然后于1360℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为1.5%。
实施例5
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第一辅助成分中Co2O3的含量为主成分的0.36wt%,辅助成分的质量为所述主成分的0.5wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例6
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第一辅助成分中Co2O3的含量为主成分的0.3wt%,辅助成分的质量为所述主成分的0.44wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例7
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第二辅助成分中V2O5的含量为主成分的0.04wt%,辅助成分的质量为所述主成分的0.54wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例8
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第二辅助成分中V2O5的含量为主成分的0.075wt%,辅助成分的质量为所述主成分的0.465wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例9
本实施例了提供一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第二辅助成分中MoO3的含量为主成分的0.005wt%外,辅助成分的质量为所述主成分的0.475wt%,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例10
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第二辅助成分中MoO3的含量为主成分的0.035wt%外,辅助成分的质量为所述主成分的0.455wt%,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
实施例11
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体的组成与实施例1相同。
除了制备方法中的烧结温度为1250℃外,所述宽温低损耗高强度MnZn功率铁氧体的其余制备方法的工艺参数均与实施例1相同。
实施例12
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体的组成与实施例1相同。
除了制备方法中的烧结温度为1390℃外,所述宽温低损耗高强度MnZn功率铁氧体的其余制备方法的工艺参数均与实施例1相同。
实施例13
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体的组成与实施例1相同。
除了制备方法中除氧气分压为2%外,所述宽温低损耗高强度MnZn功率铁氧体的其余制备方法的工艺参数均与实施例1相同。
实施例14
本实施例提供了一种宽温低损耗高强度MnZn功率铁氧体,所述宽温低损耗高强度MnZn功率铁氧体的组成与实施例1相同。
除了制备方法中氧气分压为4%外,所述宽温低损耗高强度MnZn功率铁氧体的其余制备方法的工艺参数均与实施例1相同。
对比例1
本对比例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了以主成分的质量为基准时,第一辅助成分中Co2O3的含量为主成分的0.45wt%,辅助成分的质量为所述主成分的0.59wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
对比例2
本对比例提供了一种宽温低损耗高强度MnZn功率铁氧体,除了不含有第一辅助成分Co2O3,辅助成分的质量为所述主成分的0.14wt%外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
对比例3
本对比例提供了一种宽温低损耗高强度MnZn功率铁氧体,除用等质量的Ni2O3替代Co2O3外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
对比例4
本对比例提供了一种宽温低损耗高强度MnZn功率铁氧体,除用等质量的Cr2O3替代V2O5外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
对比例5
本对比例提供了一种宽温低损耗高强度MnZn功率铁氧体,除用等质量的Cr2O3替代MoO3外,其余成分与含量与实施例1相同。
所述宽温低损耗高强度MnZn功率铁氧体的制备方法的工艺参数与实施例1相同。
对实施例1-14以及对比例1-5提供的宽温低损耗高强度MnZn功率铁氧体使用X荧光分析仪,检测铁氧体的组成与原料组成一致,测试饱和磁通密度(Bs)、功耗以及强度。使用IWATSU-8258交流B-H分析仪在50Hz、1194A/m条件下测试的宽温低损耗高强度MnZn功率铁氧体的饱和磁通密度。使用IWATSU-8218交流B-H分析仪在100kHz、200mT条件下测试铁氧体的功耗。使用NK-500强度测试仪在20mm/min、M法条件下测试铁氧体的强度,所得结果如表1所示。
表1
由表1的实施例1-4可知,本发明提供的一种宽温低损耗高强度MnZn功率铁氧体的制备方法能够得到在25-120℃范围内具有336mW/cm3以下的低损耗和102N以上的高强度的宽温低损耗高强度MnZn功率铁氧体。
由实施例5、6与实施例1的比较可知,实施例5制备的宽温低损耗高强度MnZn功率铁氧体与实施例1的性能相似,实施例6制备的宽温低损耗高强度MnZn功率铁氧体性能不如实施例1,当辅助成分Co2O3添加含量超出0.35-0.4wt%优选范围时,功耗增加且强度降低。
由实施例7、8与实施例1的比较可知,当辅助成分V2O5添加含量超出0.042-0.07wt%的优选范围时,所得宽温低损耗高强度MnZn功率铁氧体的功耗增加且强度降低。
由实施例9、10与实施例1的比较可知,实施例9、10所得宽温低损耗高强度MnZn功率铁氧体的性能较实施例1差,辅助成分MoO3的优选添加量为主成分的0.01-0.03wt%,当MoO3的添加量超出范围时,所得宽温低损耗高强度MnZn功率铁氧体的功耗增加且强度降低。
由实施例11、12与实施例1的比较可知,实施例11制备的宽温低损耗高强度MnZn功率铁氧体较实施例1功耗高且强度低,实施例12制备的宽温低损耗高强度MnZn功率铁氧体较实施例1强度低,当烧结温度超出1290-1360℃的优选范围时,所得宽温低损耗高强度MnZn功率铁氧体的功耗增加或者强度降低。
由实施例13、14与实施例1的比较可知,实施例13、14制备的宽温低损耗高强度MnZn功率铁氧体性能不如实施例1,由此可知,当氧气分压超出0.01-1.5%的优选范围时,所得宽温低损耗高强度MnZn功率铁氧体的功耗增加或者强度降低。
由对比例1-3与实施例1的比较可知,对比例1-3制备的宽温低损耗高强度MnZn功率铁氧体性能远不如实施例1,且对比例2和3的性能不如对比例1,辅助成分中Co2O3需要控制为主成分的0.1-0.4wt%,优选为0.1-0.35wt%。同时,当辅助成分中不添加Co2O3时,所得宽温低损耗高强度MnZn功率铁氧体的性能最差。
由对比例4、5与实施例1的比较可知,辅助成分中的V、Mo与Co、Ca或Nb存在协同作用,使用其它元素对V与Mo进行等质量替换,所得得宽温低损耗高强度MnZn功率铁氧体的性能降低。
综上所述,本发明通过对宽温低损耗高强度MnZn功率铁氧体中特定含量的辅助成分的添加及其协同作用,得到能够在100kHz及200mT的条件下,25℃时的功耗≤350mW/cm3,宽温25-120℃下具有低损耗、高磁通密度时的功耗≤350mW/cm3;在1194A/m及50Hz的条件下,25℃时的饱和磁通密度≥535mT;并且强度提升10%以上的宽温低损耗高强度MnZn功率铁氧体,满足汽车电子产品对宽温低损耗以及高强度的性能要求。
本发明通过上述实施例来说明本发明的详细结构特征,但本发明并不局限于上述详细结构特征,即不意味着本发明必须依赖上述详细结构特征才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明所选用部件的等效替换以及辅助部件的增加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。
Claims (25)
1.一种宽温低损耗高强度MnZn功率铁氧体,其特征在于,所述宽温低损耗高强度MnZn功率铁氧体由主成分和辅助成分组成;
所述辅助成分的质量为所述主成分的0.4-0.61wt%;
以摩尔百分数计,所述主成分包括:
Fe2O3 51-54mol%
MnO 35-38mol%
ZnO 8-14mol%;
以所述主成分的总质量为基准,所述辅助成分为:
所述宽温低损耗高强度MnZn功率铁氧体由如下方法制备得到:
(1)按配方量称取主成分制备原料,对主成分制备原料进行一次砂磨、一次喷雾造粒和预烧,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合后得到混合料,进行二次砂磨,得到二次砂磨料;
(3)步骤(2)所得二次砂磨料依次进行二次喷雾造粒、成型与烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;
所述烧结的温度为1290-1360℃,所述烧结过程在氧气和氮气的混合气体环境下进行,氧气在混合气体中的分压在致密化区域段为0.01-1.5%,烧结升温过程中的950-1100℃温度区间为烧结过程中所述的致密化区域段。
2.根据权利要求1所述的宽温低损耗高强度MnZn功率铁氧体,其特征在于,以摩尔百分数计,所述主成分包括:
Fe2O3 52-53mol%
MnO 36-38mol%
ZnO 9-12mol%。
3.一种如权利要求1或2所述宽温低损耗高强度MnZn功率铁氧体的制备方法,其特征在于,所述制备方法包括:
(1)按配方量称取主成分制备原料,对主成分制备原料进行一次砂磨、一次喷雾造粒和预烧,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合后得到混合料,进行二次砂磨,得到二次砂磨料;
(3)步骤(2)所得二次砂磨料依次进行二次喷雾造粒、成型与烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结的温度为1290-1360℃,所述烧结过程在氧气和氮气的混合气体环境下进行,所述混合气体中氧气的分压在致密化区域段为0.01-1.5%,烧结升温过程中的950-1100℃温度区间为烧结过程中所述的致密化区域段。
4.根据权利要求3所述的制备方法,其特征在于,步骤(1)中所述一次砂磨的时间为20-60min。
5.根据权利要求4所述的制备方法,其特征在于,步骤(1)中所述一次砂磨的时间为40-60min。
6.根据权利要求3所述的制备方法,其特征在于,步骤(1)所述一次砂磨时主成分制备原料与溶剂的质量比为(1.8-2.2):1。
7.根据权利要求6所述的制备方法,其特征在于,所述溶剂包括去离子水。
8.根据权利要求3所述的制备方法,其特征在于,步骤(1)所述一次砂磨后的粒度为0.6-1.5μm。
9.根据权利要求3所述的制备方法,其特征在于,步骤(1)所述一次喷雾造粒制备成颗粒料。
10.根据权利要求3所述的制备方法,其特征在于,步骤(1)所述预烧的温度为800-1030℃。
11.根据权利要求10所述的制备方法,其特征在于,步骤(1)所述预烧的温度为960-1020℃。
12.根据权利要求3所述的制备方法,其特征在于,步骤(1)所述预烧的时间为3-9h。
13.根据权利要求12所述的制备方法,其特征在于,步骤(1)所述预烧的时间为3-6h。
14.根据权利要求3所述的制备方法,其特征在于,步骤(2)所述二次砂磨时混合料与溶剂的质量比为2:(0.9-1.1)。
15.根据权利要求14所述的制备方法,其特征在于,所述溶剂包括去离子水或蒸馏水。
16.根据权利要求3所述的制备方法,其特征在于,步骤(2)所述二次砂磨的时间为1-3h。
17.根据权利要求16所述的制备方法,其特征在于,步骤(2)所述二次砂磨的时间为2-3h。
18.根据权利要求3所述的制备方法,其特征在于,步骤(2)所述二次砂磨的平均粒径为1.05-1.30μm。
19.根据权利要求3所述的制备方法,其特征在于,步骤(3)所述二次喷雾造粒的平均粒径为50-200μm。
20.根据权利要求3所述的制备方法,其特征在于,步骤(3)所述二次喷雾造粒的平均粒径为80-150μm。
21.根据权利要求3所述的制备方法,其特征在于,步骤(3)所述烧结的温度为1300-1360℃。
22.根据权利要求3所述的制备方法,其特征在于,步骤(3)所述烧结的时间为28-32h。
23.根据权利要求3所述的制备方法,其特征在于,所述混合气体中氧气的分压在致密化区域段为0.05-1.5%。
24.根据权利要求3所述的制备方法,其特征在于,所述制备方法包括:
(1)按配方量称取主成分制备原料,一次砂磨20-60min使粒度为0.6-1.5μm,然后,经一次喷雾造粒制备得到颗粒料,在800-1030℃预烧3-9h,得到预烧料;
(2)按配方量称量辅助成分,与步骤(1)所得预烧料混合添加溶剂后,二次砂磨1-3h,得到平均粒径为1.05-1.30μm的二次砂磨料;
(3)步骤(2)所得二次砂磨料进行二次喷雾造粒成平均粒径为50-200μm的颗粒,成型,然后于1290-1360℃烧结,得到所述宽温低损耗高强度MnZn功率铁氧体;所述烧结在氧气和氮气的混合气氛下进行,混合气氛中氧气的分压为0.01-1.5%。
25.一种如权利要求1或2所述宽温低损耗高强度MnZn功率铁氧体的应用,其特征在于,所述宽温低损耗高强度MnZn功率铁氧体用于变压器。
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