CN107098692B - 一种高强度镍锌软磁磁芯的制备方法 - Google Patents
一种高强度镍锌软磁磁芯的制备方法 Download PDFInfo
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- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000000498 ball milling Methods 0.000 claims abstract description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000007921 spray Substances 0.000 claims abstract description 19
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 18
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 18
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000465 moulding Methods 0.000 claims abstract description 13
- 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 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 239000004576 sand Substances 0.000 claims abstract description 11
- 238000003801 milling Methods 0.000 claims abstract description 10
- 238000005453 pelletization Methods 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 72
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 15
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000005751 Copper oxide Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910000431 copper oxide Inorganic materials 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 15
- 238000005516 engineering process Methods 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000013459 approach Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000004575 stone Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
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- 239000000443 aerosol Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种高强度镍锌软磁磁芯的制备方法，采用三氧化二铋、二氧化钛、五氧化二铌、二氧化硅适量掺杂改性配方及改变掺杂工艺途径技术，在配方中加入五氧化二铌、二氧化钛，在二次球磨中加入二氧化硅、三氧化二铋。按照混合、球磨、预烧、二次球磨、砂磨、喷雾、成型、烧结的操作程序进行工业生产，采用压力式喷雾造球、料浆配以适量粘度及比例技术，通过建立三氧化二铁纯度、比表面积等与预烧温度之间的关系曲线计算得到预烧温度，能够根据每批产品的特性精准控制预烧温度。本发明中对配方进行了优化，改进生产工艺，改善生产流程，有效提高了磁芯强度、提升了生产效率，并且大幅降低了生产能耗，大幅度提高了成品率。
Description
一种高强度镍锌软磁磁芯的制备方法
技术领域
本发明涉及电子元器件生产领域，尤其涉及的是一种高强度镍锌软磁磁芯的方法。
背景技术
随着电子技术的发展，电子元器件逐渐向小型化、轻量化、高频化、大电流、低EMI和低制造成本，以及高可靠性发展，很多镍锌软磁磁芯产品要求用智能化机器人或者机器手来制造电感。而智能设备对磁芯的机械强度普遍要求高。目前国内生产的SMD磁芯存在强度普遍偏低之缺陷，严重困扰电感制造业一直没有解决的磁芯破裂、暗裂电感进入下游机板使主机产生事故问题。与此同时，国内大多数生产镍锌软磁厂商主要设备普遍采用国内的廉价的喷塔、窑炉等。如果要采用日本昂贵的主要设备，投资壁垒较高，很难普及。满足市场要求的高强度镍锌软磁磁芯很难大工业产业化。
因而现有技术还有待改进和提高。
发明内容
鉴于以上技术缺陷和壁垒，本发明的目的在于提供一种高强度镍锌软磁磁芯的制备方法，旨在解决现有技术中磁芯强度普遍偏低，生产制造过程中磁芯破裂、暗裂电感、能耗高的问题。
为了达到上述目的，本发明采取了以下技术方案：
一种高强度镍锌软磁磁芯的制备方法，其中，包括以下步骤：
S1、筛选获取达指定纯度的三氧化二铁、氧化锌、氧化亚镍、氧化铜、三氧化二铋、五氧化二铌、二氧化硅；
S2、按照三氧化二铁48.34mol%，氧化锌24.69mol%-28mol%，氧化亚镍17.4mol%-20.52mol%，氧化铜5.68mol%-6.386mol%，五氧化二铌0.02wt%，二氧化钛0.1wt%混合0.5小时，得到初始原材料；
S3、将初始原材料按照球料比6:1球磨0.75-1.25小时，得到球磨后材料；
S4、将球磨后材料加热进行预烧，预烧温度为830℃-990℃，保温时间大于2.5小时，得到预烧后材料；
S5、将预烧后材料按照球料比6:1，同时加入三氧化二铋0.3wt%、二氧化硅0.15wt%,二次球磨0.75-1.25小时，得到二次球磨后材料；
S6、将二次球磨后材料按照球料比6:1砂磨1.75-2.25小时，得到砂磨后材料；
S7、将砂磨后材料采用压力式喷雾造球，其中压力为1.6MPa-2.0MPa，料浆粘度为18-20mpa.s，得到喷雾后材料；
S8、将喷雾后材料采用软磁磁芯模具进行成型，得到成型半成品，其中成型半成品的密度为3.0-3.2g/cm3；
S9、将成型半成品进行二次烧结得到高强度镍锌软磁磁芯，其中二次烧结温度为1060℃-1160℃，且二次烧结的保温时间大于2.5小时。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S3中将初始原材料按照球料比6:1球磨1小时，得到球磨后材料。
所述高强度镍锌软磁磁芯的制备方法，其中，所述球磨后材料的平均粒径为2µm。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S4中，当三氧化二铁纯度为99.3%、比表面积为7m2/g，预烧温度为830℃；三氧化二铁纯度为99.1%、比表面积为2 m2/g，预烧温度为990℃。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S4中采用中性烧结，氧分压为19～21%。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S5具体包括：
S501、在预烧后材料中加入三氧化二铋0.3wt%和二氧化硅0.15wt%；
S502、按照球料比6:1二次球磨1小时，得到二次球磨后材料。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S6中砂磨的时间为2小时，得到的砂磨后材料的平均粒径为1±0.3µm，砂磨后材料的固体含量为55%-62%。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S7中压力式喷雾造球采用喷塔，喷塔喷出的喷雾目数在60目-180目之间，其中80目-120目为正态分布，松装比重为1.25-1.4 g/cm3。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S9中二次烧结采用中性烧结，氧分压为19～21%。
所述高强度镍锌软磁磁芯的制备方法，其中，所述步骤S8中成型半成品的成型密度为3.0-3.2 g/mm3。
相较于现有技术，本发明采用国内普通的主要设备，采用市售的基础材料，采用廉价的仪器如光谱仪等建立对市售基础材料的简单易行的甄别及检验标准，能大幅提高甄别率；建立三氧化二铁纯度、比表面积等与预烧温度之间的关系曲线，通过关系曲线做精确推算，使每批三氧化二铁都能适合本企业模具、都能适合切削工装等预烧温度、都能符合松重标准；采用三氧化二铋、二氧化钛、五氧化二铌、二氧化硅多施主适量掺杂改性配方及改变掺杂工艺途径技术，在配方中加入五氧化二铌、二氧化钛在二次球磨中加入二氧化硅、三氧化二铋等；在预烧、烧结中采用中性烧结—氧分压19-21%烧结技术，使生产成本得到大幅降低；采用压力式喷雾造球、料浆配以适量粘度及比例技术，实现大工业产业化，使磁芯强度和生产效率得到大幅度提高，使能耗和破损率得到大幅度降低；本磁芯的研发，对我国电感行业的发展起到举足轻重的作用，将彻底解决国内一直没有解决的破裂、暗裂电感进入下游机板使主机产生事故问题，具有划时代的经济效益和社会效益。
附图说明
图1为本发明提供的高强度镍锌软磁磁芯的制备方法较佳实施例的流程图。
具体实施方式
本发明提供一种高强度镍锌软磁磁芯的制备方法，为使本发明的目的、技术方案及效果更加清楚、明确，以下参照附图并举实施例对本发明进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
请参阅图1，其为本发明提供的高强度镍锌软磁磁芯的制备方法较佳实施例的流程图。如图1所示，所述高强度镍锌软磁磁芯的制备方法，包括以下步骤：
S1、筛选获取达指定纯度的三氧化二铁、氧化锌、氧化亚镍、氧化铜、三氧化二铋、五氧化二铌、二氧化硅、二氧化钛；
S2、按照三氧化二铁48.34mol%，氧化锌24.69mol%-28mol%，氧化亚镍17.4mol%-20.52mol%，氧化铜5.68mol%-6.386mol%，五氧化二铌0.02wt%,二氧化钛0.1wt%混合0.5小时，得到初始原材料；
S3、将初始原材料按照球料比6:1球磨0.75-1.25小时，得到球磨后材料；
S4、将球磨后材料加热进行预烧，预烧温度为830℃-990℃，保温时间大于2.5小时，得到预烧后材料；
S5、将预烧后材料按照球料比6:1，同时加入三氧化二铋0.3wt%、二氧化硅0.15wt%,二次球磨0.75-1.25小时，得到二次球磨后材料；
S6、将二次球磨后材料按照球料比6:1砂磨1.75-2.25小时，得到砂磨后材料；
S7、将砂磨后材料采用压力式喷雾造球，其中压力为1.6MPa-2.0MPa，料浆粘度为18-20mpa.s，得到喷雾后材料；
S8、将喷雾后材料采用软磁磁芯模具进行成型，得到成型半成品，其中成型半成品的密度为3.0-3.2g/cm3；
S9、将成型半成品进行二次烧结得到高强度镍锌软磁磁芯，其中二次烧结温度为1060℃-1160℃，且二次烧结的保温时间大于2.5小时。
本发明的实施例中，在步骤S1中采用廉价的仪器如光谱仪等建立对市售基础材料（主要是制作软磁磁芯的材料，如三氧化二铁、氧化锌、氧化亚镍、氧化铜、三氧化二铋、五氧化二铌、二氧化硅等）的简单易行的甄别及检验标准，能大幅提高甄别率（国内同类产品没有建立对市售基础材料的简单易行的甄别及检验标准，市售基础材料甄别率低）；将通过甄别，并达到标准的基础材料用于进一步的制作高强度镍锌软磁磁芯。
更具体的，在步骤S1中对包括三氧化二铁、氧化锌、氧化亚镍、氧化铜、三氧化二铋、五氧化二铌、二氧化硅的基础材料进行筛选时，采用如表1中的仪器：
表1
三氧化二铁检测标准表如表2所示，其中的阴离子用化学的办法测量。用溶积法测定Fe2O3的纯度、用化学法测定含Cl1﹣、SO4 2-、SiO2等的含量：
表2
氧化锌检验标准表如表3所示：
表3
氧化亚镍检验标准表如表4所示：
表4
氧化铜检验标准表如表5所示：
表5
三氧化二铋检验标准表如表6所示：
表6
五氧化二铌、超细二氧化硅、二氧化钛检验标准按市售分析纯即可。
在步骤S2中采用三氧化二铋、二氧化钛、五氧化二铌、二氧化硅多施主适量掺杂改性配方及改变掺杂工艺途径技术，在配方中加入五氧化二铌、二氧化钛在二次球磨中加入二氧化硅、三氧化二铋等。优化配方及改性掺杂，各组分对感生各向异性常数K1及磁致伸缩系数λs 的影响。现有技术中，国内同类产品主要配方为三氧化二铋、三氧化二铁、氧化锌、氧化亚镍、氧化铜，没有改性掺杂，对制造设备和工艺要求苛刻。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S3中将初始原材料按照球料比6:1球磨1小时，得到球磨后材料。较佳的，所述球磨后材料的平均粒径为2µm。其中，球料比表示球磨机中球的重量与原料的重量之比。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S4中，当三氧化二铁纯度为99.3%、比表面积为7m2/g，预烧温度为830℃；三氧化二铁纯度为99.1%、比表面积为2m2/g，预烧温度为990℃。
在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S4中采用中性烧结，氧分压为19～21%。所述步骤S9中二次烧结采用中性烧结，氧分压为19～21%。步骤S4中及步骤S9中采用中性烧结，使生产成本得到大幅降低（现有技术同类产品在预烧、烧结中采用日本10～18米回转管电气窑、日本日立公司的强排风气雾连电气隧道窑烧结技术，生产成本高）。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S5具体包括：
S501、在预烧后材料中加入三氧化二铋0.3wt%和二氧化硅0.15wt%；
S502、按照球料比6:1二次球磨1小时，得到二次球磨后材料。
其中，步骤S501中加入的三氧化二铋和二氧化硅可合称为加小料。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S6中砂磨的时间为2小时，得到的砂磨后材料的平均粒径为1±0.3µm，砂磨后材料的固体含量为55%-62%，加入胶水的干胶比为1.4-2.0%。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S7中压力式喷雾造球采用喷塔，喷塔喷出的喷雾目数在60目-180目之间，其中80目-120目为正态分布，松装比重为1.25-1.4 g/cm3。采用压力式喷雾造球、料浆配以适量粘度及比例技术，实现大工业产业化，使磁芯强度和生产效率得到大幅度提高，使能耗和破损率得到大幅度降低（现有技术同类产品为了提高磁芯强度，必须使用昂贵的离心式喷塔造料技术，能耗高，破损率高，生产效率低，其能耗大约是压力式的2.5倍）。
优选的，在所述高强度镍锌软磁磁芯的制备方法中，所述步骤S8中成型半成品的成型密度为3.0-3.2 g/cm3。
通过本发明所述的高强度镍锌软磁磁芯的制备方法，制备得到的高强度镍锌软磁磁芯，检验结果如下：
1、在生产成本基本不变的前题下，磁芯强度比现有技术同类产品高40%，对于CD5845B2.2磁芯，强度为2.6～3.0㎏,检验办法按常规办法。
2、在生产成本基本不变的前题下，磁芯电气性能Bs≥ 450mT,比现有技术的同类产品的420mT高7%；其检验办法用标准环T25*15*12绕Ø0.55mm铜线10匝测试。
3、在生产成本基本不变的前题下，磁芯居里温度≥250℃，比现有技术的同类产品的220℃高13.6%；其检验办法用标准环T25*15*12绕Ø0.55铜线10匝测试。
4、在成本不变的前题下，磁芯密度ρ≥5.1g/cm3，比现有技术的同类产品的4.9g/cm3高4.1%；用密度仪测试。
5、在成本不变的前题下，磁芯表面电阻率ρ0≥109mΩ*m，比现有技术的同类产品的107 mΩ*m高10倍；用表面电阻仪测试。
可以理解的是，对本领域普通技术人员来说，可以根据本发明的技术方案及其发明构思加以等同替换或改变，而所有这些改变或替换都应属于本发明所附的权利要求的保护范围。
Claims (9)
1.一种高强度镍锌软磁磁芯的制备方法，其特征在于，包括以下步骤：
S1、筛选获取达指定纯度的三氧化二铁、氧化锌、氧化亚镍、氧化铜、三氧化二铋、五氧化二铌、二氧化硅、二氧化钛；
S2、按照三氧化二铁48.34mol%，氧化锌24.69mol%-28mol%，氧化亚镍17.4mol%-20.52mol%，氧化铜5.68mol%-6.386mol%，五氧化二铌0.02wt%，二氧化钛0.1wt%混合0.5小时，得到初始原材料；
S3、将初始原材料按照球料比6:1球磨0.75-1.25小时，得到球磨后材料；
S4、将球磨后材料加热进行预烧，预烧温度为830℃-990℃，保温时间大于2.5小时，得到预烧后材料；
S5、将预烧后材料按照球料比6:1，同时加入三氧化二铋0.3wt%、二氧化硅0.15wt%,二次球磨0.75-1.25小时，得到二次球磨后材料；
S6、将二次球磨后材料按照球料比6:1砂磨1.75-2.25小时，得到砂磨后材料；
S7、将砂磨后材料采用压力式喷雾造球，其中压力为1.6MPa-2.0MPa，料浆粘度为18-20mpa.s，得到喷雾后材料；
S8、将喷雾后材料采用软磁磁芯模具进行成型，得到成型半成品，其中成型半成品的密度为3.0-3.2g/cm3；
S9、将成型半成品进行二次烧结得到高强度镍锌软磁磁芯，其中二次烧结温度为1060℃-1160℃，且二次烧结的保温时间大于2.5小时。
2.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S3中将初始原材料按照球料比6:1球磨1小时，得到球磨后材料。
3.根据权利要求2所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述球磨后材料的平均粒径为2µm。
4.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S4中，当三氧化二铁纯度为99.3%、比表面积为7m2/g，预烧温度为830℃；三氧化二铁纯度为99.1%、比表面积为2 m2/g，预烧温度为990℃。
5.根据权利要求4所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S4中采用中性烧结，氧分压为19～21%。
6.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S5具体包括：
S501、在预烧后材料中加入三氧化二铋0.3wt%和二氧化硅0.15wt%；
S502、按照球料比6:1二次球磨1小时，得到二次球磨后材料。
7.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S6中砂磨的时间为2小时，得到的砂磨后材料的平均粒径为1±0.3µm，砂磨后材料的固体含量为55%-62%。
8.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S7中的压力式喷雾造球采用喷塔，喷塔喷出的喷雾目数在60目-180目之间，其中80目-120目为正态分布，松装比重为1.25-1.4 g/cm3。
9.根据权利要求1所述高强度镍锌软磁磁芯的制备方法，其特征在于，所述步骤S9中二次烧结采用中性烧结，氧分压为19～21%。
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| CN101891456B (zh) * | 2010-06-22 | 2013-06-05 | 广东风华高新科技股份有限公司 | 一种高抗折强度镍锌软磁铁氧体材料及其制造方法 |
| CN102276245B (zh) * | 2011-06-29 | 2013-03-27 | 广东风华高新科技股份有限公司 | 一种耐高温焊锡镍锌软磁铁氧体材料 |
| CN102690109B (zh) * | 2012-03-19 | 2014-06-04 | 横店集团东磁股份有限公司 | 一种软磁镍铜锌铁氧体材料及其制备方法 |
| CN106495677A (zh) * | 2016-10-10 | 2017-03-15 | 电子科技大学 | 一种高强度耐热冲击功率镍锌铁氧体及其制备方法 |
| CN106587977B (zh) * | 2016-11-17 | 2019-07-09 | 横店集团东磁股份有限公司 | 一种功率型镍锌铁氧体材料及其制备方法 |
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