CN116606129A - 一种高磁导率铁氧体磁性材料的制备方法 - Google Patents
一种高磁导率铁氧体磁性材料的制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 50
- 239000000696 magnetic material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 38
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000002019 doping agent Substances 0.000 claims abstract description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 19
- 239000000378 calcium silicate Substances 0.000 claims abstract description 19
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 19
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 19
- 239000011787 zinc oxide Substances 0.000 claims abstract description 19
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims abstract description 14
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 14
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 14
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 14
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 14
- 238000007689 inspection Methods 0.000 claims abstract description 12
- 230000035699 permeability Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000008676 import Effects 0.000 claims abstract description 6
- 238000012797 qualification Methods 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims description 53
- 238000005245 sintering Methods 0.000 claims description 44
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004321 preservation Methods 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 230000004907 flux Effects 0.000 abstract description 3
- 230000005415 magnetization Effects 0.000 abstract 1
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 6
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 6
- 239000011162 core material Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 230000002035 prolonged effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种高磁导率铁氧体磁性材料的制备方法,具体制备方法步骤如下:步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂具有较好的磁化强度和矫顽力,饱和磁通密度较大,可显著提高铁氧体材料的磁导率。
Description
技术领域
本发明属于磁性材料生产技术领域,具体涉及一种高磁导率铁氧体磁性材料的制备方法。
背景技术
锰锌铁氧体是软磁铁氧体的一种,属尖晶石型结构,由铁、锰、锌的氧化物及其盐类,采用陶瓷工艺制成,它具有高的起始导磁率,一般在1千赫至10兆赫的频率范围内使用,可制作电感器、变压器、滤波器的磁芯、磁头及天线棒,通常被称为铁氧体磁芯,软磁铁氧体材料是电子工业及信息产业的基础材料,应用广泛。
随着开关电源开关频率发展得越来越高,对于应用在其中的变压器而言,磁芯材料需要采用比金属磁性材料电阻率更高的软磁铁氧体材料,锰锌铁氧体因其高起始磁导率、高饱和磁感应强度、低功耗等优点一直被广泛地用作开关电源中的变压器磁芯材料,但随着开关电源的开关频率向着MHz级的高频方向发展,传统锰锌铁氧体因其较低的电阻率,其在高频环境下涡流损耗变得显著,其原有的优势也不再明显,现有化学共沉淀法制备锰锌铁氧体过程中对前驱体溶液的配制有很多种方法,但是所得前驱体的粒度较高,均匀性也较差而且最终所得的铁氧体的磁导率μi一般在10000-20000左右,对于高磁导率的锰锌铁氧体而言磁导率较低。
但是现有的高磁导率铁氧体磁性材料的制备方法,不能提高铁氧体材料的磁导率,不能使制得的铁氧体磁性材料含有的杂质少,提高铁氧体磁性材料的质量。
发明内容
本发明的目的在于提供一种高磁导率铁氧体磁性材料的制备方法,以解决上述背景技术中提出的现有的高磁导率铁氧体磁性材料的制备方法,不能提高铁氧体材料的磁导率,不能使制得的铁氧体磁性材料含有的杂质少,提高铁氧体磁性材料的质量的问题。
为实现上述目的,本发明提供如下技术方案:一种高磁导率铁氧体磁性材料的制备方法,具体制备方法步骤如下:
步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;
步骤二:按制备方法要求和产品配方进行配料称量,称取检测合格的相应重量份的三氧化二铁22.5-24.7重量份、氧化锌22.5-24.2重量份、氧化锰14-17重量份、碳酸钙3.7-7.2重量份、二氧化硅4.1-5.2重量份、硅酸钙2.1-2.9重量份、硫酸铁4.5-6.6重量份、硫酸锌4.2-4.6重量份、氧化镍6.4-7.6重量份;
步骤三:将相应重量份的三氧化二铁、氧化锌、氧化锰、碳酸钙、二氧化硅和硅酸钙一同加入到球磨机内进行一次球磨3-4h;
步骤四:将一次球磨产物置于高温电炉中进行预烧结,预烧结采用程序升温至600℃,保温反应3小时后,采用程序降温至400℃,然后自然降至室温,得到预烧结产物;
步骤五:按重量百分比加入以下掺杂剂:硫酸铁、硫酸锌、氧化镍和步骤四得到预烧结产物到球磨机内再加入占粉料总重量1.2%的等离子水进行球磨,球磨转速固定为200r/min,球磨4小时后烘干得到球磨产物;
步骤六:将步骤五得到的球磨产物进行分阶段烧结处理,第一阶段:从50℃升温到500~600℃,氧分压为18%;第二阶段:继续升温到700~850℃,氧分压为21%;第三阶段:继续升温到1200℃,氧分压为0.1%;第四阶段:保温阶段,以1200℃保温2~3h,氧分压为5~7%;
步骤七:将步骤六烧结产物加入到聚乙烯醇溶液中形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,然后将浆料注入模具中,压力机压制后送入电阻炉中进行烧结,烧结程序完成后自然冷却到室温后脱模即得高磁导率铁氧体磁性材料。
进一步的;所述步骤三中球磨转速固定为200r/min。
进一步的;所述步骤七中烧结程序由升温、降温、和保温三个阶段组成。
进一步的;所述步骤四中程序升温速率为3℃/min,降温速率为3.5℃/min。
进一步的;所述步骤七中聚乙烯醇溶液浓度为12wt%。
与现有技术相比,本发明的有益效果是:
1、选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂具有较好的磁化强度和矫顽力,饱和磁通密度较大,可显著提高铁氧体材料的磁导率,通过两次球磨,使原料微粒分散均匀,便于烧结充分,利用最终烧结产物混合聚乙烯醇溶液形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,快速提取铁氧体磁性材料,生产效率高,便于操作,制得的铁氧体磁性材料含有的杂质少,提高铁氧体磁性材料的质量。
2、将步骤五得到的球磨产物进行分阶段烧结处理,使其烧结更加充分,避免氧化,延长烧结的时间,并且烧结程序由升温、降温、和保温三个阶段组成,提高铁氧体磁性材料在制备过程中的稳定性,使制得的铁氧体磁性材料能够适应大多数电子设备的高磁导率频率特性及饱和磁感应强度的要求,实用性强,步骤简单,便于制备,适合广泛推广使用。
具体实施方式
下面将结合本发明实施例,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
一种高磁导率铁氧体磁性材料的制备方法,具体制备方法步骤如下:
步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;
步骤二:按制备方法要求和产品配方进行配料称量,称取检测合格的相应重量份的三氧化二铁22.5重量份、氧化锌22.5重量份、氧化锰14重量份、碳酸钙3.7重量份、二氧化硅4.1重量份、硅酸钙2.1重量份、硫酸铁4.5重量份、硫酸锌4.2重量份、氧化镍6.4重量份;
步骤三:将相应重量份的三氧化二铁、氧化锌、氧化锰、碳酸钙、二氧化硅和硅酸钙一同加入到球磨机内进行一次球磨3-4h;
步骤四:将一次球磨产物置于高温电炉中进行预烧结,预烧结采用程序升温至600℃,保温反应3小时后,采用程序降温至400℃,然后自然降至室温,得到预烧结产物;
步骤五:按重量百分比加入以下掺杂剂:硫酸铁、硫酸锌、氧化镍和步骤四得到预烧结产物到球磨机内再加入占粉料总重量1.2%的等离子水进行球磨,球磨转速固定为200r/min,球磨4小时后烘干得到球磨产物;
步骤六:将步骤五得到的球磨产物进行分阶段烧结处理,第一阶段:从50℃升温到500~600℃,氧分压为18%;第二阶段:继续升温到700~850℃,氧分压为21%;第三阶段:继续升温到1200℃,氧分压为0.1%;第四阶段:保温阶段,以1200℃保温2~3h,氧分压为5~7%;
步骤七:将步骤六烧结产物加入到聚乙烯醇溶液中形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,然后将浆料注入模具中,压力机压制后送入电阻炉中进行烧结,烧结程序完成后自然冷却到室温后脱模即得高磁导率铁氧体磁性材料。
其中;所述步骤三中球磨转速固定为200r/min。
其中;所述步骤七中烧结程序由升温、降温、和保温三个阶段组成。
其中;所述步骤四中程序升温速率为3℃/min,降温速率为3.5℃/min。
其中;所述步骤七中聚乙烯醇溶液浓度为12wt%。
实施例2
一种高磁导率铁氧体磁性材料的制备方法,具体制备方法步骤如下:
步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;
步骤二:按制备方法要求和产品配方进行配料称量,称取检测合格的相应重量份的三氧化二铁24.7重量份、氧化锌24.2重量份、氧化锰17重量份、碳酸钙7.2重量份、二氧化硅5.2重量份、硅酸钙2.9重量份、硫酸铁6.6重量份、硫酸锌4.6重量份、氧化镍7.6重量份;
步骤三:将相应重量份的三氧化二铁、氧化锌、氧化锰、碳酸钙、二氧化硅和硅酸钙一同加入到球磨机内进行一次球磨3-4h;
步骤四:将一次球磨产物置于高温电炉中进行预烧结,预烧结采用程序升温至600℃,保温反应3小时后,采用程序降温至400℃,然后自然降至室温,得到预烧结产物;
步骤五:按重量百分比加入以下掺杂剂:硫酸铁、硫酸锌、氧化镍和步骤四得到预烧结产物到球磨机内再加入占粉料总重量1.2%的等离子水进行球磨,球磨转速固定为200r/min,球磨4小时后烘干得到球磨产物;
步骤六:将步骤五得到的球磨产物进行分阶段烧结处理,第一阶段:从50℃升温到500~600℃,氧分压为18%;第二阶段:继续升温到700~850℃,氧分压为21%;第三阶段:继续升温到1200℃,氧分压为0.1%;第四阶段:保温阶段,以1200℃保温2~3h,氧分压为5~7%;
步骤七:将步骤六烧结产物加入到聚乙烯醇溶液中形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,然后将浆料注入模具中,压力机压制后送入电阻炉中进行烧结,烧结程序完成后自然冷却到室温后脱模即得高磁导率铁氧体磁性材料。
其中;所述步骤三中球磨转速固定为200r/min。
其中;所述步骤七中烧结程序由升温、降温、和保温三个阶段组成。
其中;所述步骤四中程序升温速率为3℃/min,降温速率为3.5℃/min。
其中;所述步骤七中聚乙烯醇溶液浓度为12wt%。
实施例3
一种高磁导率铁氧体磁性材料的制备方法,具体制备方法步骤如下:
步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;
步骤二:按制备方法要求和产品配方进行配料称量,称取检测合格的相应重量份的三氧化二铁23.6重量份、氧化锌23.35重量份、氧化锰15.5重量份、碳酸钙5.45重量份、二氧化硅4.65重量份、硅酸钙2.5重量份、硫酸铁5.55重量份、硫酸锌4.4重量份、氧化镍7重量份;
步骤三:将相应重量份的三氧化二铁、氧化锌、氧化锰、碳酸钙、二氧化硅和硅酸钙一同加入到球磨机内进行一次球磨3-4h;
步骤四:将一次球磨产物置于高温电炉中进行预烧结,预烧结采用程序升温至600℃,保温反应3小时后,采用程序降温至400℃,然后自然降至室温,得到预烧结产物;
步骤五:按重量百分比加入以下掺杂剂:硫酸铁、硫酸锌、氧化镍和步骤四得到预烧结产物到球磨机内再加入占粉料总重量1.2%的等离子水进行球磨,球磨转速固定为200r/min,球磨4小时后烘干得到球磨产物;
步骤六:将步骤五得到的球磨产物进行分阶段烧结处理,第一阶段:从50℃升温到500~600℃,氧分压为18%;第二阶段:继续升温到700~850℃,氧分压为21%;第三阶段:继续升温到1200℃,氧分压为0.1%;第四阶段:保温阶段,以1200℃保温2~3h,氧分压为5~7%;
步骤七:将步骤六烧结产物加入到聚乙烯醇溶液中形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,然后将浆料注入模具中,压力机压制后送入电阻炉中进行烧结,烧结程序完成后自然冷却到室温后脱模即得高磁导率铁氧体磁性材料。
其中;所述步骤三中球磨转速固定为200r/min。
其中;所述步骤七中烧结程序由升温、降温、和保温三个阶段组成;提高铁氧体磁性材料在制备过程中的稳定性,使制得的铁氧体磁性材料能够适应大多数电子设备的高磁导率频率特性及饱和磁感应强度的要求。
其中;所述步骤四中程序升温速率为3℃/min,降温速率为3.5℃/min。
其中;所述步骤七中聚乙烯醇溶液浓度为12wt%;用最终烧结产物混合聚乙烯醇溶液形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,快速提取铁氧体磁性材料,生产效率高。
本发明的工作效果:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂具有较好的磁化强度和矫顽力,饱和磁通密度较大,可显著提高铁氧体材料的磁导率,通过两次球磨,使原料微粒分散均匀,便于烧结充分,利用最终烧结产物混合聚乙烯醇溶液形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,快速提取铁氧体磁性材料,生产效率高,便于操作,制得的铁氧体磁性材料含有的杂质少,提高铁氧体磁性材料的质量。将步骤五得到的球磨产物进行分阶段烧结处理,使其烧结更加充分,避免氧化,延长烧结的时间,并且烧结程序由升温、降温、和保温三个阶段组成,提高铁氧体磁性材料在制备过程中的稳定性,使制得的铁氧体磁性材料能够适应大多数电子设备的高磁导率频率特性及饱和磁感应强度的要求,实用性强,步骤简单,便于制备,适合广泛推广使用。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种高磁导率铁氧体磁性材料的制备方法,其特征在于,具体制备方法步骤如下:
步骤一:选取三氧化二铁、氧化锌和氧化锰为主料,选取碳酸钙、二氧化硅、硅酸钙、硫酸铁、硫酸锌和氧化镍为掺杂剂,检验人员对主料和掺杂剂进行生产许可证检测,企业采购进口需法定检验的原料,应当向供货者索取有效的检验合格证明,来自合格供应商,查验供应商相关证明真实性;
步骤二:按制备方法要求和产品配方进行配料称量,称取检测合格的相应重量份的三氧化二铁22.5-24.7重量份、氧化锌22.5-24.2重量份、氧化锰14-17重量份、碳酸钙3.7-7.2重量份、二氧化硅4.1-5.2重量份、硅酸钙2.1-2.9重量份、硫酸铁4.5-6.6重量份、硫酸锌4.2-4.6重量份、氧化镍6.4-7.6重量份;
步骤三:将相应重量份的三氧化二铁、氧化锌、氧化锰、碳酸钙、二氧化硅和硅酸钙一同加入到球磨机内进行一次球磨3-4h;
步骤四:将一次球磨产物置于高温电炉中进行预烧结,预烧结采用程序升温至600℃,保温反应3小时后,采用程序降温至400℃,然后自然降至室温,得到预烧结产物;
步骤五:按重量百分比加入以下掺杂剂:硫酸铁、硫酸锌、氧化镍和步骤四得到预烧结产物到球磨机内再加入占粉料总重量1.2%的等离子水进行球磨,球磨转速固定为200r/min,球磨4小时后烘干得到球磨产物;
步骤六:将步骤五得到的球磨产物进行分阶段烧结处理,第一阶段:从50℃升温到500~600℃,氧分压为18%;第二阶段:继续升温到700~850℃,氧分压为21%;第三阶段:继续升温到1200℃,氧分压为0.1%;第四阶段:保温阶段,以1200℃保温2~3h,氧分压为5~7%;
步骤七:将步骤六烧结产物加入到聚乙烯醇溶液中形成悬浮液,将悬浮液进行球磨混合得到粉体浆料,然后将浆料注入模具中,压力机压制后送入电阻炉中进行烧结,烧结程序完成后自然冷却到室温后脱模即得高磁导率铁氧体磁性材料。
2.根据权利要求2所述的一种高磁导率铁氧体磁性材料的制备方法的生产方法,其特征在于:所述步骤三中球磨转速固定为200r/min。
3.根据权利要求2所述的一种高磁导率铁氧体磁性材料的制备方法的生产方法,其特征在于:所述步骤七中烧结程序由升温、降温、和保温三个阶段组成。
4.根据权利要求2所述的一种高磁导率铁氧体磁性材料的制备方法的生产方法,其特征在于:所述步骤四中程序升温速率为3℃/min,降温速率为3.5℃/min。
5.根据权利要求2所述的一种高磁导率铁氧体磁性材料的制备方法的生产方法,其特征在于:所述步骤七中聚乙烯醇溶液浓度为12wt%。
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