CN112321292A - 一种烧结铁氧体预烧料的制造方法 - Google Patents
一种烧结铁氧体预烧料的制造方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 26
- 238000005245 sintering Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 31
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 30
- 239000000654 additive Substances 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 13
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims abstract description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 14
- 229910052681 coesite Inorganic materials 0.000 claims description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 229910052682 stishovite Inorganic materials 0.000 claims description 12
- 229910052905 tridymite Inorganic materials 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 230000005415 magnetization Effects 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 235000015110 jellies Nutrition 0.000 abstract description 3
- 239000008274 jelly Substances 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 230000009257 reactivity Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229910052712 strontium Inorganic materials 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 3
- 235000012054 meals Nutrition 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 2
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910002402 SrFe12O19 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- -1 iron ions Chemical class 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
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明提供一种烧结铁氧体预烧料的制造方法,包括主原材料和添加剂,主原材料为铁红和碳酸锶。通过添加碳酸钙,能够促进液相烧结,解决摩尔比大于6时反应活性差、不能获得高的饱和磁化强度的问题。同时由于摩尔比大于6,预烧料经过微粉碎获得的料浆不产生胶状物,湿压成型过程中易于排水,成型效率明显提高。即通过添加碳酸钙,一方面提高了预烧料的饱和磁化强度,同时在微粉碎时,能够将粒度研磨到0.6μm及以下,充分发挥出材料应有的性能,从而获得了优异的磁体性能。
Description
技术领域
本发明涉及永磁材料技术领域,具体为一种烧结铁氧体预烧料的制造方法。
背景技术
M型永磁铁氧体按照化学成分可分为锶铁氧体和钡铁氧体。永磁铁氧体粉末在磁场中成型后烧结,可得到各向异性烧结铁氧体磁铁。作为烧结磁体使用的铁氧体材料,已知有六方晶系M型Sr铁氧体和Ba铁氧体。其通式可以表示为AO nFe2O3,n是摩尔比,A元素可以是Sr或Ba。目前应用最为广泛的是锶铁氧体。工业上,锶铁氧体是以铁红或铁鳞与碳酸锶为主要原料,通过陶瓷工艺制备得到。其理论分子式为:SrFe12O19,也就是原材料配比中Fe2O3和SrCO3的摩尔比理论值应为6。
按照成型方式的不同,可分为干法成型和湿法成型。干法成型就是将铁氧体粉末与粘结剂混合均匀后,直接在磁场中成型,成型效率高,但由于粉末间的摩擦力大,不利于粉末在磁场中转动,导致取向度差,产品性能低。相比干法成型,湿法成型时铁氧体粉末处于分散介质(水、酒精)的包围中,由于分散介质的存在,粉末在磁场中易于转动,能够获得很好的取向度,产品性能高,故湿法成型的磁铁应用十分广泛,应用领域遍及汽车,家电,电动工具、信息、医疗、玩具等领域。
对于湿法成型的工艺而已,要获得理想的性能,主要有两个途径:一是提高材料的饱和磁化强度;二是降低细磨粒度,一般来说,经湿式微粉碎得到的料浆的平均粒径越细,产品性能越高。
为了提高饱和磁化强度,以往从业技术人员一般将摩尔比设定为小于6,使晶格点阵上产生一定的空位,以提高离子扩散速度,即提高反应活性,已达到提高反应完全度的目的,从而提高性能。但是摩尔比设定小于6导致部分碳酸锶没有反应,而存留在铁氧体中。由于铁氧体的磁性来源于铁离子,故这部分存留的碳酸锶不仅对饱和磁化强度没有贡献,而且是对资源的浪费。
与此同时,为了进一步提高性能,一般而言粒度越细越好。但是当摩尔比设定小于6的预烧料在微粉碎时,特别是当平均粒度小于0.7μm,在晶界上残存的那部分碳酸锶被释放出来,和水发生反应,生成了氢氧化锶,当料浆经过长时间沉淀,就产生了大量的Sr(OH)2,形成胶状物,从而导致料浆在压型过程中,不利于水的排出,造成生产效率急剧下降。摩尔比越低,残存的碳酸锶也就越多,导致生成的氢氧化锶越多,排水越困难,生产效率下降越厉害。
而当摩尔比设定大于6,由于碳酸锶反应完全,因而在微粉碎时,没有碳酸锶被释放出来,不会形成胶状物,料浆在压型容易,效率极大提高。但是当摩尔比设定大于6,晶格点阵上的空位很少,离子扩散速度慢,即反应活性较差,不利于饱和磁化强度的提高,磁性能(特别是Br)较摩尔比小于6的更低。且富余的氧化铁容易生产α-Fe2O3相(软磁相),从而对磁性能产生不利影响。产品性能大大低于摩尔比设定小于6的情况。
因此现有技术的摩尔比一般设定为小于6,同时为了保证生产效率,从业人员只能成型料浆的粒度控制在0.7-0.8μm,再这个粒度下,无法发挥出材料的应有性能,这这就导致了材料的浪费。
综述所述,在不增加成本的情况下(即不添加稀土的情况下),现有技术无法既得到适合于大生产的、成型效率高的、同时性能优异的预烧料。
发明内容
本发明所解决的技术问题在于提供一种具有优异磁性能、同时易于成型的烧结铁氧体预烧料的制造方法,以解决上述背景技术中提出的问题。
本发明所解决的技术问题采用以下技术方案来实现:一种烧结铁氧体预烧料的制造方法,包括主原材料和添加剂,主原材料为铁红和碳酸锶,其制造方法包括以下步骤:
步骤一:按配比称取铁红和碳酸锶,铁红与碳酸锶的质量百分比为6.005-6.20,铁红中Fe2O3的含量为99wt%,碳酸锶z中SrCO3的含量为98wt%,同时称取定量的一次添加剂,所述一次添加剂为CaCO3和SiO2;
步骤二:将上述材料放入强混机内干式混合均匀,造粒,并于空气中在1250℃-1350℃的温度下预烧,获得预烧料;
步骤三:将上述预烧料使用干式球磨机破碎,筛分,得到粒度为3-7μm的预烧料粗粉;
步骤四:将预烧料粗粉连同二次添加剂一起投入球磨机中,以水为介质进行微粉碎,粒度控制在0.6μm;
步骤五:将微粉碎后的料浆含水率调整为40%,置于磁场中成型,施加磁场,压制成型,得到成型体;
步骤六:将成型体置于烧结炉中烧结,升温速率为6℃/min,烧结温度为1220℃,保温2小时,随炉自然冷却至室温,随后对烧结磁体的上下表面进行磨加工,获得烧结铁氧体磁体。
作为本发明的优选方案为:所述一次添加剂中的CaCO3的添加量以主原材料重量计为0.1wt%-0.6wt%,一次添加剂中的SiO2的添加量以主原材料重量计为0wt%-0.3wt%。
作为本发明的优选方案为:所述步骤四中的二次添加剂的组成为:CaCO3的添加量以粗粉重量计为1.2wt%,SiO2的添加量以粗粉重量计为0.3wt%,H3BO3的添加量以粗粉重量计为0.2wt%,Al2O3的添加量以粗粉重量计为0.3wt%。
作为本发明的优选方案为:所述步骤五中的磁场强度为8000-10000Oe,成型压力为7-9MPa。
与现有技术相比,本发明的有益效果是:通过添加碳酸钙,能够促进液相烧结,解决摩尔比大于6时反应活性差、不能获得高的饱和磁化强度的问题。同时由于摩尔比大于6,预烧料经过微粉碎获得的料浆不产生胶状物,湿压成型过程中易于排水,成型效率明显提高。即通过添加碳酸钙,一方面提高了预烧料的饱和磁化强度,同时在微粉碎时,能够将粒度研磨到0.6μm及以下,充分发挥出材料应有的性能,从而获得了优异的磁体性能。
具体实施方式
为了使本发明的实现技术手段、创作特征、达成目的与功效易于明白了解,进一步阐述本发明。
实施例1
步骤一:称取主原材料,其中铁红86.82wt%,碳酸锶13.18wt%,铁红中Fe2O3的含量为99wt%,碳酸锶z中SrCO3的含量为98wt%。同时称取0.4wt%(以主原材料重量计)的CaCO3,0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料,测量预烧料的饱和磁化强度如表1所示;
步骤二:将上述预烧料使用干式球磨机破碎,筛分,得到粒度为3-7μm的预烧料粗粉;
步骤三:将预烧料粗粉连同二次添加剂一起投入球磨机中,以水为介质进行微粉碎,粒度控制在0.6μm;所述二次添加剂的组成为:1.2wt%(以粗粉重量计)的CaCO3,0.3wt%(以粗粉重量计)的SiO2,0.2wt%(以粗粉重量计)的H3BO3,0.3wt%(以粗粉重量计)的Al2O3;
步骤四:将微粉碎后的料浆含水率调整为40%,置于磁场中成型,施加磁场,压制成型,磁场强度为8000-10000Oe,成型压力为7-9MPa,得到成型体;
步骤五:将成型体置于烧结炉中烧结,升温速率为6℃/min,烧结温度为1220℃,保温2小时,随炉自然冷却至室温,随后对烧结磁体的上下表面进行磨加工,获得烧结铁氧体磁体。测量磁性能的结果如表2所示。
对比例1
称取主原材料,其中铁红86.82wt%,碳酸锶13.18wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。同时称取0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1300℃预烧,获得预烧料;其余步骤和实施例1相同。
对比例2
称取主原材料,其中铁红86.24wt%,碳酸锶13.76wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。同时称取0.4wt%(以主原材料重量计)的CaCO3,0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料;其余步骤和实施例1相同。
对比例3
称取主原材料,其中铁红86.24wt%,碳酸锶13.76wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。同时称取0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料;其余步骤和实施例1相同。
表1实施例1和对比例1~3的饱和磁化强度对比
表2实施例1和对比例1~3的磁性和成型时间对比
实施例2
称取主原材料,其中铁红分别为86.24wt%、86.55wt%、86.63wt%、86.72wt%、86.82wt%、86.91wt%,碳酸锶分别为13.76wt%、13.45wt%、13.37wt%、13.23wt%、13.18wt%、13.09wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。同时称取0.4wt%(以主原材料重量计)的CaCO3,0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料。其余步骤和实施例1相同。测量磁性能的结果如表3所示。
表3实施例2的磁性能和成型时间统计
实施例3
称取主原材料,其中铁红86.63wt%,碳酸锶13.37wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。同时分别称取0wt%、0.1wt%、0.2wt%、0.3wt%、0.4wt%、0.5wt%、0.6wt%、1.0wtwt%(以主原材料重量计)的CaCO3,0.2wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料。其余步骤和实施例1相同。测量磁性能的结果如表4所示。
表4实施例3的磁性能和成型时间统计
实施例4
称取主原材料,其中铁红86.63wt%,碳酸锶13.37wt%,铁红中Fe2O3的含量为99wt%,碳酸锶中SrCO3的含量为98wt%。称取0.4wt%(以主原材料重量计)的CaCO3,同时分别称取0wt%、0.1wt%、0.2wt%、0.3wt%、0.4wt%(以主原材料重量计)的SiO2。用强混机干式混合均匀,造粒,于空气中1250℃预烧,获得预烧料。其余步骤和实施例1相同。测量磁性能的结果如表5所示。
表5实施例3的磁性能和成型时间统计
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明的要求保护范围由所附的权利要求书及其等效物界定。
Claims (4)
1.一种烧结铁氧体预烧料的制造方法,其特征在于:包括主原材料和添加剂,主原材料为铁红和碳酸锶,其制造方法包括以下步骤:
步骤一:按配比称取铁红和碳酸锶,铁红与碳酸锶的质量百分比为6.005-6.20,铁红中Fe2O3的含量为99wt%,碳酸锶z中SrCO3的含量为98wt%,同时称取定量的一次添加剂,所述一次添加剂为CaCO3和SiO2;
步骤二:将上述材料放入强混机内干式混合均匀,造粒,并于空气中在1250℃-1350℃的温度下预烧,获得预烧料;
步骤三:将上述预烧料使用干式球磨机破碎,筛分,得到粒度为3-7μm的预烧料粗粉;
步骤四:将预烧料粗粉连同二次添加剂一起投入球磨机中,以水为介质进行微粉碎,粒度控制在0.6μm;
步骤五:将微粉碎后的料浆含水率调整为40%,置于磁场中成型,施加磁场,压制成型,得到成型体;
步骤六:将成型体置于烧结炉中烧结,升温速率为6℃/min,烧结温度为1220℃,保温2小时,随炉自然冷却至室温,随后对烧结磁体的上下表面进行磨加工,获得烧结铁氧体磁体。
2.根据权利要求1所述的一种烧结铁氧体预烧料的制造方法,其特征在于:所述一次添加剂中的CaCO3的添加量以主原材料重量计为0.1wt%-0.6wt%,一次添加剂中的SiO2的添加量以主原材料重量计为0wt%-0.3wt%。
3.根据权利要求1所述的一种烧结铁氧体预烧料的制造方法,其特征在于:所述步骤四中的二次添加剂的组成为:CaCO3的添加量以粗粉重量计为1.2wt%,SiO2的添加量以粗粉重量计为0.3wt%,H3BO3的添加量以粗粉重量计为0.2wt%,Al2O3的添加量以粗粉重量计为0.3wt%。
4.根据权利要求1所述的一种烧结铁氧体预烧料的制造方法,其特征在于:所述步骤五中的磁场强度为8000-10000Oe,成型压力为7-9MPa。
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