CN112374879A - 一种抗电磁干扰锰锌铁氧体材料制备方法 - Google Patents
一种抗电磁干扰锰锌铁氧体材料制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 26
- 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 title claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 49
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 26
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 46
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 42
- 238000000227 grinding Methods 0.000 claims description 37
- 238000005245 sintering Methods 0.000 claims description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 22
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 20
- 229910052681 coesite Inorganic materials 0.000 claims description 20
- 229910052906 cristobalite Inorganic materials 0.000 claims description 20
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- 229910052682 stishovite Inorganic materials 0.000 claims description 20
- 229910052905 tridymite Inorganic materials 0.000 claims description 20
- 239000011268 mixed slurry Substances 0.000 claims description 19
- 238000003825 pressing Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 14
- 230000000996 additive effect Effects 0.000 claims description 14
- 238000005469 granulation Methods 0.000 claims description 13
- 230000003179 granulation Effects 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 238000004806 packaging method and process Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- 239000008188 pellet Substances 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 238000005453 pelletization Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000035699 permeability Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 6
- 238000007689 inspection Methods 0.000 claims description 6
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- 239000004576 sand Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000000344 soap Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 5
- 230000005389 magnetism Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 30
- 238000000034 method Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000004883 computer application Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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Abstract
本发明公开了一种抗电磁干扰锰锌铁氧体材料制备方法,属于锰锌铁氧体材料技术领域。该抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,所述三氧化二铁的摩尔百分比为48%‑52%,所述四氧化三锰的摩尔百分比为30%‑35%,所述氧化锌的摩尔百分比为15%‑20%,S2.原料混合:按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料。本发明通过该制备方法的流程进行产品制造,使得成品率高,并且成品的性能稳定,制备中操作也简单方便,得到的材料在100KHz~30MHZ,不仅具有高的阻抗值,并且有较强的抗电磁干扰能力。
Description
技术领域
本发明涉及锰锌铁氧体材料技术领域,具体为一种抗电磁干扰锰锌铁氧体材料制备方法。
背景技术
随着移动通信、卫星通信、计算机应用的发展,电磁干扰(EMI)在军用和民用电子信息领域的影响越来越严重,对公共环境、人生安全、信息保密等造成危害。
消除或降低电磁污染、提高设备抗EMI能力的有效方法是采用电磁兼容(EMC)设计,其中需要用到大量的抗EMI材料,即高阻抗材料。随着电磁兼容法规的建立健全,抗EMI锰锌铁氧体磁芯需求量与日俱增,为此,设计一种抗电磁干扰锰锌铁氧体材料制备方法。
发明内容
本发明的目的在于提供一种抗电磁干扰锰锌铁氧体材料制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,所述三氧化二铁的摩尔百分比为48%-52%,所述四氧化三锰的摩尔百分比为30%-35%,所述氧化锌的摩尔百分比为15%-20%,通过对原料占比的多次选择,最终确定原料在此区间范围内加工的产品性能最为优越;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡10-15min,然后将混合料捞出并进行干燥处理,经过处理时原料表面洁净,改善最终产品的美观性,在原料混合之后进行洁净处理能够满足同时清理的目的,进而减少清洗难度,节省清理的时间;
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料,经过研磨后,为后期的造球提供方便性;
S5.造球:振磨后的研磨细料投入造球机中,加入5-15wt%的纯水,最终得到球料,通过纯水的合理量加入使最终得到的球粒品质更好,对原料进行造球能够为预烧处理提供方便,降低烧结处理时的难度;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料,经过预烧处理后实现对原料的品质改善;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为1.8-2.5微米,便于后期的化浆处理,增加化浆后浆液的品质;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,所述振磨料和纯水的比例为1:0.4-0.55,经过此种配比能够保证化浆处理后所的浆料的品质,使其更容易与添加剂进行混合;
S9.加入添加剂;在混合浆料中加入Nb2O5、CaCO3、Co3O4、SiO2、TiO2,所述Nb2O5、CaCO3、Co3O4、SiO2、TiO2所占的质量百分含量为Nb2O5:0-300ppm、CaCO3:100-1000ppm、Co3O4:0-5000ppm、SiO2:0-200ppm、TiO2:0-3000ppm,混合后得到混合浆料,添加剂的合理加入能够使磁导率μi为3100±25%,并且具有较强的抗电磁干扰能力,过高或者过低的浓度会降低磁导率,以及抗电磁干扰效果;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为0.9-1.2微米,此种粒度下喷雾造粒的加工更加高效;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s,能够保证其压制品的质量;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至100-200℃开炉,保证炉内温度的正常值,不影响后期使用;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
优选的,所述S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%,此种纯度的原料有利于保证材料的品质要求。
优选的,所述S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min,使其即能够有充分的时间进行混合,有节省加工的时间。
优选的,所述S5中球料的直径为2-10mm,在此种直径更容易进行烧结加工,同时降低操作者的操作难度。
优选的,所述S6中预烧的温度为900-960℃,并且回转窑内以5-8℃/min升至预烧温度,之后并保温处理3.5-5.5h,采取匀速的升温方式,使得在烧结的过程中防止产品烧结处理不充分,或者因为温度变化剧烈对其造成损伤,增加成品率。
优选的,所述S9中所加入的Nb2O5、CaCO3、Co3O4、SiO2、TiO2等级均为电子纯。
优选的,所述S11中具体为将S10研磨后的物料加入0.5-0.7%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.05-0.5mm,在此种颗粒下后期压制成型的成品率高,容易达到要求,进而加快生产的效率。
优选的,所述S12中的毛坯密度为2.95-3.05g/cm3,此种密度能够保证材料的阻抗率,并且不会对材料的加工增加难度。
优选的,所述S13中的辅助气体为氮气,且烧结的温度为1300-1380℃,保温时长为240-360min,从入氮气能够使其快速降温,并且在1300-1380℃的区间内能够改善材料组织,并且不对组织造成损坏。
优选的,所述S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
1、与现有技术相比,本发明所达到的有益效果是:通过该制备方法的流程进行产品制造,使得成品率高,并且成品的性能稳定,品相美观,制备中操作也简单方便。
2、与现有技术相比,本发明所达到的有益效果是:通过该制备方式得到的材料在100KHz~30MHZ,不仅具有高的阻抗值,并且有较强的抗电磁干扰能力。
3、与现有技术相比,本发明所达到的有益效果是:该制备的材料具有较高的初始磁导率,磁导率μi为3100±25%(25℃1kHz,0.25V)。
4、与现有技术相比,本发明所达到的有益效果是:通过合理的制备工艺得到材料的温度适应性强,在25℃~120℃温度范围内有良好的高阻抗性能。
5、与现有技术相比,本发明所达到的有益效果是:材料具有较高的密度,典型值为4.8-4.9KG/M3×103。
具体实施方式
下面将结合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。
实施例一:
本发明提供技术方案:一种抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,其中三氧化二铁的摩尔百分比为48%,其中四氧化三锰的摩尔百分比为32%,其中氧化锌的摩尔百分比为20%;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡10-15min,然后将混合料捞出并进行干燥处理;
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料;
S5.造球:振磨后的研磨细料投入造球机中,加入5wt%的纯水,最终得到球料;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为1.8微米;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,其中振磨料和纯水的比例为1:0.4;
S9.加入添加剂;在混合浆料中加入CaCO3,其中CaCO3所占的质量百分含量为CaCO3:100ppm,混合后得到混合浆料;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为1.2微米;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至100℃开炉;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
其中S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%。
其中S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min。
其中S5中球料的直径为10mm。
其中S6中预烧的温度为900℃,并且回转窑内以5℃/min升至预烧温度,之后并保温处理3.5h。
其中S9中所加入的CaCO3等级均为电子纯。
其中S11中具体为将S10研磨后的物料加入0.5%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.5mm。
其中S12中的毛坯密度为2.95g/cm3。
其中S13中的辅助气体为氮气,且中烧结的温度为1300℃,保温时长为240min。
其中S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
实施例二:
本发明提供技术方案:一种抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,其中三氧化二铁的摩尔百分比为50%,其中四氧化三锰的摩尔百分比为32%,其中氧化锌的摩尔百分比为18%;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡10-15min,然后将混合料捞出并进行干燥处理;
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料;
S5.造球:振磨后的研磨细料投入造球机中,加入10wt%的纯水,最终得到球料;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为2.1微米;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,其中振磨料和纯水的比例为1:0.5;
S9.加入添加剂;在混合浆料中加入Nb2O5、CaCO3、Co3O4、SiO2、TiO2,所述Nb2O5、CaCO3、Co3O4、SiO2、TiO2所占的质量百分含量为Nb2O5:150ppm、CaCO3:650ppm、Co3O4:3000ppm、SiO2:100ppm、TiO2:1500ppm,混合后得到混合浆料;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为1微米;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至150℃开炉;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
其中S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%。
其中S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min。
其中S5中球料的直径为5mm。
其中S6中预烧的温度为920℃,并且回转窑内以6.5℃/min升至预烧温度,之后并保温处理4h。
其中S9中所加入的Nb2O5、CaCO3、Co3O4、SiO2、TiO2等级均为电子纯。
其中S11中具体为将S10研磨后的物料加入0.5-0.7%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.3mm。
其中S12中的毛坯密度为3g/cm3。
其中S13中的辅助气体为氮气,且烧结的温度为1350℃,保温时长为300min。
其中S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
实施例三:
本发明提供技术方案:一种抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,其中三氧化二铁的摩尔百分比为51%,其中四氧化三锰的摩尔百分比为34%,其中氧化锌的摩尔百分比为15%;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡13min,然后将混合料捞出并进行干燥处理;
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料;
S5.造球:振磨后的研磨细料投入造球机中,加入13wt%的纯水,最终得到球料;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为2.3微米;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,其中振磨料和纯水的比例为1:0.52;
S9.加入添加剂;在混合浆料中加入Nb2O5、CaCO3、Co3O4、SiO2、TiO2,所述Nb2O5、CaCO3、Co3O4、SiO2、TiO2所占的质量百分含量为Nb2O5:200ppm、CaCO3:800ppm、Co3O4:4000ppm、SiO2:150ppm、TiO2:2000ppm,混合后得到混合浆料;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为1.1微米;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至150℃开炉;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
其中S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%。
其中S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min。
其中S5中球料的直径为8mm。
其中S6中预烧的温度为950℃,并且回转窑内以6.5℃/min升至预烧温度,之后并保温处理4h。
其中S9中所加入的Nb2O5、CaCO3、Co3O4、SiO2、TiO2等级均为电子纯。
其中S11中具体为将S10研磨后的物料加入0.5-0.7%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.4mm。
其中S12中的毛坯密度为3.02g/cm3。
其中S13中的辅助气体为氮气,且S13中烧结的温度为1370℃,保温时长为340min。
其中S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
实施例四:
本发明提供技术方案:一种抗电磁干扰锰锌铁氧体材料制备方法,包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,其中三氧化二铁的摩尔百分比为52%,其中四氧化三锰的摩尔百分比为33%,其中氧化锌的摩尔百分比为15%;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡10-15min,然后将混合料捞出并进行干燥处理
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料;
S5.造球:振磨后的研磨细料投入造球机中,加入15wt%的纯水,最终得到球料;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为2.5微米;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,其中振磨料和纯水的比例为1:0.55;
S9.加入添加剂;在混合浆料中加入Nb2O5、CaCO3、Co3O4、SiO2、TiO2,所述Nb2O5、CaCO3、Co3O4、SiO2、TiO2所占的质量百分含量为Nb2O5:300ppm、CaCO3:1000ppm、Co3O4:5000ppm、SiO2:200ppm、TiO2:3000ppm,混合后得到混合浆料;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为1微米;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至200℃开炉;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
其中S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%。
其中S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min。
其中S5中球料的直径为2mm。
其中S6中预烧的温度为960℃,并且回转窑内以6.5℃/min升至预烧温度,之后并保温处理4h。
其中S9中所加入的Nb2O5、CaCO3、Co3O4、SiO2、TiO2等级均为电子纯。
其中S11中具体为将S10研磨后的物料加入0.5-0.7%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.05mm。
其中S12中的毛坯密度为3.05g/cm3。
其中S13中的辅助气体为氮气,且S13中烧结的温度为1380℃,保温时长为360min。
其中S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
实验:对实施例一至四种的产品进行实验,并与普通产品进行对比表格如下:
由实验数据能够得知本发明制成的产品性能均高于普通工艺产品,综合分析实施例三中的产品性能最为优越,实施例一至四种的产品在实验中磁导率μi为3100±25%。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:包括以下制备步骤:
S1.配方选取:选取原材料三氧化二铁、四氧化三锰、氧化锌,所述三氧化二铁的摩尔百分比为48%-52%,所述四氧化三锰的摩尔百分比为30%-35%,所述氧化锌的摩尔百分比为15%-20%;
S2.原料混合;
S3.洁净处理:将得到的混合料置于肥皂水中进行浸泡,浸泡10-15min,然后将混合料捞出并进行干燥处理;
S4.研磨:将S2中得到的一次混合料投入至通过式振动研磨机进行研磨处理,得到研磨细料;
S5.造球:振磨后的研磨细料投入造球机中,加入5-15wt%的纯水,最终得到球料;
S6.预烧处理:将得到的球料置于回转窑中预烧,经过预烧处理后得到预烧料;
S7.振磨:将预烧料用通过式振磨机振磨,得到振磨料,并且控制振磨料的平均粒径为1.8-2.5微米;
S8.化浆处理:在化浆池中注入纯水,再加入振磨料,并进行混合搅拌,得到混合浆料,所述振磨料和纯水的比例为1:0.4-0.55;
S9.加入添加剂;在混合浆料中加入Nb2O5、CaCO3、Co3O4、SiO2、TiO2,所述Nb2O5、CaCO3、Co3O4、SiO2、TiO2所占的质量百分含量为Nb2O5:0-300ppm、CaCO3:100-1000ppm、Co3O4:0-5000ppm、SiO2:0-200ppm、TiO2:0-3000ppm,混合后得到混合浆料;
S10.砂磨:浆料加入添加剂后,在砂磨机中砂磨,并控制平均粒径为0.9-1.2微米;
S11.喷雾造粒;
S12.压制:采用粉末压机,压制所需要的产品毛坯,在粉末压机对毛坯的压制时间3-5s;
S13.烧结:压制好的毛坯,采用钟罩炉烧结,烧结后并进行保温,结束后在炉体中充入辅助气体,降温至100-200℃开炉;
S14.磨加工:烧结后的坯件,采用切割机或磨床,加工成特定尺寸或形状的磁芯;
S15.检验;
S16.包装:经检验合格后对产品进行打包、入库。
2.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S1中氧化二铁的纯度≥99%、四氧化三锰的纯度≥98.5%、氧化锌的纯度≥99.7%。
3.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于;所述S2中原料混合的具体步骤为,按照比例称取原材料,然后将原材料放置在锥混器内对原料进行充分的混合,进而得到混合料,锥混器对原料的混合时间15-45min。
4.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S5中球料的直径为2-10mm。
5.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S6中预烧的温度为900-960℃,并且回转窑内以5-8℃/min升至预烧温度,之后并保温处理3.5-5.5h。
6.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S9中所加入的Nb2O5、CaCO3、Co3O4、SiO2、TiO2等级均为电子纯。
7.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S11中具体为将S10研磨后的物料加入0.5-0.7%的PVA,采用喷雾造粒干燥塔,制备成颗粒,且颗粒直径为0.05-0.5mm。
9.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S13中的辅助气体为氮气,且烧结的温度为1300-1380℃,保温时长为240-360min。
10.根据权利要求1所述的一种抗电磁干扰锰锌铁氧体材料制备方法,其特征在于:所述S15中采用SY-8219仪器检测磁芯的饱合磁通密度、剩磁和矫顽力,采用4284A型LCR仪测试磁芯的磁导率,采用CH2335功耗仪检测磁芯的功耗。
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