CN107673755A - 一种永磁铁氧体的制备方法 - Google Patents
一种永磁铁氧体的制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 71
- 238000005245 sintering Methods 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000654 additive Substances 0.000 claims abstract description 28
- 230000000996 additive effect Effects 0.000 claims abstract description 28
- 238000002485 combustion reaction Methods 0.000 claims abstract description 28
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004327 boric acid Substances 0.000 claims abstract description 19
- 230000001939 inductive effect Effects 0.000 claims abstract description 16
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- 238000001238 wet grinding Methods 0.000 claims abstract description 13
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 13
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 11
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000004227 calcium gluconate Substances 0.000 claims description 3
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- 235000013927 calcium gluconate Nutrition 0.000 claims description 3
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000005338 frosted glass Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- BJHIKXHVCXFQLS-PYWDMBMJSA-N sorbose group Chemical group OCC(=O)[C@H](O)[C@@H](O)[C@H](O)CO BJHIKXHVCXFQLS-PYWDMBMJSA-N 0.000 claims 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000012254 powdered material Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
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- 238000012913 prioritisation Methods 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
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- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical group OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
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- 241001269238 Data Species 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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Abstract
一种永磁铁氧体的制备方法,包括如下步骤:配料称量与湿磨中加入一次添加剂氧化硅和硼酸,预烧过程通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米进行预烧。加入一次添加剂,使原料在预烧时更容易预烧;通过调节助燃风机和引风机使高温区域长度增加至3米,从而在相同的预烧温度下达到更长的保温时间;通过以上方法相结合做出的预烧料在二次烧结时可适应更广的烧结温度,降低了烧结工序因温度变化造成的不良率。
Description
技术领域
本发明属于磁性材料技术领域,具体涉及一种永磁铁氧体的制备方法。
背景技术
永磁铁氧体是由二价阳离子金属氧化物和三价的铁所构成的化合物的总称,作为磁性材料的一个重要组成部分,在电子工业、信息产业、摩托车、电动工具行业、汽车工业等行业发挥着重要的作用。
在制备永磁铁氧体过程中,永磁铁氧体成型后的二次烧成是一个至关重要的环节,直接影响着永磁铁氧体的性能高低和稳定性,在烧成过程中我们设定的烧结最高温度可称为此种铁氧体的烧结温度,永磁铁氧体的烧结温度过低时,会使产品密度低,收缩小,内部分子的间距增大,铁氧体致密性低,会出现吸水现象,永磁铁氧体的烧结温度烧结过高时,会随着温度的提高造成永磁铁氧体慢慢结晶化,改变了永磁铁氧体的内部结构,造成产品性能的降低;永磁铁氧体成型后的二次烧成可适应的最高烧结温度范围我们称之为此种铁氧体具有的温度带宽。由于在大生产过程中因人为或设备的原因,会造成烧结炉体设定的最高温度段区域内温度偏高或偏低,从而导致烧结后的永磁铁氧体性能的偏差。如何进一步提高铁氧体二次烧结时的温度带宽,从而减少大生产中在烧结工序的不良率,是本领域技术人员亟待解决的问题。
发明内容
本发明为了解决以上缺陷,本发明提供了一种永磁铁氧体制备方法,通过在制备永磁铁氧体预烧粉料的过程中添加一次添加剂并更改预烧方式的方法先制作出永磁铁氧体预烧粉料,用此预烧粉制备的永磁铁氧体在二次烧结时大大提高了永磁铁氧体可适应的烧结温度范围,从而减少大生产中在烧结工序的不良率。
本发明是通过以下技术方案实现的:
一种永磁铁氧体的制备方法,具体步骤包括配料称量与湿磨,脱水,预烧,粉碎球磨,成型和烧结;
配料称量与湿磨过程中加入一次添加剂,一次添加剂为氧化硅和硼酸,添加比例为每100kg原材料,加入0.2~0.6kg氧化硅,0.05~0.25kg硼酸;
预烧是将脱水得到的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米进行预烧。
作为优化方案,配料称量与湿磨按如下操作:按分子式Sr1-xLaxFe2n-y-zCoyZnzO19的摩尔数配比,称量主相原材料碳酸锶粉末、氧化镧粉末、氧化锌粉末、氧化钴粉末及氧化铁粉末;其中,x为0.4~0.6,y为0.1~0.2,n为5.4,x/(y+z)为2;将除氧化铁粉末以外的主相原材料粉混合并加入一次添加剂,将混合物料投入到湿式球磨机中,球磨机内物料:水:球比例=1:1.6:12,磨桶转速35r/min,细磨3h,得到混合物料平均粒度不大于1.0um;在得到的混合物料中加入氧化铁粉末,再通过湿式球磨机进行混合及粉碎,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,细磨3h,得到混合粉碎后的混合物料平均粒度不大于1.0um。
作为优化方案,调节助燃空气的压力通过变频调节助燃风机使全压在4800~5000Pa、流量在2300~2500m3/h来实现,调节引风压力通过变频调节引风机使全压在5200~5400Pa、流量在4000~4200m3/h来实现。
作为优化方案,预烧得到的预烧料经干式粉碎,加入二次添加剂进行湿磨,所述二次添加剂按如下重量配比添加,每100kg所述预烧料加入碳酸钙粉末0.4~1.5kg,碳酸锶粉末0.2~1.2kg,氧化硅粉末0.1~0.6kg,氧化铝粉末0.1~1.0kg,硼酸粉末0.1~0.3kg,分散剂总量0.2~1.2kg。
作为优化方案,分散剂为山梨糖醇或葡萄糖酸钙或抗坏血酸。
作为优化方案,烧结温度为1210℃~1250℃。
本发明的有益效果包括:
1、一次添加剂,使原料在预烧时更容易预烧;通过调节助燃风机和引风机高温区域长度增加至3米,从而在相同的预烧温度下达到更长的保温时间;通过以上方法做出的预烧料在二次烧结时可适应更广的烧结温度,来减少烧结工序因温度变化造成的不良率。
2、对物料进行粒度处理,配料和氧化铁分步处理,可使混合后料浆粒度更均匀,提高混合效果,有助于原料预烧时适应更宽的高温预烧区域,更好的生成六角晶相铁氧体。
3、二次添加剂能够在烧结体中形成晶界,提高最终烧结体的磁性能。
4、加入分散剂能够改善磁场成型时的料浆粒子的取向性,如果添加量过小,得不到分散料浆粒子的作用,添加量过大,在后续的烧结过程中分散剂排出不充分,会导致烧成体密度降低。
5、适宜的烧结温度使得铁氧体剩磁(Br)随温度增加而升高,其内禀矫顽力(Hcj)随烧结温度变化较小,体现了性能的稳定性。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施方式仅仅用以解释本发明,并不用于限定本发明。
实施例1:
本实施例提供一种永磁铁氧体的制备方法,具体如下步骤:
(1)配料称量与湿磨
本制备方法配料总量按1500kg配料,按分子式Sr1-xLaxFe2n-y-zCoyZnzO19的摩尔数配比称量永磁铁氧体主相原材料:x为0.4,y为0.1,z为0.1,n为5.4,x/(y+z)为2,并由此称得碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)121.7kg,氧化镧粉末(纯度≥99.9wt%、颗粒的原始平均粒度1.5um)179.1kg,氧化锌粉末(纯度≥98.0wt%、颗粒的原始平均粒度2.0um)11.2kg,氧化钴粉末(纯度≥99wt%、颗粒的原始平均粒度2.0um)22.5kg;在所述主相原材料粉中加入一次添加剂,所述一次添加剂为氧化硅和硼酸,添加比例为主相原材料总重量每100份,加入氧化硅0.4份(纯度≥98.0wt%、颗粒的原始平均粒度1.0um),硼酸(纯度≥99.0wt%,颗粒的原始平均粒度2.0um)0.2份;将混合物料投入到湿式球磨机中,球磨机内物料:水:球比例=1:1.6:12,磨桶转速35r/min,细磨3h,得到混合物料平均粒度不大于1.0um;
加入氧化铁粉末(纯度≥99wt%、颗粒的原始平均粒度1.0um)1165.4kg,再通过湿式球磨机进行混合及粉碎,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,细磨3h,得到混合粉碎后的混合物料平均粒度不大于1.0um;
(2)脱水
将步骤(1)得到的混合物料经过卧式螺旋卸料沉降离心机脱水后放入储存桶内等待进预烧,离心机转速为2000r/min,按1.5T/h的进料量进脱水机脱水,得到料浆的含固量在65wt%;
(3)预烧
将步骤(2)获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米预烧,调节助燃空气的压力通过变频调节助燃风机使全压分别在4800Pa、流量在2500m3/h来实现,调节引风压力通过变频调节引风机使全压分别在5200Pa、流量在4200m3来实现;
(4)粉碎球磨
将步骤(3)得到的预烧料先用通过球磨机进行干式粉碎,转速29.7r/min,物料按1.5T/h的进料量通过球磨机,得到平均粒度4um的预烧粉料;称取所述预烧粉料,加入二次添加剂,二次添加剂包括碳酸钙粉末、碳酸锶粉末、氧化硅粉末、氧化铝粉末、硼酸粉末、分散剂;每100份所述预烧料加入碳酸钙粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)0.6份,碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)0.8份,氧化硅粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.0um)0.4份,氧化铝粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.0um)0.5份,硼酸粉末(纯度≥99.0wt%、颗粒的原始平均粒度2.0um)0.2份,分散剂为葡萄糖酸钙(纯度≥99.0wt%、颗粒的原始平均粒度1.0um)总量0.6份。将所得的混合物再用球磨机湿磨,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,时间为15h,得到平均粒度在0.8um的料浆;
(5)成型
将步骤(4)得到的料浆用卧式螺旋卸料沉降离心机进行脱水处理,离心机转速为1300,按1.5T/h的进料量进脱水机脱水,得到料浆的含固量在73wt%;然后在700KA/M磁场中压缩成型,成型压力为0.5T/cm3,所得成型体为直径40mm、高度15mm的圆柱体。
(6)烧结
在200℃的温度对成形体进行热处理,除去水分和有机分散剂,然后在大气中进行烧结,升温速度是100℃/h,分别在1210℃,1230℃,1250℃保温2h,获得烧结永磁体。
对比实验1:步骤(1)和步骤(3)-(6)与实施例1相同;步骤(2)获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为2米预烧,调节助燃空气的压力通过变频调节助燃风机使全压在4100、流量在1900m3/h来实现,调节引风压力通过变频调节引风机使全压在4500、流量在3200m3/h来实现。
实施例2:
本实施例提供一种永磁铁氧体的制备方法,具体如下步骤:
(1)配料处理
本制备方法配料总量按1500kg配料,按分子式Sr1-xLaxFe2n-y-zCoyZnzO19的摩尔数配比称量永磁铁氧体主相原材料:x为0.5,y为0.15,z为0.1,n为5.4,x/(y+z)为2,并由此称得碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)99.4kg,氧化镧粉末(纯度≥99.9wt%、颗粒的原始平均粒度1.5um)219.5kg,氧化锌粉末(纯度≥98.0wt%、颗粒的原始平均粒度2.0um)11kg,氧化钴粉末(纯度≥99wt%、颗粒的原始平均粒度2.0um)33.1kg;在所述主相原材料粉中加入一次添加剂,所述一次添加剂为氧化硅和硼酸,添加比例为主相原材料总重量每100份,加入氧化硅0.2份(纯度≥98.0wt%、颗粒的原始平均粒度1.Oum),硼酸(纯度≥99.0wt%,颗粒的原始平均粒度2.Oum)0.05份;将混合物料投入到湿式球磨机中,球磨机内物料:水:球比例=1:1.6:12,磨桶转速35r/min,细磨3h,得到混合物料平均粒度不大于1.0 um;
加入氧化铁粉末(纯度≥99wt%、颗粒的原始平均粒度1.0um)1137kg,再通过湿式球磨机进行混合及粉碎,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,细磨3h,得到混合粉碎后的混合物料平均粒度不大于1.0 um;
(2)脱水
将步骤(1)得到的混合物料经过卧式螺旋卸料沉降离心机脱水后放入储存桶内等待进预烧,离心机转速为1800r/min,按1.5T/h的进料量进脱水机脱水,得到料浆的含固量在60wt%;
(3)预烧
将步骤(2)获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米,调节助燃空气的压力通过变频调节助燃风机使全压分别在5000Pa、流量在2300m3/h来实现,引风压力通过变频调节引风机使全压在5400Pa、流量在4000m3/h来实现;
(4)粉碎球磨
将步骤(3)得到的预烧料先用通过球磨机进行干式粉碎,转速29.7r/min,物料按1.5T/h的进料量通过球磨机,得到平均粒度为3-5um的预烧粉料;称取所述预烧粉料,加入二次添加剂,二次添加剂包括碳酸钙粉末、碳酸锶粉末、氧化硅粉末、氧化铝粉末、硼酸粉末、分散剂;每100份所述预烧料加入碳酸钙粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)0.4份,碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)0.2份,氧化硅粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.O um)0.1份,氧化铝粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.O um)0.1份,硼酸粉末(纯度≥99.0wt%、颗粒的原始平均粒度2.O um)0.1份,分散剂为山梨糖醇(纯度≥99.0wt%、颗粒的原始平均粒度1.O um)总量0.2份。将所得的混合物再用球磨机湿磨,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,时间为15h,得到平均粒度0.65-0.9um的料浆;
(5)成型
将步骤(4)得到的料浆用卧式螺旋卸料沉降离心机进行脱水处理,离心机转速为1500r/min,按1.5T/h的进料量进行脱水处理,得到料浆的含固量在80wt%;然后在500KA/M磁场中压缩成型,成型压力为0.5T/cm3,所得成型体为直径40mm、高度15mm的圆柱体。
(6)烧结
在100℃的温度对成形体进行热处理,除去水分和有机分散剂,然后在大气中进行烧结,升温速度是100℃/h,分别在1210℃,1230℃,1250℃保温2h,获得烧结永磁体。
对比实验2:步骤(1)和步骤(3)-(6)与实施例2相同;步骤(2)中获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为2米预烧,调节助燃空气的压力通过变频调节助燃风机使全压在4300Pa、流量在1700m3/h来实现,调节引风压力通过变频调节引风机使全压在4700Pa、流量在3000m3/h来实现;
实施例3:
本实施例提供一种永磁铁氧体的制备方法,具体如下步骤:
(1)配料处理
本制备方法配料总量按1500kg配料,按分子式Sr1-xLaxFe2n-y-zCoyZnzO19的摩尔数配比称量永磁铁氧体主相原材料:x为0.6,y为0.2,z为0.1,n为5.4,x/(y+z)为2,并由此称得碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)78kg,氧化镧粉末(纯度≥99.9wt%、颗粒的原始平均粒度1.5um)258.2kg,氧化锌粉末(纯度≥98.0wt%、颗粒的原始平均粒度2.0um)10.8kg,氧化钴粉末(纯度≥99wt%、颗粒的原始平均粒度2.0um)43.3kg;在所述主相原材料粉中加入一次添加剂,所述一次添加剂为氧化硅和硼酸,添加比例为主相原材料总重量每100份,加入氧化硅0.6份(纯度≥98.0wt%、颗粒的原始平均粒度1.Oum),硼酸(纯度≥99.0wt%,颗粒的原始平均粒度2.O um)0.25份;将混合物料投入到湿式球磨机中,球磨机内物料:水:球比例=1:1.6:12,磨桶转速35r/min,细磨3h,得到混合物料平均粒度不大于1.0um;
加入氧化铁粉末(纯度≥99wt%、颗粒的原始平均粒度1.0um)1109.7kg,再通过湿式球磨机进行混合及粉碎,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,细磨3h,得到混合粉碎后的混合物料平均粒度不大于1.0um;
(2)脱水
将步骤(1)得到的混合物料经过卧式螺旋卸料沉降离心机脱水后放入储存桶内等待进预烧,离心机转速为2300r/min,按1.5T/h的进料量进脱水机脱水,得到料浆的含固量在70wt%;
(3)预烧
将步骤(2)获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米预烧,调节助燃空气的压力通过变频调节助燃风机使全压在4900Pa、流量在2400m3/h,调节引风压力通过变频调节引风机使全压在5300Pa、流量在4100m3/h来实现;
(4)粉碎球磨
将步骤(3)得到的预烧料先用通过球磨机进行干式粉碎,转速29.7r/min,物料按1.5T/h的进料量通过球磨机,得到平均粒度为5um的预烧粉料;称取预烧粉料,加入二次添加剂,二次添加剂包括碳酸钙粉末、碳酸锶粉末、氧化硅粉末、氧化铝粉末、硼酸粉末、分散剂;每100份所述预烧料加入碳酸钙粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)1.5份,碳酸锶粉末(纯度≥98wt%、颗粒的原始平均粒度2.0um)1.2份,氧化硅粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.O um)0.6份,氧化铝粉末(纯度≥98.0wt%、颗粒的原始平均粒度1.O um)1.0份,硼酸粉末(纯度≥99.0wt%、颗粒的原始平均粒度2.O um)0.3份,分散剂为抗坏血酸(纯度≥99.0wt%、颗粒的原始平均粒度1.O um)总量1.2份。将所得的混合物再用球磨机湿磨,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,时间为15h,得到平均粒度0.65~0.9um的料浆;
(5)成型
将步骤(4)得到的料浆用卧式螺旋卸料沉降离心机进行脱水处理,离心机转速为1200r/min,按1.5T/h的进料量进行脱水处理,得到料浆的含固量在60wt%;然后在800KA/M磁场中压缩成型,成型压力为0.5T/cm3,所得成型体为直径40mm、高度15mm的圆柱体。
(6)烧结
在350℃的温度对成形体进行热处理,除去水分和有机分散剂,然后在大气中进行烧结,升温速度是100℃/h,分别在1210℃,1230℃,1250℃保温2h,获得烧结永磁体。
对比实验3:步骤(1)和步骤(3)-(6)与实施例3相同;步骤(2)中获得的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为2米预烧,调节助燃空气的压力通过变频调节助燃风机使全压在4200、流量在1800m3/h来实现,调节引风压力可通过变频调节引风机使全压在4600Pa、流量在3100m3/h来实现。
表1
如表1所示,3米为实施例1-3的实验数据结果,2米为对比试验1-3的实验数据结果。对物料进行粒度处理,并添加一次添加剂,使原料在预烧时更容易预烧;当x的值为0.4,0.5,0.6时,实施例与对比试验相比,通过调节助燃风机和引风机高温区域长度增加至3米,从而在相同的预烧温度下达到更长的保温时间,使得预烧料在1210-1250℃二次烧结成内禀矫顽力变化较小,剩磁较高的高温度带宽的永磁铁氧体,而只添加一次添加剂未更改高温区域长度的对比实验并不能达到这样的效果。通过以上方法做出的预烧料在二次烧结时可适应更广的烧结温度,来减少烧结工序因温度变化造成的不良率。通过扫描电子显微镜分析知x低于0.4时,La对六角晶M相的置换不充分,六角晶M型铁氧体结构变得不稳定,SrO·Fe2O3、SrO·2Fe203等的异相生成,磁性能大大降低。若x超过0.6,则未反应的La氧化物增加,还会生成正铁氧体等不为优选的相。
本领域的技术人员容易理解,以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种永磁铁氧体的制备方法,具体步骤包括配料称量与湿磨,脱水,预烧,粉碎球磨,成型和烧结;其特征在于:
所述配料称量与湿磨过程中加入一次添加剂,所述一次添加剂为氧化硅和硼酸,添加比例为每100kg配料,加入0.2~0.6kg氧化硅,0.05~0.25kg硼酸;
所述预烧是将脱水得到的混合物料在回转窑中进行预烧,回转窑转速0.85r/min,物料通过速度4.5m/h,通过调节助燃空气的压力和引风压力使预烧区高温区域段的长度为3米进行预烧。
2.根据权利要求1所述的永磁铁氧体的制备方法,其特征在于:所述配料称量与湿磨按如下操作:
按分子式Sr1-xLaxFe2n-y-zCoyZnzO19的摩尔数配比,称量主相原材料碳酸锶粉末、氧化镧粉末、氧化锌粉末、氧化钴粉末及氧化铁粉末;其中,x为0.4~0.6,y为0.1~0.2,n为5.4,x/(y+z)为2;将除氧化铁粉末以外的主相原材料粉混合并加入一次添加剂,将混合物料投入到湿式球磨机中,球磨机内物料:水:球比例=1:1.6:12,磨桶转速35r/min,细磨3h,得到混合物料平均粒度不大于1.0um;在得到的混合物料中加入氧化铁粉末,再通过湿式球磨机进行混合及粉碎,球磨机内物料:水:球比例=1:1.6:12,磨桶转速28r/min,细磨3h,得到混合粉碎后的混合物料平均粒度不大于1.0um。
3.根据权利要求2所述的永磁铁氧体的制备方法,其特征在于:调节助燃空气的压力通过变频调节助燃风机使全压在4800~5000Pa、流量在2300~2500m3/h来实现,调节引风压力通过变频调节引风机使全压在5200~5400Pa、流量在4000~4200m3/h来实现。
4.根据权利要求3所述的永磁铁氧体的制备方法,其特征在于,预烧得到的预烧料经干式粉碎,加入二次添加剂进行湿磨,所述二次添加剂按如下重量配比添加,每100kg所述预烧料加入碳酸钙粉末0.4~1.5kg,碳酸锶粉末0.2~1.2kg,氧化硅粉末0.1~0.6kg,氧化铝粉末0.1~1.0kg,硼酸粉末0.1~0.3kg,分散剂总量0.2~1.2kg。
5.根据权利要求4所述的永磁铁氧体的制备方法,其特征在于,所述步分散剂为山梨糖醇或葡萄糖酸钙或抗坏血酸。
6.根据权利要求5所述的永磁铁氧体的制备方法,其特征在于,烧结温度为1210℃~1250℃。
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