CN105702411A - 一种铜渣回收制备铜锌铁氧体软磁材料的方法 - Google Patents
一种铜渣回收制备铜锌铁氧体软磁材料的方法 Download PDFInfo
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Abstract
本发明公开了一种铜渣回收制备铜锌铁氧体软磁材料的方法,属于铁氧体软磁材料制备技术领域领域。本发明通过将含锌量2%的废弃铜渣碾磨并还原煅烧,制备磁性合金,将铜铁合金溶于硫酸,通过氢氧化钠进行沉淀,制备离子级铁氧体粉末,随后将其与磁性凝胶中间体混合煅烧制备软磁复合材料,通过少量铜离子进入软磁材料晶格,使饱和磁化强度不断增加,制备得一种高饱和磁化强度铜锌铁氧体软磁材料。本发明的有益效果是:本发明制备步骤简单,所得产品磁导率和居里温度高较其他同类产品提高10~15%;在成型过程中分散性好,材料密度分布均匀,饱和场强度高达32000A/m。
Description
技术领域
本发明涉及一种铜渣回收制备铜锌铁氧体软磁材料的方法,属于铁氧体软磁材料制备技术领域领域。
背景技术
当磁化发生在Hc不大于100A/m,这样的材料称为软磁体。典型的软磁材料,可以用最小的外磁场实现最大的磁化强度。软磁材料主要有以金属软磁材料和铁氧体软磁材料为代表的晶体材料,目前应用最多的是铁氧体软磁材料,软磁铁氧体材料按其晶体结构可分为立方晶系的尖晶石(适用于低频、中频和高频)和平面六角晶系的磁铅石(适用于特高频,可到200MHz~2GHz)等两种。最常用的软磁铁氧体主要是MnZn、NiZn和MgZn三大系列。软磁铁氧体材料电阻率高(10-2~1010Ω·m),中高频损耗低,成本低,但饱和磁通密度低,磁导率低(<100),居里温度低,且由于铁氧体纳米粉体具有较高的表面活性,在成型过程中极易团聚,导致材料密度分布不均匀,经烧结后,材料性能较差。因此在此基础上研究出一种性能优异的铁氧体软磁材料,具有重要的意义,且在相关领域具有很好的发展前景和社会效益。
发明内容
本发明所要解决的技术问题:针对目前软磁铁氧体材料饱和磁通密度低,磁导率和居里温度低,经烧结材料性能较差的弊端,提供了一种通过将废弃铜渣碾磨并还原煅烧,制备复合铜铁合金,将铜铁合金溶于硫酸,通过氢氧化钠进行沉淀,制备离子级铁氧体粉末,随后将其与磁性凝胶中间体混合煅烧制备软磁复合材料,通过少量铜离子进入软磁材料晶格,使饱和磁化强度不断增加,制备得一种高饱和磁化强度铜锌铁氧体软磁材料的方法。本发明制备步骤简单,所得产品饱和磁化强度高。
为解决上述技术问题,本发明采用如下所述的技术方案是:
(1)收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得50~60目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1180~1250℃后,保温煅烧2~3h;
(2)待煅烧完成后,停止加热并静置冷却至20~30℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;
(3)收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于78~85℃下水浴加热2~3h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于450~600℃下煅烧2~3h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;
(4)按重量份数计,分别称量20~45份氯化铁、30~35份钛酸四丁酯、20~25份冰醋酸和5~20份聚乙烯醇与三口烧杯中,搅拌混合并置于70~85℃下水浴加热45~60min,待其加热完成后,对其过滤并收集滤液,再将滤液置于40~60℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;
(5)按重量份数计,分别称量30~55份去离子水、10~15份聚乙烯醇、10~15份上述制备的磁性凝胶中间体、20~30份步骤(3)中制备的铜锌铁氧体粉末和5~10份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于65~80℃下水浴加热45~60min,制备得软磁前驱体;
(6)将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至600~800℃后,保温煅烧2~3h,随后停止加热,静置冷却至20~30℃,再将其置于不锈钢模具中冷压25~30min,即可制备得一种铜锌铁氧体软磁材料。
本发明制得的铜锌铁氧体软磁材料饱和磁感>1.2,居里温度为576~800℃,电阻率为1.25~1.45μΩ·m,饱和场强度为32000~32500A/m,磁导率为115~130mH/m,损耗为10.8~12.3W/kg,灵敏度为0.3%/(A·m-1)。
本发明与其他方法相比,有益技术效果是:
(1)本发明制备步骤简单,所得产品磁导率和居里温度高较其他同类产品提高10~15%;
(2)在成型过程中分散性好,材料密度分布均匀,饱和场强度高达32000A/m。
具体实施方式
首先收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得50~60目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1180~1250℃后,保温煅烧2~3h;待煅烧完成后,停止加热并静置冷却至20~30℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;再收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于78~85℃下水浴加热2~3h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于450~600℃下煅烧2~3h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;再按重量份数计,分别称量20~45份氯化铁、30~35份钛酸四丁酯、20~25份冰醋酸和5~20份聚乙烯醇与三口烧杯中,搅拌混合并置于70~85℃下水浴加热45~60min,待其加热完成后,对其过滤并收集滤液,再将滤液置于40~60℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;然后按重量份数计,分别称量30~55份去离子水、10~15份聚乙烯醇、10~15份上述制备的磁性凝胶中间体、20~30份备用的铜锌铁氧体粉末和5~10份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于65~80℃下水浴加热45~60min,制备得软磁前驱体;最后将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至600~800℃后,保温煅烧2~3h,随后停止加热,静置冷却至20~30℃,再将其置于不锈钢模具中冷压25~30min,即可制备得一种铜锌铁氧体软磁材料。
实例1
首先收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得50目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1180℃后,保温煅烧2h;待煅烧完成后,停止加热并静置冷却至20℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;再收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于78℃下水浴加热2h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于450℃下煅烧2h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;再按重量份数计,分别称量20份氯化铁、35份钛酸四丁酯、25份冰醋酸和20份聚乙烯醇与三口烧杯中,搅拌混合并置于70℃下水浴加热45min,待其加热完成后,对其过滤并收集滤液,再将滤液置于40℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;然后按重量份数计,分别称量30份去离子水、15份聚乙烯醇、15份上述制备的磁性凝胶中间体、30份备用的铜锌铁氧体粉末和10份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于65℃下水浴加热45min,制备得软磁前驱体;将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至600℃后,保温煅烧2h,随后停止加热,静置冷却至20℃,再将其置于不锈钢模具中冷压25min,即可制备得一种铜锌铁氧体软磁材料。本发明制备步骤简单,所得产品磁导率和居里温度高;在成型过程中分散性好,材料密度分布均匀,烧结后材料性能好;制得的铜锌铁氧体软磁材料饱和磁感为1.25,居里温度为576℃,电阻率为1.25μΩ·m,饱和场强度为32000A/m,磁导率为115mH/m,损耗为10.8W/kg,灵敏度为0.3%/(A·m-1)。
实例2
首先收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得55目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1210℃后,保温煅烧3h;待煅烧完成后,停止加热并静置冷却至25℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;再收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于82℃下水浴加热3h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于520℃下煅烧3h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;再按重量份数计,分别称量33份氯化铁、32份钛酸四丁酯、23份冰醋酸和12份聚乙烯醇与三口烧杯中,搅拌混合并置于77℃下水浴加热52min,待其加热完成后,对其过滤并收集滤液,再将滤液置于50℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;然后按重量份数计,分别称量43份去离子水、12份聚乙烯醇、13份上述制备的磁性凝胶中间体、24份备用的铜锌铁氧体粉末和8份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于72℃下水浴加热52min,制备得软磁前驱体;将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至700℃后,保温煅烧3h,随后停止加热,静置冷却至25℃,再将其置于不锈钢模具中冷压28min,即可制备得一种铜锌铁氧体软磁材料。本发明制备步骤简单,所得产品磁导率和居里温度高;在成型过程中分散性好,材料密度分布均匀,烧结后材料性能好;制得的铜锌铁氧体软磁材料饱和磁感为1.31,居里温度为688℃,电阻率为1.35μΩ·m,饱和场强度为32250A/m,磁导率为122mH/m,损耗为11.5W/kg,灵敏度为0.3%/(A·m-1)。
实例3
首先收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得60目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1250℃后,保温煅烧3h;待煅烧完成后,停止加热并静置冷却至30℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;再收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于85℃下水浴加热3h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于600℃下煅烧3h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;再按重量份数计,分别称量45份氯化铁、30份钛酸四丁酯、20份冰醋酸和5份聚乙烯醇与三口烧杯中,搅拌混合并置于85℃下水浴加热60min,待其加热完成后,对其过滤并收集滤液,再将滤液置于60℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;然后按重量份数计,分别称量55份去离子水、10份聚乙烯醇、10份上述制备的磁性凝胶中间体、20份备用的铜锌铁氧体粉末和5份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于80℃下水浴加热60min,制备得软磁前驱体;将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至800℃后,保温煅烧3h,随后停止加热,静置冷却至30℃,再将其置于不锈钢模具中冷压30min,即可制备得一种铜锌铁氧体软磁材料。本发明制备步骤简单,所得产品磁导率和居里温度高;在成型过程中分散性好,材料密度分布均匀,烧结后材料性能好;制得的铜锌铁氧体软磁材料饱和磁感为1.38,居里温度为800℃,电阻率为1.45μΩ·m,饱和场强度为32500A/m,磁导率为130mH/m,损耗为12.3W/kg,灵敏度为0.3%/(A·m-1)。
Claims (1)
1.一种铜渣回收制备铜锌铁氧体软磁材料的方法,其特征在于具体制备步骤为:
(1)收集炼铜厂含锌量2%的废弃铜渣,对其碾磨并过筛,制备得50~60目铜渣颗粒,随后将铜渣颗粒置于马弗炉中,对其通CO排除空气,再在CO气氛下,按8℃/min升温速率升温加热,待升温加热至1180~1250℃后,保温煅烧2~3h;
(2)待煅烧完成后,停止加热并静置冷却至20~30℃,随后用电磁铁装置将其进行筛分,回收磁性合金,按固液比1:5,将铜铁合金与质量浓度为75%硫酸溶液搅拌混合,制备得铜锌铁离子混合液;
(3)收集上述制备的铜锌铁离子混合液于烧杯中,向其中缓慢滴加3mol/L氢氧化钠,调节pH至9.5,待调节完成后,将其置于78~85℃下水浴加热2~3h,随后静置冷却并对其过滤,收集滤饼并用磁铁进行二次筛选,收集筛选物,用去离子水洗涤筛选物pH至7.0后,将其置于450~600℃下煅烧2~3h,再自然冷却并碾磨制备得铜锌铁氧体粉末,备用;
(4)按重量份数计,分别称量20~45份氯化铁、30~35份钛酸四丁酯、20~25份冰醋酸和5~20份聚乙烯醇与三口烧杯中,搅拌混合并置于70~85℃下水浴加热45~60min,待其加热完成后,对其过滤并收集滤液,再将滤液置于40~60℃下旋转蒸发至原有液体体积的1/8,制备得磁性凝胶中间体;
(5)按重量份数计,分别称量30~55份去离子水、10~15份聚乙烯醇、10~15份上述制备的磁性凝胶中间体、20~30份步骤(3)中制备的铜锌铁氧体粉末和5~10份γ-氨丙基三乙氧基硅烷置于烧杯中,搅拌混合并置于65~80℃下水浴加热45~60min,制备得软磁前驱体;
(6)将上述制备的软磁前驱体置于马弗炉中,对其通氮气排除空气,再在氮气气氛下,对其升温加热,控制升温速率为10℃/min,待升温至600~800℃后,保温煅烧2~3h,随后停止加热,静置冷却至20~30℃,再将其置于不锈钢模具中冷压25~30min,即可制备得一种铜锌铁氧体软磁材料。
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CN115626821A (zh) * | 2022-11-10 | 2023-01-20 | 杭州电子科技大学 | 一种用于肿瘤热疗的铁氧体材料及其制备方法 |
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CN106278224B (zh) * | 2016-08-19 | 2018-12-21 | 横店集团东磁股份有限公司 | 一种低温共烧用软磁铜锌铁氧体材料及其制备方法 |
CN115626821A (zh) * | 2022-11-10 | 2023-01-20 | 杭州电子科技大学 | 一种用于肿瘤热疗的铁氧体材料及其制备方法 |
CN115626821B (zh) * | 2022-11-10 | 2023-03-31 | 杭州电子科技大学 | 一种用于肿瘤热疗的铁氧体材料及其制备方法 |
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