CN107098694A - 一种磁伸缩转能器用宽带吸波铁氧体材料及其制备方法 - Google Patents

一种磁伸缩转能器用宽带吸波铁氧体材料及其制备方法 Download PDF

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CN107098694A
CN107098694A CN201710341784.8A CN201710341784A CN107098694A CN 107098694 A CN107098694 A CN 107098694A CN 201710341784 A CN201710341784 A CN 201710341784A CN 107098694 A CN107098694 A CN 107098694A
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瞿德林
王久如
王晓祥
李丛俊
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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Abstract

本发明公开了一种磁伸缩转能器用宽带吸波铁氧体材料的制备方法,包括如下步骤:S1、称取硝酸铁、醋酸锌、硝酸锰,加入草酸和去离子水搅拌溶解得到混合溶液1;S2、称取柠檬酸和EDTA,加入去离子水溶解得到混合溶液2;S3、按重量份取100份混合溶液1,调节pH至6.5‑8,静置,取混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取混合溶液2继续滴加至混合物料1中,得到混合物物料2;S4、将混合物料2加热搅拌胶凝,预烘得到预烘物料;S5、将预烘物料中加入参杂料混合均匀,升温至1000‑1200℃进行烧结,水淬,二次升温保温,随炉冷却至室温得到产品。本发明提高了磁伸缩转能器用铁氧体材料的磁致伸缩性能和吸波宽度,满足了实际使用要求。

Description

一种磁伸缩转能器用宽带吸波铁氧体材料及其制备方法
技术领域
本发明涉及磁伸缩转能器用铁氧体材料制备技术领域,尤其涉及一种磁伸缩转能器用宽带吸波铁氧体材料及其制备方法。
背景技术
超声是近年来科学技术中发展较快的领域之一,已取得了许多卓越的成果。现在有很多科学和技术部门正在兴趣盎然地应用着超声方法或是正在力求引用这一新的技术成就。超声工程的中应用最多的是压电换能器和磁伸缩转能器,而后者在大功率超声的应用中占着重要的地位。因此这是现在人们努力研究的一个方面,在寻求优良的磁伸缩材料,以代替或超越当前应用最多的钝镍或镍合金的研究主要集中在铁铝合金和铁氧体材料上,而后者以具有良好的电磁性能、制备方法易控成为理想的磁伸缩材料。但是目前用于磁伸缩转能器的铁氧体材料的伸缩性能和吸波带宽性能越来越不能满足实际使用要求。
发明内容
本发明提出了一种磁伸缩转能器用宽带吸波铁氧体材料及其制备方法,提高了铁氧体的磁致伸缩性能和转能效率,拓宽了吸波宽度,满足了实际使用要求。
本发明提出的一种磁伸缩转能器用宽带吸波铁氧体材料的制备方法,包括如下步骤:
S1、按摩尔分数称取10-15份硝酸铁、5-8份醋酸锌、3-5份硝酸锰,加入8-15份草酸和12-20份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1-1.2倍的去离子水溶解得到混合溶液2;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至6.5-8,静置,取40-50份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取20-30份混合溶液2继续滴加至混合物料1中,得到混合物物料2;
S4、将混合物料2加热至70-80℃,搅拌胶凝,预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1000-1200℃进行烧结,水淬,二次升温至700-800℃保温,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料。
优选地,S2中,柠檬酸和EDTA的摩尔比为10:2-3。
优选地,S3中,改性黄麻与混合溶液1的重量比为5-10:100。
优选地,S3中,改性黄麻的制备过程包括:将黄麻置于均苯四甲酸二酐和N,N-二甲基甲酰胺的混合溶液中,升温至60-70℃,在微波条件下反应20-30min,冷却,洗涤过滤,烘干后加入石墨烯进行超声混合,球磨后干燥得到改性黄麻。
优选地,黄麻和均苯四甲酸二酐质量体积比为1-3:4。
优选地,黄麻和均苯四甲酸二酐质量体积比为1:2。
优选地,均苯四甲酸二酐和N,N-二甲基甲酰胺的体积比为4-6:10。
优选地,所述黄麻经过预处理,预处理的具体操作为:将麻黄在碱液中浸泡,过滤,水洗至中性,干燥后备用。
优选地,S4中,预烘温度为120-150℃。
优选地,S5中,烧结时间为2-4h,优选地,保温时间为1-2h。
本发明提出了一种磁伸缩转能器用宽带吸波铁氧体材料,由所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法制得。
本发明在溶胶-凝胶的基础上,以硝酸铁、醋酸锌和硝酸锰为主料,采用EDTA配合作用络合剂,柠檬酸作为凝胶剂,两者与铁、锌、锰、铟、镓、钽离子具有很好的配位作用,形成稳定的多元结构,保证了铁氧体材料电磁性能的稳定性,同时两者配合作用促进了铁氧体晶粒的传质和生长,晶体结构更加紧密,可促进材料的晶粒生长、致密化并降低损耗,拓宽了铁氧体材料的温域;加入改性黄麻,对金属离子具有很好的吸附能力,黄麻改性后具有一定的空间孔径结构提高了铁氧体的吸波性能,在凝胶中期加入黄麻形成大型网状支撑结构,促进主料中黄麻表面晶粒生长,并在烧结阶段,促进主料和参杂料的复合,提高了铁氧体材料的等效电磁参数,拓宽材料的吸波带宽;黄麻来源广,价格低廉,降低了生产成本;本发明在烧结后进行热处理,通过保温-水淬-二次升温-随炉冷却工艺,提高了氧化铟、氧化镓、氧化钽、氧化钙、氧化钡的参杂效果,提高了单空位缺陷浓度,铁氧体材料的磁致伸缩性能相应提高,从而提高了铁氧体的转能效率,同时进一步扩宽了吸波宽度。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种磁伸缩转能器用宽带吸波铁氧体材料,由如下步骤制得:
S1、按摩尔分数称取10份硝酸铁、8份醋酸锌、3份硝酸锰,加入8份草酸和12份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1倍的去离子水溶解得到混合溶液2;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至6.5,静置,取40份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取20份混合溶液2继续滴加至混合物料1中,得到混合物物料2;
S4、将混合物料2加热至70℃,搅拌胶凝,预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1000℃进行烧结,水淬,二次升温至800℃保温,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料。
实施例2
一种磁伸缩转能器用宽带吸波铁氧体材料,由如下步骤制得:
S1、按摩尔分数称取15份硝酸铁、5份醋酸锌、5份硝酸锰,加入15份草酸和20份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1.2倍的去离子水溶解得到混合溶液2;其中,柠檬酸和EDTA的摩尔比为10:2;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至8,静置,取50份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取30份混合溶液2继续滴加至混合物料1中,得到混合物物料2;其中,改性黄麻与混合溶液1的重量比为5:100;
S4、将混合物料2加热至80℃,搅拌胶凝,在120℃下预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1200℃进行烧结2h,水淬,二次升温至700℃保温2h,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料。
实施例3
一种磁伸缩转能器用宽带吸波铁氧体材料,由如下步骤制得:
S1、按摩尔分数称取12份硝酸铁、6份醋酸锌、4份硝酸锰,加入12份草酸和17份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1.2倍的去离子水溶解得到混合溶液2;其中,柠檬酸和EDTA的摩尔比为10:3;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至7,静置,取45份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取25份混合溶液2继续滴加至混合物料1中,得到混合物物料2;其中,改性黄麻与混合溶液1的重量比为10:100;
S4、将混合物料2加热至80℃,搅拌胶凝,在120℃下预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1000℃进行烧结4h,水淬,二次升温至800℃保温1h,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料;
改性黄麻的制备过程包括:将黄麻置于均苯四甲酸二酐和N,N-二甲基甲酰胺的混合溶液中,升温至60℃,在微波条件下反应30min,冷却,洗涤过滤,烘干后加入石墨烯进行超声混合,球磨后干燥得到改性黄麻。
实施例4
一种磁伸缩转能器用宽带吸波铁氧体材料,由如下步骤制得:
S1、按摩尔分数称取12份硝酸铁、6份醋酸锌、4份硝酸锰,加入12份草酸和17份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1.2倍的去离子水溶解得到混合溶液2;其中,柠檬酸和EDTA的摩尔比为10:2.5;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至7,静置,取45份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取25份混合溶液2继续滴加至混合物料1中,得到混合物物料2;其中,改性黄麻与混合溶液1的重量比为7.5:100;
S4、将混合物料2加热至80℃,搅拌胶凝,在150℃下预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1000℃进行烧结4h,水淬,二次升温至800℃保温1h,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料;
改性黄麻的制备过程包括:将黄麻置于均苯四甲酸二酐和N,N-二甲基甲酰胺的混合溶液中,升温至70℃,在微波条件下反应20min,冷却,洗涤过滤,烘干后加入石墨烯进行超声混合,球磨后干燥得到改性黄麻;其中,黄麻和均苯四甲酸二酐质量体积比为1-3,均苯四甲酸二酐和N,N-二甲基甲酰胺的体积比为4:10。
实施例5
一种磁伸缩转能器用宽带吸波铁氧体材料,由如下步骤制得:
S1、按摩尔分数称取12份硝酸铁、6份醋酸锌、4份硝酸锰,加入12份草酸和17份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1.2倍的去离子水溶解得到混合溶液2;其中,柠檬酸和EDTA的摩尔比为10:2.5;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至7,静置,取45份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取25份混合溶液2继续滴加至混合物料1中,得到混合物物料2;其中,改性黄麻与混合溶液1的重量比为7.5:100;
S4、将混合物料2加热至80℃,搅拌胶凝,在140℃下预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1100℃进行烧结3h,水淬,二次升温至750℃保温1.5h,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料;
改性黄麻的制备过程包括:将麻黄在碱液中浸泡,过滤,水洗至中性,干燥后备用;将预处理过的黄麻置于均苯四甲酸二酐和N,N-二甲基甲酰胺的混合溶液中,升温至70℃,在微波条件下反应20min,冷却,洗涤过滤,烘干后加入石墨烯进行超声混合,球磨后干燥得到改性黄麻;其中,黄麻和均苯四甲酸二酐质量体积比为1-2,均苯四甲酸二酐和N,N-二甲基甲酰胺的体积比为6:10。
将实施例3-5制得磁伸缩转能器用宽带吸波铁氧体材料进行性能测试,测试结果如下所示:
性能参数 实施例3 实施例4 实施例5
有效带宽/GHz 5.0-16.9 3.5-15.6 4.5-17.2
反射损耗/dB <-10 <-10 >-10
磁致伸缩量(8000A/m)/(ppm) 1259 1294 1280
从测试结果可以看出,本发明采用采用EDTA配合作用络合剂并加入改性黄麻,提高了铁氧体的磁致伸缩性能和吸波宽度,满足了实际使用要求。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。

Claims (9)

1.一种磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,包括如下步骤:
S1、按摩尔分数称取10-15份硝酸铁、5-8份醋酸锌、3-5份硝酸锰,加入8-15份草酸和12-20份去离子水搅拌溶解得到混合溶液1;
S2、称取柠檬酸和EDTA,加入取柠檬酸和EDTA总摩尔份数1-1.2倍的去离子水溶解得到混合溶液2;
S3、按重量份取100份混合溶液1,向其中滴加氨水调节pH至6.5-8,静置,取40-50份混合溶液2滴加至混合溶液1中,加入改性黄麻得到混合物料1,另取20-30份混合溶液2继续滴加至混合物料1中,得到混合物物料2;
S4、将混合物料2加热至70-80℃,搅拌胶凝,预烘得到预烘物料;
S5、将预烘物料中加入氧化铟、氧化镓、氧化钽、氧化钙、氧化钡混合均匀,升温至1000-1200℃进行烧结,水淬,二次升温至700-800℃保温,随炉冷却至室温得到磁伸缩转能器用宽带吸波铁氧体材料。
2.根据权利要求1所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,S2中,柠檬酸和EDTA的摩尔比为10:2-3。
3.根据权利要求1所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,S3中,改性黄麻与混合溶液1的重量比为5-10:100。
4.根据权利要求1-3任一项所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,S3中,改性黄麻的制备过程包括:将黄麻置于均苯四甲酸二酐和N,N-二甲基甲酰胺的混合溶液中,升温至60-70℃,在微波条件下反应20-30min,冷却,洗涤过滤,烘干后加入石墨烯进行超声混合,球磨后干燥得到改性黄麻。
5.根据权利要求4所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,黄麻和均苯四甲酸二酐质量体积比为1-3:4;优选地,黄麻和均苯四甲酸二酐质量体积比为1:2;优选地,均苯四甲酸二酐和N,N-二甲基甲酰胺的体积比为4-6:10。
6.根据权利要求4所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,所述黄麻经过预处理,预处理的具体操作为:将麻黄在碱液中浸泡,过滤,水洗至中性,干燥后备用。
7.根据权利要求1-3任一项所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,S4中,预烘温度为120-150℃。
8.根据权利要求1-3任一项所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法,其特征在于,S5中,烧结时间为2-4h,优选地,保温时间为1-2h。
9.一种磁伸缩转能器用宽带吸波铁氧体材料,其特征在于,由权利要求1-8任一项所述的磁伸缩转能器用宽带吸波铁氧体材料的制备方法制得。
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