CN116444262A - 一种高性能Bi2223前驱粉末的制备方法 - Google Patents
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- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 6
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- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 238000000034 method Methods 0.000 claims description 26
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
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Abstract
本发明公开了一种高性能Bi2223前驱粉末的制备方法,该方法包括:一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,配制Bi2223热解粉末和Pb3321或Pb3221热解粉末;二、将Pb3321或Pb3221热解粉末与Bi2223热解粉末混合后研磨,经热处理得到Bi2223前驱粉末。本发明在Bi2223前驱粉末中引入Pb3321或Pb3221粉末,促使Bi2223带材在热处理时Pb更容易进入Bi2223晶格中,提高Bi2223前驱粉末的均匀性和反应活性及转化效率,并调节Bi2223带材在后退火时析出小尺寸点状Pb3321相或Pb3221相,提升Bi2223前驱粉末的综合性能及其带材性能。
Description
技术领域
本发明属于高温超导材料技术领域,具体涉及一种高性能Bi2223前驱粉末的制备方法。
背景技术
(Bi,Pb)2Sr2Ca2Cu3Ox(Bi2223)在77K具有良好的载流性能,是重要的实用化高温超导材料。Bi2223高温超导材料可以采用粉末装管法加工成千米级长带,满足实用化要求。在Bi2223高温超导材料制备过程中,前驱粉末、加工和热处理是影响带材性能的三个主要关键因素。其中前驱粉末的性质尤其重要,是影响带材性能的核心因素。Bi2223芯丝中的前驱粉末的特性决定了最终芯丝的反应速度、超导相含量、超导晶粒的排布、微裂纹等,进而影响到带材的性能。
为了提升Bi2223前驱粉末的综合性能,研究人员通过多种方法制备前驱粉末,例如共沉淀方法,固相烧结法,喷雾干燥法等。通过改变元素化学计量比的方式,优化粉末中的元素比例,提高前驱粉末的性能;优化前驱粉末的热处理工艺参数等,提升前驱粉末的相纯度等;以及通过传统共沉淀方法分别合成Bi2212和CaCuO2粉末相混合,制备Bi2223前驱粉末,这些方法部分改善了前驱粉末的性能。但是,当较大范围改变元素比例时,出现不可控制的第二相,例如碱土铜酸盐相(AEC),铅酸钙相(Ca2PbO4)等。铅酸钙具有较高的熔化反应温度,导致Bi2223带材在热处理过程中Pb难以进入Bi2223的晶格,Bi2223的成相率降低。同时,Bi2223带材的热处理过程中,AEC颗粒的尺寸容易发生长大情况,阻碍超导电流传输。因此,传统制备方法较难控制热处理过程中芯丝的微液相的形成,难以调节Bi2223反应速率,难以调控第二相的种类和尺寸,前驱粉末的性能难以进一步提升。
发明内容
本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种高性能Bi2223前驱粉末的制备方法。本发明通过在Bi2223前驱粉末中引入Pb3321粉末或者Pb3221粉末,使得Bi2223带材在热处理过程中Pb更加容易进入Bi2223晶格中,提高Bi2223前驱粉末的均匀性和反应活性及转化效率,Bi2223带材在后退火过程中析出形成小尺寸点状Pb3321相或Pb3221相,可以提升Bi2223带材的磁通钉扎性能,进一步提升Bi2223前驱粉末的综合性能,解决了第二相种类难控制及尺寸较大导致Bi2223带材的性能降低的难题。
为解决上述技术问题,本发明采用的技术方案为:一种高性能Bi2223前驱粉末的制备方法,其特征在于,该方法包括以下步骤:
步骤一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,按照金属离子比例Bi:Pb:Sr:Ca:Cu=1.8:0.3:1.9:2:3选择原料溶解于硝酸溶液中,经喷雾热解得到(Bi1.8Pb0.3)Sr1.9Ca2Cu3Oy即Bi2223热解粉末,同时按照金属离子比例Pb:Bi:Sr:Ca:Cu=3:0.5:2.5:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到Pb3(Bi0.5Sr2.5)Ca2CuOx即Pb3321热解粉末,或者按照金属离子比例Pb:Bi:Sr:Ca:Cu=2.5:0.5:2:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到(Pb2.5Bi0.5)Sr2Ca2CuOz即Pb3221热解粉末;
步骤二、将步骤一中得到的Pb3321热解粉末或Pb3221热解粉末与Bi2223热解粉末按照0.01~0.03:1的质量比混合后研磨,经热处理得到Bi2223前驱粉末。
上述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,步骤二中所述热处理的温度为790℃,时间为10h~60h,采用的气氛为氧氩混合气,其中氧气的体积百分比为7.5%。
上述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,采用粉末装管法将步骤二中得到的Bi2223前驱粉末装管后加工,经轧制得到Bi2223带材,再经热处理得到高性能Bi2223多芯带材。
上述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,将Bi2223前驱粉末装入Ag管中,经拉拔加工得到单芯线,然后将单芯线截断后组装到AgMn包套中,经拉拔加工得到37芯线,再经轧制得到37芯的高性能Bi2223带材。
本发明与现有技术相比具有以下优点:
1、与传统前驱粉末中形成的高熔点Ca2PbO4第二相相比,本发明在Bi2223前驱粉末中引入Pb3321粉末或者Pb3221粉末,在热处理初期阶段,由于Pb3321或者Pb3221粉末的熔点更低,可以精确控制反应过程中的微液相,促使Pb更加容易进入Bi2223晶格中,提高Bi2223前驱粉末的均匀性和反应活性及转化效率;在热处理末期后退火阶段,部分Pb又会从Bi2223晶粒中析出,在局域元素配比调节的情况下,形成小尺寸点状Pb3321相或者Pb3221相第二相,小尺寸的第二相可以提升Bi2223带材的磁通钉扎性能,从而提升Bi2223前驱粉末的综合性能。
2、传统方法中直接改变溶液元素比例,非常容易在前驱粉末中形成其他杂相,同时在后续热处理过程中形成大尺寸颗粒而影响超导电流传输。与之相比较,本发明通过在Bi2223前驱粉末中引入Pb3321粉末或者Pb3221粉末,形成部分元素富集区域,且热处理反应过程中形成微液相促进Bi2223晶粒生长,并在降温过程中析出形成小尺寸的第二相,解决传统大尺寸第二相抑制Bi2223性能的问题,提升Bi2223前驱粉末的综合性能。
下面通过实施例对本发明的技术方案作进一步的详细描述。
具体实施方式
实施例1
本实施例包括以下步骤:
步骤一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,按照金属离子比例Bi:Pb:Sr:Ca:Cu=1.8:0.3:1.9:2:3选择原料溶解于硝酸溶液中,经喷雾热解得到(Bi1.8Pb0.3)Sr1.9Ca2Cu3Oy即Bi2223热解粉末,同时按照金属离子比例Pb:Bi:Sr:Ca:Cu=3:0.5:2.5:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到Pb3(Bi0.5Sr2.5)Ca2CuOx即Pb3321热解粉末;
步骤二、将步骤一中得到的Pb3321热解粉末与Bi2223热解粉末按照0.01:1的质量比混合后研磨,经热处理得到Bi2223前驱粉末;所述热处理的温度为790℃,时间为10h,采用的气氛为氧氩混合气,其中氧气的体积百分比为7.5%;
步骤三、采用粉末装管法将步骤二中得到的Bi2223前驱粉末装入Ag管中,经拉拔加工得到单芯线,然后将单芯线截断后组装到AgMn包套中,经拉拔加工得到37芯线,再经轧制得到37芯的高性能Bi2223带材。
经检测,本实施例得到的Bi2223前驱粉末中含有质量分数1%的Pb3321相,且加工得到的37芯的高性能Bi2223带材在液氮温度下临界电流为120A,具有优异的超导性能。
实施例2
本实施例包括以下步骤:
步骤一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,按照金属离子比例Bi:Pb:Sr:Ca:Cu=1.8:0.3:1.9:2:3选择原料溶解于硝酸溶液中,经喷雾热解得到(Bi1.8Pb0.3)Sr1.9Ca2Cu3Oy即Bi2223热解粉末,同时按照金属离子比例Pb:Bi:Sr:Ca:Cu=2.5:0.5:2:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到(Pb2.5Bi0.5)Sr2Ca2CuOz即Pb3221热解粉末;
步骤二、将步骤一中得到的Pb3221热解粉末与Bi2223热解粉末按照0.02:1的质量比混合后研磨,经热处理得到Bi2223前驱粉末;所述热处理的温度为790℃,时间为30h,采用的气氛为氧氩混合气,其中氧气的体积百分比为7.5%;
步骤三、采用粉末装管法将步骤二中得到的Bi2223前驱粉末装入Ag管中,经拉拔加工得到单芯线,然后将单芯线截断后组装到AgMn包套中,经拉拔加工得到37芯线,再经轧制得到37芯的高性能Bi2223带材。
经检测,本实施例得到的Bi2223前驱粉末中含有质量分数2%的Pb3221相,且加工得到的37芯的高性能Bi2223带材在液氮温度下临界电流为140A,具有优异的超导性能。
实施例3
本实施例包括以下步骤:
步骤一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,按照金属离子比例Bi:Pb:Sr:Ca:Cu=1.8:0.3:1.9:2:3选择原料溶解于硝酸溶液中,经喷雾热解得到(Bi1.8Pb0.3)Sr1.9Ca2Cu3Oy即Bi2223热解粉末,同时按照金属离子比例Pb:Bi:Sr:Ca:Cu=2.5:0.5:2:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到(Pb2.5Bi0.5)Sr2Ca2CuOz即Pb3221热解粉末;
步骤二、将步骤一中得到的Pb3221热解粉末与Bi2223热解粉末按照0.03:1的质量比混合后研磨,经热处理得到Bi2223前驱粉末;所述热处理的温度为790℃,时间为60h,采用的气氛为氧氩混合气,其中氧气的体积百分比为7.5%;
步骤三、采用粉末装管法将步骤二中得到的Bi2223前驱粉末装入Ag管中,经拉拔加工得到单芯线,然后将单芯线截断后组装到AgMn包套中,经拉拔加工得到37芯线,再经轧制得到37芯的高性能Bi2223带材。
经检测,本实施例得到的Bi2223前驱粉末中含有质量分数3%的Pb3221相,且加工得到的37芯的高性能Bi2223带材在液氮温度下临界电流为130A,具有优异的超导性能。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化,均仍属于本发明技术方案的保护范围内。
Claims (4)
1.一种高性能Bi2223前驱粉末的制备方法,其特征在于,该方法包括以下步骤:
步骤一、以氧化铋、硝酸铅、碳酸锶、碳酸钙、无氧铜为原料,按照金属离子比例Bi:Pb:Sr:Ca:Cu=1.8:0.3:1.9:2:3选择原料溶解于硝酸溶液中,经喷雾热解得到(Bi1.8Pb0.3)Sr1.9Ca2Cu3Oy即Bi2223热解粉末,同时按照金属离子比例Pb:Bi:Sr:Ca:Cu=3:0.5:2.5:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到Pb3(Bi0.5Sr2.5)Ca2CuOx即Pb3321热解粉末,或者按照金属离子比例Pb:Bi:Sr:Ca:Cu=2.5:0.5:2:2:1选择原料溶解于硝酸溶液中,经喷雾热解得到(Pb2.5Bi0.5)Sr2Ca2CuOz即Pb3221热解粉末;
步骤二、将步骤一中得到的Pb3321热解粉末或Pb3221热解粉末与Bi2223热解粉末按照0.01~0.03:1的质量比混合后研磨,经热处理得到Bi2223前驱粉末。
2.根据权利要求1所述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,步骤二中所述热处理的温度为790℃,时间为10h~60h,采用的气氛为氧氩混合气,其中氧气的体积百分比为7.5%。
3.根据权利要求1所述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,采用粉末装管法将步骤二中得到的Bi2223前驱粉末装管后加工,经轧制得到Bi2223带材,再经热处理得到高性能Bi2223多芯带材。
4.根据权利要求3所述的一种高性能Bi2223前驱粉末的制备方法,其特征在于,将Bi2223前驱粉末装入Ag管中,经拉拔加工得到单芯线,然后将单芯线截断后组装到AgMn包套中,经拉拔加工得到37芯线,再经轧制得到37芯的高性能Bi2223带材。
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