CN116444262A - 一种高性能Bi2223前驱粉末的制备方法 - Google Patents
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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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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1701395A (zh) * | 2003-06-26 | 2005-11-23 | 住友电气工业株式会社 | 铋基氧化物超导线材及其制备方法 |
| JP2006082992A (ja) * | 2004-09-14 | 2006-03-30 | Sumitomo Electric Ind Ltd | 原料粉末の製造方法 |
| JP2007149416A (ja) * | 2005-11-25 | 2007-06-14 | Sumitomo Electric Ind Ltd | 酸化物超電導材料およびその製造方法ならびに超電導線材、超電導機器 |
| JP2007214070A (ja) * | 2006-02-13 | 2007-08-23 | Sumitomo Electric Ind Ltd | 超電導線材およびその製造方法ならびに超電導機器 |
| CN102503402A (zh) * | 2011-09-19 | 2012-06-20 | 北京英纳超导技术有限公司 | 一种铋系超导粉的制备方法 |
| CN103896576A (zh) * | 2014-03-06 | 2014-07-02 | 北京英纳超导技术有限公司 | 一种改性铋系超导粉及其制备方法 |
| CN113593765A (zh) * | 2021-07-06 | 2021-11-02 | 西部超导材料科技股份有限公司 | 一种铋系高温超导线/带材的制备方法 |
-
2023
- 2023-04-28 CN CN202310475533.4A patent/CN116444262B/zh active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1701395A (zh) * | 2003-06-26 | 2005-11-23 | 住友电气工业株式会社 | 铋基氧化物超导线材及其制备方法 |
| JP2006082992A (ja) * | 2004-09-14 | 2006-03-30 | Sumitomo Electric Ind Ltd | 原料粉末の製造方法 |
| JP2007149416A (ja) * | 2005-11-25 | 2007-06-14 | Sumitomo Electric Ind Ltd | 酸化物超電導材料およびその製造方法ならびに超電導線材、超電導機器 |
| JP2007214070A (ja) * | 2006-02-13 | 2007-08-23 | Sumitomo Electric Ind Ltd | 超電導線材およびその製造方法ならびに超電導機器 |
| CN102503402A (zh) * | 2011-09-19 | 2012-06-20 | 北京英纳超导技术有限公司 | 一种铋系超导粉的制备方法 |
| CN103896576A (zh) * | 2014-03-06 | 2014-07-02 | 北京英纳超导技术有限公司 | 一种改性铋系超导粉及其制备方法 |
| CN113593765A (zh) * | 2021-07-06 | 2021-11-02 | 西部超导材料科技股份有限公司 | 一种铋系高温超导线/带材的制备方法 |
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