CN106024196B - Nb3Al超导材料的制备方法 - Google Patents
Nb3Al超导材料的制备方法 Download PDFInfo
- Publication number
- CN106024196B CN106024196B CN201610481932.1A CN201610481932A CN106024196B CN 106024196 B CN106024196 B CN 106024196B CN 201610481932 A CN201610481932 A CN 201610481932A CN 106024196 B CN106024196 B CN 106024196B
- Authority
- CN
- China
- Prior art keywords
- niobium powder
- nb3al
- powder
- superconductors
- pretreatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- 239000002887 superconductor Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 139
- 239000010955 niobium Substances 0.000 claims abstract description 132
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium Chemical compound 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[Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 110
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 110
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 238000007781 pre-processing Methods 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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- 238000005245 sintering Methods 0.000 claims abstract description 7
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 20
- 229910052904 quartz Inorganic materials 0.000 claims description 19
- 239000010453 quartz Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials 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Classifications
-
- H—ELECTRICITY
- H01—BASIC ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—BASIC ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Abstract
本发明公开一种Nb3Al超导材料的制备方法，以铌粉和氢气的物理化学作用作为细化铌粉的预处理过程，所述方法包括在氢氩混合气氛中加热铌粉，经过预处理的铌粉与铝粉按照Nb3Al的化学计量比混合均匀后压片，烧结即得到Nb3Al超导材料。这种Nb3Al超导材料制备过程中不会引入其他金属杂质，纯度高，超导性能优良。本发明制备工艺简单，制备周期短，能耗低，设备简单，大大降低了生产成本，适合不同大小规模的生产。
Description
Nb3AI超导材料的制备方法
技术领域
[0001]本发明涉及一种Nb3Al超导材料的制备方法。
背景技术
[0002]高场超导磁体在诸如核磁共振、ITER热核聚变、高能粒子加速器等技术领域起着 无可替代的重要作用。在现有超导磁体制备技术中，10T及以下磁体采用机械延展性能优异 的NbTi合金超导线绕制而成。由于NbTi合金的临界磁场较低，10T以上的更高磁场则需要使 用具备更高临界磁场特性的A-15型金属间化合物超导材料建造磁体。现有的l〇—20T磁体多 采用由低温超导体的NbTi合金和Nb：3Sn超导体的混合线圈嵌套构成。A-15型金属间化合物 Nb：3Sn超导材料具有较好的经济性和较高的技术成熟度，但是其缺点在于临界性能有限，且 机械性能尤其脆弱。高场磁体线圈要求在承受较大的应力同时能够维持较高的电流密度， 同属A-15型晶体结构的Nb：3Al相比Nb3Sn具备超导临界性能高、应力敏感性低、耐辐照性能 好等技术优点，是未来商用热核聚变堆、高能粒子加速器、NMR等高场应用中替代Nb3Sn的理 想材料。
[0003] 由于Nb3Al成相温度高，低于成相温度时存在化学计量比偏移的现象，目前仍未有 商业制备的NbMl出售。超导磁体的电缆线中一般用铜来作为稳定化材料，一定量铜的存在 可以帮助超导体在扰动失超的情况下减小焦耳热的产生。目前，Nb3Al超导材料的优化制备 技术主要有:快热快冷法和机械合金化法。
[0004] 快热快冷法:将Nb和A1进行机械复合后，加工成长线，然后在真空环境下进行快速 加热和冷却，使Nb和A1反应生成Nb (Al) ss过饱和固溶体，进而在800°C左右退火将Nb (Al) ss 转变为Nb3Al。上述过程中需要通过特殊的设备在2000°C左右的高温下进行热处理，；原料 须将铌和铝加工成管状，带状或板状，然后进行加工和复合再拉丝和热处理，工艺极其复 杂，周期长。另外，用叠层卷制法或管中棒法制成的前驱体线材外层为铜，欧姆加热处理时 的温度明显高于铜的熔点，所以在进行欧姆加热之前须用酸洗方法除去这层铜，去铜操作 复杂;若前驱体线材采用难融的Nb或Ta作为基体材料，起稳定化作用的Cu只能通过其他方 式附加到线材上，热稳定效果下降，股线制造成本大幅度增加。利用这种方法合成的Nb3Al 线材的性能高度依赖于欧姆加热处理过程中线材获得的最高温度(Tmax)。由于被加热股线 的弯曲、振动和熔融Ga浴液面的随时变化，因此，即使欧姆加热电流保持不变，也不能保证 线材获得的最高温度(Tmax)不变，合成线材的性能也得不到保证。此外，在进行转变退火时 由于线材升温速度的差异会产生A15相的堆垛层错，偏离化学计量比，导致Tc和Bc2下降。除 了上面提到的问题外，Nb/Al先驱线截面配置、退火前有助于提高晶界密度的机械变形制度 和适合减小堆垛层错密度的退火制度等也都还需进一步的优化。可见，RHQT方法工艺复杂， 对设备要求太高，周期长，效率低下，反应条件难以控制，很难满足大规模应用的需求。
[0005] 机械合金化法:通过机械-化学作用，把混合的Nb和A1粉末放入球磨机中进行机械 合金化，然后对机械合金化后的粉末进行热处理得到铌铝化合物。此法物相纯度不高，且设 备不普及，在磨球型号，球磨介质，球料比，转速及时间等方面需进行多番调试，为充分混合 及避免在球磨罐底形成合金壳层，球磨罐还需要间歇处理，且不可避免原料粉末被磨球污 染的可能，很难用于扩大规模生产。
[0006]尚温合成的工艺普遍复杂难度大，或对设备要求高。基于密度泛函的一系列计算 表明颗粒细小的反应物使反应中的活化能大幅减少，降低合成难度。本发明利用铌粉吸收 气体的特性，首先通过氢气与铌粉的物理化学作用，产生含有氢气的铌粉与微量铌氢化合 物，达到细化铌粉的目的，使反应中的活化能大幅减少，降低合成难度。后续的热处理过程 中氢气及少量氢化物会抑制铌粉和铝粉与烧结环境中存在的微量空气发生氧化反应，避免 引入氧化物，氮化物等杂质，确保产品质量。细化的铌粉与铝粉按配比模压成形，在140(rc 烧结得到具有AI5结构的Nb3Al超导材料。
发明内容
[0007]针对上述问题，本发明提供一种制备工艺简单、制备周期短、制备效率高，且值得 的超导材料性能优良的Nb3Al超导材料的制备方法。
[0008]为达到上述发明目的，本发明Nb3Al超导材料的制备方法，包括：
[0009] a、镅粉预处理 •
[0010]将纯度为99.99%的Nb粉均匀铺洒在石英舟内，放入管式炉，通入配比为4.7%_ 100%的氢气和95.3%-0的氩气混合气，在3〇〇-38(TC的温度区间加热，保温3小时，随炉冷 却后取出，得到预处理铌粉；
[00川 b、压片制备
[0012]按Nb3Al分子式中Nb与A1原子摩尔比3:1进行配料，称取纯度为99.99%的々1粉和& 步制得的预处理铌粉，将预处理过的铌粉、铝粉装入玛瑙研钵中，研磨混合均匀，然后使用 模具压制成形，压制压力为lOMPa，制成块片状料坯，用铌箱包裹，将包裹好的块片状料坯装 入石英舟中；
[0013] c、烧结
[00M]将装有b步制得的块片状料坯的石英舟放在管式炉中，在4 • 7 %的氢气与95.3 %的 氩气混合气保护中，将炉温升温至1400-C，保温10小时进行烧结反应，然后快速冷却至室 温，即制得Nb3Al超导材料。
[0015] 具体地，a、铌粉预处理具体包括:将纯度为99.99 %的Nb粉均匀铺洒在石英舟内， 放入管式炉，通入纯度为99.99%的氢气，升温至38(TC，保温3小时，随炉冷却后取出，得到 预处理铌粉。
[0016] 具体地，a、铌粉预处理具体包括:将纯度为99.99%的Nb粉均匀铺洒在石英舟内， 放入管式炉，通入配比为4.7%的氢气和％•3%的氩气混合气，升温至38(TC，保温3小时，随 炉冷却后取出，得到预处理铌粉。
[0017] 具体地，a、铌粉预处理具体包括:将纯度为的Nb粉均匀铺洒在石英舟内， 放入管式炉，通入配比为4.7%的氢气和95 •3%的氩气混合气，升温至34"7-C，保温3小时，随 炉冷却后取出，得到预处理铌粉。 t0018]具体地，a、铌粉预处理具体包括:将纯度为99.99%的Nb粉均匀铺洒在石英舟内， 放入管式炉，通入配比为4• 7%的氢气和％ •3%的氩气混合气，升温至30(TC，保温3小时，随 炉冷却后取出，得到预处理铌粉。 L0019」有益效果
[0020]本发明Nb3Al超导材料的制备方法与现有技术具备如下有益效果：
[0021] 1、本发明利用铌粉吸收气体的特性，首先通过氢气与铌粉的物理化学作用，产生 含有氢气的铌粉与微量铌氢化合物，达到细化铌粉的目的，使反应中的活化能大幅减少，降 低合成难度。后续的热处理过程中氢气及少量氢化物会抑制铌粉和铝粉与烧结环境中存在 的微量空气发生氧化反应，避免引入氧化物，氮化物等杂质，确保产品质量。
[0022] 2、本发明错粉和细化的铌粉通过扩散反应直接形成所需的Nb3Al超导相，避免了 快热快冷法及机械化合金法需要特殊设备的要求以及成分不稳定的情况，所得Nb3A1超导 材料成分均匀，性能优良。
[0023] 3、本发明使用通用的管式炉有效降低了成本，简化制备工艺，避免引入其他杂质， 不同的制备工艺参数的变化对制得材料的性能影响较小，满足工业化生产的要求，便于大 规模生产，具有广泛的应用前景。
附图说明
[0024]图1是本发咖麗超导材料的制备方法的实翻—碰理后的雜与原料银粉 的XRD对比图； D025j ® 2 g H 0j^b 3 A1 ® •料的齡方法的实n例—祕的 3 A i超导材料的XRD 指标化图； _6]图墙賴_b3A_钟料_恪施的实麵二觀理后随购原料讎 的XRD对比图； _7] ’是本发0jNb3Al®导材料咖备方法的实酬：齡咖應超导材料的 图；
[0028]图5是本发明Nb 3 A1超导材料的制备方法的实施例三预处理后的与原料银粉 的XRD对比图； _9]图6是本发_麗超导材料_丨」备方法的实删王制細廳心超导材料的xrd 图； 是本发_3A1超导材料的制备方法的实施例四预处理后的银粉与原料铜粉 的XRD对比图； =〇31]图8疋本发明Nb3All导材料的制备方法的实施例四制备超导材料的 图； 注:图U图3、图5、图7中上方的曲线为预处理后的银粉曲线，下方的曲线为原料银
具体实施方式
[0033]下面结合附图对本发明做进〜步的描述 [0034] 实施例1 、 。
[0035]本实施例NMAl超导材料的制备方 [0036] a、铌粉预处理 ’
[0_觀度为"_娜的轉均勾铺洒在石英舟内，放入管式炉，通入纯度为"遍 的氢气，升温至380°C，保温3小时，随炉冷却后取出，得到预处理铌粉。
[0038] b、压片制备
[0039] 按Nb3Al分子式中Nb与A1原子摩尔比3:1进行配料，称取纯度为99 •99 %的A1粉和a 步制得的预处理铌粉，将预处理过的铌粉、铝粉装入玛瑙研钵中，研磨混合均匀，然后使用 模具压制成形，压制压力为lOMPa，制成块片状料坯，用铌箔包裹，将包裹好的块片状料坯装 入石英舟中。
[0040] C、烧结
[0041]将装有b步制得的块片状料坯的石英舟放在管式炉中，在4.7 %的氢气与95.3 %的 氩气混合气保护中，将炉温升温至140(TC，保温10小时进行烧结反应，然后快速冷却至室 温，即制得Nb：3Al超导材料。
[0042]所述的a，c步的热处理的升温速度不限。
[0043] 图1为本例方法制得的预处理后的铌粉与原料铌粉的XRD对比图，从图中可以看 出，经过预处理的铌粉衍射峰宽化明显，存在微量杂质。根据XRD数据可得三强峰的半峰宽， 原料铌粉的平均半峰宽为0.1288 (29/。），预处理后的铌粉平均半峰宽为0.2〇8 (20/。）。根据 谢乐公式计算，原料铌粉的平均晶粒度是?3.5nm，预处理后铌粉的平均晶粒度是43.6nm，达 到细化铌粉的目的。
[0044] 图功采用本实施例所述的方法制得的他謝超导材料的图，对具有M5相结构 的Nb3Al进行指标化标示，除他和A1以外没有其他元素存在，预处理后的铌粉所含的微量杂 质对NbMl样品没有影响，所制得的他^丨超导材料整体成分均匀。取本实施例中制得的 Nb3Al超导材料进行测试，其超导转变温度为15.2K。
[0045] 实施例2
[0046]本例与实施例Nb3Al超导材料的制备方法，在实施例丨的基础上，不同之处仅在于. [0047] a、铌粉预处理 • J°〇48]将纯度为的池粉均匀铺洒在石英舟内，放入管式炉，通入配比为4.7%的 虱气和95 • 3%的氩气混合气，升温至38〇°c，保温3小时，随炉冷却后取出，得到预处理铌粉。
[0049]图3为本例方法制得的预处理后的铌粉与原料铌粉的XRD对比图，从图中可以看 出’ fen过预处理的银粉衍射峰宽化明显，存在微量杂质。根据XRD数据可得三强峰的半峰宽， 原料银粉的平均半峰宽为〇• I288⑽/。），碰理后的働^平均半峰宽加.468⑽/。）。根据 谢乐公式计算，原料铌粉的平均晶粒度是73 _ 5nm，预处理后铌粉的平均 到细化铜粉的目的。 」日日做疋y.ynm，® _] S4为采用本实施例所述的方法制肖的NbMl超导材料的XRD图，主要成分为 腦所含的觀細麻3Al關㈣，所制得的 寸材料整体成分均匀。取本买施例中制得的廳“超导材料进行测试，其超导转变 温度为16.8K。 、
[0051] 实施例3 =]]腿1麵職臟，在麵_祉，碰处仅在于： 将纯度为的Nb粉均勾铺洒在石英舟内，放入管式炉，通入配比为4 M和95 •3⑽氩气混合气，升温至3仍，保温3小时，随炉冷却后取出，得到预f理银粉的 |±|b乃耳:例万法制侍的预处理后的铌粉与原料铌粉的XRD对比图，从图中可以看 出，经过预处理的铌粉衍射峰宽化明显，存在微量杂质。根据XRD数据可得三强峰的半峰宽， 原料铌粉的平均半峰宽为〇.1288 (20/。），预处理后的铌粉平均半峰宽为〇.4〇56(20/。）。根 据谢乐公式计算，原料铌粉的平均晶粒度是73 • 5nm，预处理后铌粉的平均晶粒度是26 〇_ 达到细化铌粉的目的。
[0056]图6为采用本实施例所述的方法制得的NbM1超导材料的XRD图，主要成分为 Nb3A 1，含有少量Nb2A 1，预处理后的铌粉所含的微量杂质对Nb;3A1样品没有影响，所制得的 Nb3Al超导材料整体成分均匀。取本实施例中制得的池^丨超导材料进行测试，宜超导 温度为15.7K。
[0057] 实施例4
[0058]本例与实施例他说1超导材料的制备方法，在实施例丨的基础上，不同之处仅在于. [0059] a、铌粉预处理 ’ ^〇6〇]将纯度为99 •99%的他粉均匀铺洒在石英舟内，放入管式炉，通入配比为4 • 7%的 氢气和％ •3 %的氩气混合气，升温至30(rc，保温3小时，随炉冷却后取出，得到预处理铌粉。 [0061]图7为本例方法制得的预处理后的铌粉与原料铌粉的XRD对比图，从图中可以看 出，经过预处理的铌粉衍射峰宽化明显，存在微量杂质。根据XRD数据可得三强峰的半峰宽， 原料铌粉的平均半峰宽为0.1288 (20/。），预处理后的铌粉平均半峰宽为〇_2〇8 (20/。）。根据 谢乐公式计算，原料银粉的平均晶粒度是73.5nm，预处理后银粉的平均晶粒度是43 9nm达 到细化铌粉的目的。 _
[0062]图8为采用本实施例所述的方法制得的Nb3Al超导材料的XRD图，主要成分为 Nb3Al，含有少量Nb2Al，预处理后的铌粉所含的微量杂质对Nb3A1样品没有影响，所制得的 Nb3Al超导材料整体成分均匀。取本实施例中制得的他^丨超导材料进行测试，其超导转变 温度为15.2K。 ' '
[0063]^对本发明应当理解的是，以上所述的实施例，对本发明的目的、技术方案和有益效 果进行了进一步详细的说明，以上仅为本发明的实施例而已，并不用于限定本发明，凡是在 本发明的精神原则之内，所作出的任何修改、等同替换、改进等，均应包含在本发明的保护 范围之内，本发明的保护范围应该以权利要求所界定的保护范围为准。
Claims (5)
1.一种Nb3Al超导材料的制备方法，其特征在于，包括： a、 铌粉预处理 将纯度为99.99%的Nb粉均匀铺洒在石英舟内，放入管式炉，通入配比为4.7%_1〇〇% 的氢气和95.3%-0的氩气混合气，在300—38〇1的温度区间加热，保温3小时，随炉冷却后取 出，得到预处理铌粉，预处理铌粉为氢化铌粉，该氢化铌粉用于后续的Nb3A1制备； b、 压片制备 按NMA1分子式中Nb与A1原子摩尔比3:1进行配料，称取纯度为⑽⑽^乂的“粉和a步制 得的预处理铌粉，将预处理过的铌粉、铝粉装入玛瑙研钵中，研磨混合均匀，然后使用模具 压制成形，压制压力为lOMPa，制成块片状料坯，用铌箔包裹，将包裹好的块片状料坯装入石 英舟中； c、 烧结 、将装有制得的块片状料坯的石英舟放在管式炉中，在4.7%的氢气与95.3%的氩气 混合气保护中，将炉温升温至1400°C，保温10小时进行烧结反应，然后快速冷却至室温，即 制得Nb3Al超导材料。 …
2.根据权利要求1所述的Nb3Al超导材料的制备方法，其特征在于，a、铌粉预处理具体 包括:将纯度为99 • 99%的Nb粉均勾铺洒在石英舟内，放入管式炉，通入纯度为99 • 99%的氢 气，升温至380 C，保温3小时，随炉冷却后取出，得到预处理铌粉，预处理铌粉为氢化铌粉， 该氢化铌粉用于后续的Nb3Al制备。
3.根据权利要求1所述的Nb：3Al超导材料的制备方法，其特征在于，a、银粉预处理具体 包括:将纯度为99 _"%的Nb粉均勾铺洒在石英舟内，放入管式炉，通入配比为4.7%的氢气 和95.3%的氩气混合气，升温至380 C，保温3小时，随炉冷却后取出，得到预处理银粉，预处 理铌粉为氢化铌粉，该氢化铌粉用于后续的Nb3Al制备。 ' '
4.根据权利要求1所述的Nb：BAl超导材料的制备方法，其特征在于，锯粉预处理具体 包括:将纯度为"的Nb粉均匀铺洒在石英舟内，放入管式炉，通入配比为4• 7%的氢气 和95.3%的風气混合气，升温至347 C，保温3小时，随炉冷却后取出，得到预处理银粉，预处 理铌粉为氢化铌粉，该氢化铌粉用于后续的Nb3Al制备。 ' '
5.根驗利要求1臟的Nb3Al超导材料的制备方法，其特征在于，a、银粉预处理具体 包括:将纯度为"•"％ _b粉均娜洒在石英舟内，放人管式炉，通人为纟•7%的氢气 和95.3%的氩气混合气，升温至3〇(TC，保温3小时，随炉冷却后取出得 理银粉为氢化铜粉，该氢化银粉用于后续的Nb3Al制备。 ’mi
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