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Article(id=1241064279848309149, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241064275599479114, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2025.05.030, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1745078400000, receivedDateStr=2025-04-20, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773822382175, onlineDateStr=2026-03-18, pubDate=1759248000000, pubDateStr=2025-10-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773822382175, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773822382175, creator=13701087609, updateTime=1773822382175, updator=13701087609, issue=Issue{id=1241064275599479114, tenantId=1146029695717560320, journalId=1235980550691926019, year='2025', volume='45', issue='5', pageStart='1', pageEnd='201', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773822381162, creator=13701087609, updateTime=1773822785847, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241065973038501946, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241064275599479114, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241065973038501947, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241064275599479114, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=170, endPage=175, ext={EN=ArticleExt(id=1241064280200630705, articleId=1241064279848309149, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Preparation of Manganese-Containing Master Alloy and Its Application in Rare-Earth-Based Hydrogen Storage Alloys, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Manganese-containing master alloy was prepared by vacuum induction melting. Effects of factors, such as manganese source, Mn/Al mass ratio, preheating time, and refining time on the composition of the manganese-containing master alloy were studied, and the influence of manganese-containing master alloys replacing the traditional “Mn + Al” feed on the prepared manganese-containing AB5-type rare-earth-based hydrogen storage alloy was also discussed. The experimental results show that compared to manganese powder, manganese flakes as manganese source can bring higher melting yield. Manganese-containing master alloys can be formed with different Mn/Al mass ratios. As the preheating time is prolonged, the melting yield firstly increases and then decreases, and the optimal condition for preheating is 10 minutes at a power of 4 kW. As the refining time increases, the melting yield decreases slightly, and the optimal condition for refining is 1 minute at a power of 15 kW. The average melting yields of rare-earth-based hydrogen storage alloy prepared with MnAlNi alloy and MnAl alloy are increased by 0.37% and 0.78% respectively than that with “Mn + Al” as raw material. The preparation of AB5-type rare-earth-based hydrogen storage alloy with manganese-containing master alloy can optimize the yield, with the hydrogen storage performance not influenced. The application of this method in practical industrial production brings good effect.

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采用真空感应熔炼法制备了含锰中间合金，研究了锰源、Mn/Al质量比、预热时间和精炼时间等因素对含锰中间合金组成的影响，探讨了含锰中间合金替代传统“Mn+Al”投料对制备含锰AB5型稀土储氢合金的影响。结果表明，采用锰片作锰源比锰粉作锰源具有更高的熔炼收率；不同Mn/Al质量比下均能形成含锰中间合金；随着预热时间增加，熔炼收率先增加后减小，适宜的预热条件为：4 kW功率下预热10 min；随着精炼时间增加，熔炼收率略有降低，适宜的精炼条件为：15 kW功率下精炼1 min。与“Mn+Al”为原料相比，采用MnAlNi合金和MnAl合金制备稀土储氢合金的平均熔炼收率分别提高了0.37%和0.78%。使用含锰中间合金制备AB5型稀土储氢合金在优化收率的同时不影响储氢性能，在实际工业生产中具有较好效果。

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谢懋良（1998—），男，江西赣州人，硕士，助理工程师，研究方向为金属功能材料。E-mail：
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郑波（1981—），男，重庆合川人，助理工程师，研究方向为储氢材料以及器件。E-mail：

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郑波（1981—），男，重庆合川人，助理工程师，研究方向为储氢材料以及器件。E-mail：

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郑波（1981—），男，重庆合川人，助理工程师，研究方向为储氢材料以及器件。E-mail：

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journalId=1235980550691926019, articleId=1241064279848309149, language=CN, label=图9, caption=不同原料制备的含锰AB5型稀土储氢合金的性能, figureFileSmall=3LTSUo+uQL5pWMIQZvf94Q==, figureFileBig=EWG0hAOCwpJGFwnT+4q+qw==, tableContent=null), ArticleFig(id=1241064295648252204, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241064279848309149, language=EN, label=Table 1, caption=

Experimental preparation of MnAl master alloys with different Mn sources

, figureFileSmall=null, figureFileBig=null, tableContent=
锰源种类投入/g产出/g熔炼收率/%合金Mn/Al质量比
锰片锰粉铝块合金炉渣
锰粉01 8013771 516.0674.669.614.28
锰片1 80103772 044.6112.093.884.88
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不同锰源制备MnAl中间合金实验情况

, figureFileSmall=null, figureFileBig=null, tableContent=
锰源种类投入/g产出/g熔炼收率/%合金Mn/Al质量比
锰片锰粉铝块合金炉渣
锰粉01 8013771 516.0674.669.614.28
锰片1 80103772 044.6112.093.884.88
), ArticleFig(id=1241064296105431353, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241064279848309149, language=EN, label=Table 2, caption=

Experimental preparation of MnAl master alloys with different refining time

, figureFileSmall=null, figureFileBig=null, tableContent=
精炼时间/min质量/g熔炼收率/%Mn/Al质量比
投入金属产出合金产出炉渣
1.02 016.01 938.077.696.134.85
1.52 016.01 931.280.595.794.82
2.02 016.01 929.481.795.704.86
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不同精炼时间制备MnAl中间合金的试验情况

, figureFileSmall=null, figureFileBig=null, tableContent=
精炼时间/min质量/g熔炼收率/%Mn/Al质量比
投入金属产出合金产出炉渣
1.02 016.01 938.077.696.134.85
1.52 016.01 931.280.595.794.82
2.02 016.01 929.481.795.704.86
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含锰中间合金的制备及其在稀土储氢合金中的应用
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郑波 1 , 谢懋良 2 , 任权兵 1 , 赖华生 2 , 冯兰 1 , 刘雯雯 2 , 皮雄 1 , 李荣华 1 , 林昊 1
矿冶工程杂志 | 材料 2025,45(5): 170-175
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矿冶工程杂志 | 材料 2025, 45(5): 170-175
含锰中间合金的制备及其在稀土储氢合金中的应用
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郑波1 , 谢懋良2 , 任权兵1, 赖华生2, 冯兰1, 刘雯雯2, 皮雄1, 李荣华1, 林昊1
作者信息
  • 1.江西江钨浩运科技有限公司，江西　南昌　330096
  • 2.赣州有色冶金研究所有限公司，江西　赣州　341000

    • 郑波（1981—），男，重庆合川人，助理工程师，研究方向为储氢材料以及器件。E-mail：

通讯作者:

谢懋良（1998—），男，江西赣州人，硕士，助理工程师，研究方向为金属功能材料。E-mail：
Preparation of Manganese-Containing Master Alloy and Its Application in Rare-Earth-Based Hydrogen Storage Alloys
Bo ZHENG1 , Maoliang XIE2 , Quanbing REN1, Huasheng LAI2, Lan FENG1, Wenwen LIU2, Xiong PI1, Ronghua LI1, Hao LIN1
Affiliations
  • 1.Jiangxi Jiangwu Haoyun Technology Co., Ltd., Nanchang 330096, Jiangxi, China
  • 2.Ganzhou Nonferrous Metallurgy Research Institute Co., Ltd., Ganzhou 341000, Jiangxi, China
出版时间: 2025-10-01 doi: 10.3969/j.issn.0253-6099.2025.05.030
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摘要
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采用真空感应熔炼法制备了含锰中间合金，研究了锰源、Mn/Al质量比、预热时间和精炼时间等因素对含锰中间合金组成的影响，探讨了含锰中间合金替代传统“Mn+Al”投料对制备含锰AB5型稀土储氢合金的影响。结果表明，采用锰片作锰源比锰粉作锰源具有更高的熔炼收率；不同Mn/Al质量比下均能形成含锰中间合金；随着预热时间增加，熔炼收率先增加后减小，适宜的预热条件为：4 kW功率下预热10 min；随着精炼时间增加，熔炼收率略有降低，适宜的精炼条件为：15 kW功率下精炼1 min。与“Mn+Al”为原料相比，采用MnAlNi合金和MnAl合金制备稀土储氢合金的平均熔炼收率分别提高了0.37%和0.78%。使用含锰中间合金制备AB5型稀土储氢合金在优化收率的同时不影响储氢性能，在实际工业生产中具有较好效果。

真空感应熔炼  /  稀土储氢合金  /  中间合金  /  锰  /  AB5型储氢合金

Manganese-containing master alloy was prepared by vacuum induction melting. Effects of factors, such as manganese source, Mn/Al mass ratio, preheating time, and refining time on the composition of the manganese-containing master alloy were studied, and the influence of manganese-containing master alloys replacing the traditional “Mn + Al” feed on the prepared manganese-containing AB5-type rare-earth-based hydrogen storage alloy was also discussed. The experimental results show that compared to manganese powder, manganese flakes as manganese source can bring higher melting yield. Manganese-containing master alloys can be formed with different Mn/Al mass ratios. As the preheating time is prolonged, the melting yield firstly increases and then decreases, and the optimal condition for preheating is 10 minutes at a power of 4 kW. As the refining time increases, the melting yield decreases slightly, and the optimal condition for refining is 1 minute at a power of 15 kW. The average melting yields of rare-earth-based hydrogen storage alloy prepared with MnAlNi alloy and MnAl alloy are increased by 0.37% and 0.78% respectively than that with “Mn + Al” as raw material. The preparation of AB5-type rare-earth-based hydrogen storage alloy with manganese-containing master alloy can optimize the yield, with the hydrogen storage performance not influenced. The application of this method in practical industrial production brings good effect.

vacuum induction melting  /  rare-earth-based hydrogen storage alloy  /  master alloy  /  manganese  /  AB5-type hydrogen storage alloy
郑波, 谢懋良, 任权兵, 赖华生, 冯兰, 刘雯雯, 皮雄, 李荣华, 林昊. 含锰中间合金的制备及其在稀土储氢合金中的应用. 矿冶工程杂志, 2025 , 45 (5) : 170 -175 . DOI: 10.3969/j.issn.0253-6099.2025.05.030
Bo ZHENG, Maoliang XIE, Quanbing REN, Huasheng LAI, Lan FENG, Wenwen LIU, Xiong PI, Ronghua LI, Hao LIN. Preparation of Manganese-Containing Master Alloy and Its Application in Rare-Earth-Based Hydrogen Storage Alloys[J]. Mining and Metallurgical Engineering, 2025 , 45 (5) : 170 -175 . DOI: 10.3969/j.issn.0253-6099.2025.05.030
正文
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储氢合金的性能与其元素组成有很大关联[1-3]，AB5型稀土储氢合金常用Co[4]、Mn[5-6]、Al[7-8]等代替Ni获得更好的性能。其中，Co元素可改善AB5型储氢合金循环寿命，因此传统商用AB5型储氢合金含有质量分数约10%的Co。当前，锂电池的大量应用挤压了镍氢电池市场[9]，市场对镍氢电池用储氢合金的成本提出了更高要求。钴价格昂贵，高钴含量的AB5型稀土储氢合金成本高，难以适应市场需求变化[10]，因此开发具有良好性能的低钴储氢合金以降低合金成本，是AB5型稀土储氢合金研究的重要内容[11-14]。提高Mn含量并减少Co含量是降低AB5型稀土储氢合金成本的常用策略，而且Mn的加入可降低储氢合金平台氢压、减小滞后、改善活化性能[15-17]。含锰AB5型稀土储氢合金通常采用电解锰片作为原料，金属锰的熔点相对较高（1 244 ℃），在制备储氢合金过程中易漂浮在熔点较低的稀土熔液表面，导致熔化时间长、金属收率低、稳定性差等，对于锰含量较高的AB5型稀土储氢合金这种影响尤为严重。
为解决上述问题，本文采用含锰中间合金作为AB5型稀土储氢合金的原料，研究了制备工艺参数对含锰中间合金的影响，探讨了含锰中间合金替代纯金属锰投料制备含锰AB5型稀土储氢合金的影响。在制备MnAl/MnAlNi中间合金时，一方面利用铝热还原锰片表面的氧化膜，减少合金氧含量，保证配方准确；另一方面含锰中间合金熔点低于单质锰熔点，可缩短熔炼时间，减少金属烧损。研究成果可为含锰中间合金的制备及其在AB5型稀土储氢合金的应用方面提供借鉴。
1　实验材料与方法
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实验使用原材料包括金属镧、铈、镍、铝、钴、电解锰片、锰粉等，纯度均大于99.5%。
采用ZG-PT203型电子天平称量总质量约2 kg的原材料，其中含锰中间合金以金属铝、金属锰、金属镍为原料；AB5型稀土储氢合金以含锰中间合金或锰、铝以及镧、铈、钇、镍等作为原料。采用ZG-10型真空中频感应熔炼炉熔炼合金。加入原料后，启动真空系统，待真空达到5 mPa后，启动中频电源，在功率4 kW条件下预热一定时间（脱除原料表面吸附的气体）；预热完毕后关闭真空系统，充入氩气至-0.02 MPa，随后升高功率至20 kW，原料全部熔化后保持功率2 min，然后降低功率至14 kW精炼一定时间；精炼完毕后进行浇铸，冷却后取出合金样品和炉渣称重并取样检测。
使用Horiba Ultima2型ICP原子发射光谱仪检测合金样品的元素组成及含量；使用X’pert Power型X射线衍射仪表征合金的物相组成；使用4SDWIN型PCT测试仪检测合金气态储氢性能；使用CT-3008W-5V3A型电池测试系统检测合金的电化学性能，详细方法为：取0.2 g合金粉与0.8 g羰基镍粉混合，使用MK-60J型压片机在20 MPa压力下保持3 min得到负极片，使用泡沫镍包覆负极片，在6 mol/L氢氧化钾为电解液、烧结氢氧化镍为对电极、Hg/HgO电极为参比电极的条件下测试合金的电化学性能。
2　结果与讨论
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2.1　不同锰源制备MnAl中间合金
锰的蒸汽压高，熔炼时易挥发且易氧化。锰源形貌可能对合金收率和成分有很大影响，因此分别使用电解锰片和锰粉作为锰源，在功率4 kW下预热10 min，在功率15 kW下精炼1 min，固定投料Mn/Al质量比为4.78，考察不同形态的锰源对合金收率的影响，结果如表1所示。从表1可知，使用锰片制备MnAl中间合金的收率可达93.88%，使用锰粉时收率只有69.61%。这是由于锰粉颗粒小、表面积大，熔炼时更易氧化且更易挥发。
不同锰源制备的MnAl中间合金XRD图见图1。锰粉或锰片制备的MnAl中间合金均由Al2Mn3相和Mn单质相构成，锰源仅影响收率，并不影响MnAl中间合金相结构。对比可知，选择锰片作为锰源制备含锰中间合金更好。
2.2　预热时间对制备MnAl中间合金熔炼收率的影响
金属锰在工业上是电解法制备的，为片状。锰片与电解阴极板接触的一面光滑，另一面具有枝晶结构，表面粗糙，易吸附气体，因此，在真空感应熔炼炉中需要先小功率预热以脱除吸附气体（尤其是氧和水），减少熔炼渣产生，提高熔炼收率。在功率15 kW下精炼1 min，投料Mn/Al质量比5.0条件下，固定预热功率为4 kW，预热时间对制备MnAl中间合金熔炼收率的影响见图2。从图2可见，随着预热时间增加，熔炼收率先升高后降低。预热时间10 min时，熔炼收率达到峰值，为96.13%；继续增加预热时间，熔炼收率反而下降。随着预热时间增加，实际Mn/Al质量比偏差先变小后趋于稳定，预热时间较短时，锰片吸附的气体未完全脱除，后续熔炼时形成锰氧化物，造成Mn/Al质量比偏差较大。因此，在功率4 kW条件下预热10 min为宜。
2.3　精炼时间对制备MnAl中间合金熔炼收率的影响
真空感应熔炼过程中，待金属物料熔化后需进行精炼，使熔体与炉渣充分分离。在功率4 kW下预热10 min、投料Mn/Al质量比5.0条件下，固定精炼功率为15 kW，研究精炼时间对制备MnAl中间合金熔炼收率的影响，结果见表2。可以看出，随着精炼时间增加，熔炼收率略有降低，但变化不明显。精炼功率15 kW条件下精炼1 min即可。
2.4　不同Mn/Al质量比制备MnAl中间合金研究
不同AB5型储氢合金产品具有不同的Mn/Al质量比，因此设计了不同Mn/Al质量比的MnAl中间合金，并在功率4 kW下预热10 min，在功率15 kW下精炼1 min，对产出的合金进行成分分析和XRD检测，结果见图3～4。
从图3看出，配料Mn/Al质量比为1.20时，熔炼收率达到98.26%；随着配料Mn/Al质量比增加，熔炼收率逐渐降低，配料Mn/Al质量比为9.60时，熔炼收率降低至93.55%。MnAl中间合金实际Mn/Al质量比略低于配料Mn/Al质量比，这与锰片表面存在的氧化层在熔炼过程中造渣有关。
由图4可见，配料Mn/Al质量比为1.20和1.90时，MnAl中间合金样品的主相为Mn8Al5。随着Mn/Al质量比增大，MnAl中间合金的主相为Al2Mn3和单质Mn，衍射峰位置随着Mn/Al质量比增大向高角度偏移。这是因为Mn的原子半径（130 pm）小于Al的原子半径（143 pm），Mn含量增多导致晶格间距变小，衍射峰向高角度方向移动。
2.5　不同掺Ni量制备MnAlNi中间合金研究
Ni是AB5型储氢合金中的主要元素，因此选择镍作为中间合金元素之一，在功率4 kW下预热10 min，在功率15 kW下精炼1 min，制备不同Ni含量的MnAlNi中间合金，Ni含量对MnAlNi中间合金熔炼收率的影响见图5，图6为所制备的MnAlNi中间合金的XRD图谱。
熔炼收率随掺镍量增加而单调增加。主要原因是Ni在熔炼中几乎不损失，Ni添加越多，收率自然越高。随着Ni含量增加，Al2Mn3相和Mn相的衍射峰强度降低，而Ni2AlMn相的衍射峰强度增强，这归因于Al2Mn3相和Mn相逐渐转化为Ni2AlMn相。归属于Al2Mn3相和Mn相的衍射峰位置向高角度偏移，这是因为Ni原子半径（124 pm）小于Mn和Al原子半径（130 pm和143 pm），部分Ni以掺杂的形式进入Al2Mn3相和Mn相的晶格中，晶体膨胀导致的。含锰中间合金掺入Ni后，合金硬度增加且脆性降低，合金难破碎，在后续制备储氢合金时较难控制MnAlNi中间合金的添加量，因此含锰中间合金应该尽量少掺或不掺金属镍。
2.6　采用含锰中间合金制备含锰AB5型稀土储氢合金
分别采用“Mn+Al”、MnAlNi合金和MnAl合金作为原料，按照RE1.0Ni4.7Mn0.62Al0.26配方制备含锰AB5型稀土储氢合金，实验结果见图7。对3组收率数据进行t检验[图7（b）和（c）]，3组数据之间的p<0.05，具有显著差异，表明三者收率的变化并非实验偶然因素，而是实验条件改变导致的。以“Mn+Al”为原料时，平均收率97.83%；以MnAlNi合金为原料时，平均收率98.20%；以MnAl合金为原料时，平均收率98.61%，分别比“Mn+Al”为原料提高0.37%和0.78%，具有一定的经济价值。
对“Mn+Al”和MnAl合金制备的含锰AB5型稀土储氢合金的元素含量、气态储氢性能、电化学性能进行分析检测，结果如图8～9所示。结果表明，“Mn+Al”和MnAl合金制备的储氢合金在元素含量上没有显著差异（P>0.05）。图9表明不同原料制备的储氢合金在性能上差异较小，吸氢量在1.270%附近小幅波动，放电容量在323.0 mAh/g附近小幅波动。采用MnAl合金替代“Mn+Al”投料在提高合金收率的同时不影响储氢合金的性能，使用含锰中间合金制备含锰AB5型稀土储氢合金具有一定效果。
3　结论
收起
1）在含锰中间合金的锰源选择方面，锰片作为锰源比锰粉具有更高的熔炼收率。在含锰中间合金制备条件方面，熔炼收率随预热时间增加，先增加后减小，在功率4 kW下预热10 min效果较好；熔炼收率随着精炼时间增加略有降低，在功率15 kW下精炼1 min为佳。不同Mn/Al质量比条件下均能形成合金，根据不同产品的Mn/Al质量比制备中间合金的方案可行。
2）在制备含锰AB5型稀土储氢合金方面，以MnAlNi合金为原料收率为98.20%，以MnAl合金为原料收率为98.61%，分别比“Mn+Al”为原料的收率提高0.37%和0.78%。
3）采用含锰中间合金制备储氢合金对其性能几乎无影响，不同原料制备的AB5型稀土储氢合金的放电容量均在323.0 mAh/g附近小幅波动，吸氢量均在1.270%附近小幅波动，使用含锰中间合金制备AB5型稀土储氢合金可在优化合金收率的同时不影响合金性能。
基金
收起
  • 江西省重点研发计划项目(20203BBE53055)
  • 南昌市科技重大项目(洪科字(2023)137号)
  • 江西钨业控股集团有限公司科技计划项目(JXTC-25A-04)
文献
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参考文献 引证文献
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2025年第45卷第5期
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doi: 10.3969/j.issn.0253-6099.2025.05.030
  • 接收时间：2025-04-20
  • 首发时间：2026-03-18
  • 出版时间：2025-10-01
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  • 收稿日期：2025-04-20
基金
江西省重点研发计划项目(20203BBE53055)
南昌市科技重大项目(洪科字(2023)137号)
江西钨业控股集团有限公司科技计划项目(JXTC-25A-04)
作者信息
    1.江西江钨浩运科技有限公司，江西　南昌　330096
    2.赣州有色冶金研究所有限公司，江西　赣州　341000

通讯作者:

谢懋良（1998—），男，江西赣州人，硕士，助理工程师，研究方向为金属功能材料。E-mail：
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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