CN106637932A - 一种制备储氢物质镁镍合金纳米纤维的方法 - Google Patents
一种制备储氢物质镁镍合金纳米纤维的方法 Download PDFInfo
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Abstract
本发明属于氢气存储材料制备技术领域,具体为制备储氢物质镁镍合金纳米纤维的方法。本发明通过改变静电纺丝法制备Ni(NO3)2/PVP纤维的煅烧条件,合成竹节状的Ni纳米纤维作为Ni源,利用高温热蒸发法将Mg蒸发到Ni纳米纤维表面进行原位反应,制备得到Mg‑Ni纳米纤维。本发明合成的Mg‑Ni纳米纤维总储氢量为2.25 wt.%,在100℃,100 min内即可吸附1.31 wt.%的氢气,吸完氢后,在265℃,1 min内能够快速放出1.5 wt.%的氢气,总放氢量为2.13 wt.%,具有较高的吸放氢动力学性能。
Description
技术领域
本发明属于氢气存储材料制备技术领域,具体涉及制备储氢物质镁镍合金纳米纤维的方法。
背景技术
不可再生化石能源的大量消耗,人类生存环境的日益恶化换得了人类经济的迅猛发展,能源是人类赖以生存、生产和生活的重要源泉,为了满足全球对清洁能源的需求,解决日益严重的能源危机,寻找合适的可替代能源是各国的战略目标。[1] 在各种可替代能源中,氢能因其储量丰富,燃烧能量密度值高,燃烧产物(水)清洁无污染等一系列优势成为最理想的二次能源。如何安全高效地储存氢能是当前氢能应用的瓶颈问题。[2,3] 随着氢经济的发展,许多储氢材料不断被开发,如合金,轻金属氢化物,碳纳米管等。镁基储氢材料以其丰富的储备,低廉的价格,以及容量高,可逆性好等特点而备受关注,但是它还存在高的吸放氢温度和缓慢的动力学这两个主要应用障碍,MgH2具有极高的热力学稳定性,分解焓变高达74.6 KJ/(mol·H2)。放氢温度往往在350 ℃以上,这限制了其在储氢方面的实际应用,而通过与Ni,Cu,Al等合金化能够改变MgH2的分解路径,降低其热力学稳定性,从而能够显著改善MgH2的热力学性能,Ni作为一种廉价易得的金属,其与Mg的二元合金产物Mg2Ni具有相对较高的理论含氢量(3.6 wt.%)和快速可逆吸放氢的性能受到广泛研究。但是目前合成Mg2Ni的方法存在种种不足。比如常规的共熔法由于Mg的低熔点、高挥发性以及MgNi金属间高的熔点差异受到限制很难制备高纯度的Mg2Ni合金。[4-6]有研究表明机械球磨的方法可以合成Mg2Ni。[7-10]但是此法耗时长,并且最终产物均一性和纯度会受到球磨转速,球料比,球磨时间等多种因素的影响。此外,长的球磨时间容易使样品发生氧化。为了解决这个问题,Sun课题组提出了两步法合成Mg2Ni。先将Mg粉与Ni粉简单球磨20 min后再在500 ℃,Ar气氛下进行固相反应合成Mg2Ni。[11]但是此法步骤较为繁琐。后来Li等人采用H等离子体法合成Mg,Ni纳米颗粒,然后在4 MPa氢压,350 ℃条件下,利用Mg,Ni纳米颗粒反应合成Mg2NiH4,再经后续脱氢后便得到纯Mg2Ni。[12,13]但此法引进了H等离子体设备,目前只能应用于实验室合成,不适合工业化批量生产。本发明开创性的利用高温热蒸发法将Mg蒸发到Ni纳米纤维表面进行原位反应制备Mg-Ni纳米纤维。
参考文献:
【1】. Schmitz, B., Virtual Reality: On the Brink of Greatness [J].Computer Aided Engineering, Vol. 12, No. 4, 1993, pp.26~32.
【2】. Jayaram, S., Connacher, H.I., and Lyons, K.W., Virtual AssemblyUsing Virtual Reality Techniques [J]. Computer Aided Design, Vol. 29, No. 8,1997, pp. 575~584.
【3】. Jung, B., Hoffhenke, M., and Wachsmuth, I., Virtual Assembly WithConstruction Kits [M]. Proceedings of 1997 ASME Design Engineering TechnicalConference, September 14-17, 1997, Sacramento, DETC97/DFM-4363.
【4】. Hsu C-W, Lee S-L, Jeng R-R, Lin J-C. Mass production of Mg2Ni alloybulk by isothermal evaporation casting process [J]. Int J Hydrogen Energy,2007,32:4907-4911.
【5】. Sun D, Enoki H, Gingl F, Akiba E. New approach for synthesizing Mg-based alloys [J]. J Alloys Compd., 1999, 285:279-283.
【6】. Knight Jr L, Brittain R, Duncan M, Joyner C. Unusual behavior ofvaporaized magnesium under low pressure conditions [J]. J Phys Chem., 1975,79: 1183-1190.
【7】. Ebrahimi-Purkani A, Kashani-Bozorg SF, Nanocrystalline Mg2Ni-basedpowders produced by high-energy ball milling and subsequent annealing [J]. JAlloys Compd., 2008,456:211-215.
【8】. Simicic MV, Zdujic M, Dimitrijevic R, Nikolic-Bujanovic L, PopovicNH. Hydrogen absorption and elecdtrochemical properties of Mg2Ni-type alloyssynthesized by mechanical alloying [J]. J Power Sources, 2006, 158: 730-734.
【9】. Zaluski L, Zaluska A, Stromolsen JO. Hydrogen absorption innanocrystalling Mg2Ni formed by mechanical alloying [J]. J Alloys Compd.,1995, 217: 245-249.
【10】. Lee HY, Goo NH, Jeong WT, Lee KS. The surface state ofnanocrystalline and amorphous Mg2Ni alloys prepared by mechanical alloying[J]. J Alloys Compd., 2000, 313: 258-262.
【11】. Zhao B, Fang F, Sun D, Zhang Q, Wei S, Cao F, er al. Formation ofMg2Ni with enhanced kinetics: Using MgH2 instead of Mg as a starting material[J]. J Solid State Chem., 2012, 192: 210-214.
【12】. Shao H, Liu T, Li X. Preparation of the Mg2Ni compound fromultrafine particles and its hydrogen storage properties [J]. Nanotechnology,2003,14: L1-L3.
【13】. Shao HY, Liu T, Wang YT, Xu HR, Li XG. Preparation of Mg-basedhydrogen storage materials from metal nanoparticles [J]. J Alloys Compd.,2008, 456: 527-533.。
发明内容
本发明目的是提供一种工艺简单的制备镁镍(Mg-Ni)合金纳米纤维的方法。
本发明提供的制备镁镍合金纳米纤维的方法,通过改变静电纺丝法制备Ni(NO3)2/PVP纤维的煅烧条件,合成竹节状的Ni纳米纤维作为Ni源,利用高温热蒸发法将Mg蒸发到Ni纳米纤维表面进行原位反应,制备得到Mg-Ni纳米纤维。具体步骤为:
(1)用静电纺丝法合成竹节状的Ni纳米纤维:
将溶有Ni(NO3)2和PVP的DMF/乙醇溶液用静电纺丝法制备Ni(NO3)2/PVP纤维,然后,在管式炉中将Ni(NO3)2/PVP纤维在空气中煅烧成NiO纤维,最后在H2/N2混合气保护下将NiO纤维还原为Ni纤维;
(2)用热蒸发法将Mg粉蒸发到Ni纳米纤维表面:
将装有Ni纤维的瓷舟置于铺满Mg粉的大瓷舟内,密封,然后在保护气体Ar下,用管式炉对其煅烧,将Mg粉蒸到Ni纳米纤维表面,并与Ni进行原位反应,生成Mg-Ni纳米纤维。
本发明步骤(1)中,所述煅烧Ni(NO3)2/PVP纤维的条件为:以1~5 ℃/min速率升温到190~220 ℃,保温1~3 h;然后继续以此速率升温至500~550 ℃,在此温度下保温2~4 h;所述还原NiO纤维的条件为:H2/N2混合气的保护下,以1~5 ℃/min速率升温至380-420℃,在此温度下保温2~4 h,结束后冷却至室温。
本发明步骤(2)中,所述煅烧条件为:以1~5 ℃/min速率升温至500 -550℃,随即再从此温度以2-3 ℃/min速率升温至600~650 ℃,在此温度保温2~3h,然后冷却至室温。
本发明所合成的Mg-Ni合金纳米纤维,由许多纳米晶粒堆积而成,纤维尺寸在80-200 nm不等。
本发明所合成的Mg-Ni合金纳米纤维是一中理想的储氢物质,在氢压30 bar,100℃下,100 min内即可吸附1.31 wt.%的氢气;在235 ℃,1 min内吸氢量就能达到1 wt.%,总的储氢容量为2.25 wt.%;吸完氢后,在265 ℃,1 min内能够快速放出1.5 wt.%的氢气,总放氢量为2.13 wt.%。
本发明具有以下几个方面显著优点:
(1)使用Mg-Ni合金纳米纤维作为氢源材料,可于较低的加热温度下获得大量高纯氢气;
(2)制备设备简单,易于实现;
(3)工艺简单,合成方便,成本适中。
附图说明
图1静电纺丝法合成的NiO纳米纤维(NiO NFs),还原后的Ni纤维(Ni NFs), Mg-Ni合金纳米纤维(Mg-Ni NFs)的XRD图。
图2为NiO纳米纤维、Ni纳米纤维、Mg-Ni合金纳米纤维的有关图片。其中, a为 静电纺丝法制备的NiO纳米纤维的TEM照片;b为竹节状的Ni纳米纤维的TEM照片;c 为Mg-Ni合金纳米纤维的TEM照片;d为Mg-Ni合金纳米纤维的HRTEM照片;e为单根的TEM照片,f为e中元素Ni谱图,g 为e中的元素Mg谱图。
图3 Mg-Ni合金纳米纤维热分解性能谱图。其中,黑线,为Mg-Ni合金纳米纤维的加氢产物的质谱图;红线为 Mg-Ni粉末样品的加氢产物的质谱图。
图4产物吸放氢后的XRD谱图,其中,a为Mg-Ni合金纳米纤维吸氢后的产物;b 为Mg-Ni合金纳米纤维放氢后的产物。
图5 Mg-Ni合金纤维不同温度条件下的吸氢曲线(上)。
图6 Mg-Ni合金纤维不同温度条件下的放氢曲线(下)。
具体实施方式
下面通过实施例进一步说明本发明。
实施例1:
1.Ni纳米纤维的制备:共分为三步。首先,量取1.25 ml的DMF和乙醇,混合均匀。然后在混合的有机溶剂中,加入0.17 g的PVP,搅拌几分钟溶解,再加入0.101g的Ni(NO3)2·6H2O,继续搅拌5 h后得到澄清的绿色溶液,用于静电纺丝。参数设置:电压12 KV,喷丝头距接收板15 cm,液体流速为0.25 ml/h,在室温条件下纺丝。第二步,将负极板上接受的Ni(NO3)2/PVP前驱纤维在空气中煅烧得到NiO纤维。煅烧程序为1 ℃/min到190 ℃,保温2 h后继续升温至500 ℃,保温3 h。第三步,还原NiO纤维,在400 ℃,H2/N2混合气的保护下保温2 h,可以使NiO还原成Ni纤维。
2.Mg-Ni合金纳米纤维制备:称取Ni线25 mg于小瓷舟 A中,将瓷舟 A置于底部铺满Mg粉(400 mg) 大瓷舟 B内部,盖上瓷舟盖密封。将瓷舟 B移入石英管内,置于管式炉加热,通保护气体Ar。热处理程序为:先5 ℃/min 到500 ℃,再以2 ℃/min到650 ℃保温2 h,后冷却至室温。作为对比,称取等量Ni粉按照相同方法合成Mg2Ni粉末样品。
3.Mg-Ni纳米纤维加氢过程:称取20 mg样品与高压反应釜中,加入30 bar的氢压,在300℃保温5 h后冷却至室温。按照相同方法对合成的Mg-Ni粉末样品进行加氢操作作为对比试验。产物的XRD如图1所示,合成产物的形貌表征如图2所示,图3为Mg-Ni纳米纤维及其对比样品的热分解性能图谱,而Mg-Ni纳米纤维吸氢和放氢后的产物分析如图4所示,最后,Mg-Ni纳米纤维的吸放氢性能如图5-6所示。
实施例2:
1.Ni纳米纤维的制备:共分为三步。首先,量取2.5 ml的DMF和乙醇,混合均匀。然后在混合的有机溶剂中,加入0.34g的PVP,搅拌几分钟溶解,再加入0.202g的Ni(NO3)2·6H2O,继续搅拌5 h后得到澄清的绿色溶液,用于静电纺丝。参数设置:电压12 KV,喷丝头距接收板15 cm,液体流速为0.25 ml/h,在室温条件下纺丝。第二步,将负极板上接受的Ni(NO3)2/PVP前驱纤维在空气中煅烧得到NiO纤维。煅烧程序为3 ℃/min到220 ℃,保温2 h后继续以此速率升温至550 ℃,保温3 h。第三步,还原NiO纤维,在H2/N2混合气的保护下,以5 ℃/min升到400 ℃,在400 ℃下保温3 h,可以使NiO还原成Ni纤维。
2.Mg-Ni合金纳米纤维制备:称取Ni线25 mg于小瓷舟 A中,将瓷舟 A置于底部铺满Mg粉(400 mg) 大瓷舟 B内部,盖上瓷舟盖密封。将瓷舟 B移入石英管内,置于管式炉加热,通保护气体Ar。热处理程序为:先5 ℃/min 到500 ℃,再以2 ℃/min到600 ℃保温3 h,后冷却至室温。作为对比,称取等量Ni粉按照相同方法合成Mg2Ni粉末样品。
3.Mg-Ni纳米纤维加氢过程:称取20 mg样品与高压反应釜中,加入30 bar的氢压,在300℃保温5 h后冷却至室温。按照相同方法对合成的Mg-Ni粉末样品进行加氢操作作为对比试验。
Claims (3)
1.一种制备储氢物质镁镍合金纳米纤维的方法,其特征在于,通过改变静电纺丝法制备Ni(NO3)2/PVP纤维的煅烧条件,合成竹节状的Ni纳米纤维作为Ni源,利用高温热蒸发法将Mg蒸发到Ni纳米纤维表面进行原位反应,制备得到Mg-Ni纳米纤维;具体步骤为:
(1)用静电纺丝法合成竹节状的Ni纳米纤维:
将溶有Ni(NO3)2和PVP的DMF/乙醇溶液用静电纺丝法制备Ni(NO3)2/PVP纤维,然后,在管式炉中将Ni(NO3)2/PVP纤维在空气中煅烧成NiO纤维,最后在H2/N2混合气保护下将NiO纤维还原为Ni纤维;
(2)用热蒸发法将Mg粉蒸发到Ni纳米纤维表面:
将装有Ni纤维的瓷舟置于铺满Mg粉的大瓷舟内,密封,然后在保护气体Ar下,用管式炉对其煅烧,将Mg粉蒸到Ni纳米纤维表面,并与Ni进行原位反应,生成Mg-Ni纳米纤维;
步骤(1)中所述煅烧Ni(NO3)2/PVP纤维的条件为:以1~5 ℃/min速率升温到190~220℃,保温1~3 h;然后继续以此速率升温至500~550 ℃,在此温度下保温2~4 h;所述还原NiO纤维的条件为:H2/N2混合气的保护下,以1~5 ℃/min速率升温至380-420℃,在此温度下保温2~4 h,结束后冷却至室温。
2. 根据权利要求1所述的方法,其特征在于,步骤(2)所述煅烧条件为:以1~5 ℃/min速率升温至500 -550℃,随即再从此温度以2-3 ℃/min速率升温至600~650 ℃,在此温度保温2~3h,然后冷却至室温。
3. 根据权利要求1所述的方法,其特征在于,所合成的Mg-Ni合金纳米纤维由许多纳米晶粒堆积而成,纤维尺寸为80-200 nm。
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CN114918421A (zh) * | 2022-04-21 | 2022-08-19 | 北京航空航天大学 | 一种ZrCo合金的纤维空间限域制备方法及其应用 |
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