CN103570067A - 以蒸发结晶法制备铜钒氧纳米结构材料的方法 - Google Patents
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000002086 nanomaterial Substances 0.000 title abstract description 6
- JKLVRIRNLLAISP-UHFFFAOYSA-N [O-2].[V+5].[Cu+2] Chemical compound [O-2].[V+5].[Cu+2] JKLVRIRNLLAISP-UHFFFAOYSA-N 0.000 title abstract 5
- FDHXJXORQOCVFU-UHFFFAOYSA-N [V].[Cu]=O Chemical compound [V].[Cu]=O FDHXJXORQOCVFU-UHFFFAOYSA-N 0.000 claims description 32
- 239000010949 copper Substances 0.000 claims description 15
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- 230000008025 crystallization Effects 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 9
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 8
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 239000012267 brine Substances 0.000 claims description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- 229910016508 CuCl22H2O Inorganic materials 0.000 claims description 3
- PAJMKGZZBBTTOY-UHFFFAOYSA-N 2-[[2-hydroxy-1-(3-hydroxyoctyl)-2,3,3a,4,9,9a-hexahydro-1h-cyclopenta[g]naphthalen-5-yl]oxy]acetic acid Chemical compound C1=CC=C(OCC(O)=O)C2=C1CC1C(CCC(O)CCCCC)C(O)CC1C2 PAJMKGZZBBTTOY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 5
- 239000010406 cathode material Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 229910016383 CuV2O6 Inorganic materials 0.000 description 4
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000010405 anode material Substances 0.000 description 3
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- 239000002070 nanowire Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910017656 Ag2V4O11 Inorganic materials 0.000 description 1
- 229910003206 NH4VO3 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000004202 carbamide Substances 0.000 description 1
- 230000000747 cardiac effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 0.000 description 1
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- Y02E60/10—Energy storage using batteries
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Abstract
本发明公开了以蒸发结晶法制备铜钒氧纳米结构材料的方法,首先以蒸发结晶法制备铜钒氧纳米结构材料的前驱体,然后将其在空气氛围中煅烧制备了颗粒均匀、微结构可控的铜钒氧纳米结构材料。本发明方法简单、条件温和,所制备的铜钒氧纳米结构材料形貌均匀、结构稳定和导电性好,是一种很有希望的正极材料。
Description
技术领域
本发明涉及锂离子电池正极材料的制备方法,尤其涉及一种以蒸发结晶法制备铜钒氧(CVO)纳米结构材料的方法。
背景技术
铜钒氧(CVO)作为一种有潜力的锂离子电池材料,由于其优异的电子电导率和Cu的高氧化态,它可以提供比Ag2V4O11更高的放电比容量和能量密度。同时,相对于银钒氧(SVO),铜钒氧(CVO)的原料成本更低。近年来,铜钒氧(CVO)作为锂离子电池正极材料引起了关注。
常见的制备铜钒氧纳米结构材料(CVO)的方法有水热法、固相法和溶胶凝胶法。Yu等人报道了以V2O5、H2O2、尿素和Cu(NO3)2·3H2O为原料,在200℃水热反应24h,制备了由纳米片组装的具有多级结构的Cu4V2.1509.38,结果显示这种材料在5mA g-1的电流密度下,其放电比容量可达471mAh g-1(Hierarchical Cu4V2.1509.38micro/nanostructures:a lithiumintercalating electrode material[J].Nanoscale,2011,3,999-1003.)。Chen等人报道了以CuCl2·2H2O和NH4VO3为原料,在210℃水热反应12h,制备了直径约为100nm、长为十几微米的α-CuV2O6纳米线,结果显示在20mAg-1的电流密度下,所制备的α-CuV2O6纳米线的首次放电比容量达到了514mAh g-1,比其它三种形貌的α-CuV2O6都高,这表明α-CuV2O6纳米线是一种有希望应用于可植入心脏起搏器(ICD)的电极材料。(α-CuV2O6nanowires:hydrothermal synthesis and primary lithium battery application[J].Journal of the American Chemical Society,2008,130,5361-5367.)
本发明是在低成本、条件温和、高效率的前提下,采用蒸发结晶法制备铜钒氧纳米结构材料。
发明内容
本发明要解决的技术问题是提供一种以蒸发结晶法制备铜钒氧(CVO)纳米结构材料的方法。
为了解决上述技术问题,本发明采用的技术方案是:以蒸发结晶法制备铜钒氧(CVO)纳米结构材料的方法,包括如下步骤:
(1)铜钒氧纳米结构材料的前驱体制备:分别配制0.1~2mol/L的可溶性偏钒酸盐水溶液,和0.05~2mol/L的可溶性的二价Cu盐水溶液,按摩尔比V:Cu=1~10:1把可溶性偏钒酸盐水溶液逐滴加入可溶性的二价Cu盐水溶液中,或将可溶性的二价Cu盐水溶液逐滴加入可溶性偏钒酸盐水溶液中,搅拌均匀后,将其置于50~160℃的鼓风干燥箱内,水分蒸发完后将烧其取出,用水和酒精离心洗涤产物并干燥,得到前驱体;
(2)铜钒氧纳米结构材料的制备:将步骤(1)制备出的前驱体在空气中煅烧,于350~650℃焙烧2~15小时,得到铜钒氧纳米结构材料。
作为优选,可溶性偏钒酸盐为偏钒酸铵、偏钒酸钠、偏钒酸钾的一种或两种及以上混合物。
作为优选,可溶性的二价Cu盐选自CuCl2·2H2O、硝酸铜、硫酸铜的一种或两种及以上混合物。
本发明的有益效果是:
1)合成方法简单、形貌可控。
2)采用蒸发结晶法制备了锂离子电池正极材料铜钒氧纳米结构材料,与固相合成的铜钒氧(CVO)粉体相比,具有更好的结构稳定性与导电性,可明显提高材料的放电容量、减小不可逆容量损失、提高循环性能与倍率性能。
3)铜钒氧纳米结构材料相比于铜钒氧(CVO)块体材料,比表面积相对较大,若将其应用于锂离子电池中,可增加了材料与电解液之间的接触面积,从而提高该材料的放电比容量。
附图说明
下面结合附图和具体实施方式对本发明作进一步详细的说明。
图1为本发明以蒸发结晶法制备的铜钒氧纳米结构材料的方法实施例1前驱体的FESEM照片。
图2为本发明以蒸发结晶法制备的铜钒氧纳米结构材料的方法实施例1前驱体经煅烧后所得样品的X射线衍射(XRD)图。
图3为本发明以蒸发结晶法制备的铜钒氧纳米结构材料的方法实施例1前驱体经煅烧后所得样品的FESEM照片。
具体实施方式
实施例1:
(1)铜钒氧纳米结构材料的前驱体制备
在2个120mL的烧杯中,分别配制0.1mol/L的偏钒酸铵水溶液40mL,和0.1mol/L的硝酸铜水溶液40mL,按摩尔比(V:Cu=1:1)把偏钒酸铵水溶液逐滴加入硝酸铜水溶液中,搅拌均匀后,将烧杯置于120℃的鼓风干燥箱内,水分蒸发完后将烧杯取出,用水和酒精离心洗涤产物并干燥。
蒸发结晶反应所制备的铜钒氧纳米结构材料的前驱体,经过FESEM照片(图1)分析表明,所得前驱体的形貌为纳米棒组装而成的团簇。
(2)铜钒氧纳米结构材料的制备
将步骤(1)制备出的前驱体在空气中煅烧,于550℃焙烧5小时,得到铜钒氧纳米结构材料。
蒸发结晶反应所制备的前驱体经过煅烧后得到的样品,经X射线衍射(XRD(图2)和FESEM照片(图3)分析表明该样品是Cu2V2O7纳米棒,该纳米棒是团簇前驱体在煅烧下裂解而成的。
实施例2:
(1)铜钒氧纳米结构材料的前驱体制备
在2个120mL的烧杯中,分别配制0.1mol/L的偏钒酸铵水溶液50mL,和0.05mol/L的CuCl2水溶液20mL,按摩尔比(V:Cu=5:1)把偏钒酸铵水溶液逐滴加入CuCl2水溶液中,搅拌均匀后,将烧杯置于100℃的鼓风干燥箱内,水分蒸发完后将烧杯取出,用水和酒精离心洗涤产物并干燥。
(2)铜钒氧纳米结构材料的制备
将步骤(1)制备出的前驱体在空气中煅烧,于450℃焙烧8小时,得到铜钒氧纳米结构材料。
以上所述的本发明实施方式,并不构成对本发明保护范围的限定。任何在本发明的精神和原则之内所作的修改、等同替换和改进等,均应包含在本发明的权利要求保护范围之内。
Claims (3)
1.以蒸发结晶法制备铜钒氧纳米结构材料的方法,其特征是包括如下步骤:
(1)铜钒氧纳米结构材料的前驱体制备:分别配制0.1~2mol/L的可溶性偏钒酸盐水溶液,和0.05~2mol/L的可溶性的二价Cu盐水溶液,按摩尔比V:Cu=1~10:1把可溶性偏钒酸盐水溶液逐滴加入可溶性的二价Cu盐水溶液中,或将可溶性的二价Cu盐水溶液逐滴加入可溶性偏钒酸盐水溶液中,搅拌均匀后,将其置于50~160℃的鼓风干燥箱内,水分蒸发完后将烧其取出,用水和酒精离心洗涤产物并干燥,得到前驱体;
(2)铜钒氧纳米结构材料的制备:将步骤(1)制备出的前驱体在空气中煅烧,于350~650℃焙烧2~15小时,得到铜钒氧纳米结构材料。
2.根据权利要求1所述以蒸发结晶法制备铜钒氧纳米结构材料的方法,其特征在于:所述可溶性偏钒酸盐为偏钒酸铵、偏钒酸钠、偏钒酸钾的一种或两种及以上混合物。
3.根据权利要求1所述以蒸发结晶法制备铜钒氧纳米结构材料的方法,其特征在于:所述可溶性的二价Cu盐选自CuCl2·2H2O、硝酸铜、硫酸铜的一种或两种及以上混合物。
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CN107512740A (zh) * | 2017-08-29 | 2017-12-26 | 合肥国轩电池材料有限公司 | 一种锂离子电池负极材料FeVO4纳米线的制备方法 |
CN110482604A (zh) * | 2019-07-25 | 2019-11-22 | 广东工业大学 | 一种Cu2V2O7纳米棒钾离子电池正极材料、钾离子电池及其制备方法 |
CN110482604B (zh) * | 2019-07-25 | 2022-01-25 | 广东工业大学 | 一种Cu2V2O7纳米棒钾离子电池正极材料、钾离子电池及其制备方法 |
CN111847509A (zh) * | 2020-06-16 | 2020-10-30 | 北京科技大学 | 一种铜铁矿型铜钒氧化物材料及其制备方法 |
CN111847509B (zh) * | 2020-06-16 | 2021-08-13 | 北京科技大学 | 一种铜铁矿型铜钒氧化物材料及其制备方法 |
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