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
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- 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
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- 238000004458 analytical method Methods 0.000 description 2
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- 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
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- 238000009830 intercalation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 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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| CN105576206B (zh) * | 2016-01-07 | 2017-12-05 | 陕西科技大学 | 一种用于锂离子电池负极的Cu2V2O7‑石墨烯复合材料的制备方法 |
| 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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