CN111039268A - 一种CoP/C纳米复合材料、制备方法以及用途 - Google Patents
一种CoP/C纳米复合材料、制备方法以及用途 Download PDFInfo
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- C01B25/08—Other phosphides
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
本发明属于钠离子电池电极材料制备领域,公开一种CoP/C纳米复合材料、制备方法以及用途。所述CoP/C纳米复合材料的制备方法:以质量体积比计,Co(CH3COO)2·4H2O∶硫脲∶植酸∶水=(0.3~0.7)g∶(3~5)g∶2 mL∶2 mL,将Co(CH3COO)2·4H2O、硫脲、植酸加入水中,60~80℃下搅拌至干,获得螯合物;然后在保护气氛下,将所得螯合物分两阶段升温:第一阶段升温至180℃恒温30 min,第二阶段升温至900℃恒温2 h;最后冷却至室温,即得CoP/C纳米复合材料。所述CoP/C纳米复合材料可以用作钠离子电池的电极材料。本发明整个反应过程在水溶液中进行,无需外加其他添加剂,工艺简单,成本低廉且节能环保,易于产业化生产料。
Description
技术领域
本发明属于钠离子电池电极材料制备领域,具体涉及一种CoP/C纳米复合材料、制备方法以及用途。
技术背景
随着人们生活水平的不断提高,以往所依赖的化石燃料已远远不能满足我们目前的需求。然而,以锂离子电池为代表的二次储能设备具有环境友好型、功率密度高、能量密度高等特点,引起人们极大的关注。但是锂在自然界中的丰度低以及分布不均匀等特点,严重限制了锂离子电池的进一步发展。相比而言,金属钠在自然界中丰度高,具有与锂离子电池相似的反应机理,受到人们广泛的关注。目前大量的研究集中在电极材料的研究上,如一些具有高理论容量的过渡金属氧化物、硫化物及磷化物的研究成为研究热点。研究结果表明,如CN201710319311.8发明专利公开了一种二氧化锡-氧化亚钴复合薄膜材料、锂电池及制备方法,采用交替沉积的方法制备出氧化锡-氧化亚钴复合薄膜,用于锂离子电池负极时可以表现出优异的电化学性质。一方面是由于二氧化锡和氧化亚钴交替分布,有效地缓冲了体积变化所导致的应力,进而保持了结构的完整性,提高了循环稳定性,另一方面CoO储能反应中生成的金属Co具有催化电极充放电反应活性的功能,提高了电池倍率性能。镍/钴掺杂二硫化三镍储能电极材料作为储能材料具有较高的比容量,如CN201611247251.5发明了两步水热反应制备镍/钴掺杂二硫化三镍储能电极材料的方法并将其应用于储能材料进行测试,结果表明镍/钴掺杂二硫化三镍储能电极材料具有730 C/cm3高体积容量并且具有良好的倍率性能。再如CN201910063119.6发明专利公开一种磷化二钴/碳复合材料及其制备方法,首先将钴源、磷源和表面活性剂与水混合后,进行水热反应,得到Co2P前驱体;然后将Co2P前驱体与有机碳源混合进行水热;最后将得到的样品高温煅烧得到磷化二钴/碳复合材料;该材料用于储能材料表现出良好的循环和倍率性能。上述制备过程步骤繁琐、原料使用种类多,导致工业化程度复杂,对产品性能及应用产生严重影响,在生产的过程中会耗时耗力且成本较高。
发明内容
本发明的目的旨在提供一种CoP/C纳米复合材料、制备方法以及用途。
为实现上述目的,本发明采取的技术方案如下:
一种CoP/C纳米复合材料,所述复合材料是指一磷化钴纳米粒子负载在碳纳米片上。
所述CoP/C纳米复合材料的制备方法:以质量体积比计,Co(CH3COO)2·4H2O∶硫脲∶植酸∶水=(0.3~0.7) g∶(3~5) g∶2 mL∶2 mL,将Co(CH3COO)2·4H2O、硫脲、植酸加入水中,60~80 ℃下搅拌至干,获得螯合物;然后在保护气氛下,将所得螯合物分两阶段升温:第一阶段升温至180 ℃恒温30 min,第二阶段升温至900 ℃恒温2 h;最后冷却至室温,即得CoP/C纳米复合材料。
较好地,第一阶段升温速率为2~5 ℃/ min,第二阶段升温速率为5~10 ℃/min。
所述CoP/C纳米复合材料可以用作钠离子电池的电极材料。
本发明整个反应过程在水溶液中进行,无需外加其他添加剂,工艺简单,成本低廉且节能环保,易于产业化生产料。
附图说明
图1为实施例1~3制备的CoP/C纳米复合材料的扫描电镜图:a--CoP/C-0.3,b--CoP/C-0.5,c--CoP/C-0.7。
图2为实施例1~3制备的CoP/C纳米复合材料的X射线衍射图。
图3为实施例1~3制备的CoP/C纳米复合材料的循环性能图。
图4为实施例1~3制备的CoP/C纳米复合材料不同倍率下的充放电容量。
具体实施方式
下面结合具体实施例对本发明的技术方案作进一步解释说明,但本发明的保护范围并不局限于此。
实施例1
一种CoP/C纳米复合材料的制备方法,步骤如下:
(1)、螯合物的制备:
取0.3 g的Co(CH3COO)2·4H2O和5 g硫脲加入2 mL去离子水于干燥洁净的容器中,将2mL植酸加入上述溶液,在80 ℃下搅拌至干,获得螯合物;
(2)、螯合物的分解:
将步骤(1)制得的螯合物置于瓷舟中,放置于管式炉中,在氩气氛围下,以5 ℃/min的升温速率升温至180 ℃,恒温30 min;
(3)、硫脲的高温碳化:
在步骤(2)基础上,继续以10 ℃/min的升温速率升温至900 ℃,恒温2 h,恒温结束后随炉冷却至室温,制得CoP/C纳米复合材料,该材料命名为CoP/C-0.3。
实施例2
与实施例1的不同之处在于:步骤(1)中,Co(CH3COO)2·4H2O的用量为0.5 g;其它均同实施例1。所得材料命名为CoP/C-0.5。
实施例3
与实施例1的不同之处在于:步骤(1)中,Co(CH3COO)2·4H2O的用量为0.7 g;其它均同实施例1。所得材料命名为CoP/C-0.7。
结构表征
图1为实施例1~3制备的CoP/C纳米复合材料的扫描电镜图:a--CoP/C-0.3,b--CoP/C-0.5,c--CoP/C-0.7。由图1可以看出:CoP纳米粒子负载于C纳米片上。
图2为实施例1~3制备的CoP/C纳米复合材料的X射线衍射图。图2表明:图中出现了单一相的CoP纳米粒子(JCPDS:29-0497),而碳由于是无定型,所以图中并未出现碳的特征峰。
性能测试
实验步骤如下:
(一)、以实施例1~3制备的CoP/C纳米复合材料作为电极活性材料,制备电极片,具体过程为:将70 wt%活性物质、20 wt%导电剂(Super-P)和10 wt%聚合物粘合剂(PVDF)与N-甲基-2-吡咯烷酮(NMP)混合,研磨均匀,得到料浆;将得到的料浆涂在铜箔集流体上,在120℃下真空干燥12 h,每块铜箔上的活性物质平均负载量为1 mg cm-1,烘干后的铜箔用冲片机冲压成圆形极片,即得电极片;
(二)、半电池组装:电池的组装过程都是在充满氩气的手套箱中完成,并且手套箱中水和氧的值都小于等于0.1 ppm,以金属钠片作为对电极,以玻璃纤维隔膜(Whatman)为钠离子电池隔膜,以1mol/L NaPF6/(EC+DEC)为电解液(EC和DEC的体积比为1∶1),电解液中按体积比计添加有5%的FEC,按照正极壳-步骤(一)制备的电极片-电解液-隔膜-电解液-钠片-垫片-负极壳-封口顺序依次完成CR-2032型扣式电池的组装,然后用液压封口机密封,最后放置12 h;
(三)、电化学性能是由武汉蓝电电子有限公司研发的蓝电系列电池测试系统(CT3001B)测试的;循环性能测试条件为:0.2 A g-1,循环150圈;倍率性能测试条件:0.1C,0.2C,0.5C,1C,2C,5C和0.1A g-1下各循环10圈。
图3为实施例1~3制备的CoP/C纳米复合材料的循环性能图。从图3可以看出:本发明实施例1~3制备的CoP/C纳米复合材料具有较高的首次充放电容量和库伦效率,并且在循环150次后,依然保持较高的充放电容量和库伦效率,尤其是实施例2制备的CoP/C-0.5的复合材料显出最优的循环性能。这是因为相比于CoP/C-0.3和CoP/C-0.7而言,CoP/C-0.5复合材料具有合适的CoP负载量,能明显抑制一磷化钴纳米粒子的聚集。
图4为实施例1~3制备的CoP/C纳米复合材料不同倍率下的充放电容量。从图4可以看出:本发明实施例1~3制备的CoP/C纳米复合材料表现出优异的倍率性能,尤其是实施例2制备的CoP/C-0.5的复合材料显出最优的倍率性能。
实验结果表明:本发明制备的CoP/C纳米复合材料可用作制备钠离子电池的负极材料,具有优异的电化学性能。
Claims (4)
1.一种CoP/C纳米复合材料,其特征在于:所述复合材料是指一磷化钴纳米粒子负载在碳纳米片上。
2.一种如权利要求1所述的CoP/C纳米复合材料的制备方法,其特征在于:以质量体积比计,Co(CH3COO)2·4H2O∶硫脲∶植酸∶水=(0.3~0.7) g∶(3~5) g∶2 mL∶2 mL,将Co(CH3COO)2·4H2O、硫脲、植酸加入水中,60~80 ℃下搅拌至干,获得螯合物;然后在保护气氛下,将所得螯合物分两阶段升温:第一阶段升温至180 ℃恒温30 min,第二阶段升温至900℃恒温2 h;最后冷却至室温,即得CoP/C纳米复合材料。
3.如权利要求1所述的CoP/C纳米复合材料的制备方法,其特征在于:第一阶段升温速率为2~5 ℃/ min,第二阶段升温速率为5~10 ℃/min。
4.一种如权利要求1所述的CoP/C纳米复合材料的用途,其特征在于:作为钠离子电池的电极材料。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111924843A (zh) * | 2020-08-19 | 2020-11-13 | 中国海洋大学 | 一种氰根修饰生物质衍生碳的方法及其在储钾领域的应用 |
CN114852979A (zh) * | 2022-04-26 | 2022-08-05 | 广东工业大学 | 一种磷化钴材料及其制备方法与应用 |
CN115141031A (zh) * | 2022-05-18 | 2022-10-04 | 安徽大学 | 电磁波吸收复合材料及其制备方法和应用 |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105895886A (zh) * | 2016-06-21 | 2016-08-24 | 中南大学 | 一种钠离子电池过渡金属磷化物/多孔碳负极复合材料及其制备方法 |
US20170015558A1 (en) * | 2015-07-13 | 2017-01-19 | Agency For Science, Technology And Research | Method for preparing transition metal phosphide |
CN107275639A (zh) * | 2017-06-30 | 2017-10-20 | 武汉理工大学 | 纳米颗粒组装的CoP/C分级纳米线及其制备方法和应用 |
CN107362818A (zh) * | 2017-07-12 | 2017-11-21 | 武汉理工大学 | 氮磷双掺杂碳包覆过渡金属二磷化物析氢催化剂及制备方法 |
CN108598450A (zh) * | 2018-06-29 | 2018-09-28 | 陕西师范大学 | 一种CoP/氮掺杂碳/石墨烯纳米复合材料及其制备方法 |
CN109569683A (zh) * | 2018-10-19 | 2019-04-05 | 郑州大学 | 一种氮磷共掺杂的多孔碳片/过渡金属磷化物复合材料的制备方法及应用 |
CN109590002A (zh) * | 2019-01-11 | 2019-04-09 | 中南大学 | 一种过渡金属磷化物析氢复合材料及其制备方法和应用 |
CN110215930A (zh) * | 2019-06-17 | 2019-09-10 | 西南石油大学 | 氮掺杂碳包覆的Co基MOF衍生材料和制备方法及其应用 |
-
2019
- 2019-12-19 CN CN201911313894.9A patent/CN111039268A/zh active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20170015558A1 (en) * | 2015-07-13 | 2017-01-19 | Agency For Science, Technology And Research | Method for preparing transition metal phosphide |
CN105895886A (zh) * | 2016-06-21 | 2016-08-24 | 中南大学 | 一种钠离子电池过渡金属磷化物/多孔碳负极复合材料及其制备方法 |
CN107275639A (zh) * | 2017-06-30 | 2017-10-20 | 武汉理工大学 | 纳米颗粒组装的CoP/C分级纳米线及其制备方法和应用 |
CN107362818A (zh) * | 2017-07-12 | 2017-11-21 | 武汉理工大学 | 氮磷双掺杂碳包覆过渡金属二磷化物析氢催化剂及制备方法 |
CN108598450A (zh) * | 2018-06-29 | 2018-09-28 | 陕西师范大学 | 一种CoP/氮掺杂碳/石墨烯纳米复合材料及其制备方法 |
CN109569683A (zh) * | 2018-10-19 | 2019-04-05 | 郑州大学 | 一种氮磷共掺杂的多孔碳片/过渡金属磷化物复合材料的制备方法及应用 |
CN109590002A (zh) * | 2019-01-11 | 2019-04-09 | 中南大学 | 一种过渡金属磷化物析氢复合材料及其制备方法和应用 |
CN110215930A (zh) * | 2019-06-17 | 2019-09-10 | 西南石油大学 | 氮掺杂碳包覆的Co基MOF衍生材料和制备方法及其应用 |
Non-Patent Citations (2)
Title |
---|
JING BAI ET AL.: "One-Step Construction of N,P-Codoped Porous Carbon Sheets/CoP Hybrids with Enhanced Lithium and Potassium Storage", 《ADVANCED MATERIALS》 * |
TAO MENG ET AL.: "Organophosphoric acid-derived CoP quantum dots@S,N-codoped graphite carbon as a trifunctional electrocatalyst for overall water splitting and Zn-air batteries", 《NANOSCALE》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111924843A (zh) * | 2020-08-19 | 2020-11-13 | 中国海洋大学 | 一种氰根修饰生物质衍生碳的方法及其在储钾领域的应用 |
CN114852979A (zh) * | 2022-04-26 | 2022-08-05 | 广东工业大学 | 一种磷化钴材料及其制备方法与应用 |
CN115141031A (zh) * | 2022-05-18 | 2022-10-04 | 安徽大学 | 电磁波吸收复合材料及其制备方法和应用 |
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