CN110364365B - 一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法 - Google Patents
一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法 Download PDFInfo
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Abstract
本发明涉及电化学领域,尤其是一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法。将经分散剂分散的钴盐于水热釜中150‑220℃下反应3~24h,反应后降至室温,将悬浊液离心获得沉淀,沉淀经有机溶剂反复洗涤,所得沉淀干燥再将其于碱性溶液的电解液中,恒电流密度下电催化氧化即可得到单层多孔羟基氧化钴纳米片。本发明具有反应条件温和、工艺流程简单、能耗低、可规模化生产等优点,所得产品具有孔径分布窄、孔隙率高、比表面积大、批次间重复性好等优势,有望在锂离子电池、超级电容器以及电催化等领域得到广泛应用。
Description
技术领域
本发明涉及电化学领域,尤其是一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法。
背景技术
近年来,羟基氧化钴因在锂离子电池、超级电容器以及电催化等诸多领域有较广泛应用而备受关注。在锂离子电池领域,羟基氧化钴常作为钴源来生产锂离子电池的正极活性材料——钴酸锂,同时,它还可以作为电池添加剂改善电池容量及循环寿命。在超级电容器的应用方面,直接利用羟基氧化钴作为电极材料制备出的超级电容器,通常会表现出较高的电容特性。在电催化领域,羟基氧化钴则在电催化析氧反应中展现出了优异的催化活性,并且被认为是钴基催化剂的电催化析氧反应的活性中心。因此,制备高活性的羟基氧化钴在电化学领域具有重要作用。
众所周知,纳米催化剂的活性和用途会因纳米材料的形貌、粒度和粒度分布而受到显著影响。目前公开的专利和文献报道中制备羟基氧化钴最常用的方法是先将钴盐与碱溶液进行混合得到沉淀,然后再对沉淀进行氧化处理,得到羟基氧化钴。研究者通过控制反应条件,制备出了不同形状的羟基氧化钴。例如,专利申请201510589714.5公开了一种空心六边形状羟基氧化钴纳米材料的制备方法;专利申请201210578760.1公开了一种球形羟基氧化钴的制备方法;文献“CoOOH Nanosheets with High Mass Activity for WaterOxidation,Huang,J.;Chen,J.;Yao,T.;He,J.;Jiang,S.;Sun,Z.;Liu,Q.;Cheng,W.;Hu,F.;Jiang,Y.;Pan,Z.;Wei,S.,Angew Chem Int Ed Engl 2015,54(30),8722-7.”报道了一种超薄羟基氧化钴纳米片;文献“Synthesis of CoOOH nanorods and application ascoating materials of nickel hydroxide for high temperature Ni-MH cells”(WuW.,Gao X.,Geng M.,Gong Z.,Noreus D.,J.Phys.Chem.B 19(2005)5392-5394)报道了一种羟基氧化钴纳米棒。由此可见,研究人员目前已经成功制备出了球形、棒状和片状等多种形貌的羟基氧化钴纳米材料,但是,关于制备单层多孔纳米片状的羟基氧化钴目前却尚未报道。
发明内容
本发明的目的在于提供一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法。
为实现上述目的,本发明所采用的技术方案为:
一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法,将经分散剂分散的钴盐于水热釜中150-220℃下反应3~24h,反应后降至室温(反应后用自来水冲洗水热釜快速降温至室温),将悬浊液离心获得沉淀,沉淀经有机溶剂反复洗涤,所得沉淀干燥再将其于碱性溶液的电解液中,恒电流密度下电催化氧化即可得到单层多孔羟基氧化钴纳米片。
所述将经分散剂分散的钴盐为将按质量比为1:1~3:1的钴盐和分散剂混合后溶解于过量的乙二醇和去离子水的混合液中,充分溶解,待用;其中,钴盐为硫酸钴,硝酸钴,醋酸钴或氯化钴中的一种或几种,分散剂为聚乙烯吡咯烷酮。
所述乙二醇和去离子水按质量比为50:1~20:1的比例混合得混合液;钴盐在混合液中的质量分数为0.6~3.2%;分散剂在混合液中的质量分数为0.2~1.8%。
所述将经分散剂分散的钴盐置于聚四氟乙烯内衬的水热晶化釜中,密封反应,反应后降温,离心获得沉淀,并用有机溶剂洗涤沉淀2~3次,干燥,得粉色前驱体;其中,有机溶剂为无水乙醇、异丙醇、叔丁醇的一种或几种。
所述离心转速为6500~9000r/min,时间为5~20min;干燥温度为30~90℃,干燥时间为1~10h。
将所得前驱体滴在碳纸上为工作电极,以碱性溶液作为电解液,于5~50mA cm-2的恒电流密度下电催化氧化1~6h,即可得到单层多孔羟基氧化钴纳米片;所述电解液为氢氧化钾、氢氧化钠或氢氧化锂中的一种或几种混合物,电解液浓度为0.1M~5M。
所述碳纸大小为1×1cm~3×3cm。
相对于现有技术,本发明所提供的制备方法具有以下优势:
(1)采用本发明方法首次合成了单层多孔羟基氧化钴纳米片,该产品具有孔径分布窄、孔隙率高、比表面积大、批次间重复性好等优势。这种具有特殊形貌的材料有望在锂离子电池、超级电容器以及电催化领域发挥重要作用。
(2)本发明所利用的电化学氧化法制备单层多孔羟基氧化钴纳米片,具有反应条件温和、工艺流程简单、能耗低、可规模化生产等优点。
附图说明
图1为本发明实施例提供的实施例1合成的单层多孔羟基氧化钴纳米片的扫描电子显微镜(SEM)照片。
图2为本发明实施例提供的实施例2合成的单层多孔羟基氧化钴纳米片的高透射电镜(TEM)照片。
图3为本发明实施例提供的实施例3合成的单层多孔羟基氧化钴X射线衍射(XRD)谱图。
具体实施方式
以下结合附图和实施例对本发明做进一步详细说明,但该实施例并不以任何形式限制本发明。
一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法,包括以下步骤:
(1)分别称取一定质量的钴盐、分散剂溶解于乙二醇和去离子水的混合液中,搅拌均匀。
(2)将步骤(1)所得混合液置于聚四氟乙烯内衬的水热晶化釜中,密封。将反应釜放置于高温环境中反应,一定时间后,将反应釜取出,快速降温,将所得沉淀离心分离,并用有机溶剂洗涤2-3次,再分离,干燥,得粉色前驱体。
(3)将步骤(2)所得前驱体定量滴在碳纸上,作为工作电极,碱性溶液为电解液,恒电流密度下进行电化学氧化,一定时间后,即可得到单层多孔羟基氧化钴纳米片。
本发明反应条件温和、工艺流程简单、能耗低、可规模化生产等优点,制备出的羟基氧化钴具有孔径分布窄(平均孔径3.8纳米)、孔隙率高、比表面积大(198m2g-1)、批次间重复性好等优势。
实施例1
取1.8g四水合乙酸钴溶解在100ml的乙二醇中,加入0.6g聚乙烯吡络烷酮,5ml蒸馏水,充分搅拌30min至全部溶解形成透明澄清溶液。将上述透明溶液转移至250ml晶化釜中,密封,在220℃反应6h。反应结束后,将水热釜用自来水冲洗快速降温至室温。将所得悬浊液进行离心分离得到沉淀,然后将所得沉淀用无水乙醇洗涤3次,在50℃下干燥10h,即可得粉色前驱体。
取上述粉色前驱体100mg,分散到1*1cm的碳纸上,作为工作电极,0.1M KOH溶液为电解液。在恒电流密度(10mA cm-2)下电解3h即可得到单层多孔羟基氧化钴纳米片。产品的SEM图见附图1。由图1可见,通过实施例1可以获得单层羟基氧化钴纳米片,表面具有大量的纳米颗粒。
实施例2
取0.9g硝酸钴溶解在100ml的乙二醇中,加入0.3g聚乙烯吡络烷酮,充分搅拌均匀到全部溶解。加入5ml蒸馏水,搅拌30min,形成透明溶液。将上述透明溶液转移至250ml晶化釜中,密封,在200℃反应12h。反应结束后,将水热釜用自来水冲洗快速降温至室温。将所得悬浊液进行离心分离得到沉淀,将所得沉淀用异丙醇洗涤3次,在50℃下干燥10h,即可得粉色前驱体。
取上述粉色前驱体120mg,分散到2*2cm的碳纸上,作为工作电极,1M KOH溶液为电解液。在恒电流密度(5mA cm-2)下电解6h即可得到单层多孔羟基氧化钴纳米片,其TEM图见附图2。由图2可见,通过实施例2我们可以获得单层多孔的羟基氧化钴纳米片。
实施例3
取0.5g氯化钴溶解在50ml的乙二醇中,加入0.3g聚乙烯吡络烷酮,充分搅拌均匀到全部溶解。加入5ml蒸馏水,搅拌30min,形成透明溶液。将上述透明溶液转移至250ml晶化釜中,密封,在150℃反应24h。反应结束后,将水热釜用自来水冲洗快速降温至室温。将所得悬浊液进行离心分离得到沉淀,将所得沉淀用叔丁醇洗涤3次,在50℃下干燥10h,即可得粉色前驱体。
取上述粉色前驱体200mg,分散到3*3cm的碳纸上,作为工作电极,5M KOH溶液为电解液。在恒电流密度(20mA cm-2)下电解1h即可得到单层多孔羟基氧化钴纳米片,其XRD图见附图3。由图3可见,通过实施例3所获得的样品晶型与标准羟基氧化钴卡片是完全一致的,即获得单层多孔羟基氧化钴纳米片。
Claims (1)
1.一种电化学氧化法制备单层多孔羟基氧化钴纳米片的方法 ,其特征在于:将经分散剂分散的钴盐于水热釜中150-220℃下反应3~24h,反应后降至室温,将悬浊液离心获得沉淀,沉淀经有机溶剂反复洗涤,所得沉淀干燥再将其于碱性溶液的电解液中,恒电流密度下电催化氧化即可得到单层多孔羟基氧化钴纳米片;其中,有机溶剂为无水乙醇、异丙醇、叔丁醇的一种或几种;
所述将经分散剂分散的钴盐为将按质量比为1:1~3:1的钴盐和分散剂混合后溶解于过量的乙二醇和去离子水的混合液中,充分溶解,待用;其中,钴盐为硫酸钴,硝酸钴,醋酸钴或氯化钴中的一种或几种,分散剂为聚乙烯吡咯烷酮;
所述乙二醇和去离子水按质量比为50:1~20:1的比例混合得混合液;钴盐在混合液中的质量分数为0.6~3.2%;分散剂在混合液中的质量分数为0.2~1.8%;
所述离心转速为6500~9000r/min,时间为5~20 min;干燥温度为30~90℃,干燥时间为1~10 h;
所述恒电流密度下电催化氧化为将所得前驱体滴在碳纸上为工作电极,以碱性溶液作为电解液,于5~50 mA cm-2的恒电流密度下电催化氧化1~6h,即可得到单层多孔羟基氧化钴纳米片; 所述电解液为氢氧化钾、氢氧化钠或氢氧化锂中的一种或几种混合物,电解液浓度为0.1M~5M。
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