CN109110827B - 一种二硫化镍纳米球的制备方法及其应用 - Google Patents
一种二硫化镍纳米球的制备方法及其应用 Download PDFInfo
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 44
- NKHCNALJONDGSY-UHFFFAOYSA-N nickel disulfide Chemical compound [Ni+2].[S-][S-] NKHCNALJONDGSY-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940078494 nickel acetate Drugs 0.000 claims abstract description 13
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000001509 sodium citrate Substances 0.000 claims abstract description 12
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 12
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims abstract description 5
- 239000007772 electrode material Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- WTURHYSHERRQHM-UHFFFAOYSA-N [Ni].[Ni]=S Chemical compound [Ni].[Ni]=S WTURHYSHERRQHM-UHFFFAOYSA-N 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- -1 sulfide ions Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
本发明提供一种二硫化镍纳米球的制备方法及其应用,制备时,按比例取乙酸镍、柠檬酸三钠和硫代乙酰胺分散于混合溶剂中,再加入聚乙烯吡咯烷酮K30,并添加正丙胺调节反应体系的pH值至7~9,搅拌均匀后,于170‑190℃反应12‑24 h,反应结束后,后处理即得二硫化镍纳米球;其中,乙酸镍、柠檬酸三钠和硫代乙酰胺的摩尔比为1:(0.5‑2):2。该二硫化镍纳米材料“一锅法”即可制备得到,且尺寸显著缩小、形貌均匀,可作为超级电容器的电极材料使用。
Description
技术领域
本发明属于二硫化镍纳米材料制备技术领域,具体涉及一种二硫化镍纳米球的制备方法及其应用。
背景技术
到目前为止,已被报道的镍的硫化物的合成方法虽然已有多种,但大多需要借助模板或多步转化的方法,一步合成的例子不多。例如赵等人首先在180℃的条件下合成由氢氧化镍纳米片组成的微米球,再以该微米球为前体,加入硫代乙酰胺,通过金属氢氧化物与硫离子的阴离子交换反应,在120℃条件下转换成多孔硫化镍微米球,此方法合成的三维多孔硫化镍微球尺寸为3 μm,形貌均匀,但该制备方法需要两步完成,且合成的样品尺寸较大[ACS Nano2014, 8: 10909–10919]。楼雄文课题组通过牺牲模板的方法,合成了盒子套盒子结构的硫化镍,制备过程需要预先合成硬模板SiO2 [Adv. Funct. Mater. 2014, 24:7440–7446],此外,通过该球形SiO2模板转化法,还可以得到中空球形的硫化镍[RSC Adv.,2011, 1: 397–400]。曹等人以NiCl2·6H2O和硫脲为原料,通过简单的一步水热法,在180℃反应12 h 的条件下合成了尺寸为2~3 μm的Ni7S6纳米花[J. Mater. Chem., 2010, 20:1078–1085]。综上所述,一步法合成镍的硫化物,方法虽然简单,但是得到的晶体结晶度不高,形貌不规则,且尺寸比较大,而两步法合成的镍硫化物,得到的产物形貌较均匀,但是合成过程较为复杂。
发明内容
本发明针对二硫化镍制备存在的问题,提供一种二硫化镍纳米球的制备方法及其应用,该二硫化镍纳米材料“一锅法”即可制备得到,且尺寸显著缩小、形貌均匀,可作为超级电容器的电极材料使用。
本发明采用如下技术方案:
一种二硫化镍纳米球的制备方法,包括以下步骤:按比例取乙酸镍、柠檬酸三钠和硫代乙酰胺分散于混合溶剂中,再加入聚乙烯吡咯烷酮K30,并添加正丙胺调节反应体系的pH值至7~9,搅拌均匀后,于170-190℃反应12-24 h,反应结束后,后处理即得二硫化镍纳米球;
其中,乙酸镍、柠檬酸三钠和硫代乙酰胺的摩尔比为1: (0.5-2): 2;聚乙烯吡咯烷酮K30作为表面活性剂使用,聚乙烯吡咯烷酮K30与乙酸镍的摩尔比优选为1: 0.033。
优选地,所述混合溶剂由体积比为1:1的去离子水和N, N-二甲基乙酰胺混合而成。
上述制备方法得到的二硫化镍纳米球。
所述二硫化镍纳米球可作为超级电容器电极材料使用。
本发明的有益效果如下:
本发明采用简单的溶剂热法,并通过正丙胺调节体系至适宜反应的pH值范围,一步合成得到了形貌规则、结晶度好、尺寸均匀的二硫化镍(NiS2)纳米球,且所得二硫化镍纳米球的平均尺寸可以缩小至280 nm,显著低于目前报道的尺寸。经测试,该二硫化镍纳米球在碱性电解质中循环可逆性良好,且在0.5 A/g电流密度下,比容量达到1457.8 F/g,同时表现出较好的倍率性能,有望作为超级电容器电极材料使用。
附图说明
图1为不同正丙胺用量得到NiS2的XRD图: (a) 0 μL (b) 25 μL (c) 50 μL;
图2为不同正丙胺用量得到NiS2的SEM图:(a) 0 μL (b) 25 μL (c) 50 μL;
图3为NiS2纳米球的吸附等温线及孔分布图;
图4为NiS2纳米球在不同扫描速率下的CV曲线;
图5为NiS2纳米球在不同电流密度时的恒电流充放电曲线。
图6为NiS2纳米球在电流密度为时4 A/g时的循环寿命测试。
具体实施方式
为了使本发明的技术目的、技术方案和有益效果更加清楚,下面结合附图和具体实施例对本发明的技术方案作出进一步的说明。
实施例1
一种二硫化镍纳米球的制备方法,包括以下步骤:取乙酸镍24.88 mg(0.1 mmol),PVP-K30 100 mg(0.0033 mmol),柠檬酸三钠29.41 mg (0.1 mmol)和硫代乙酰胺15.03 mg(0.2 mmol)分散于4 mL去离子水和4 mL N, N-二甲基乙酰胺 (DMA)混合而成的混合溶剂中,磁力搅拌20 min,测得体系的pH值为7,转移至50 mL反应釜中,在180℃反应12 h,自然冷却到室温,得到的黑色沉淀用无水乙醇和去离子水交替洗涤数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球。
实施例2
一种二硫化镍纳米球的制备方法,包括以下步骤:取乙酸镍24.88 mg (0.1mmol),PVP-K30 100 mg (0.0033 mmol),柠檬酸三钠29.41 mg (0.1 mmol)和硫代乙酰胺15.03 mg (0.2 mmol)分散于4 mL去离子水和4 mL N, N-二甲基乙酰胺 (DMA)混合而成的混合溶剂中,再加入25 μL正丙胺,磁力搅拌20 min,测得体系的pH值为8,转移至50 mL反应釜中,在180℃反应12 h,自然冷却到室温,得到的黑色沉淀用无水乙醇和去离子水交替洗涤数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球。
实施例3
一种二硫化镍纳米球的制备方法,包括以下步骤:取乙酸镍24.88 mg(0.1 mmol),PVP-K30 100 mg (0.0033 mmol),柠檬酸三钠29.41 mg (0.1 mmol)和硫代乙酰胺15.03mg (0.2 mmol)分散于4 mL去离子水和4 mL N, N-二甲基乙酰胺 (DMA)混合而成的混合溶剂中,再加入50 μL正丙胺,磁力搅拌20 min,测得体系的pH值为9,转移至50 mL反应釜中,在180℃反应12 h,自然冷却到室温,得到的黑色沉淀用无水乙醇和去离子水交替洗涤数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球。
实施例4
一种二硫化镍纳米球的制备方法,包括以下步骤:取乙酸镍24.88 mg(0.1 mmol),PVP-K30 100 mg (0.0033 mmol),柠檬酸三钠14.71 mg (0.05 mmol)和硫代乙酰胺15.03mg (0.2 mmol)分散于4 mL去离子水和4 mL N, N-二甲基乙酰胺 (DMA)混合而成的混合溶剂中,再加入25 μL正丙胺,磁力搅拌20 min,测得体系的pH值为8,转移至50 mL反应釜中,在190℃反应12 h,自然冷却到室温,然后用无水乙醇和去离子水交替洗涤黑色沉淀数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球。
实施例5
一种二硫化镍纳米球的制备方法,包括以下步骤:取乙酸镍24.88 mg(0.1 mmol),PVP-K30 100 mg (0.0033 mmol),柠檬酸三钠58.82 mg (0.2 mmol)和硫代乙酰胺15.03mg (0.2 mmol)分散于4 mL去离子水和4 mL N, N-二甲基乙酰胺 (DMA)混合而成的混合溶剂中,再加入25 μL正丙胺,磁力搅拌20 min,测得体系的pH值为8,转移至50 mL反应釜中,在170℃反应24 h,自然冷却到室温,得到的黑色沉淀用无水乙醇和去离子水交替洗涤数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球。
以实施例1、 2和3制备得到的二硫化镍纳米球为例,其结构由XRD确定,如图1所示,可以看出,实施例2制备的二硫化镍纳米球的特征峰与标准PDF卡片号为65-3325的立方晶相匹配度较高,说明本发明制备得到的二硫化镍纳米球为立方晶相。
以实施例1、 2和3制备得到的二硫化镍纳米球为例,扫描电镜测试如图2所示,当反应体系中不加入正丙胺时,如图2a所示,纳米球的产率很低;当正丙胺的用量为25 μL时,得到的样品均为球形形貌,且平均尺寸约280 nm(图2b);当正丙胺的用量达到50 μL时,产物中出现了少许片状形貌(图2c)。由此可知,要得到尺寸和形貌较为均匀的二硫化镍纳米球,选择正丙胺用量为25 μL,此时调节体系最佳pH值为8 。
以实施例2制备得到的二硫化镍纳米球为例,如图3所示,NiS2纳米球的吸附等温线属于IV型中的H3型,样品的孔可能是由球形材料堆积缝隙所产生的,所测样品BET表面积为5.34 m2/g,主要孔径分布约为37 nm。
二硫化镍纳米球的电化学性能测试
以实施例2得到的样品进行如下测试。
图4为二硫化镍纳米球作为工作电极在2 mol/L KOH溶液中的CV曲线,采用铂丝作为对电极,饱和甘汞电极为参比电极。样品的扫描速率为 5~50 mV/s,电位窗口在0~0.6V范围内。由图中曲线可看出,氧化还原峰对称,阴极峰电流与阳极峰电流近似相等,且当扫描速度增加时,曲线的形状维持不变,只是峰电流增加,说明本发明二硫化镍纳米球具有较好的循环可逆性。
图5为在不同电流密度(0.5~6 A/g)下工作电极的恒电流充放电测试曲线,测试电压为0.42 V。在0.5 A/g、1 A/g、2 A/g、4 A/g、6 A/g的比电容值分别为1457.79 F/g、1273.26 F/g、1118.43 F/g、961.34 F/g、841.72 F/g,说明NiS2纳米球具有高的比电容值,且表现出较好的倍率性能。
图6为电流密度为4 A/g下的循环稳定性图,循环1000圈后,电容量为722.47 F/g。
最后所应说明的是:上述实施例仅用于说明而非限制本发明的技术方案,任何对本发明进行的等同替换及不脱离本发明精神和范围的修改或局部替换,其均应涵盖在本发明权利要求保护的范围之内。
Claims (3)
1.一种二硫化镍纳米球的制备方法,其特征在于,包括以下步骤:按比例取乙酸镍、柠檬酸三钠和硫代乙酰胺分散于混合溶剂中,再加入聚乙烯吡咯烷酮K30,并添加正丙胺调节反应体系的pH值至7~9,搅拌均匀后,于170-190℃下反应12-24 h,反应结束后,自然冷却到室温,得到的黑色沉淀用无水乙醇和去离子水交替洗涤数次,离心分离取固体产物,将所收集到的固体样品在60℃下干燥20 min,即得二硫化镍纳米球;
其中,乙酸镍、柠檬酸三钠和硫代乙酰胺的摩尔比为1: (0.5-2): 2;所述混合溶剂由体积比为1:1的去离子水和N, N-二甲基乙酰胺混合而成。
2.权利要求1所述制备方法得到的二硫化镍纳米球。
3.权利要求2所述二硫化镍纳米球作为超级电容器电极材料的应用。
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