CN112062169A - 一种镍钴锰硫化物纳米片的制备方法 - Google Patents
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 27
- MBUJIFHANTWAKB-UHFFFAOYSA-N [S-2].[Mn+2].[Co+2].[Ni+2].[S-2].[S-2] Chemical compound [S-2].[Mn+2].[Co+2].[Ni+2].[S-2].[S-2] MBUJIFHANTWAKB-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011572 manganese Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 15
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 15
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 15
- 239000010941 cobalt Substances 0.000 claims abstract description 14
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- -1 molybdenum-niobium-tin-carbon Chemical compound 0.000 claims abstract description 5
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims abstract description 4
- INILCLIQNYSABH-UHFFFAOYSA-N cobalt;sulfanylidenemolybdenum Chemical compound [Mo].[Co]=S INILCLIQNYSABH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 4
- MRDDPVFURQTAIS-UHFFFAOYSA-N molybdenum;sulfanylidenenickel Chemical compound [Ni].[Mo]=S MRDDPVFURQTAIS-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZOCLAPYLSUCOGI-UHFFFAOYSA-M potassium hydrosulfide Chemical compound [SH-].[K+] ZOCLAPYLSUCOGI-UHFFFAOYSA-M 0.000 claims abstract description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 4
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 4
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 2
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 4
- 229910003266 NiCo Inorganic materials 0.000 description 3
- 238000003491 array Methods 0.000 description 3
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- IWHAVVGLVXIYBA-UHFFFAOYSA-N [S-2].[Mn+2].[Co+2].[S-2] Chemical compound [S-2].[Mn+2].[Co+2].[S-2] IWHAVVGLVXIYBA-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
- C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/10—Energy storage using batteries
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Abstract
本发明公开了一种镍钴锰硫化物纳米片的制备方法，以二维材料为载体，以镍、钴、锰可溶性盐为原料，水热反应生成镍钴锰氢氧化物，再与硫化物混合，水热反应获得镍钴锰硫化物纳米片；二维材料为碳化钛、钼铌锡碳、石墨烯、镍‑钼硫化物、钴‑钼硫化物的一种；硫化物为硫化钠、硫化钾、硫化铵、硫化氢钠、硫化氢钾、硫化氢铵的一种；镍、钴、锰的摩尔比为1：(1.5‑2.5)：(1‑3)；二维材料为镍钴锰总摩尔数的0.001‑0.2；硫化物与镍钴锰总摩尔比为2‑5。该镍钴锰硫化物纳米片制备工艺简单可控、操作方便，适于工业化生产。
Description
技术领域
本发明专利涉及一种电极材料的制备方法，具体涉及一种镍钴锰硫化物纳米片的制备方法。
背景技术
过渡金属硫化物具有电导率高和稳定性好等优点，是非常有应用前景的超级电容器材料。目前科研人员主要集中在单金属或双金属硫化物的制备与性能改性，如Ni3S2、CuS、NiS、NiCo2S4、ZnCo2S4等。
Xu et al0采用电沉积法制备泡沫镍负载Ni3S2纳米片阵列实现高达309.4C·g-1的比容量。(Xu J,Sun Y,Lu M,et al.One-step electrodeposition fabrication ofNi3S2 nanosheet arrays on Ni foam as an advanced electrode for asymmetricsupercapacitors[J].Science China Materials,2019,62(5):699-710.)
Zhao et al.采用电沉积法制备CuS微球实现高达222.1C·g-1的比容量；(Zhao TK,Peng X R,Zhao X,et al.Facile preparation and high capacitance performanceof copper sulfide microspheres as supercapacitor electrodematerial.Composites Part B:Engineering,2019,163:26-35.)
Guo et al制备出NiCo2S4纳米管获得高达3.5C·cm-2的比容量，当电流密度增大25倍时保留66.1％的比容量；(Guo M L,Gao H X,Huang W,et al.Microwave-assistedrapid synthesis of NiCo2S4 nanotube arrays on Ni foam for highcyclingstabilitysupercapacitors.Journal of Alloys and Compounds,2019,780:164-169.
Cheng et al采溶剂热法合成ZnCo2S4实现418.1C·g-1的比容量，在功率密度1700W·kg-1时具有51.7Wh·kg-1的能量密度和在功率密度6.8kW·kg-1时具有42.5Wh·kg-1的能量密度；(Cheng C,Zhang X Y,Wei C Z,et al.Mesoporous hollow ZnCo2S4 core-shell nanospheres for high performance supercapacitors.CeramicInternational.2018,44:17464-17472.)
但单金属和双金属硫化物的能量密度不高，如何通过多金属的协同作用，提高其能量密度是亟待解决的问题。
发明内容
针对现有技术方案的缺陷，本发明的目的是提供一种镍钴锰硫化物纳米片的制备方法。
本发明涉及一种镍钴锰硫化物纳米片的制备方法，其特征在于：以二维材料为载体，以镍、钴、锰可溶性盐为原料，水热反应生成镍钴锰氢氧化物，再与硫化物混合，水热反应获得镍钴锰硫化物纳米片；二维材料为碳化钛、钼铌锡碳、石墨烯.镍-钼硫化物、钴-钼硫化物的一种；硫化物为硫化钠、硫化钾、硫化铵、硫化氢钠、硫化氢钾、硫化氢铵的一种；镍、钴、锰的摩尔比为1：(1.5-2.5)：(1-3)；一种镍钴锰硫化物纳米片的制备方法包括：
1)称量一定质量的二维材料、镍、钴、锰可溶性盐，放入水/乙醇溶剂，搅拌，然后在80-150℃水热反应5-10h，获得镍钴锰氢氧化物；
2)将步骤1)产物与硫化物混合，搅拌，然后在120-250℃水热反应5-10h；
所述的二维材料为镍钴锰总摩尔数的0.001-0.2；
所述的硫化物与镍钴锰总摩尔比为2-5。
本专利以二维材料为模板，吸附镍、钴、锰在其表面沉积，形成镍钴锰氢氧化物纳米片；再用硫化物与镍钴锰氢氧化物置换反应，生成镍钴锰硫化物纳米片。
与现有技术相比，本发明专利提供的一种镍钴锰硫化物纳米片制备方法，具有以下优势：
1)制备工艺简单、工序可控、可产业化生产；
2)以片状二维材料为模板，引导镍钴锰离子在其表面沉积，再与硫化物置换反应，生成纳米片状镍钴锰硫化物，极大地改善了镍钴锰硫化物的导电率。
3)镍钴锰三金属的协同作用，提高了材料的比容量；本专利制备的纳米片状镍钴锰硫化物具有很好的电化学性能；在电流密度1A·g-1具有大于600C·g-1的比容量。
具体实施方式
为能进一步了解本发明的发明内容、特点及功效，兹举以下实施例详细说明如下：
实例1
一种镍钴锰硫化物纳米片的制备方法，包括：
1)称量一定质量的二维材料、镍、钴、锰可溶性盐，放入水/乙醇溶剂，搅拌，然后在90℃水热反应6h；
2)将步骤1)产物与硫化物混合，搅拌，然后在180℃水热反应5h。
一种镍钴锰硫化物纳米片的成分设计，包括：
1)NiCl2·6H2O,0.02mol；CoCl2·6H2O,0.04mol；MnCl2·4H2O,0.03mol；碳化钛，0.0009mol；硫化钠，0.21mol；
结果显示：镍钴锰硫化物纳米片在电流密度1A·g-1时，具有大于600C·g-1的比容量，在电流密度为50A·g-1时，保留了大于300C·g-1的比容量。
实例2
操作同实例1.
一种镍钴锰硫化物纳米片的成分设计，包括：
2)NiCl2·6H2O,0.02mol；CoCl2·6H2O,0.04mol；MnCl2·4H2O,0.04mol；钼铌锡碳，0.00125mol；硫化钾，0.27mol；
镍钴锰硫化物纳米片在电流密度1A·g-1具有657.7C·g-1的比容量，电流密度为50A·g-1，保留339.5C·g-1的比容量，经1100次循环，保留97.8％的比容量。
实例3
一种镍钴锰硫化物纳米片的制备方法，包括：
3)称量一定质量的二维材料、镍、钴、锰可溶性盐，放入水/乙醇溶剂，搅拌，然后在120℃水热反应5h；
4)将步骤1)产物与硫化物混合，搅拌，然后在200℃水热反应5h。
一种镍钴锰硫化物纳米片的成分设计，包括：
3)Ni(CH3COO)2·4H2O,0.02mol；Co(CH3COO)2·4H2O,0.03mol；
Mn(CH3COO)2·4H2O,0.02mol；石墨烯，0.001mol；硫化钾，0.27mol；
4)Ni(CH3COO)2·4H2O,0.02mol；Co(CH3COO)2·4H2O,0.05mol；
Mn(CH3COO)2·4H2O,0.02mol；镍-钼硫化物，0.009mol；硫化铵，0.22mol；
5)Ni(CH3COO)2·4H2O,0.02mol；Co(CH3COO)2·4H2O,0.04mol；
Mn(CH3COO)2·4H2O,0.06mol；钴-钼硫化物，0.00125mol；硫化氢钾，0.5mol；
镍钴锰硫化物纳米片在电流密度1A·g-1具有657.7C·g-1的比容量，电流密度为50A·g-1，保留339.5C·g-1的比容量，经1100次循环，保留97.8％的比容量。
上述专利的具体实施方式是示例性的，是为了更好的使本领域技术人员能够理解本专利，不能理解为是对本专利包括范围的限制；只要是根据本专利所揭示精神的所作的任何等同变更或修饰，均落入本专利包括的范围。
Claims (3)
1.本发明涉及一种镍钴锰硫化物纳米片的制备方法，其特征在于：以二维材料为载体，以镍、钴、锰可溶性盐为原料，水热反应生成镍钴锰氢氧化物，再与硫化物混合，水热反应获得镍钴锰硫化物纳米片；二维材料为碳化钛、钼铌锡碳、石墨烯、镍-钼硫化物、钴-钼硫化物的一种；硫化物为硫化钠、硫化钾、硫化铵、硫化氢钠、硫化氢钾、硫化氢铵的一种；镍、钴、锰的摩尔比为1：(1.5-2.5)：(1-3)；一种镍钴锰硫化物纳米片的制备方法包括：
1)称量一定质量的二维材料、镍、钴、锰可溶性盐，放入水/乙醇溶剂，搅拌，然后在80-150℃水热反应5-10h，获得镍钴锰氢氧化物；
2)将步骤1)产物与硫化物混合，搅拌，然后在120-250℃水热反应5-10h。
2.根据权利要求1所述的一种镍钴锰硫化物纳米片制备方法，其特征在于：二维材料为镍钴锰总摩尔数的0.001-0.2。
3.根据权利要求1所述的一种镍钴锰硫化物纳米片制备方法，其特征在于：硫化物与镍钴锰总摩尔比为2-5。
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| CN114360918A (zh) * | 2021-11-22 | 2022-04-15 | 沈阳工程学院 | 一种高性能超级电容器异质结构的电极材料的制备方法 |
| CN114590850A (zh) * | 2022-03-17 | 2022-06-07 | 中国长江三峡集团有限公司 | 硫化物全固态锂电池用新型硫化正极材料及其制备方法 |
| CN114974916A (zh) * | 2022-07-04 | 2022-08-30 | 桂林电子科技大学 | 一种纤维状MXene负载NiCoS复合材料及其制备方法和应用 |
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| CN114974916A (zh) * | 2022-07-04 | 2022-08-30 | 桂林电子科技大学 | 一种纤维状MXene负载NiCoS复合材料及其制备方法和应用 |
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