CN111204814A - 一种棒状结构硫铁钠材料及其制备方法 - Google Patents
一种棒状结构硫铁钠材料及其制备方法 Download PDFInfo
- Publication number
- CN111204814A CN111204814A CN202010023860.2A CN202010023860A CN111204814A CN 111204814 A CN111204814 A CN 111204814A CN 202010023860 A CN202010023860 A CN 202010023860A CN 111204814 A CN111204814 A CN 111204814A
- Authority
- CN
- China
- Prior art keywords
- sodium
- rod
- containing material
- sulfate
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 42
- HVKQCFGSHOWUMW-UHFFFAOYSA-N [S].[Na].[Fe] Chemical compound [S].[Na].[Fe] HVKQCFGSHOWUMW-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011734 sodium Substances 0.000 claims abstract description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 15
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 235000019820 disodium diphosphate Nutrition 0.000 claims description 5
- GYQBBRRVRKFJRG-UHFFFAOYSA-L disodium pyrophosphate Chemical compound [Na+].[Na+].OP([O-])(=O)OP(O)([O-])=O GYQBBRRVRKFJRG-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011019 hematite Substances 0.000 claims description 5
- 229910052595 hematite Inorganic materials 0.000 claims description 5
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 5
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 5
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229960004887 ferric hydroxide Drugs 0.000 claims description 2
- 229940032950 ferric sulfate Drugs 0.000 claims description 2
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 2
- 229960001781 ferrous sulfate Drugs 0.000 claims description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- 229910052683 pyrite Inorganic materials 0.000 claims description 2
- 239000011028 pyrite Substances 0.000 claims description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 2
- 229910021646 siderite Inorganic materials 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 abstract description 6
- 238000004146 energy storage Methods 0.000 abstract description 6
- 239000007772 electrode material Substances 0.000 abstract description 5
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 abstract description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- -1 aluminum ion Chemical class 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 239000002001 electrolyte material Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 208000028659 discharge Diseases 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Compounds Of Iron (AREA)
Abstract
本发明提供了一种棒状结构硫铁钠材料及其制备方法，制备的硫铁钠材料，稳定性高，初始容量高，最高达22888mAh g‑1，这些都表明硫铁钠材料将在储能材料中具有潜在的应用。该硫铁钠材料可以用于储能电池的电极材料、电解质材料，比如可以应用在钠离子电池、锂离子电池、钾离子电池、铝离子电池、铅酸电池、超级电容器等储能电池的电极、电解质，也可以作为太阳能电池的重要组件，未来可能会应用于生物医药领域。
Description
技术领域
本发明涉及化工技术领域，尤其涉及一种棒状结构硫铁钠材料及其制备方法。
背景技术
目前，风电水电，核能等受到越来越多的关注，发电技术的进步导致了旺季电力储备的持续下滑，促进了储能材料的蓬勃发展。新型能源材料的研发将在一定程度上推动着能源领域的快速发展。
为了稳定电极和缩短钠离子的扩散长度，锂电池中采用的许多策略正在启发钠电池电极的设计，包括纳米化和复合材料的制备。纳米结构材料具有两种效应：(1)“微小尺寸效应”，取决于纳米颗粒直径的减小或单层膜的厚度和表面体积比的增加；(2)“真实尺寸效应”，取决于材料局部性质的变化。例如，高比表面积的纳米结构电极材料可以增加电解质的副反应，降低库仑效率。单相体系同时获得高容量、长循环寿命和良好的速率性能是很少见的，因此，将单个材料的独特性能结合起来形成复合材料，可能在钠电池电极材料中产生协同效应。纳米材料的组合为先进电极的发展开辟了新的前景。通常有以下选择：(1)引入不适合作为电极材料本身的新材料；(2)增加活性材料与电解液之间的接触表面积；(3)使用导电材料作为结构剂，减少电子和离子的传输路径长度。因此，使用新材料是获得高性能新型钠电池的一个好方法。
发明内容
针对上述现有技术中所存在的技术问题，本发明提供了一种棒状结构硫硫铁钠新材料，包括以下制备步骤：
1)准备制备原料摩尔百分比为：含铁材料10-50％，含钠材料10-50％，含硫材料10-50％，且上述材料的摩尔百分比总和为100％；
2)将原料加入有机溶剂/超纯水中搅拌均匀后转移至反应釜中；
3)将产物用有机溶剂或超纯水洗涤后干燥；
4)将产物在氮气保护中，进行热处理，制得棒状结构硫铁钠。
优选地，所述含铁材料选自：赤铁矿、磁铁矿、菱铁矿、黄铁矿、硫酸铁、硫酸亚铁、硫酸亚铁铵、氢氧化铁、氢氧化亚铁中的一种或几种。
优选地，所述含钠材料选自：磷酸钠、酸式焦磷酸钠、磷酸二氢钠、磷酸氢二钠、焦磷酸钠、乙酸钠、醋酸钠、碳酸钠、氢氧化钠、氯化钠、硫酸钠、硫代硫酸钠、碳酸氢钠、硝酸钠中的一种或几种。
优选地，所述含硫材料选自：硫单质、硫酸盐、亚硫酸和亚硫酸盐中的一种或几种。
优选地，所述反应釜中的条件为：反应温度100-200℃，反应时间2-48h。
优选地，所述有机溶剂选自：醇、乙二醇、异丙醇。
优选地，所述热处理条件为：在氮气下，烧结温度200-1000℃，反应时间2-48h。
一种棒状结构的硫铁钠材料由以上所述方法制备。
优选地，所述棒状结构长度为300-500nm，直径约为50-80nm。
初始容量高，最高达22888mAh g-1，比能量最高达17016Wh kg-1。
该硫铁钠材料可以用于储能电池的电极材料、电解质材料，比如可以应用在钠离子电池、锂离子电池、钾离子电池、铝离子电池、铅酸电池、超级电容器等储能电池的电极、电解质，也可以作为太阳能电池的重要组件，未来可能会应用于生物医药领域。
有益效果包括:
本发明提出了硫铁钠材料及其制备方法，制备的硫铁钠材料，稳定性高，初始容量高，最高达22888mAh g-1，比能量最高达17016Wh kg-1。所有这些都表明硫铁钠材料将在固体电解质中具有潜在的应用。
附图说明
图1为溶剂热法制备硫铁钠材料SEM形貌图；
图2为硫铁钠材料X射线衍射图；
图3为比容量随电压的变化关系；
图4为电池循环性能。
具体实施方式
下面结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护范围。
溶剂热法制备硫铁钠材料SEM形貌如图1所示，图2为硫铁钠材料X射线衍射图，图3为比容量随电压的变化关系,电池初始放电比容量高达22888mAh g-1,经过6圈循环后容量下降至12mAh g-1。这主要是由于初始放电阶段电解质在电极表面形成一层SEI膜，使其具有较高的不可逆容量。
实施例1
选择一种棒状结构硫铁钠材料硫铁钠材料优选地实施方案，包括以下制备步骤：
(1)准备制备原料摩尔百分比为：赤铁矿20％，酸式焦磷酸钠50％，硫酸盐30％；
(2)将原料加入超纯水中搅拌均匀后转移至反应釜中；
(3)将产物用超纯水洗涤后干燥；
(4)将产物在氮气保护中，100℃烧结6小时，即可得产物。
如图2所示，100℃烧结6小时得到的产物经XRD衍射后，特征峰33°、35°很弱，说明，此条件下，产物结晶性很差。
实施例2
选择一种棒状结构硫铁钠材料硫铁钠材料优选地实施方案，包括以下制备步骤：
(1)准备制备原料摩尔百分比为：赤铁矿20％，酸式焦磷酸钠50％，硫酸盐30％；
(2)将原料加入超纯水中搅拌均匀后转移至反应釜中；
(3)将产物用超纯水洗涤后干燥；
(4)将产物在氮气保护中，400℃烧结6小时，即可得产物。
如图2所示，400℃烧结6小时得到的产物经XRD衍射后，特征峰33°、35°很强，说明，此条件下，产物结晶性很好。如图4所示在相同的电化学循环测试条件下，电池初始放电比容量高达22888mAh g-1,经过6圈循环后容量下降至12mAh g-1。这主要是由于初始放电阶段电解质在电极表面形成一层SEI膜，使其具有较高的不可逆容量。初始的库伦效率也相对较高，经过几个循环的活化后，后趋于稳定约为100％，说明可逆的充放电过程。
实施例2
选择一种棒状结构硫铁钠材料硫铁钠材料优选地实施方案，包括以下制备步骤：
(1)准备制备原料摩尔百分比为：赤铁矿20％，酸式焦磷酸钠50％，硫酸盐30％；
(2)将原料加入超纯水中搅拌均匀后转移至反应釜中；
(3)将产物用超纯水洗涤后干燥；
(4)将产物在氮气保护中，600℃烧结6小时，即可得产物。
如图2所示，600℃烧结6小时得到的产物经XRD衍射后，特征峰33°、35°变弱并发生微小的偏移，说明，此条件下，产物结晶性很差，产物可能发生了分解或晶相转变。
最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在形式上和细节上对其作出各种各样的改变，而不偏离本发明权利要求书所限定的范围。
Claims (8)
1.一种棒状结构硫铁钠材料的制备方法，其特征在于，包括以下制备步骤：
1)准备制备原料摩尔百分比为：含铁材料10-50％，含钠材料10-50％，含硫材料10-50％，且上述材料的摩尔百分比总和为100％；
2)将原料加入有机溶剂/超纯水中搅拌均匀后转移至反应釜中；
3)将产物用有机溶剂或超纯水洗涤后干燥；
4)将产物在氮气保护中，进行热处理，制得棒状结构硫铁钠材料。
2.如权利要求1所述的制备方法，其特征在于，所述含铁材料选自：赤铁矿、磁铁矿、菱铁矿、黄铁矿、硫酸铁、硫酸亚铁、硫酸亚铁铵、氢氧化铁、氢氧化亚铁中的一种或几种。
3.如权利要求1所述的制备方法，其特征在于，所述含钠材料选自：磷酸钠、酸式焦磷酸钠、磷酸二氢钠、磷酸氢二钠、焦磷酸钠、乙酸钠、醋酸钠、碳酸钠、氢氧化钠、氯化钠、硫酸钠、硫代硫酸钠、碳酸氢钠、硝酸钠中的一种或几种。
4.如权利要求1所述的制备方法，其特征在于，所述含硫材料选自：硫单质、硫酸盐、亚硫酸和亚硫酸盐中的一种或几种。
5.如权利要求1所述的制备方法，其特征在于，所述反应釜中的条件为：反应温度100-200℃，反应时间2-48h。
6.如权利要求1所述的制备方法，其特征在于，所述有机溶剂选自：醇、乙二醇、异丙醇。
7.如权利要求1所述的制备方法，其特征在于，所述热处理条件为：在氮气下，烧结温度200-1000℃，反应时间2-48h。
8.一种棒状结构硫铁钠材料由权利要求1-7所述任一方法制备，其特征在于，所述棒状结构长度为300-500nm，直径约为50-80nm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010023860.2A CN111204814B (zh) | 2020-01-09 | 2020-01-09 | 一种棒状结构硫铁钠材料及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010023860.2A CN111204814B (zh) | 2020-01-09 | 2020-01-09 | 一种棒状结构硫铁钠材料及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111204814A true CN111204814A (zh) | 2020-05-29 |
| CN111204814B CN111204814B (zh) | 2022-11-15 |
Family
ID=70780548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010023860.2A Active CN111204814B (zh) | 2020-01-09 | 2020-01-09 | 一种棒状结构硫铁钠材料及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111204814B (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114429865A (zh) * | 2022-01-10 | 2022-05-03 | 重庆文理学院 | 一种镍丝/三氧化二铁/二氧化锰复合纤维的制备方法 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603856A (zh) * | 2018-11-07 | 2019-04-12 | 东北师范大学 | 由废水制备Erdite棒状颗粒应用于水处理的方法 |
-
2020
- 2020-01-09 CN CN202010023860.2A patent/CN111204814B/zh active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603856A (zh) * | 2018-11-07 | 2019-04-12 | 东北师范大学 | 由废水制备Erdite棒状颗粒应用于水处理的方法 |
Non-Patent Citations (2)
| Title |
|---|
| FENG HUANG等: ""Synthesis of NaFeS2 Nanorods by Solvothermal Technique"", 《ADVANCED MATERIALS RESEARCH》 * |
| 王延来等: "《新材料研究系列丛书 太阳电池光吸收层铜基薄膜的制备技术研究》", 30 April 2019 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114429865A (zh) * | 2022-01-10 | 2022-05-03 | 重庆文理学院 | 一种镍丝/三氧化二铁/二氧化锰复合纤维的制备方法 |
| CN114429865B (zh) * | 2022-01-10 | 2023-10-13 | 重庆文理学院 | 一种镍丝/三氧化二铁/二氧化锰复合纤维的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111204814B (zh) | 2022-11-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101662021B (zh) | 一种纳米包覆的正极材料及其二次铝电池的制备方法 | |
| Deng et al. | Ultrathin cobalt nickel selenides (Co0. 5Ni0. 5Se2) nanosheet arrays anchoring on Ti3C2 MXene for high-performance Na+/K+ batteries | |
| CN113410440B (zh) | 一种二硒化钴@多孔氮掺杂碳纳米复合材料、钾离子电池及其制备方法 | |
| CN105514378B (zh) | 一种仿细胞结构锂硫电池正极复合材料及其制备方法 | |
| CN107026256B (zh) | 一种热电池正极材料FexCo1-xS2粉体及其制备方法 | |
| CN108832114B (zh) | 一种石墨烯包覆CuFeO2复合负极材料的制备方法 | |
| CN101662022A (zh) | 一种负极材料的纳米包覆及其二次铝电池制备方法 | |
| CN107204437A (zh) | 一种锂硒电池正极材料的制备方法 | |
| WO2018095202A1 (zh) | 一种复合锂电池及其制备方法 | |
| CN110311111B (zh) | N掺杂CNT原位包覆Co纳米颗粒复合材料及制备与应用 | |
| CN112010291B (zh) | 一种镍掺杂二硫化钼/石墨烯三维复合材料的制备方法及应用 | |
| CN111056544B (zh) | 一种磷酸铁钠复合材料及其制备方法、应用 | |
| CN114639809B (zh) | 一种复合硬碳负极材料、制备方法及应用 | |
| CN111196600A (zh) | 一种空心球状结构磷酸铁材料及其制备方法 | |
| CN116281922A (zh) | 富钠型氟掺杂焦磷酸磷酸铁钠复合材料及制备方法和应用 | |
| CN111204814B (zh) | 一种棒状结构硫铁钠材料及其制备方法 | |
| CN108321390B (zh) | 三维花状单晶磷酸铁锂及其制备方法 | |
| Fu et al. | One-step hydrothermal synthesis of CoNi bimetallic phosphide nanoflowers for high-performance quasi-solid-state zinc-ion batteries | |
| Zeng et al. | Nano-Ni/Co-PBA as high-performance cathode material for aqueous sodium-ion batteries | |
| CN111816853B (zh) | CuS-Cu7.2S4纳米复合材料、锂电池及制备方法 | |
| CN107611420A (zh) | 一种锂电池纳米电极材料LiNaV2O6及其制备方法 | |
| CN1564347A (zh) | 一种锂离子电池复合正极材料及其制备方法 | |
| CN112960663A (zh) | 一种LiFeXCo1-XPO4/N-C/CC复合材料的制备方法 | |
| CN106935842B (zh) | 电镀硒的镀液、锂硒电池正极材料及锂硒电池 | |
| CN103117385B (zh) | 一种缺陷结构LiFePO4表面改性富锂层-层正极材料及制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230330 Address after: No. 1088, Xueyuan Avenue, Taoyuan Street, Nanshan District, Shenzhen City, Guangdong Province Patentee after: Southern University of Science and Technology Address before: Taizhou building, No. 1088, Xueyuan Avenue, Xili University Town, Nanshan District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN THIRD GENERATION SEMICONDUCTOR Research Institute |