CN109604626B - 一种锡负极材料的制备方法 - Google Patents
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000010405 anode material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 5
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 3
- AFVFQIVMOAPDHO-UHFFFAOYSA-M Methanesulfonate Chemical compound CS([O-])(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-M 0.000 claims abstract 2
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 6
- 239000010406 cathode material Substances 0.000 abstract description 6
- 239000010949 copper Substances 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910009819 Ti3C2 Inorganic materials 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 229910019762 Nb4C3 Inorganic materials 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 2
- 229910017052 cobalt Inorganic materials 0.000 abstract description 2
- 239000010941 cobalt Substances 0.000 abstract description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 2
- 239000004332 silver Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- QWJYDTCSUDMGSU-UHFFFAOYSA-N [Sn].[C] Chemical compound [Sn].[C] QWJYDTCSUDMGSU-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 241000255789 Bombyx mori Species 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- WSSMOXHYUFMBLS-UHFFFAOYSA-L iron dichloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Fe+2] WSSMOXHYUFMBLS-UHFFFAOYSA-L 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- AICMYQIGFPHNCY-UHFFFAOYSA-J methanesulfonate;tin(4+) Chemical compound [Sn+4].CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O AICMYQIGFPHNCY-UHFFFAOYSA-J 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BJDDAXVXMQYXHL-UHFFFAOYSA-J tris(ethylsulfonyloxy)stannyl ethanesulfonate Chemical compound [Sn+4].CCS([O-])(=O)=O.CCS([O-])(=O)=O.CCS([O-])(=O)=O.CCS([O-])(=O)=O BJDDAXVXMQYXHL-UHFFFAOYSA-J 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
本发明涉及一种锡负极材料的制备方法,以二维材料为载体,以可溶性双金属盐为原料,水解共沉积、干燥、烧结、高温还原,制备锡负极材料;二维材料为Ti3C2,MoNb2SnC2,Ti2C,Ti3CN,Nb2C,Nb4C3,(Ti0.5Nb0.5)2C,(V0.5Cr0.5)3C2的一种或多种;双金属盐包括可溶性的锡盐和辅助金属盐;锡源为氯化锡、氯化亚锡、硝酸亚锡、磺酸锡、甲基磺酸锡、乙基磺酸锡的一种;辅助金属盐为镍、铜、银、铁、钴、锑的可溶性氯盐、硝酸盐、醋酸盐、硫酸盐、溴盐的一种;辅助金属与锡的摩尔比为0.05~1.5;二维材料与锡的质量比0.1~10;该负极材料具有很好的电化学性能,在锂离子电池领域具有很好的应用前景。
Description
技术领域
本发明涉及储能领域,具体涉及一种锡负极材料的制备方法。
背景技术
锡具有理论容量高、成本低、低毒、应用广等优点,是非常有发展前景的锂离子电池负极材料。但锡在充放电过程中,体积膨胀、收缩,导致电极材料粉化,影响了锡材料的循环性能和应用。专利1(金周,俞海龙,黄学杰。一种复合包覆的纳米锡负极材料及其制备方法和应用,申请号2017113176636.)采用纳米铜和碳协同包覆纳米锡,避免纳米锡与电解液的直接接触,形成稳定的SEI、增加电极的导电性,该材料作为锂离子电池负极材料时,具有优异的电化学性能。专利2(吴孟强,陈治,单双,徐自强等。生物质碳-锡储能材料及其制备方法,201810028108X)提供一种生物质碳-锡储能材料及其制备方法,以蚕沙为载体,通过四氯化锡水解沉积二氧化锡,然后高温碳化,生成碳-锡材料;该材料比现有的石墨类负极材料拥有更高的比容量。
二维材料MXenen具有优异的稳定性、较大的比表面积和机械性能,可作为纳米金属氧化物的良好载体。二维材料还具有良好的导电性和层状结构,可作为锂离子电池负极材料。专利3(罗剑敏,金成滨,陶新永等。一种氧化物柱撑MXene复合材料及其应用,申请号201610733989.6)和专利4(张炳森,李浩杰,鲁铭等。一种MXene/双金属氧化物复合材料及其制备方法和锂离子电池负极材料,申请号201810466140.6)介绍了MXene/氧化物复合材料具有较好的电化学性能和循环性能。但二维材料MXenen电化学容量低,而纳米氧化物作为电极材料时,在首次充放电时,存在较大的不可逆容量。
发明内容
本发明目的在于提供一种锡负极材料的制备方法,克服现有制备技术的缺陷,提高锡负极的电化学容量。为实现上述发明目的,本发明的技术方案是:以二维材料为载体,以可溶性双金属盐为原料,水解共沉积、干燥、烧结、高温还原,制备锡负极材料;二维材料为Ti3C2,MoNb2SnC2,Ti2C,Ti3CN,Nb2C,Nb4C3,(Ti0.5Nb0.5)2C,(V0.5Cr0.5)3C2的一种或多种;双金属盐包括可溶性的锡盐和辅助金属盐;锡源为氯化锡、氯化亚锡、硝酸亚锡、磺酸锡、甲基磺酸锡、乙基磺酸锡的一种;辅助金属盐为镍、铜、银、铁、钴、锑的可溶性氯盐、硝酸盐、醋酸盐、硫酸盐、溴盐的一种;辅助金属与锡的摩尔比为0.05~1.5;二维材料与锡的质量比0.1~10;一种锡负极材料的制备方法包括:
1)称量一定质量的二维材料、辅助金属盐、锡盐和表面活性剂,浸入乙醇水溶液;搅拌1~10h,超声波0.5~5h;
2)在步骤1)的产物中加入碱溶液,搅拌1~20h,离心、分离、洗涤、烘干;
3)将步骤2)的产物放入气氛炉中抽真空烧结,烧结温度为200~500℃,烧结时间为1~20h;
4)将步骤3)中的产物,粉碎、碾磨,再放入气氛炉中高温还原,还原温度500~1000℃、搁置时间1~20h,还原气体为氢氩混合气、氢氮混合气、一氧化碳和氩气混合气、一氧化碳和氮气混合气、氢气和甲醇混合气、一氧化碳和甲醇混合气的一种;
5)将步骤4)中的产物,粉碎、碾磨,获得锡负极材料。
与现有锡负极材料制备技术相比,本发明具有如下优点:
1)本发明工艺简单、操作方便,有利于工业化生产。
2)本发明将二维材料与锡合金复合,提高了锡合金的电化学容量和循环寿命。
3)本发明以二维材料为载体,均匀分散纳米金属氧化物;以还原性气体与金属氧化物反应,并高温烧结获得纳米合金;二维材料和辅助金属协同提高了锡的电化学性能。因此该方法制备的锡负极在锂离子电池领域具有很好的应用前景。
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,并详细说明如下:
实施例1
一种锡负极材料的成分设计:
1)MoNb2SnC2,0.236g;SnCl4,0.04mol,Ni(CH3COO)2.4H2O,0.015mol
一种锡负极材料的制备方法:
1)称量一定质量的MoNb2SnC2、Ni(CH3COO)2.4H2O、SnCl4和表面活性剂,浸入乙醇水溶液;搅拌2h,超声波1h;
2)在步骤1)的产物中加入氢氧化钠溶液,搅拌3h,离心、分离、洗涤、烘干;
4)将步骤2)的产物放入气氛炉中抽真空烧结,烧结温度为300℃,烧结时间为3h;
4)将步骤3)中的产物,粉碎、碾磨,再放入气氛炉中、氢氩混合气、还原温度800℃、搁置时间5h;
5)将步骤4)中的产物,粉碎、碾磨,获得锡负极材料。
该材料用于锂离子电池负极时,具有很好的电化学性能。
实施例2
一种锡负极材料的成分设计:
2)Ti3C2,0.3g;SnCl2,0.01mol,NiCl2.6H2O,0.075mol
一种锡负极材料的制备方法:
1)称量一定质量的Ti3C2、NiCl2.6H2O、SnCl2和表面活性剂,浸入乙醇水溶液;搅拌2h,超声波1h;
2)在步骤1)的产物中加入氢氧化钠溶液,搅拌3h,离心、分离、洗涤、烘干;
5)将步骤2)的产物放入气氛炉中抽真空烧结,烧结温度为250℃,烧结时间为3h;
4)将步骤3)中的产物,粉碎、碾磨,再放入气氛炉中、氢气和甲醇混合气、还原温度750℃、搁置时间5h;
5)将步骤4)中的产物,粉碎、碾磨,获得锡负极材料。
该材料用于锂离子负极时,具有很好的电化学性能。
实施例3
一种锡负极材料的成分设计:
3)Nb2C,0.15g;SnCl2,0.01mol,Cu(CH3COO)2·H2O,0.012mol
一种锡负极材料的制备方法:
1)称量一定质量的Nb2C、Cu(CH3COO)2·H2O、SnCl2和表面活性剂,浸入乙醇水溶液;搅拌3h,超声波0.5h;
2)在步骤1)的产物中加入氢氧化钠溶液,搅拌2h,离心、分离、洗涤、烘干;
6)将步骤2)的产物放入气氛炉中抽真空烧结,烧结温度为350℃,烧结时间为2h;
4)将步骤3)中的产物,粉碎、碾磨,再放入气氛炉中、氢气和氮气混合气、还原温度850℃、搁置时间10h;
5)将步骤4)中的产物,粉碎、碾磨,获得锡负极材料。
实施例4
同实施例2操作
一种锡负极材料的成分设计:
4)Ti2C,0.118g;SnCl2,0.01mol;FeCl2.4H2O,0.003mol;
5)Ti3CN,1.0g;(CH3SO3)2Sn,0.01mol;CoCl2.6H2O,0.015mol;
6)Nb4C3,5.0g;SnCl4,0.01mol;CoCl2.6H2O,0.002mol;
7)(Ti0.5Nb0.5)2C,2.0g;Sn(NO3)2,0.01mol;AgNO3,0.01mol;
该材料用于锂离子负极时,具有很好的电化学性能。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (1)
1.一种锡负极材料的制备方法,包括:
1)称量一定质量的MoNb2SnC2、辅助金属盐、锡盐和表面活性剂,浸入乙醇水溶液;搅拌1~10h,超声波0.5~5 h;锡源为氯化锡、氯化亚锡、硝酸亚锡、磺酸锡、甲基磺酸锡、乙基磺酸锡的一种;辅助金属盐为锑的可溶性氯盐、硝酸盐、醋酸盐、硫酸盐、溴盐的一种;辅助金属与锡的摩尔比为0.05~1.5;二维材料与锡的质量比0.1~10;
2)在步骤1)的产物中加入碱溶液,搅拌1~20h,离心、分离、洗涤、烘干;
3)将步骤2)的产物放入气氛炉中抽真空烧结,烧结温度为200~500℃,烧结时间为1~20 h;
4)将步骤3)中的产物,粉碎、碾磨,再放入气氛炉中高温还原,还原温度750~1000℃、搁置时间1~20 h,还原气体为氢气和甲醇混合气、一氧化碳和甲醇混合气的一种;
5)将步骤4)中的产物,粉碎、碾磨,获得锡负极材料。
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Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012142257A (ja) * | 2010-12-14 | 2012-07-26 | Dowa Holdings Co Ltd | 二次電池用電極材およびその製造方法 |
CN102800849A (zh) * | 2012-07-23 | 2012-11-28 | 浙江大学 | 过渡金属锡化物/石墨烯复合材料及其制备方法和应用 |
CN103178248A (zh) * | 2013-04-18 | 2013-06-26 | 厦门大学 | 锂离子电池锡-钴合金负极材料的制备方法 |
CN103715406A (zh) * | 2014-01-13 | 2014-04-09 | 中国科学院宁波材料技术与工程研究所 | 一种锡基合金-碳复合负极活性材料的制备及应用 |
CN104064739A (zh) * | 2014-07-02 | 2014-09-24 | 长沙国容新能源有限公司 | 锡钴合金/石墨烯复合材料及其制备方法 |
CN104143632A (zh) * | 2014-07-30 | 2014-11-12 | 吉林大学 | 一种锡基铁碳复合锂电池负极材料、制备方法及应用 |
CN104868104A (zh) * | 2015-03-27 | 2015-08-26 | 浙江工业大学 | 一种二维层状碳化钛/金属离子复合材料及其应用 |
WO2016012275A1 (en) * | 2014-07-22 | 2016-01-28 | Basf Se | Composites comprising mxenes for cathodes of lithium sulfur cells |
CN105470486A (zh) * | 2015-12-25 | 2016-04-06 | 陕西科技大学 | 颗粒状二氧化锡/二维纳米碳化钛复合材料的制备方法 |
WO2017044262A1 (en) * | 2015-09-08 | 2017-03-16 | Drexel University | Improved routes to mx-ene carbides |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104022270B (zh) * | 2014-06-10 | 2016-07-06 | 中国计量学院 | 一种镍锡合金/碳复合电极材料的制备方法 |
CN105720246B (zh) * | 2015-12-25 | 2019-05-24 | 陕西科技大学 | 颗粒状二氧化锡/二维纳米碳化钛复合材料及应用 |
CN105870421A (zh) * | 2016-05-31 | 2016-08-17 | 陕西科技大学 | 一种C-SnO2/Ti3C2二维纳米锂离子电池负极材料及其制备方法 |
CN106229488B (zh) * | 2016-08-26 | 2019-01-08 | 浙江工业大学 | 一种氧化物柱撑MXene复合材料及其应用 |
-
2018
- 2018-12-06 CN CN201811484147.7A patent/CN109604626B/zh not_active Expired - Fee Related
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012142257A (ja) * | 2010-12-14 | 2012-07-26 | Dowa Holdings Co Ltd | 二次電池用電極材およびその製造方法 |
CN102800849A (zh) * | 2012-07-23 | 2012-11-28 | 浙江大学 | 过渡金属锡化物/石墨烯复合材料及其制备方法和应用 |
CN103178248A (zh) * | 2013-04-18 | 2013-06-26 | 厦门大学 | 锂离子电池锡-钴合金负极材料的制备方法 |
CN103715406A (zh) * | 2014-01-13 | 2014-04-09 | 中国科学院宁波材料技术与工程研究所 | 一种锡基合金-碳复合负极活性材料的制备及应用 |
CN104064739A (zh) * | 2014-07-02 | 2014-09-24 | 长沙国容新能源有限公司 | 锡钴合金/石墨烯复合材料及其制备方法 |
WO2016012275A1 (en) * | 2014-07-22 | 2016-01-28 | Basf Se | Composites comprising mxenes for cathodes of lithium sulfur cells |
CN104143632A (zh) * | 2014-07-30 | 2014-11-12 | 吉林大学 | 一种锡基铁碳复合锂电池负极材料、制备方法及应用 |
CN104868104A (zh) * | 2015-03-27 | 2015-08-26 | 浙江工业大学 | 一种二维层状碳化钛/金属离子复合材料及其应用 |
WO2017044262A1 (en) * | 2015-09-08 | 2017-03-16 | Drexel University | Improved routes to mx-ene carbides |
CN105470486A (zh) * | 2015-12-25 | 2016-04-06 | 陕西科技大学 | 颗粒状二氧化锡/二维纳米碳化钛复合材料的制备方法 |
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