CN114538517A - 一种Mo2C和碳包夹的钼基异质结构材料及其制备方法和应用 - Google Patents
一种Mo2C和碳包夹的钼基异质结构材料及其制备方法和应用 Download PDFInfo
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- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 68
- 239000011733 molybdenum Substances 0.000 title claims abstract description 68
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910003178 Mo2C Inorganic materials 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
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- 238000000034 method Methods 0.000 claims abstract description 12
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
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- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- 229910001415 sodium ion Inorganic materials 0.000 claims description 5
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 4
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- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 4
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 4
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- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 3
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
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- ZKXBDPZAQUNPOY-UHFFFAOYSA-N 1-azaniumylhexylazanium;hexanedioate Chemical compound CCCCCC(N)N.OC(=O)CCCCC(O)=O ZKXBDPZAQUNPOY-UHFFFAOYSA-N 0.000 claims description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 2
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- 230000001351 cycling effect Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
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- 239000006230 acetylene black Substances 0.000 description 4
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- 239000000047 product Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
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- 238000001000 micrograph Methods 0.000 description 2
- -1 molybdenum ions Chemical class 0.000 description 2
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- 239000002245 particle Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- GZIJWFRSBSKSQT-UHFFFAOYSA-N [Mo](=O)=O.[Mo](=O)(=O)=O Chemical compound [Mo](=O)=O.[Mo](=O)(=O)=O GZIJWFRSBSKSQT-UHFFFAOYSA-N 0.000 description 1
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- 239000013590 bulk material Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
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- 239000001569 carbon dioxide Substances 0.000 description 1
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- 238000010168 coupling process Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
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- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Images
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
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Abstract
本发明公开了一种Mo2C和碳包夹的钼基异质结构材料及其制备方法和应用,通过表面原位生长的方式在Mo2CTX表面构筑钼基材料,然后在上述材料表面将聚合物碳化,得到Mo2C和碳包夹的钼基异质结构材料。该材料具有二维片状结构自组装形成的三维结构,通过在钼基材料两侧分别引入高导电性Mo2C和碳构筑夹层状钼基异质结构,不仅可提高该异质结构材料的导电性,还可缓冲该异质结构材料在充放电过程中的体积变化。
Description
技术领域
本发明涉及新材料技术领域,具体涉及一种Mo2C和碳包夹的钼基异质结构材料及其制备方法和应用。
背景技术
锂离子电池具有能量密度高、循环寿命长、环境友好等优点备受关注。然而,商业化石墨负极的比容量较低,限制了高能量密度锂离子电池的开发。钼基材料具有比容量高、价格低廉等优点,被认为是有望替代石墨负极的候选材料之一。然而,钼基材料导电性差、充放电过程中体积膨胀大等缺点限制了其工业化应用。
目前通常通过将钼基材料纳米化以缩短离子扩散路径,从而提高其电化学动力学,然而充过电过程中纳米材料的团聚和体积膨胀仍然难以避免。将钼基材料与其他导电性物质复合,可明显改善钼基材料的导电性,从而提高材料的电化学性能。然而,受限于钼基材料本身较低的导电性,往往离子的嵌入和脱出仅发生在材料表面,体相材料中离子的嵌入和脱出仍然受限。
通过耦合不同结构的材料构筑异质结构,可改善材料的电子结构并提升材料的导电性,因而异质结构电极材料引起了研究者的广泛关注。如申请号为CN202010358796.3的专利文件公开了一种三氧化钼-二氧化钼异质结构复合体,该复合材料表现出卓越的电化学性能。MXene作为一种新型的二维材料,表面具有丰富的官能团,可为纳米材料的原位生长提供场所;同时其较高的导电性也可提升电极材料的导电性。再如申请号为CN201910377882.6的专利文件公开了一种表面均匀负载赝电容型过度金属氧化物纳米颗粒的碳包MXene二维纳米薄片,该二维材料作为钠离子电池负极时,具有较高的比容量、优异的循环性能和倍率性能。然而将过度金属氧化物纳米颗粒负载于导电基体表面仍难以解决材料在充放电过程中的体积膨胀、颗粒破碎现象。若构筑三明治状夹层结构,可明显抑制电极材料在充放电过程中的体积膨胀和颗粒破碎现象,从而提升材料的电化学性能。
发明内容
本发明的目的是为解决上述技术问题及不足,提供一种Mo2C和碳包夹的钼基异质结构材料及其制备方法和应用,该材料具有二维片状结构自组装形成的三维结构,通过在钼基材料两侧分别引入高导电性Mo2C和碳构筑夹层状钼基异质结构,不仅可提高该异质结构材料的导电性,还可缓冲该异质结构材料在充放电过程中的体积变化。
本发明为解决上述技术问题的不足,所采用的技术方案是:一种Mo2C和碳包夹的钼基异质结构材料的制备方法:通过表面原位生长的方式在Mo2CTX表面构筑钼基材料,然后在上述材料表面将聚合物碳化,得到Mo2C和碳包夹的钼基异质结构材料。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:具体包括以下步骤:
S1、将钼源和络合剂溶于Mo2CTx分散液中,经水热处理后,过滤、干燥得到中间产物A;
S2、将中间产物A溶于引发剂溶液,搅拌均匀并加入聚合物单体,然后在搅拌条件下进行聚合反应,反应结束后,过滤、干燥得到中间产物B;
S3、将中间产物B进行焙烧处理,即得到Mo2C和碳包夹的钼基异质结构材料。
作为本发明一种含Mo2C的钼基异质结构材料的制备方法的进一步优化:所述钼源为钼酸铵、钼酸盐、钼酸或磷钼酸中的一种或几种,络合剂为三聚氰胺、苯胺、硫脲、植酸、乙二胺、已二酸已二胺、2-甲基咪唑、对苯二甲酸或尿素中的一种或几种。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:所述步骤S1中钼源、络合剂与Mo2CTX的加入质量比为1:0.1-10:0.1-2。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:所述引发剂为三羟甲基氨基甲烷、三氯化铁、过硫酸盐、重铬酸盐或双氧水中的一种或几种,所述聚合物单体为盐酸多巴胺、苯胺、吡咯或噻吩中的一种或几种。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:所述步骤S2中中间产物A、引发剂和聚合物单体的加入质量比为1:1-30:1-20。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:所述水热处理的条件为:在100-200℃温度下处理时间2-40h。
作为本发明一种Mo2C和碳包夹的钼基异质结构材料的制备方法的进一步优化:所述焙烧处理的条件为:在气氛保护下,以0.5-10℃/min的升温速率升温至300-900℃焙烧0.1-12h。
一种Mo2C和碳包夹的钼基异质结构材料,由上述制备方法得到,该材料由Mo2C负载的碳包覆钼基纳米颗粒组成,具有二维片状结构自组装形成的三维结构,二维纳米片厚度为10-300nm。
一种Mo2C和碳包夹的钼基异质结构材料在制备锂离子电池和钠离子电池的负极材料方面的应用。
本发明具有以下有益效果:
1、本发明钼基异质结构材料中的Mo2C和碳可提高钼基材料的分散性,并将钼基材料纳米化,缩短离子扩散路径,从而有利于离子扩散过程。
2、本发明钼基异质结构材料中的Mo2C和碳为钼基材料提供了额外的离子存储位点,有利于提升复合材料的储锂容量。
3、本发明钼基异质结构材料中Mo2C和碳夹层的存在还可提高该异质结构材料的导电性,促进电化学动力学的提升;缓冲该异质结构材料在充放电过程中的体积变化,提升材料的循环稳定性。
附图说明
图1为实施例1制备得到钼基异质结构材料的扫描电镜图;
图2为实施例2制备得到钼基异质结构材料的扫描电镜图;
图3为实施例1和实施例2制备得到钼基异质结构材料的X射线衍射图;
图4为试验电池1在50mAh/g电流密度下的充放电曲线;
图5为试验电池2和3的500mAh/g循环曲线;
图6为试验电池4和5的倍率曲线及其1000mAh/g循环曲线。
具体实施方式
下面将结合具体实施例,对本发明的技术方案进行清楚、完整地描述。
一种Mo2C和碳包夹的钼基异质结构材料的制备方法,包括以下步骤:
S1、将钼源、络合剂溶于20-100mL一定浓度的Mo2CTX分散液中,所得溶液于100-200℃水热处理2-40h。用去离子水过滤至滤液呈中性后,将所得固体在40-100℃干燥10-40h。其中钼离子在溶液中的浓度为1-15mg/mL。
S2、将0.1-2g上述固体溶于30-600mL浓度为5mmol/L-1mol/L的引发剂溶液中搅拌0.1-12h,并加入0.1-2g聚合物单体。在搅拌条件下,聚合2-48h后,用去离子水过滤悬浊液至滤液为中性,所得固体在40-150℃干燥2-48h。最后将固体置于管式炉中,在气氛保护下,以0.5-10℃/min的升温速率升温至300-900℃焙烧0.1-12h。
所述的煅烧气氛为氩气、氮气、氢气、氨气或二氧化碳中的一种或几种。
所述的Mo2CTX分散液(Tx代表表面官能团,T=O2-,F-,OH-)可购买也可通过如下方法制备:将0.1-5g的Mo2Ga2C加入到浓度为20-50%的HF中,其中Mo2Ga2C与HF的质量比为1:(20-60)。上述混合物于40-100℃搅拌20-200h。用去离子水过滤至滤液呈中性后,将所得固体超声分散到四甲基氢氧化铵或二甲基亚砜中,室温搅拌1-50h;固体与四甲基氢氧化铵或二甲基亚砜的质量比为1:(5-50)。去离子水洗涤至中性后,得到Mo2CTX粉末。按照0.1-5mg/mL的浓度将制备的Mo2CTX超声分散入水中,得到Mo2CTX分散液。
Mo2C和碳包夹的钼基异质结构材料在制备锂离子电池和钠离子电池的负极材料方面的应用:以质量比为Mo2C和碳包夹的钼基结构电极材料:乙炔黑:聚偏氟乙烯=(7-9):(0.5-2):(0.5-2)的比例制备浆料,并将浆料涂敷在铜箔上,经干燥、切片之后得到电极片。在手套箱中以上述电极片为负极组装锂/钠离子电池。
实施例1
将200mg钼酸铵、100mg三聚氰胺溶于30mL浓度为2.5mg/mL的Mo2CTX分散液中,所得溶液于120℃水热处理12h。用去离子水过滤至滤液呈中性后,将所得固体在60℃干燥24h。将0.2g上述固体溶于60mL浓度为10mmol/L的三羟甲基氨基甲烷溶液中搅拌0.2h,并加入0.2g盐酸多巴胺。在搅拌条件下,聚合12h后,用去离子水过滤悬浊液至滤液为中性,所得固体在80℃干燥12h。最后将固体置于管式炉中,在氩气氛保护下,以2℃/min的升温速率升温至600℃焙烧3h,得到Mo2C和碳包夹的钼基异质结构材料。
图1为制得产物的扫描电镜图,从图中可以看出该材料呈现出二维纳米片组成的三维球状形貌,二维纳米片的厚度大约为10nm左右。
制得产物的X射线衍射图见图3,图中给出了MoO2的标准卡片,样品的部分衍射图曲线与MoO2匹配良好,其余未匹配到的衍射峰为Mo2C的衍射峰;说明形成了含有Mo2C的MoO2异质结构材料。
实施例2
将400mg钼酸铵、200mg三聚氰胺溶于60mL浓度为2mg/mL的Mo2CTX分散液中,所得溶液于120℃水热处理12h。用去离子水过滤至滤液呈中性后,将所得固体在60℃干燥24h。将0.2g上述固体溶于60mL浓度为10mmol/L的三羟甲基氨基甲烷溶液中搅拌0.2h,并加入0.2g盐酸多巴胺。在搅拌条件下,聚合12h后,用去离子水过滤悬浊液至滤液为中性,所得固体在100℃干燥12h。最后将固体置于管式炉中,在氩气气氛保护下,以2℃/min的升温速率升温至600℃焙烧3h,得到Mo2C和碳包夹的钼基异质结构材料。
图2为制得产物的扫描电镜图,从图中可以看出该材料呈现出二维纳米片组成的三维扇形形貌,二维纳米片的厚度大约为20-100nm左右。
制得产物的X射线衍射图见图3,图中给出了MoO2的标准卡片,样品的部分衍射图曲线与MoO2匹配良好,其余未匹配到的衍射峰为Mo2C的衍射峰;说明形成了含有Mo2C的MoO2异质结构材料。
<性能试验1>
按照重量比为7:2:1的比例取实施例1制得的电极材料、乙炔黑以及聚偏氟乙烯制备浆料,并将浆料涂敷在铜箔上,经干燥、切片之后得到电极片。在手套箱中以上述电极片为负极组装锂离子电池,制得试验电池1。
在50mAh/g电流密度下试验电池1的充放电性能,图4中给出了试验电池1前三次充放电过程中的充放电曲线,其首次放电容量为733.5mAh/g,首次库伦效率为73.5%,具有高容量、高首效的特点;第二圈和第三圈的充放电曲线重合,说明材料具有较高的电化学可逆性。
<性能试验2>
按照重量比为7:2:1的比例分别取实施例1和实施例2制得的电极材料、乙炔黑以及聚偏氟乙烯制备浆料,并将浆料涂敷在铜箔上,经干燥、切片之后得到电极片。在手套箱中以上述电极片为负极组装锂离子电池,得到试验电池2和试验电池3。
测试电池在500mAh/g条件下的循环性能,图5为试验电池2和试验电池3在500mAh/g条件下的循环曲线。从曲线上可以看出,试验电池2在500mAh/g的电流密度下循环500次,比容量为854.5mAh/g,试验电池3在500mAh/g的电流密度下循环500次,比容量为565.9mAh/g,由此可以看出,本发明的材料具有良好的充放电稳定性(容量稳定),说明该异质结构可以明显改善材料的充放电结构稳定性,并抑制材料充放电过程中的膨胀。
<性能试验3>
按照重量比为7:2:1的比例分别取实施例1和实施例2制得的电极材料、乙炔黑以及聚偏氟乙烯制备浆料,并将浆料涂敷在铜箔上,经干燥、切片之后得到电极片。在手套箱中以上述电极片为负极组装锂离子电池,得到试验电池4和试验电池5。
测试电池在1000mAh/g条件下的循环性能,图6为试验电池4和试验电池5的倍率曲线和在1000mAh/g条件下的循环曲线。从曲线上可以看出,试验电池4在1000mAh/g的电流密度下循环1000次,比容量为640.9mAh/g,试验电池5在1000mAh/g的电流密度下循环1000次,比容量为475.8mAh/g,由此可以看出,本发明的材料具有良好的充放电稳定性(容量稳定)和倍率性能,说明该异质结构具有较高的导电性,可以大电流放电。
实施例3
将400mg钼酸铵、200mg硫脲溶于30mL浓度为3mg/mL的Mo2CTX分散液中,所得溶液于180℃水热处理24h。用去离子水过滤至滤液呈中性后,将所得固体在80℃干燥30h。将0.5g上述固体溶于80mL浓度为0.5mol/L的过硫酸铵溶液中搅拌0.2h,并加入0.5g苯胺。在搅拌条件下,聚合12h后,用去离子水过滤悬浊液至滤液为中性,所得固体在120℃干燥24h。最后将固体置于管式炉中,在氩气气氛保护下,以1℃/min的升温速率升温至800℃焙烧5h,得到Mo2C和碳包夹的钼基异质结构材料。
实施例4
将200mg钼酸钠、200mg植酸溶于30mL浓度为1mg/mL的Mo2CTX分散液中,所得溶液于200℃水热处理40h。用去离子水过滤至滤液呈中性后,将所得固体在100℃干燥20h。将0.2g上述固体溶于30mL浓度为1molL-1的三氯化铁溶液中搅拌0.2h,并加入0.3g噻吩。在搅拌条件下,聚合12h后,用去离子水过滤悬浊液至滤液为中性,所得固体在100℃干燥12h。最后将固体置于管式炉中,在氩气气氛保护下,以0.5℃/min的升温速率升温至700℃焙烧2h,得到Mo2C和碳包夹的钼基异质结构材料。
实施例5
将200mg钼酸、200mg苯胺溶于30mL浓度为1mg/mL的Mo2CTX分散液中,所得溶液于120℃水热处理40h。用去离子水过滤至滤液呈中性后,将所得固体在60℃干燥12h。将0.2g上述固体溶于60mL浓度为1mol/L的重铬酸钾溶液中搅拌2h,并加入0.3g吡咯。在搅拌条件下,聚合24h后,用去离子水过滤悬浊液至滤液为中性,所得固体在60℃干燥24h。最后将固体置于管式炉中,在氩气气氛保护下,以0.5℃/min的升温速率升温至600℃焙烧2h,得到Mo2C和碳包夹的钼基异质结构材料。
实施例6
将200mg钼酸、100mg苯胺、100mg对苯二甲酸溶于30mL浓度为1mg/mL的Mo2CTX分散液中,所得溶液于120℃水热处理40h。用去离子水过滤至滤液呈中性后,将所得固体在60℃干燥12h。将0.2g上述固体溶于60mL浓度为1mol/L的双氧水中搅拌2h,并加入0.3g吡咯。在搅拌条件下,聚合24h后,用去离子水过滤悬浊液至滤液为中性,所得固体在60℃干燥24h。最后将固体置于管式炉中,在氩气气氛保护下,以0.5℃/min的升温速率升温至900℃焙烧2h,得到Mo2C和碳包夹的钼基异质结构材料。
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变形或修改,这并不影响本发明的实质内容。
Claims (10)
1.一种Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:通过表面原位生长的方式在Mo2CTX表面构筑钼基材料,然后在上述材料表面将聚合物碳化,得到Mo2C和碳包夹的钼基异质结构材料。
2.如权利要求1所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:具体包括以下步骤:
S1、将钼源和络合剂溶于Mo2CTx分散液中,经水热处理后,过滤、干燥得到中间产物A;
S2、将中间产物A溶于引发剂溶液,搅拌均匀并加入聚合物单体,然后在搅拌条件下进行聚合反应,反应结束后,过滤、干燥得到中间产物B;
S3、将中间产物B进行焙烧处理,即得到Mo2C和碳包夹的钼基异质结构材料。
3.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述钼源为钼酸铵、钼酸盐、钼酸或磷钼酸中的一种或几种,络合剂为三聚氰胺、苯胺、硫脲、植酸、乙二胺、已二酸已二胺、2-甲基咪唑、对苯二甲酸或尿素中的一种或几种。
4.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述步骤S1中钼源、络合剂与Mo2CTx的加入质量比为1:0.1-10:0.1-2。
5.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述引发剂为三羟甲基氨基甲烷、三氯化铁、过硫酸盐、重铬酸盐或双氧水中的一种或几种,所述聚合物单体为盐酸多巴胺、苯胺、吡咯或噻吩中的一种或几种。
6.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述步骤S2中中间产物A、引发剂和聚合物单体的加入质量比为1:1-30:1-20。
7.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述水热处理的条件为:在100-200℃温度下处理时间2-40h。
8.如权利要求2所述Mo2C和碳包夹的钼基异质结构材料的制备方法,其特征在于:所述焙烧处理的条件为:在气氛保护下,以0.5-10℃/min的升温速率升温至300-900℃焙烧0.1-12h。
9.权利要求1-8中任一权利要求所述制备方法得到的Mo2C和碳包夹的钼基异质结构材料,其特征在于:该材料由Mo2C负载的碳包覆钼基纳米颗粒组成,具有二维片状结构自组装形成的三维结构,二维纳米片厚度为10-300nm。
10.如权利要求9所述Mo2C和碳包夹的钼基异质结构材料在制备锂离子电池和钠离子电池的负极材料方面的应用。
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