CN109037652A - 一种氮掺杂碳包覆分等级锗结构的制备方法及应用 - Google Patents
一种氮掺杂碳包覆分等级锗结构的制备方法及应用 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 28
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000005253 cladding Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011701 zinc Substances 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 21
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- BEAZKUGSCHFXIQ-UHFFFAOYSA-L zinc;diacetate;dihydrate Chemical class O.O.[Zn+2].CC([O-])=O.CC([O-])=O BEAZKUGSCHFXIQ-UHFFFAOYSA-L 0.000 claims description 3
- 241000208340 Araliaceae Species 0.000 claims description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 2
- 235000008434 ginseng Nutrition 0.000 claims description 2
- 238000007599 discharging Methods 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 229910010633 Li22Ge5 Inorganic materials 0.000 description 1
- 229910002986 Li4Ti5O12 Inorganic materials 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
本发明提供了一种氮掺杂碳包覆分等级锗结构的制备方法及应用,该方法工艺简单,成本廉价,重现性好,性能优异。本发明首先合成了锗酸锌,然后在浓硝酸中反应获得分等级椭圆形GeO2,最后在氮气氛围下煅烧获得氮掺杂碳包覆分等级锗。所制备的Ge@NC作锂离子电池负极,得到的锂离子电池具有很高的比容量和循环稳定性,在电流密度为1A/g时充放电循环300圈容量稳定在1067.9 mAh/g。同时表现出优异的倍率放电性能,即使在电流密度为20 A/g时其充放电容量也能稳定在605.0 mAh/g。
Description
技术领域
本发明属于锂离子电池领域,具体涉及一种氮掺杂碳包覆分等级锗结构的制备方法及应用。
背景技术
90年代初,Sony公司首先发研制出以碳材料为负极,以LiCoO2作正极的锂电池。该电池在充放电过程中,没有金属锂的存在,只有锂离子,又称为锂离子电池。但是要得到循环性能好,比容量高,大电流充放电性能好的锂离子电池负极材料一直以来是科学家的研究重点。现在常用的负极材料有金属锂、碳材料、硅材料、TiO2和Li4Ti5O12等。金属锂和碳材料存在安全性能隐患和倍率性能差等缺点。Ge单质相比于Si单质,价格相对较高,并且理论容量相对较低,为1623 mAh/g(Li22Ge5),但比碳负极材料高出许多。该材料具有较高的电子导电率,比Si负极材料高4个数量级,同时,还具有较高的锂离子扩散率,室温下是Si负极材料的400倍。因此,Ge也是很有潜力的高能锂离子负极材料。
目前还未有制备用氮掺杂的碳包覆的分等级Ge颗粒的相关专利报道。
发明内容
本发明的目的在于提供一种氮掺杂碳包覆分等级锗结构的制备及应用。本发明合成了分等级结构的锗,并进行了氮掺杂的碳包覆。所制备的Ge@NC作锂电池负极,得到的锂电池具有很高的比容量和循环稳定性,在电流密度为1A/g时充放电循环300圈容量稳定在1067.9 mAh/g。同时表现出优异的倍率放电性能,即使在电流密度为20 A/g时其充放电容量也能稳定在605.0 mAh/g。
为实现上述目的,本发明采用如下技术方案:
一种氮掺杂碳包覆分等级锗结构制备的方法,包括以下步骤:
(1)将0.52克GeO2,1.1克二水合醋酸锌,0.1克CTAB加入到20毫升水中,调节pH至8,移入50毫升的反应釜中,置于140℃的烘箱中,反应24小时,将所得产品用水洗涤数次,烘干,将所得锗酸锌用适量的浓硝酸混合搅拌1h得到分等级椭圆形GeO2;
(2)将0.065克分等级椭圆形GeO2超声30min分散于50毫升甲醇中,再加入0.1克盐酸多巴胺,调节pH至8,室温搅拌24小时,无水乙醇洗涤后烘干,得到GeO2@PDA;
(3)将所得GeO2@PDA于700℃,N2气氛下煅烧3h后,再在体积浓度5%H2/95%Ar气氛下,于350℃煅烧1.5h,然后升温到650℃,煅烧2.5h,得到氮掺杂碳包覆分等级锗Ge@NC。
所述的氮掺杂碳包覆分等级锗在锂离子电池中的应用,该锂离子电池的制备方法为:按质量比Ge@NC:聚偏氟乙烯:乙炔黑=8:1:1混合研磨后均匀地涂在铜箔上做负极,参比电极和对电极均为金属锂,电解质为1M LiPF6的EC+DMC+EMC溶液,其中体积比EC/DMC/EMC=1/1/1,所有组装均在手套箱里进行。
本发明的显著优点在于:本发明提供了一种氮掺杂碳包覆分等级锗结构的制备方法,该方法工艺简单,成本廉价,重现性好,性能优异。本发明合成了分等级结构的锗,并进行了氮掺杂的碳包覆。所制备的Ge@NC作锂离子电池负极,得到的锂离子电池具有很高的比容量和循环稳定性,在电流密度为1A/g时充放电循环300圈容量稳定在1067.9 mAh/g。同时表现出优异的倍率放电性能,即使在电流密度为20 A/g时其充放电容量也能稳定在605.0mAh/g。
附图说明
图1是氮掺杂碳包覆分等级锗的X射线衍射图;
图2是氮掺杂碳包覆分等级锗的扫描电镜图;
图3是氮掺杂碳包覆分等级锗的透射电镜图;
图4是电流密度为1A/g时, 氮掺杂碳包覆分等级锗的电化学性能图。
具体实施方式
本发明用下列实施例来进一步说明本发明,但本发明的保护范围并不限于下列实施例。
实施例1 氮掺杂碳包覆分等级锗的制备
一种氮掺杂碳包覆分等级锗结构制备的方法,包括以下步骤:
(1)将0.52克GeO2,1.1克二水合醋酸锌,0.1克CTAB加入到20毫升水中,调节pH至8,移入50毫升的反应釜中,置于140℃的烘箱中,反应24小时,将所得产品用水洗涤数次,烘干,将所得锗酸锌用适量的浓硝酸混合搅拌1h得到分等级椭圆形GeO2;
(2)将0.065克分等级椭圆形GeO2超声30min分散于50毫升甲醇中,再加入0.1克盐酸多巴胺,调节pH至8,室温搅拌24小时,无水乙醇洗涤后烘干,得到GeO2@PDA;
(3)将所得GeO2@PDA于700℃,N2气氛下煅烧3h后,再在体积浓度5%H2/95%Ar气氛下,于350℃煅烧1.5h,然后升温到650℃,煅烧2.5h,得到氮掺杂碳包覆分等级锗Ge@NC。
由图1、2、3可知,本发明制得的材料确为氮掺杂碳包覆分等级锗。
实施例2 氮掺杂碳包覆分等级锗在锂离子电池中的应用
将实施例1制得的氮掺杂碳包覆分等级锗用于锂离子电池的制备,并进行电化学性能测试。
该锂离子电池的制备方法为:按质量比Ge@NC:聚偏氟乙烯:乙炔黑=8:1:1混合研磨后均匀地涂在铜箔上做负极,参比电极和对电极均为金属锂,电解质为1M LiPF6的EC+DMC+EMC (EC/DMC/EMC=1/1/1 v/v)溶液,所有组装均在手套箱里进行。
所制备的Ge@NC作锂离子电池负极,得到的锂离子电池具有很高的比容量和循环稳定性,由图4可知,在电流密度为1A/g时充放电循环300圈容量稳定在1067.9 mAh/g。同时表现出优异的倍率放电性能,即使在电流密度为20 A/g时其充放电容量也能稳定在605.0mAh/g。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (3)
1.一种氮掺杂碳包覆分等级锗结构制备的方法,其特征在于,包括以下步骤:
(1)将0.52克GeO2,1.1克二水合醋酸锌,0.1克CTAB加入到20毫升水中,调节pH至8,移入50毫升的反应釜中,置于140℃的烘箱中,反应24小时,将所得产品用水洗涤数次,烘干,将所得锗酸锌用适量的浓硝酸混合搅拌1h得到分等级椭圆形GeO2;
(2)将0.065克分等级椭圆形GeO2超声30min分散于50毫升甲醇中,再加入0.1克盐酸多巴胺,调节pH至8,室温搅拌24小时,无水乙醇洗涤后烘干,得到GeO2@PDA;
(3)将所得GeO2@PDA于700℃,N2气氛下煅烧3h后,再在体积浓度5%H2/95%Ar气氛下,于350℃煅烧1.5h,然后升温到650℃,煅烧2.5h,得到氮掺杂碳包覆分等级锗Ge@NC。
2.一种如权利要求1所述的制备方法制得的氮掺杂碳包覆分等级锗。
3.一种如权利要求2所述的氮掺杂碳包覆分等级锗的应用,其特征在于,所述的氮掺杂碳包覆分等级锗在锂离子电池中的应用,该锂离子电池的制备方法为:按质量比氮掺杂碳包覆分等级锗Ge@NC:聚偏氟乙烯:乙炔黑=8:1:1混合研磨后均匀地涂在铜箔上做负极,参比电极和对电极均为金属锂,电解质为1M LiPF6的EC+DMC+EMC溶液,其中体积比EC/DMC/EMC=1/1/1,所有组装均在手套箱里进行。
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CN110790304A (zh) * | 2019-11-13 | 2020-02-14 | 福州大学 | 一种海胆状结构的二氧化锗/氮掺杂碳复合材料制备及其锂离子电池应用 |
CN115036505A (zh) * | 2022-05-27 | 2022-09-09 | 江苏科技大学 | 一种锂离子电池用碳包覆锗复合负极材料及其制备方法与应用 |
CN115548311A (zh) * | 2022-10-20 | 2022-12-30 | 福州大学 | 氟掺杂TiO2(B)/rGO复合材料及其制备方法和应用 |
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