CN110931741A - 硫化锡量子点负载的碳化钛复合纳米材料及其制备方法 - Google Patents
硫化锡量子点负载的碳化钛复合纳米材料及其制备方法 Download PDFInfo
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- 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 title claims abstract description 59
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 27
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 title claims abstract description 19
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Abstract
本发明涉及一种硫化锡量子点负载的碳化钛复合纳米材料,该材料是以碳化钛纳米片(Ti3C2)为基体材料,硫化锡量子点负载在该碳化钛纳米片上而形成的复合纳米材料。本发明以热解还原的碳化钛、L‑半胱氨酸和氯化亚锡为原料,N‑甲基‑2‑吡咯烷酮和水为共溶剂,采用简单的水热合成方法,可得形貌均一的SnS2量子点/碳化钛复合纳米材料。从电镜结果来看,平均粒径为3 nm的SnS2量子点均匀负载在超薄的碳化钛纳米片上且高度分散。XRD谱图显示,所得材料结晶度良好,为典型的六方晶系的硫化锡。本发明合成工艺简单易操作,重复性好,在钠(锂、钾等)离子二次电池等领域具有广阔的应用前景。
Description
技术领域
本发明涉及一种硫化锡量子点/碳化钛复合纳米材料及其制备方法,属于材料化学和新能源等领域。
背景技术
随着便携式电子设备,混合动力车辆以及智能电网等的兴起,新能源技术的开发和应用引起了工业界和学术界的广泛关注。可充电的锂离子电池因其突出的优势,已成为较成熟的能源存储技术之一,并被广泛应用于各种电动设备和电子器件中。然而,锂资源的相对匮乏导致的高成本等问题,严重限制了锂离子电池的深入发展。因此,众多研究都致力于探索低成本和可靠的可充电电池系统。其中,钠具有与锂相似的电化学机制且其资源相对丰富等优点,使得钠离子电池成为了最有潜力替代锂离子电池的新型二次电池。然而,受限于钠离子较大的离子半径,很多用于钠离子电池的电极材料表现出了缓慢的扩散动力学,从而导致有限的可逆容量及循环稳定性差等问题。因此,研究和开发具有良好的可逆Na+嵌入/脱出性能以及令人满意的容量的钠离子电池负极材料是非常必要的。
在众多负极材料中,二硫化锡(SnS2)因其较大的理论容量和独特的CdI2层状六方结构而受到广泛关注。然而,SnS2固有的低电导率和迟滞的反应动力学等缺点导致了可逆容量的快速衰减以及较差的循环寿命。因此,为了提高材料的电化学性能,可以通过材料微纳结构的调控或与导电性优异的基体材料复合以及引入杂原子掺杂等方法来增强其导电性,缓解体积膨胀和改善循环稳定性等。其中,Ti3C2TxMXene作为一种新兴的二维材料,凭借其优异的导电性、低的扩散壁垒、锂(钠)离子嵌入/脱出过程中体积变化小等独特优势在能源存储和转化等领域有着较好的应用前景,已成为很多硫化物或氧化物理想的载体材料。
发明内容
本发明的目的之一在于提供一种硫化锡量子点负载的碳化钛复合纳米材料。
本发明的目的之二在于提供该复合纳米材料的制备方法。
本发明以少层的碳化钛(Ti3C2)为基体材料,通过简单的一步水热合成法制备了SnS2量子点/碳化钛复合纳米材料,其中SnS2量子点均匀地负载在二维的碳化钛纳米片上,在改善碳化钛堆叠的同时,也可以有效地缓解SnS2在充放电过程中产生的体积膨胀,从而更好地发挥二者之间的协同效应,提高电化学性能。
为达到上述目的,本发明采用以下技术方案:
一种硫化锡量子点负载的碳化钛复合纳米材料,其特征在于该材料是以碳化钛纳米片(Ti3C2)为基体材料,硫化锡量子点负载在该碳化钛纳米片上而形成的复合纳米材料;所述的硫化锡量子点与碳化钛纳米片的质量比为:0.15 ~ 0.40。
一种制备上述的硫化锡量子点负载的碳化钛复合纳米材料的方法,其特征在于该方法的具体步骤为:
a.将少层的碳化钛加入到N-甲基-2-吡咯烷酮(NMP)和水的混合溶剂中,配置成浓度为1.0 ~3.0 mg mL-1的混合溶液,超声0.5 ~ 2 h;
b.将二水合氯化亚锡加入到步骤b所得混合溶液中,搅拌0.5 ~ 1 h;再继续加入L-半胱氨酸,再搅拌0.5 ~ 1 h;所述的Ti3C2、氯化亚锡、L-半胱氨酸的质量比为:1.2 ~2.0:0.6~0.8:1;
c.将步骤c所得混合溶液在140~180 ℃条件下水热反应2 ~ 12 h;将产物用去离子水和乙醇反复洗涤、离心分离后,真空烘干,最终得到硫化锡量子点负载的碳化钛复合纳米材料。
本发明通过简单的水热合成法以氯化亚锡为锡源,L-半胱氨酸为硫源,在N-甲基-2-吡咯烷酮和水作为共溶剂的条件下,与二维碳化钛材料进行有效复合,制备出形貌均一的SnS2量子点/碳化钛复合纳米材料。本发明工艺过程中,水解后的Sn2+首先通过静电作用吸附在带负电的碳化钛上;随后,与L-半胱氨酸在高温下进行反应生成二硫化锡量子点,并均匀地负载到超薄的碳化钛纳米片上。本发明得到的材料粒径均一且分散性好。
与现有的合成技术相比,本发明技术具有以下显著优点:合成工艺简单易操作,形貌均匀且为高度分散的量子点复合材料,在钠(锂、钾等)离子二次电池等领域具有一定的应用前景。
附图说明
图1为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料的TEM图片。
图2为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料的SEM图片。
图3为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料的XRD谱图。
图4为本发明实施例1和对比例所得SnS2/碳化钛复合纳米材料的电化学循环性能图。
具体实施方式
所有实施例均按上述技术方案的操作步骤进行操作。本发明所使用的少层Ti3C2MXene参考文献来制备(Gogotsi et al. Chem. Mater.,2017, 29, 1632-1640.)。合成过程简要如下:将LiF溶解在HCl中,然后逐步加入Ti3AlC2粉末,并将所得混合物在40℃下反应24 h。反应完成后,将产物离心洗涤至上层清液pH > 6。将得到的沉淀加入去离子水,超声1 h后再以3500 rpm离心1 h,得到的上层悬浮液冻干即得少层的碳化钛(Ti3C2)。
实施例1
a.用电子天平称取30 mg上述制备的碳化钛,加入到20 ml N-甲基-2-吡咯烷酮(NMP)和10 ml的去离子水的混合溶液中,超声30 min使其分散均匀;
b.向上述混合溶液中加入17 mg二水合氯化亚锡,搅拌1 h,充分溶解;
c.将25 mg L-半胱氨酸加入上述混合溶液中,继续搅拌1 h;
d.将反应后的混合溶液倒入带聚四氟乙烯内衬的高压反应釜中,在180 ℃条件下反应6 h;
e.反应完成后,将产物从反应釜中取出,用去离子水和乙醇反复洗涤、离心后,将其在60℃下真空烘干,即得本发明制备的SnS2量子点/碳化钛复合纳米材料。
将所制得的样品进行物性表征,其部分结果如附图所示。由结果可知,所得SnS2量子点/碳化钛复合纳米材料形貌均一,粒径约为3 nm且均匀地负载在超薄的碳化钛纳米片上。
实施例2
本实施例的制备过程和步骤与实施例1基本相同,不同在于a步骤:
将30 mg碳化钛加入到30 ml异丙醇中,超声30 min使其均匀分散;
所得结果与实施例1有较大差异,产品为大小不一的颗粒且明显团聚。
实施例3
本实施例的制备过程和步骤与实施例1基本相同,不同在于b步骤:
将20 mg五水合四氯化锡加入上述混合溶液中,继续搅拌1 h;
所得结果与实施例1有明显差异,制备的复合材料,形貌不均一且粒径较大。
对比例
本实施例的制备过程和步骤与实施例1基本相同,不同在于a步骤:
将30 mg碳化钛加入到30 ml去离子水中,超声30 min使其均匀分散;
所得结果与实施例1有较大差异,所得产品为大小不一的片状结构且有明显地聚集现象。
参见附图,图1为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料的透射电镜(TEM)图片。TEM分析:采用日立Hitachi HT7700型透射电子显微镜观察材料的形貌和内部结构。从TEM结果可知,所得复合材料中,SnS2为粒径在3 nm左右的量子点,且在超薄的碳化钛纳米片上高度均匀负载。
参见附图,图2为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料的扫描电镜(SEM)图片。SEM分析:采用日立Hitachi SU8200型发射扫描电子显微镜观察材料的表面形貌。从中可以看出,大量的SnS2量子点均匀生长在碳化钛表面上,与TEM的结果相一致。
参见附图,图3为本发明实施例1所得SnS2量子点/碳化钛复合纳米材料XRD谱图。XRD分析:在日本Riga KuD/max-2550型X射线衍射仪上进行,采用CuKα衍射。从图谱中可知,本发明所得复合纳米材料中,衍射峰的出峰位置与标准谱图(JCPDS Card No.23-0677)相一致,是典型的六方晶系SnS2晶相。此外,在2q = 6.4°左右出现的宽峰对应于刻蚀后的碳化钛的(002)晶面。说明所得复合材料为结晶良好的高纯度的硫化锡量子点负载的碳化钛复合材料。
参见附图,图4为本发明实施例1和对比例所得SnS2/碳化钛复合纳米材料的电化学循环性能图。其中,电化学性能测试的方法如下:将炭黑和合成的SnS2量子点/碳化钛复合纳米材料加入到PVDF(聚偏二氟乙烯,2.5 wt.% NMP溶液)中混合搅拌均匀,用涂膜法将材料均匀的涂覆在铜片上制成钠离子电池的负极;正极材料为金属钠片,微孔玻璃纤维材料作为隔膜,电解液是由NaClO4溶解在相应质量比为1:1:1的乙烯碳酸脂(EC)、丙烯碳酸脂(DMC)和碳酸乙酯(DEC)溶液中配制而成的。模拟电池是在充满氩气的手套箱中组装而成。根据电化学性能测试的结果,当作为钠离子电池的负极材料时,实施例1所得的SnS2量子点/碳化钛复合材料表现出较高的可逆容量和优异的循环稳定性:在电流密度为100 mAg-1的条件下首次放电容量为795 mAhg-1,100次循环后的放电容量为346.3 mAhg-1。而对比例所得复合材料在相同的测试条件下首次放电容量为645.6 mAhg-1,100次循环后的放电容量仅为79mAhg-1。该结果表明,本发明制备的SnS2量子点/碳化钛复合纳米材料具有优异的储钠性能。
Claims (2)
1.一种硫化锡量子点负载的碳化钛复合纳米材料,其特征在于该材料是以碳化钛纳米片(Ti3C2)为基体材料,平均粒径为3nm的硫化锡量子点均匀负载在超薄的二维碳化钛纳米片上而形成;所述的硫化锡量子点与碳化钛纳米片的质量比为:0.15 ~ 0.40。
2.一种制备根据权利要求1所述的硫化锡量子点负载的碳化钛复合纳米材料的方法,其特征在于该方法的具体步骤为:
a.将少层的碳化钛加入到N-甲基-2-吡咯烷酮和水的混合溶剂中,配置成浓度为1.0~3.0 mg mL-1的混合溶液,超声0.5 ~ 2h;
b.将二水合氯化亚锡加入到步骤b所得混合溶液中,搅拌0.5 ~ 1 h;再继续加入L-半胱氨酸,再搅拌0.5 ~ 1 h;所述的Ti3C2、氯化亚锡、L-半胱氨酸的质量比为:1.2 ~2.0:0.6~0.8:1;
c.将步骤c所得混合溶液在140~180 ℃条件下水热反应2 ~ 12 h;将产物用去离子水和乙醇反复洗涤、离心分离后,真空烘干,最终得到硫化锡量子点负载的碳化钛复合纳米材料。
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