CN109331844A - 一种MoS2微球/PtCo合金纳米颗粒复合材料及其制备方法 - Google Patents
一种MoS2微球/PtCo合金纳米颗粒复合材料及其制备方法 Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
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- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 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 1
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- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 29
- 230000003197 catalytic effect Effects 0.000 abstract description 18
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 13
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- 239000011684 sodium molybdate Substances 0.000 description 3
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- 235000015393 sodium molybdate Nutrition 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910015667 MoO4 Inorganic materials 0.000 description 1
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- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- AVMBSRQXOWNFTR-UHFFFAOYSA-N cobalt platinum Chemical compound [Pt][Co][Pt] AVMBSRQXOWNFTR-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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Abstract
本发明公开了一种MoS2微球/PtCo合金纳米颗粒复合材料及其制备方法,所述MoS2微球/PtCo合金纳米颗粒复合材料以MoS2微球为基体材料,在MoS2微球表面负载PtCo合金纳米颗粒,具体制备步骤如下:首先通过水热法制备MoS2微球;然后通过PVP产生自组装所需的结合力;最后通过共还原的方式制备PtCo合金纳米颗粒,并使其负载于MoS2微球表面,得到MoS2微球/PtCo合金纳米颗粒复合材料。MoS2/PtCo合金纳米颗粒复合材料具有与铂相近的催化能力且含铂量很低,并具有强于铂的催化稳定性,这对代替主流的贵金属催化剂具有重要意义。
Description
技术领域
本发明属于纳米材料制备技术领域,涉及一种MoS2微球/PtCo合金纳米颗粒复合材料及其制备方法。
背景技术
二硫化钼(MoS2)作为一种新型的二维材料最早被应用于润滑领域。随着对其研究的深入,科研人员发现MoS2因其特殊的性质也可成为出色的光电、催化材料。根据以往的文献报道,MoS2已经在二维晶体管、锂离子电池、加氢脱硫催化及光催化制氢等领域都有了不错的应用。MoS2与石墨烯有相似的原子层结构,但是与石墨烯不同的是,组成MoS2的是三原子层而非单原子层,它是有两个硫原子包夹一个钼原子形成的原子层结构。正是由于这种结构使得MoS2拥有许多独特的化学位点,并且层上的载流子迁移速度是层间的2200倍。根据以往的文献报道,MoS2体材料表面是由热力学有利的原子平面组成,这些位置催化能力较弱。而MoS2原子层的边界具有催化活性很高的活性位点。一种材料的催化能力主要由两方面决定:(1)材料本身的固有催化能力;(2)材料上的活性位点数量。因此催化活性较高的MoS2在其表面(与反应物接触区域)应具有较多的活性位点数,即:在表面暴露更多的MoS2片层边界。
合金纳米颗粒是一种整体尺寸在纳米尺度的,两种或两种以上金属、金属与非金属组成的具有金属特性的材料。合金纳米颗粒具有明显区别于体合金与纯金属的性质:(1)由于价电子在不同元素原子核建立的势场中重新分布,实现了电子重构。(2)两种不同原子的错配能产生缺陷态,这可以丰富材料的催化活性位点;(3)第二种原子的加入可以提升材料的化学稳定性。目前复合催化材料发展迅速,并且应用于燃料电池、光催化制氢、染料敏化太阳能对电极,但是尚未有MoS2/PtCo合金复合材料的文献报道。
发明内容
本发明的目的是提供一种高催化活性的MoS2微球/PtCo合金纳米颗粒复合材料及其制备方法。本发明利用自组装的方式将PtCo合金纳米颗粒负载于MoS2微球上,构成一种含铂量极少的高催化活性复合材料,该材料具有与铂相近的催化能力且含铂量很低,并具有强于铂的催化稳定性,这对代替主流的贵金属催化剂具有重要意义。
本发明的目的是通过以下技术方案实现的:
一种高催化活性的MoS2微球/PtCo合金纳米颗粒复合材料,以MoS2微球为基体材料,在MoS2微球表面负载PtCo合金纳米颗粒。
一种上述高催化活性的MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,包括如下步骤:
一、配制浓度为4.0~6.0g/ml的PVP溶液80~100ml,并向其中分别加入0.95~0.10g钼酸钠和1.90~1.95g硫脲,得到混合溶液;
二、将步骤一配制的混合溶液为反应物,通过水热法制备MoS2微球,控制温度为180~220℃,时间为20~25h;
三、将步骤二制备的0.2~0.4g MoS2微球与0.05~0.2g PVP在30~50ml溶剂(乙二醇或去离子水)中混合形成混合溶液,随后根据所需的负载量按摩尔比1:1加入H2PtCl6与CoCl2溶液;
四、以NaBH4作为还原剂,向步骤三的溶液中加入足量NaBH4,通过共还原法制备MoS2微球/PtCo合金纳米颗粒复合材料。所谓共还原法,指的是同时将两种元素还原成零价原子并形成合金的方法。共还原法可在还原剂的作用下将氧化还原电位相近的离子在常温同时还原。
上述方法中,所用化学试剂均为分析纯,没有经过进一步提纯。
上述方法中,PVP在步骤一、步骤二制备MoS2微球时的作用是在溶液中形成囊泡,作为MoS2微球形成的模板,其中:PVP加入量会影响微球的大小,可根据需要的微球尺寸加入适量的PVP。
上述方法中,PVP在步骤三、步骤四中作为自组装的连接剂,将还原出的钴铂合金组装到MoS2微球表面,其中:PVP加入量通过加入的MoS2微球粉末与溶剂的量决定。
上述方法中,水热法采用的反应物是钼酸钠和硫脲,制备MoS2微球的基本过程如下:
MoO4 2++2S2-+6e-→MoS2+4O2-。
上述方法中,共还原法采用的铂源和钴源为H2PtCl6和CoCl2,还原剂为NaBH4,制备PtCo纳米颗粒的基本过程如下:
Pt+4+Co2++6H-→PtCo+3H2;
其中:H2PtCl6与CoCl2混合溶液的加入量根据所需负载的金属质量分数计算,NaBH4的加入量根据所加入H2PtCl6与CoCl2混合溶液的量推算。
上述方法中,使用PVP连接并组装的过程为:
(1)PVP中羰基中的孤对电子与金属离子配位,经还原后形成PVP包裹的PtCo合金纳米颗粒PVP-PtCo NPs;
(2)MoS2表面的PVP与PVP-PtCo NPs通过PVP上的氮原子在溶液中形成互相吸引的氢键,将PVP-PtCo NPs通过弱结合力吸引其上,完成自组装;
相比于现有技术,本发明具有如下优点:
1、常见的块体硫化钼在大多数溶剂中无法分散,不具备通过液相共还原制备MoS2/PtCo合金纳米颗粒复合材料的基本条件。本发明采用PVP作为连接剂自组装负载/PtCo合金纳米颗粒,负载量大,纳米颗粒分布均匀。
2、MoS2/PtCo合金纳米颗粒复合材料的催化性能与大面积的铂相近,但含铂量非常少,是铂的一种性能优异、成本低廉的替代材料。
附图说明
图1为市售MoS2块体图像;
图2为MoS2微球SEM图像,a为MoS2微球,b为MoS2/PtCo合金纳米颗粒复合材料(在乙二醇中制备);
图3为MoS2/PtCo合金纳米颗粒复合材料TEM图像;
图4为MoS2/PtCo合金纳米颗粒复合材料与其他材料对比的CV曲线;
图5为100次循环CV曲线,a为MoS2/Pt纳米颗粒复合材料,b为MoS2/PtCo合金纳米颗粒复合材料。
图6在去离子水中制备的MoS2/PtCo合金纳米颗粒复合材料的SEM图像。
图7在去离子水中制备的MoS2/PtCo合金纳米颗粒复合材料的TEM图像。
具体实施方式
下面结合附图对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
实施例1:
本实施例提供了一种高催化活性的MoS2微球/PtCo合金纳米颗粒复合材料制备方法,所述方法首先通过水热法制备MoS2微球;然后通过PVP产生自组装所需的结合力;最后通过共还原的方式制备PtCo合金纳米颗粒,并使其负载于MoS2微球表面。具体实施步骤如下:
步骤一:称量0.4g PVP(k30),将其加入到80ml去离子水中,并搅拌30min,得到5.0g/LPVP溶液。
步骤二:将0.96g Na2MoO4和1.92g硫脲加入到步骤一得到的PVP溶液中,得到前驱体溶液。
步骤三:将步骤二得到的前驱体溶液加入到带有100ml聚四氟乙烯内胆的反应釜中,在200℃反应24h,反应完成后离心收集并用去离子水清洗并干燥,得到直径约300nm的MoS2微球。
步骤四:将步骤三制备的0.3g MoS2微球粉末加入到40ml乙二醇中,搅拌30min;然后加入0.2g PVP并搅拌30min;接着加入分别含有0.295mmol H2PtCl6与CoCl2混合溶液并搅拌30min,随后加入200mg NaBH4并搅拌4h。静置6h,然后离心清洗收集,得到MoS2/PtCo合金纳米颗粒复合材料。
通过对比图1与图2a可以看出,与市售MoS2相比,该方法制备的MoS2微球为表面暴露有大量MoS2片层边界的MoS2微球。由于MoS2的片层边缘为催化活性位点,因此该材料具有形貌及结构上的优势。通过图2可以明显看出:用该方法合成并负载在MoS2微球上的合金纳米颗粒负载量大、分布均匀无团聚出现;通过图3可看出:大量细小的PtCo纳米颗粒均匀负载在MoS2微球表面;通过图4可看出:在循环伏安曲线(CV)中,该复合材料的电流密度与阴极峰电势均与纯铂相近,说明其催化能力相当;通过图5可看出:相较于MoS2/Pt纳米颗粒复合材料,MoS2/PtCo合金纳米颗粒复合材料,在催化过程中的稳定性极佳,这是钴原子加入使金属电子结构改变的缘故。
实施例2:
本实施例证明了在水中亦可制备MoS2/PtCo合金纳米颗粒复合材料,但纳米颗粒负载量及分散度稍低,具体实施步骤如下:
步骤一:利用实施例1的方法制备MoS2微球。
步骤二:将步骤一制备的0.3g MoS2微球粉末加入到40ml去离子水中,搅拌30min;然后加入0.2g PVP并搅拌30min;接着加入分别含有0.295mmol H2PtCl6与CoCl2混合溶液并搅拌30min,随后加入200mg NaBH4并搅拌4h。静置6h,然后离心清洗收集,得到MoS2/PtCo合金纳米颗粒复合材料。
通过图6、7可以看出在水中也可制备出MoS2/PtCo合金纳米颗粒复合材料,但负载量和分散度稍逊于在乙二醇中制备的复合材料。
Claims (6)
1.一种MoS2微球/PtCo合金纳米颗粒复合材料,其特征在于所述复合材料以MoS2微球为基体材料,在MoS2微球表面负载PtCo合金纳米颗粒。
2.一种权利要求1所述MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,其特征在于所述方法包括如下步骤:
一、将0.2~0.4gMoS2微球与0.05~0.2gPVP在30~50ml溶剂中混合形成混合溶液,随后根据所需的负载量加入H2PtCl6与CoCl2溶液;
二、以NaBH4作为还原剂,向步骤三的溶液中加入足量NaBH4,通过共还原法制备MoS2微球/PtCo合金纳米颗粒复合材料。
3.根据权利要求2所述的MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,其特征在于所述MoS2微球的制备方法如下:
(1)配制浓度为4.0~6.0g/ml的PVP溶液80~100ml,并向其中分别加入0.95~0.10g钼酸钠和1.90~1.95g硫脲,得到混合溶液;
(2)以步骤(1)配制的混合溶液为反应物,通过水热法制备MoS2微球。
4.根据权利要求3所述的MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,其特征在于所述水热法的温度为180~220℃,时间为20~25h。
5.根据权利要求2所述的MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,其特征在于所述步骤一中,Pt+4与Co2+的摩尔比为1:1。
6.根据权利要求2所述的MoS2微球/PtCo合金纳米颗粒复合材料的制备方法,其特征在于所述溶剂为乙二醇或去离子水。
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