CN107999093A - 一种钴掺杂二维硒化钨电催化剂及其制备方法 - Google Patents
一种钴掺杂二维硒化钨电催化剂及其制备方法 Download PDFInfo
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Abstract
本发明属于电催化剂制备领域,公开一种钴掺杂二维硒化钨电催化剂的制备方法。将硒粉、硼氢化钠分散于N,N‑二甲基甲酰胺中,在40~60℃条件下搅拌均匀;将二水合钨酸钠和四水合乙酸钴溶解于水中;混合两溶液,搅拌均匀;于160~200℃条件下反应8~12 h;反应结束后,离心洗涤,将所得沉淀在真空下干燥;所得产物在惰性气体保护下300~500℃碳化3~5 h,即得。本发明方法制备的钴掺杂二维硒化钨在广泛的pH范围内都展现出比商业硒化钨优异的电催化析氢性能,这在催化领域具有良好的应用前景。
Description
技术领域
本发明属于电催化剂制备领域,具体涉及一种钴掺杂二维硒化钨电催化剂的制备方法。
背景技术
过渡金属硫族化合物作为一种新型的二维层状材料,具有类似于石墨烯的特性,广泛用于场效应晶体管、传感、储能和催化等方面。实验和理论研究表明,过渡金属硫族化合物暴露的边缘具有可媲美贵金属铂的电催化性能。但是由于过渡金属硫族化合物二维层状结构的特性,很容易在范德华力作用下聚集重叠在一起,大大降低了其边缘活性位点的暴露。因此如何制备具有高密度活性位点的过渡金属硫族化合物存在难题。截至目前,提高过渡金属硫族化合物活性位点密度的制备方法主要是剥离分散和减小尺寸,但是该过程的操作产量低且复杂,并且提高的活性位点密度有限,极大地限制了其在催化领域方面的应用。硒化钨作为一个未被广泛开发的过渡金属硫族化合物,是具有前景的非贵金属催化剂,它的性能同样受活性位点的密度的影响。因此,寻找一种行之的方法得到高活性的二维硒化钨的电催化剂仍然是一个挑战。此外,氢气作为一种高效、可再生的清洁燃料,二维材料催化剂对其电化学制备多局限在酸性条件下。 因此,开发成本低且在碱性水电解条件下工作的新型高效析氢电催化剂具有重要意义。
发明内容
针对上述现有技术的缺陷与不足,本发明的目的在于提供一种钴掺杂二维硒化钨电催化剂的制备方法。
为实现上述目的,本发明采取的技术方案如下:
一种钴掺杂二维硒化钨电催化剂的制备方法,步骤如下:
(1)、将硒粉、硼氢化钠分散于 N,N-二甲基甲酰胺中,在40~60 ℃条件下搅拌均匀,配成硒粉、硼氢化钠的质量浓度分别为(10~15)×10-3 g/mL、(5~6)×10-3 g/mL的溶液;
(2)、将二水合钨酸钠和四水合乙酸钴溶解于水中, 配成二水合钨酸钠和四水合乙酸钴的质量浓度为(100~150)×10-3 g/mL、(10~30)×10-3 g/mL的溶液;其中N,N-二甲基甲酰胺和水的体积比为(4~5)∶1,
(3)、将步骤(2)所得溶液加入步骤(1)所得溶液中,搅拌均匀;
(4)、将步骤(3)所得溶液于160~200 ℃条件下反应8~12 h;
(5)、步骤(4)反应结束后,离心洗涤,将所得沉淀在真空下干燥;
(6)、将步骤(5)所得产物在惰性气体保护下300~500 ℃碳化3~5 h,即得钴掺杂二维硒化钨电催化剂。
较好地,离心洗涤时,先用水洗涤再用乙醇洗涤;每次离心时,速度为7000~9000rpm,时间为5~10 min。
更好地,水和乙醇各自洗涤三次。
较好地,真空干燥的温度为40~60 ℃。
利用所述制备方法制备的钴掺杂二维硒化钨电催化剂。
本发明相对于现有技术,有以下优点:
1、本发明制备方法工艺简单、操作简便、后处理简单、安全,具有重复性;
2、本发明制备方法提供了一种钴掺杂二维硒化钨电催化剂的制备方法,相对于气相金属掺杂方法的高温长时间等苛刻的操作环境,此方法较温和安全而且产量大,有应用在器件上的潜力;
3、本发明方法制备的钴掺杂二维硒化钨在广泛的pH范围内都展现出比商业硒化钨优异的电催化析氢性能,这在催化领域具有良好的应用前景。
附图说明
图1:本发明实施例1制备的钴掺杂二维硒化钨的扫描电镜图。
图2:本发明实施例1制备的钴掺杂二维硒化钨的X射线光电子能谱图,(a)钨元素,(b)硒元素,(c)钴元素。
图3:本发明实施例1制备的钴掺杂二维硒化钨的透射电镜照片。
图4:本发明实施例1制备的钴掺杂二维硒化钨的X射线衍射谱图(a)和拉曼谱图(b)。
图5:商业硒化钨与本发明实施例1-3制备的钴掺杂二维硒化钨在0.5 M H2SO4酸性(a)和1 M KOH碱性(b)电解液中的极化曲线对比。
具体实施方式
以下以具体实施例来说明本发明的技术方案,但本发明的保护范围并不局限于此:
实施例1
(1)、将640 mg硒粉和300 mg硼氢化钠分散在50 mL N,N-二甲基甲酰胺中,封上保鲜膜在60 ℃条件下搅拌两个小时直至溶液变为棕黄色,形成硒粉、硼氢化钠的质量浓度分别为12.8×10-3 g/mL、6×10-3 g/mL的溶液;
(2)、将1320 mg二水合钨酸钠和200 mg 四水合乙酸钴加入10 mL去离子水中,超声0.5小时,形成二水合钨酸钠和四水合乙酸钴的质量浓度为132×10-3 g/mL、20×10-3 g/mL的溶液;
(3)、将步骤(2)所得溶液加入步骤(1)所得溶液中,继续60 ℃搅拌0.5小时;
(4)、将步骤(3)所得溶液转至反应釜中,在200 ℃条件下反应12小时;
(5)、分别用去离子水和无水乙醇洗涤三次,每次离心时,速度为7000 rpm,时间为10分钟,提取离心管下层沉淀在40 ℃下真空干燥;
(6)、将步骤(5)所得产物在氮气保护下炭化炉300 ℃碳化5小时,即得钴掺杂二维硒化钨电催化剂。
实施例2
与实施例1的不同之处在于:将步骤(2)中的四水合乙酸钴调至100 mg,其它均同实施例1。
实施例3
与实施例1的不同之处在于:将步骤(2)中的四水合乙酸钴调至300 mg,其它均同实施例1。
结构表征和性能测试
(一)结构表征
图1为本发明实施例1制备的钴掺杂二维硒化钨的扫描电子显微镜图,从图中可以看出合成的产物为二维片状结构,横向尺寸为100 nm,纵向尺寸为25 nm。
图2为本发明实施例1制备的钴掺杂二维硒化钨的X射线光电子能谱图,分别为(a)W 4f和(b)Se 3d以及(c) Co 2p谱图,从图中可以看出钴是以正二价态的形式掺杂进原有的硒化钨结构中。
图3为本发明实施例1制备的钴掺杂二维硒化钨的透射电子显微镜图,掺杂后的材料仍是尺寸较小的片状结构。
图4为本发明实施例1制备的钴掺杂二维硒化钨的X射线衍射谱图(a)和拉曼谱图(b),(a)图中除了保留原有硒化钨的特征峰以外都还有新峰的出现,并且通过对比PDF卡片可以将新峰归属为Co9Se8,(b)图中除了原来250 cm-1位置处的硒化钨特征振动模式外还有新峰的出现同样表明钴成功掺杂进硒化钨。
(二)性能测试
分别把实施例1-3制备的钴掺杂二维硒化钨与商业硒化钨作为催化剂加载到玻碳电极上作为工作电极,银/氯化银电极为参比电极,碳棒为对电极,组装三电极体系测试析氢性能,电解液为0.5 M H2SO4或1 M KOH,扫描速度为5 mv/s。工作电极的制备过程为:将5 mg样品溶解于1 mL无水乙醇中并加入5 μL 5wt%萘酚溶液超声1 小时左右直至均匀分散,用移液枪取10 μL均匀涂敷在玻碳电极上,在室温下干燥。
图5为商业硒化钨与本发明实施例1-3制备的钴掺杂二维硒化钨在0.5 M H2SO4酸性(a)和1 M KOH碱性(b)电解液中的极化曲线对比,从图中可以看到:相对于商业硒化钨,少量钴掺杂催化剂(实施例2)的析氢性能无论在酸性还是碱性条件下都有很大提高,但是当钴掺杂量相对较大时,催化剂(实施例1、实施例3)析氢性能相对商业硒化钨虽然有很大提高,但是催化剂析氢性能并不与钴掺杂量成正比,而是存在一个最合适的掺杂量;本发明实施例1制备的掺钴硒化钨不仅在酸性条件下比商业硒化钨和实施例2以及实施例3制备的钴掺杂硒化钨的催化性能高,在碱性条件下析氢性能也最优。
Claims (5)
1.一种钴掺杂二维硒化钨电催化剂的制备方法,其特征在于,步骤如下:
(1)、将硒粉、硼氢化钠分散于 N,N-二甲基甲酰胺中,在40~60 ℃条件下搅拌均匀,配成硒粉、硼氢化钠的质量浓度分别为(10~15)×10-3 g/mL、(5~6)×10-3 g/mL的溶液;
(2)、将二水合钨酸钠和四水合乙酸钴溶解于水中, 配成二水合钨酸钠和四水合乙酸钴的质量浓度为(100~150)×10-3 g/mL、(10~30)×10-3 g/mL的溶液;其中N,N-二甲基甲酰胺和水的体积比为(4~5)∶1,
(3)、将步骤(2)所得溶液加入步骤(1)所得溶液中,搅拌均匀;
(4)、将步骤(3)所得溶液于160~200 ℃条件下反应8~12 h;
(5)、步骤(4)反应结束后,离心洗涤,将所得沉淀在真空下干燥;
(6)、将步骤(5)所得产物在惰性气体保护下300~500 ℃碳化3~5 h,即得钴掺杂二维硒化钨电催化剂。
2.如权利要求1所述的制备方法,其特征在于:离心洗涤时,先用水洗涤再用乙醇洗涤;每次离心时,速度为7000~9000 rpm,时间为5~10 min。
3.如权利要求2所述的制备方法,其特征在于:水和乙醇各自洗涤三次。
4.如权利要求1所述的制备方法,其特征在于:真空干燥的温度为40~60 ℃。
5.一种利用如权利要求1~4任意一项所述制备方法制备的钴掺杂二维硒化钨电催化剂。
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