CN113522298B - 一种钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料及其制备方法和应用 - Google Patents
一种钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料及其制备方法和应用 Download PDFInfo
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- CN113522298B CN113522298B CN202110786338.4A CN202110786338A CN113522298B CN 113522298 B CN113522298 B CN 113522298B CN 202110786338 A CN202110786338 A CN 202110786338A CN 113522298 B CN113522298 B CN 113522298B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 52
- 239000006260 foam Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910018921 CoO 3 Inorganic materials 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 36
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000002243 precursor Substances 0.000 claims description 14
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 14
- 238000002207 thermal evaporation Methods 0.000 claims description 11
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 6
- 239000013535 sea water Substances 0.000 claims description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 5
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- 229910001385 heavy metal Inorganic materials 0.000 claims description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 4
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- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明公开了一种钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料及其制备方法和应用,属于光热与电化学领域。将零维LaxSr1‑xCoO3纳米颗粒与2D Ti3C2MXene纳米片负载在导电泡沫镍上,制得光热协同电催化析氧的泡沫镍复合材料。该复合材料中Ti3C2MXene光热材料可以将太阳光谱转化为热能,从而高效地进行净水蒸发,同时产生的热能加速电化学反应动力学,有效提高电催化材料的氧析出性能,实现高效产氧。该复合材料提供的制备原料不含贵金属元素,造价成本低,工艺简便,可重复性高,易于大批量生产,在海水淡化协同电解水产氧的多学科交叉领域具有广泛的应用前景。
Description
技术领域
本发明属于光热转化与电化学技术领域,具体涉及一种钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料及其制备方法和应用。
背景技术
近年来,随着我国经济的迅速发展,对淡水资源的需求也逐年增长。目前,发展较为成熟的空气蒸馏渗透淡化工艺技术和反应式渗透淡化技术在全球较大范围内已经得到了广泛的研究应用,但它们仍然普遍存在大量能源消耗大、维修维护成本高等技术缺陷。因此,探索出高效的太阳能转换技术与材料对太阳能的利用至关重要。太阳能光热转换是通过反射、吸收或其他方式把太阳辐射能集中起来,转换成足够高温度的过程,是直接利用太阳能的有效途径。通过太阳能转化产生的热能可以应用在多个领域,如光热蒸汽转化、光热发电、光热催化以及光热化学转化等。
在过去的几十年里,随着电池技术的快速发展,传统的铅蓄电池日渐不能满足现代产业的用电需求,逐步被需要氧气作为反应物的金属空气电池和燃料电池取代。电化学水分解法是一种通过氧释放反应(OER)产生氧气的便捷方法,它涉及复杂的四电子过程(2H2O→O2+4H++4e),而且不同基本反应之间的相关性通常会限制反应速率。目前,Ru/Ir基氧化物通常被认为是实现OER性能的有效电催化剂,但其实际应用受到储量低和成本高的限制。因此,迫切需要开发在恶劣环境下有效、稳定且不含贵金属的电催化剂。钙钛矿氧化物LaCoO3固有的电导率和活性表面积,被研究者们应用于电化学分解水领域。近年来,研究人员将多种形貌的LaxSr1-xCoO3与各种导电基材(例如碳纳米纤维、多孔碳和还原的氧化石墨烯)结合以提高电导率,进一步促进电催化活性。二维层状过渡金属碳化物(2D Ti3C2MXenes)具有优异的金属导电性,出色的亲水性和多种表面官能团,使其在高效电催化方面具有很大的潜能。此外,其负电荷表面和超低功函的超薄分层为构建强界面相互作用的受限杂化电催化剂提供了平台,有利于优化电催化剂的活性中心。Ti3C2 MXene的独特二维形貌可以大大缩短进行质量扩散和电荷转移的途径,并获得高度暴露的活性位点的异质结电催化剂。因此,如何将LaxSr1-xCoO3纳米材料与2D Ti3C2 MXene纳米片复合,以提高LaxSr1- xCoO3的OER性能成为需要解决的问题。
发明内容
针对现有技术中存在的问题,本发明要解决的技术问题在于提供一种钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料。本发明解决的另一个技术问题在于提供一种钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料的制备方法。本发明要解决的技术问题还有一个在于提供一种钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料在电催化析氧中的应用和在海水和重金属、强酸碱性废水光热蒸发净化中的应用。该材料具有突出的全太阳光谱利用率、光热蒸汽转化以及光电协同催化效率。
为了解决上述问题,本发明所采用的技术方案如下:
一种钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,将零维LaxSr1- xCoO3纳米颗粒与2D Ti3C2 MXene纳米片负载在导电泡沫镍上,制得钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料。包括以下步骤:
(1)分别称量硝酸镧、硝酸锶、硝酸钴、六亚甲基四胺,并加入超纯水和甲醇溶液,配置前驱体溶液;
(2)向步骤(1)所述前驱体溶液中,加入Ti3C2 MXene光热材料,并缓慢加入氢氧化钾粉末,低速搅拌,使其混合均匀,调整pH=10;
(3)将泡沫镍基底材料用1.0mol L-1的盐酸溶液清洗后浸没在步骤(2)所述溶液中进行水热反应,反应结束后冷冻干燥,然后进行高温煅烧,得到钙钛矿氧化物/Ti3C2 MXene/泡沫镍基复合材料。
所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,配制前驱体溶液时,硝酸镧、硝酸锶、硝酸钴和六亚甲基四胺的质量比为3.9:0.2:2.9:2.8,去离子水和甲醇的体积比为1:1。
所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,所述Ti3C2 MXene与硝酸钴的质量比为0.5:2.9。
所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,所述水热反应温度为200℃,反应时间为48h。
所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,所述高温煅烧过程使用管式炉,并在氮气氛下,煅烧温度为600℃,煅烧2h。
上述方法制备得到的钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料。
上述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料在海水和重金属、强酸碱性废水光热蒸发净化中的应用。
上述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料在高效电催化析氧(OER)中的应用。
有益效果:与现有的技术相比,本发明的优点包括:
(1)将零维(0D)LaxSr1-xCoO3纳米颗粒与2D Ti3C2 MXene纳米片负载在导电泡沫镍上,利用2D MXene的光热性能提高LaxSr1-xCoO3的电催化性能。LaxSr1-xCoO3/Ti3C2 MXene/泡沫镍复合材料是通过金属离子与MXene表面的负电荷之间的静电作用在泡沫镍上原位生长钙钛矿型氧化物。通过强界面和电子耦合相互作用,LaxSr1-xCoO3/Ti3C2 MXene纳米片牢固地生长在泡沫镍表面上。
(2)在标准太阳光照射下,该光热-电化学协同催化的泡沫镍复合材料具有高达81.2%的转换效率和1.58kg m-2h-1的水蒸发速率。
(3)在标准太阳光照射下,该复合材料在三电极系统中的1.0mol L-1KOH溶液中,10mA cm-2的电流密度下的过电势低至290mV,Tafel斜率为83.2mV dec-1。
(4)本发明光热协同电催化复合材料能够在盐水、重金属、强酸碱性废水中均具有优异的光热蒸发性能。
(5)本发明泡沫镍基复合材料具有突出的光热蒸发速率和效率以及电催化性能,制备原料不含贵金属元素,制备工艺简单,造价成本低,可重复性高,易于大批量生产,在海水淡化、污水处理、电催化等领域具有广泛的应用前景。
附图说明
图1为光热协同电催化La0.9Sr0.1CoO3/Ti3C2 MXene/NF复合材料合成流程图;
图2为LMN的透射显微镜图像(2a),LMN复合材料的扫描电子显微镜图像(2b),Ti3C2MXene、La0.9Sr0.1CoO3、Ti3C2 MXene/La0.9Sr0.1CoO3功能材料的X射线衍射图(2c);
图3为LMN复合材料表面亲水性测试图(3a),泡沫镍、LSC1、LSC1-NF与LMN复合材料在250-2500nm太阳光波长范围内的吸收光谱(3b),在光功率密度为1kW m-2的光照强度下,使用泡沫镍、LSC1、LSC1-NF与LMN复合材料制备的光热蒸发器,水的蒸发重量损失结果图(3c),在光功率密度为1kW m-2的光照强度下,使用泡沫镍、LSC1、LSC1-NF与LMN复合材料制备的光热蒸发器对应的光热蒸发水速率和蒸发效率结果图(3d);
图4为一个光功率密度为1kW m-2的光照强度下,LMN复合材料光热蒸发器的循环稳定性测试结果图(4a),使用LMN复合材料光热蒸发器进行光热蒸发前后海水和废水中的离子浓度变化结果图(4b);
图5为在1mol L-1KOH溶液中,Ti3C2 MXene、LSC1-NF与LMN催化剂在无光和有光照射下的线性扫描伏安图(5a),在1mol L-1KOH溶液中,Ti3C2 MXene、LSC1-NF、LMN在无光和有光照射下的Tafel拟合曲线图(5b),在1mol L-1KOH溶液中,Ti3C2 MXene、LSC1-N、LMN复合光热电催化剂在光功率密度为1kW/m2的光照强度下的CV循环曲线图(5c),催化剂在OER反应式的长期稳定性测试结果图(5d);
图6为光热协同电催化产氧一体化装置示意图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。
实施例1
如图1所示,光热协同电催化La0.9Sr0.1CoO3/Ti3C2 MXene/NF复合材料的制备方法,包括以下步骤:
(1)称取0.5g Ti3AlC2(MAX),2.96g的NH4F,并量取20mL的HCl,在60℃水浴搅拌持续48h,得到黑色糊状液体。待完全冷却至室温后,将高压反应釜内黑色糊状液体转移至离心管内,用9000rpm转速离心8min,并用去离子水清洗,如此重复三次,直到pH=6,将离心的底物冷冻干燥14h,得到Ti3C2 MXene固体纳米片;
(2)取二甲亚砜(DMSO)50mL,倒入锥形瓶内,并加入Ti3C2 MXene固体,通入氮气(N2)保护并保持在25℃,同时用磁力搅拌子以15rpm转速搅拌48h;然后以9000rpm的转速离心8min,用去离子水清洗,并震荡5min,如此洗涤三次后冷冻干燥12h,得到剥离后的Ti3C2MXene纳米片;
(3)将泡沫镍剪裁至25mm*25mm大小的片状,浸泡在1mol L-1的盐酸溶液中,低速搅拌,去除泡沫镍表面氧化物,然后用去离子水反复浸泡去除表面盐酸,冷冻干燥,得到泡沫镍基底材料;
(4)称取0.39g六水合硝酸镧(La(NO3)3·6H2O),0.291g六水合硝酸钴(Co(NO3)2·6H2O),0.0212g硝酸锶(Sr(NO3)2),0.280g六亚甲基四胺,加入20mL去离子水和20mL甲醇,获得前驱体溶液,然后加入0.05g剥离后的Ti3C2 MXene纳米片充分搅拌,加入KOH粉末,调整pH至10;
(5)将泡沫镍基底材料加入步骤(4)溶液中,水热反应200℃保持48h;然后,以5℃min-1的升温速率升温至600℃,在氮气氛下热处理120min,得到La0.9Sr0.1CoO3/Ti3C2MXene/NF复合材料,该样品记为LMN。
通过透射电子显微镜图像(图2a)与LMN的X射线衍射图(图2c)可以看出,在泡沫镍上形成了La0.9Sr0.1CoO3/Ti3C2 MXene纳米片。通过对冷冻干燥后复合材料的扫描电子显微镜图(图2b),可得钙钛矿纳米片表面具有多孔结构,可以显著提高催化剂的比表面积,提高活性位点。
通过对复合材料进行表面接触角测试(图3a),LMN催化剂表现出较好的亲水性。通过紫外-可见-近红外吸收光谱分析可以发现,LMN催化剂对波长范围为250-2500nm的光谱均具有较好的吸收能力,吸收率高达91.21%(图3b)。在光功率密度为1kW/m2的光照强度下,LMN功能光热蒸发器呈现出较好的光热蒸发性能,蒸发速率能够达到1.58kg m-2h-1(图3d),光热转换效率为81.2%(图3d)。
通过测试LMN功能光热蒸发器的光热循环稳定性(图4a),可得LMN在光功率密度为1kW/m2的光照强度下,10小时内表现出较好的光热蒸发稳定性。
与此同时,测试LMN复合催化剂的电化学分解水性能,可得该催化剂在无光和有光照射下的OER极化曲线(图5a)和Tafel斜率测试(图5b)。实验结果可得,LMN复合光热催化剂在光功率密度为1kW/m2的光照强度下,在1.0mol L-1KOH溶液中,10mAcm-2的电流密度下的过电势仅为290mV,Tafel斜率为83.2mV dec-1。因此,光热效应有效增强LMN催化剂的电催化析氧特性。该性能测试结果证明了La0.9Sr0.1CoO3/Ti3C2 MXene/Ni复合光热催化剂可以应用于光热海水淡化的同时,进行电化学分解水产氧,实现纯水与能源的协同产出,有效缓解淡水资源匮乏和绿色能源紧缺。
图6为光热协同电催化产氧一体化装置示意图。采用高透亚克力材料作为装置外壳,太阳能电池板为LMN复合材料电解水析氧提供清洁电能,同时产生的氧气通过软管用排水集气法收集,太阳光驱动LMN复合材料光热污水净化协同氧气能源收集。
采用复合材料La0.9Sr0.1CoO3/Ti3C2 MXene/NF(LMN)作为测试样品,在1mol L-1KOH溶液中评估OER活性。与单相La0.9Sr0.1CoO3电催化剂相比,LMN在10mA cm-2的电流密度下,它的过电势低至300mV。并且,该复合材料的Tafel斜率低于La0.9Sr0.1CoO3纳米片,意味着复合材料发生的OER动力学要快得多。结果表明,LMN复合材料的优异OER性能归因于导电Ti3C2MXene、La0.9Sr0.1CoO3纳米片以及泡沫镍之间的协同增强作用。
对比例1
钙钛矿La0.9Sr0.1CoO3的制备方法,包括以下步骤:
(1)称取0.39g六水合硝酸镧(La(NO3)3·6H2O),0.291g六水合硝酸钴(Co(NO3)2·6H2O),0.0212g硝酸锶(Sr(NO3)2)和0.05g剥离后的Ti3C2 MXene纳米片,加入20mL去离子水和20mL甲醇,充分搅拌获得前驱体溶液;
(2)称取少量的KOH固体,用研钵研磨成颗粒较小的粉末,然后逐渐加入前驱体溶液内,同时用pH计测量其酸碱浓度,直到获得pH=10的前驱体溶液;
(3)将前驱体液倒入反应釜进行高温水热反应,在200℃的条件下水热48h,然后将液体以用8000rpm转速离心8min,得到离心的底物;
(4)将底物冷冻干燥14h,然后平铺在刚玉磁舟内,放入箱式炉内,以10℃min-1的升温速率在空气氛围中1000℃煅烧120min,得到钙钛矿La0.9Sr0.1CoO3,该粉体记为LSC1。
通过紫外可见近红外吸收光谱分析可以发现,LSC1功能粉体对波长250-2500nm的光谱具有较强的光吸收能力,吸收率为82.32%(图3b)。在光功率密度为1kW/m2的光照强度下,LSC1功能光热蒸发器呈现出较好的光热蒸发性能,蒸发速率能够达到1.24kg m-2h-1(图3d),光热转换效率为67.3%(图3d)。
对比例2
La0.9Sr0.1CoO3/NF复合材料的制备方法,包括以下步骤:
(1)称取0.39g六水合硝酸镧(La(NO3)3·6H2O),0.291g六水合硝酸钴(Co(NO3)2·6H2O),0.0212g硝酸锶(Sr(NO3)2)和0.05g剥离后的Ti3C2 MXene纳米片,加入20mL去离子水和20mL甲醇,充分搅拌获得前驱体溶液;
(2)将泡沫镍片用4.0mol L-1的盐酸溶液超声清洗,后用去离子水冲洗;
(3)将泡沫镍片加入前驱体溶液,加入KOH粉末,调节pH至10,水热反应200℃保持48h。然后将含有前驱体物质的泡沫镍取出,冷冻干燥12h;
(4)将干燥的复合泡沫镍放入气氛炉中,在氮气氛围内,以5℃min-1的升温速率升温至600℃煅烧保温120min,得到La0.9Sr0.1CoO3/NF复合材料,该样品记为LSC1-NF。
通过紫外可见近红外吸收光谱分析可以发现,LSC1-NF对波长250-2500nm的光谱具有较好的吸收能力,吸收率为90.32%(图3b)。在光功率密度为1kW/m2的光照强度下,LSC1-NF功能光热蒸发器呈现出较好的光热蒸发性能,蒸发速率能够达到1.42kg m-2h-1(图3d),光热转换效率为73.2%(图3d)。同时,通过测试复合催化剂的极化曲线(图5a)和Tafel斜率(图5b),LSC1-NF在1.0mol L-1KOH溶液中,10mA cm-2的电流密度下的过电势为390mV,Tafel斜率为117.8mV dec-1。
Claims (7)
1.一种钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,其特征在于,将零维La x Sr1-x CoO3纳米颗粒与2D Ti3C2 MXene纳米片负载在导电泡沫镍上,制得钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料;包括以下步骤:
(1)分别称量硝酸镧、硝酸锶、硝酸钴、六亚甲基四胺,并加入超纯水和甲醇溶液,配置前驱体溶液;
(2)向步骤(1)所述前驱体溶液中,加入Ti3C2 MXene光热材料,并缓慢加入氢氧化钾粉末,低速搅拌,使其混合均匀,调整pH=10;
(3)将泡沫镍基底材料用1.0 mol L-1的盐酸溶液清洗后浸没在步骤(2)所述溶液中进行水热反应,反应结束后冷冻干燥,然后进行高温煅烧,得到钙钛矿氧化物/Ti3C2 MXene/泡沫镍基复合材料;水热反应温度为200℃,反应时间为48 h。
2.根据权利要求1所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,其特征在于,配制前驱体溶液时,硝酸镧、硝酸锶、硝酸钴和六亚甲基四胺的质量比为3.9:0.2:2.9:2.8,去离子水和甲醇的体积比为1:1。
3.根据权利要求1所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,其特征在于,所述Ti3C2 MXene与硝酸钴的质量比为0.5:2.9。
4.根据权利要求1所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料的制备方法,其特征在于,所述高温煅烧过程使用管式炉,并在氮气氛下,煅烧温度为600 ℃,煅烧2 h。
5.权利要求1~4任一所述方法制备得到的钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料。
6.权利要求5所述钙钛矿氧化物/Ti3C2 MXene/泡沫镍复合材料在海水和重金属、强酸碱性废水光热蒸发净化中的应用。
7.权利要求5所述钙钛矿氧化物/Ti3C2MXene/泡沫镍复合材料在高效电催化析氧中的应用。
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