CN115449840A - 一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其电催化应用 - Google Patents
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Abstract
本发明涉及一种P‑MoO2/P‑Fe3O4异质结构纳米带的制备方法及其电催化应用，具体的说是将α‑MoO3粉末溶解在H2O2溶液中，采用水热合成法得到α‑MoO3纳米带；然后将α‑MoO3纳米带和Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在Ar氛围中加热，得到P‑MoO2/P‑Fe3O4异质结构纳米带；该P‑MoO2/P‑Fe3O4异质结构纳米带在电催化水氧化反应和电催化水分解反应中的应用。
Description
技术领域
本发明涉及一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其电催化应用，属于材料的制备及其应用领域。
背景技术
Mo基氧化物包含MoO3、MoO2等形式，价格低廉，制备方法简单，引起了人们极大的研究兴趣。其中，MoO2是因Mo的价电子为4d2，具有一定的导电性。电催化分解水是绿色制备氢气的重要途径。MoO2电催化分解水能力较弱，因此调控MoO2表面结构实现高效催化水分解，具有重要的理论和现实意义。
杂原子掺杂、构建异质结构、形成缺陷位等方法可以有效调控材料电子结构，暴露更多的活性位点。例如：Lyu等利用ZIF-67和Na2MoO4合成了CoO-MoO2纳米笼，实现了在低电压下催化水分解氧气，当电压为312mV时，电催化水氧化为10mA/cm2(Advanced FunctionalMaterials,2017；27(34):1702324)。Wang等利用(NH4)6Mo7O2·4H2O、Na2WO4·2H2O和NaH2PO2合成了(P,W)-MoO2/NF，实现了在低电压下表现出良好的电解水反应活性，当电压为308mV时，电催化水氧化为40mA/cm2(Applied Surface Science，2020；529:146987)。Zhou等通过构建Ni-MoO2@SCG复合材料，在常温下催化水反应中具有较高的活性，当电压为278mV时，电催化水氧化为10mA/cm2(Journal of Electroanalytical Chemistry，2021；897:115555)。综上所述，形貌可控调变MoO2实现高效电催化水氧化反应、电催化分解水反应的研究较少。
研究表明电解水可以高效制备氢气，是实现绿色能源解决环境问题的挑战。因此P掺杂、增加空位、构建P-MoO2/P-Fe3O4异质界面结构，对调控MoO2制备高活性、高稳定性的电解水分解催化剂具有重要的现实意义。
发明内容：
本发明旨在提供一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其电催化应用。
基于上述目的，本发明所涉及的技术方案如下：
(1)一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法：将α-MoO3粉末溶解在H2O2溶液中，采用水热合成法在140-200℃下反应2-24h，将反应得到的产物离心，干燥得到α-MoO3纳米带；然后将α-MoO3纳米带和Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在Ar氛围中加热，得到P-MoO2/P-Fe3O4异质结构纳米带。
上述的制备方法，所述α-MoO3粉末质量为0.5-2g，H2O2溶液体积为5-20mL。
上述的制备方法，所述α-MoO3纳米带的宽度为90-300nm、长度为400-6000nm。
上述的制备方法，所述α-MoO3纳米带的质量为20-40mg，Fe(NO3)3·9H2O的质量为20-40g，NaH2PO2·H2O的质量为0.5-2g。
上述的制备方法，所述然后将α-MoO3纳米带和Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在10-30mL/min Ar氛围中加热，加热温度为200-400℃，加热时间为1-5小时。
上述的制备方法，所述P-MoO2/P-Fe3O4异质结构纳米带宽度为120-300nm、长度为350-7000nm，P/Mo/Fe摩尔比为(1-2):(10-13):(0.05-2)。
上述的制备方法，所述P-MoO2/P-Fe3O4异质结构纳米带中P掺杂MoO2、P掺杂Fe3O4形成异质结构，MoO2晶相归属于标准卡片JCPDS#32-0671，Fe3O4晶相归属于标准卡片JCPDS#19-0629。
(2)一种上述的制备方法制备得到的P-MoO2/P-Fe3O4异质结构纳米带在电催化水氧化反应和电催化水分解反应中的应用；电催化水氧化反应，电压为1.48-1.5V时电流密度为10mA/cm2；电催化水分解反应，电压为1.7-1.72V时电流密度为10mA/cm2。
本发明具有如下优点：
1)利用α-MoO3、Fe(NO3)3·9H2O为前驱体，采用磷化的工艺制备了P-MoO2/P-Fe3O4异质结构纳米带，开发了P-MoO2/P-Fe3O4异质结构纳米带的新合成路径。
2)P-MoO2/P-Fe3O4异质结构纳米带在电催化水氧化反应和电催化水分解反应中具有较好的性能。
3)本发明具有方法简单易操作的优点。
附图说明：
图1是P-MoO2/P-Fe3O4异质结构纳米带的表征结果；(a)XRD，(b,c)SEM，(d-f)TEM，(g-j)P、Mo、O、Fe的Mapping。
具体实施方式
下列实施例用来进一步说明本发明，但不因此而限制本发明。
实施例1
一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法：将1.4gα-MoO3粉末溶解在11mLH2O2溶液中，采用水热合成法在170℃下反应12h，将反应得到的产物离心，干燥得到宽度为90-260nm、长度为500-6000nm的α-MoO3纳米带；然后将25mgα-MoO3纳米带和25mg Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取1g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在20mL/min流速的Ar氛围中350℃加热2h，得到140-240nm、长度为400-6500nm的P-MoO2/P-Fe3O4异质结构纳米带，P/Mo/Fe摩尔比为1:10:0.05。将该P-MoO2/P-Fe3O4异质结构纳米带、Nafion、乙醇按照5mg、25μL、500μL比例混合，将0.6mg/cm2混合液涂到Ni电极上，将其在电催化水氧化反应和电催化水分解反应中应用；电催化水氧化反应，电压为1.5V时电流密度为10mA/cm2；电催化水分解反应，电压为1.72V时电流密度为10mA/cm2。
实施例2
一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法：将0.5gα-MoO3粉末溶解在5mLH2O2溶液中，采用水热合成法在140℃下反应2h，将反应得到的产物离心，干燥得到宽度为90-300nm、长度为400-6000nm的α-MoO3纳米带；然后将20mgα-MoO3纳米带和20mg Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取0.5g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在10mL/min流速的Ar氛围中200℃加热1h，得到120-300nm、长度为350-7000nm的P-MoO2/P-Fe3O4异质结构纳米带，P/Mo/Fe摩尔比为2:13:2。将该P-MoO2/P-Fe3O4异质结构纳米带、Nafion、乙醇按照5mg、25μL、500μL比例混合，将0.6mg/cm2混合液涂到Ni电极上，将其在电催化水氧化反应和电催化水分解反应中应用；电催化水氧化反应，电压为1.48V时电流密度为10mA/cm2；电催化水分解反应，电压为1.71V时电流密度为10mA/cm2。
实施例3
一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法：将2gα-MoO3粉末溶解在20mLH2O2溶液中，采用水热合成法在200℃下反应24h，将反应得到的产物离心，干燥得到宽度为100-300nm、长度为400-5000nm的α-MoO3纳米带；然后将40mgα-MoO3纳米带和40mg Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取2g NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在30mL/min流速的Ar氛围中400℃加热5h，得到120-240nm、长度为350-6500nm的P-MoO2/P-Fe3O4异质结构纳米带，P/Mo/Fe摩尔比为1.5:11:1.5。将该P-MoO2/P-Fe3O4异质结构纳米带、Nafion、乙醇按照5mg、25μL、500μL比例混合，将0.6mg/cm2混合液涂到Ni电极上，将其在电催化水氧化反应和电催化水分解反应中应用；电催化水氧化反应，电压为1.49V时电流密度为10mA/cm2；电催化水分解反应，电压为1.7V时电流密度为10mA/cm2。
Claims (5)
1.一种P-MoO2/P-Fe3O4异质结构纳米带的制备方法其特征在于，包括以下步骤：
将α-MoO3粉末溶解在H2O2溶液中，采用水热合成法在140-200℃下反应2-24h，将反应得到的产物离心，干燥得到α-MoO3纳米带；然后将α-MoO3纳米带和Fe(NO3)3·9H2O的混合物研磨均匀，然后放入瓷舟中；取NaH2PO2·H2O放入另一个瓷舟中，将两个瓷舟放入管式炉中，其中装有NaH2PO2·H2O的瓷舟放置在上游，在Ar氛围中加热，得到P-MoO2/P-Fe3O4异质结构纳米带。
2.如权利要求1所述的制备方法，其特征在于，α-MoO3粉末的质量为0.5-2g，H2O2溶液体积为5-20mL，所得到α-MoO3纳米带宽度为90-300nm，长度为400-6000nm。
3.如权利要求1所述的制备方法，其特征在于，20-40mgα-MoO3纳米带和20-40mg Fe(NO3)3·9H2O的混合物研磨均匀，NaH2PO2·H2O的质量为0.5-2g，Ar流速为10-30mL/min，加热1-5小时。
4.一种由权利要求1-3任一项所述的制备方法制备得到的P-MoO2/P-Fe3O4异质结构纳米带，其特征在于，所述P-MoO2/P-Fe3O4异质结构纳米带宽度为120-300nm、长度为350-7000nm，P/Mo/Fe摩尔比为(1-2):(10-13):(0.05-2)，所述P-MoO2/P-Fe3O4异质结构纳米带中P掺杂MoO2、P掺杂Fe3O4形成异质结构，MoO2晶相归属于标准卡片JCPDS#32-0671，Fe3O4晶相归属于标准卡片JCPDS#19-0629。
5.一种由权利要求1-3任一项所述的制备方法制备得到的P-MoO2/P-Fe3O4异质结构纳米带在电催化中的应用；电催化水氧化反应，电压为1.48-1.5V时电流密度为10mA/cm2；电催化水分解反应，电压为1.7-1.72V时电流密度为10mA/cm2。
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|---|---|---|---|---|
| CN115608387A (zh) * | 2022-09-21 | 2023-01-17 | 青岛科技大学 | P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用 |
| CN115608387B (zh) * | 2022-09-21 | 2024-03-12 | 青岛科技大学 | P-MoO3/P-MoO2/P-Fe3O4异质结构纳米带的制备方法及其光催化应用 |
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