CN108855193B - TaN/BiVO4异质结复合材料及其制备方法和应用 - Google Patents
TaN/BiVO4异质结复合材料及其制备方法和应用 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims abstract description 28
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 25
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000004070 electrodeposition Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 4
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 229940037003 alum Drugs 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 125000005595 acetylacetonate group Chemical group 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
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- 230000008021 deposition Effects 0.000 claims description 2
- 150000007529 inorganic bases Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
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- 239000004065 semiconductor Substances 0.000 abstract description 10
- 238000005215 recombination Methods 0.000 abstract description 4
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- 239000000243 solution Substances 0.000 description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000008363 phosphate buffer Substances 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 239000003504 photosensitizing agent Substances 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- CSWCIDWEGIREGN-UHFFFAOYSA-N [Bi].[W](=O)(=O)=O Chemical compound [Bi].[W](=O)(=O)=O CSWCIDWEGIREGN-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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Abstract
本发明涉及TaN/BiVO4异质结复合材料及其制备方法和应用。TaN/BiVO4异质结复合材料是采用浸渍的方法将氮化钽负载在钒酸铋上形成的异质结构的复合材料。本发明改善了单独半导体在光激发电子后，其电子和空穴再结合速率快的缺点，制备了一种TaN/BiVO4异质结复合材料，间接地加快了电荷与空穴的分离效率，进一步地提高了光激发的电子利用率，提高了光电催化效率。本发明通过修饰半导体，实现高效光电分解水。
Description
技术领域
本发明涉及光电解水催化领域，具体为通过制备Z-型异质结改善孤立半导体的缺陷，从而实现高效光电解水。
背景技术
全球化石能源的日益枯竭，能源危机已经日益显现出来。为了解决这一难题，人们将研究目光转移到可再生的和清洁的太阳能，利用太阳光分解水制氢已经逐渐成熟起来。但是由于种种限制因素，单纯的光解水制氢效率低，对材料的要求高，于是光电解水技术应用而生。光电解水体系主要由光敏剂、催化剂、电子受体三部分组成。
由于半导体具有良好的吸光性能，经常作为光敏剂材料，因此人们在不断地修饰改造半导体，用于实现光电解水产氢。但是半导体在光激发后产生的电子空穴对，其重结合效率较快，因此在半导体表面修饰催化剂是一种提高催化效果的方法，也可以通过形成异质结构，降低电子空穴对的再结合率，提高光电解水性能。常见的异质结结构，比如常见的三氧化钨钒酸铋异质结等其制备过程繁琐，并且光电催化效果低。
发明内容
为了解决上述技术问题，本发明的目的是改善单独半导体在光激发电子后，其电子和空穴再结合速率快的缺点，制备一种TaN/BiVO4异质结复合材料，间接地加快了电荷与空穴的分离效率，进一步地提高了光激发的电子利用率，提高了光电催化效率。
本发明采用的技术方案是：TaN/BiVO4异质结复合材料，所述的TaN/BiVO4异质结复合材料是采用浸渍的方法将氮化钽负载在钒酸铋上形成的异质结构的复合材料。
TaN/BiVO4异质结复合材料的制备方法，包括如下步骤：
1)制备钒酸铋基底：于含有硝酸铋、碘化钾和对苯醌的电沉积溶液中，采用三电极体系，在导电载体FTO上沉积一层BiOI膜，水洗，氮气吹干后，于BiOI膜上均匀滴加乙酰丙酮氧矾的DMSO溶液后，于450℃保温2h，冷却至室温后，放入无机碱溶液中浸泡 30min，取出，用水冲洗，氮气吹干，得钒酸铋基底；
2)制备TaN/BiVO4异质结复合材料：将钒酸铋基底浸入氮化钽水溶胶中，60℃保持30- 60min后，置于马弗炉中500℃煅烧2h。
上述的TaN/BiVO4异质结复合材料的制备方法，步骤1)中，所述的电沉积溶液的制备方法是：取适量去离子水，用硝酸调节其pH到1.7，加入硝酸铋和碘化钾，充分溶解后，加入对苯醌的乙醇溶液，充分搅拌，制成电沉积溶液。
上述的TaN/BiVO4异质结复合材料的制备方法，步骤1)中，采用三电极体系，沉积条件为：外加-0.1V vs Ag/AgCl的偏压沉积5分钟。
上述的TaN/BiVO4异质结复合材料的制备方法，步骤1)中，所述的无机碱为氢氧化钠或氢氧化钾。
上述的TaN/BiVO4异质结复合材料的制备方法，步骤2)中，所述的氮化钽的制备方法是：在氨气的条件下，将氧化钽于500℃下煅烧4h，形成氮化钽。
上述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤2)中，所述的氮化钽水溶胶的制备方法是：取氮化钽溶解于水中，超声，形成氮化钽水溶胶。优选的，氮化钽与水的料液比为：1g：(10-15)mL。
TaN/BiVO4异质结复合材料作为修饰电极在光催化分解水制氢中的应用。
本发明的有益效果是：本发明采用高温煅烧氧化钽的方法制备氮化钽。基于多孔性的钒酸铋，采用简单的浸渍法将氮化钽镶嵌在钒酸铋的空隙中形成异质结，相比于其他的方法，本方法在于操作简单，催化效果显著。
附图说明
图1为钒酸铋的扫描电镜图(SEM)。
图2为氮化钽的X射线衍射图(XRD)。
图3为TaN/BiVO4异质结复合材料的扫描电镜图(SEM)。
图4为TaN/BiVO4异质结复合材料在含有亚硫酸钠的线性扫描图(LSV)。
图5为TaN/BiVO4异质结复合材料在磷酸缓冲液中的线性扫描图(LSV)。
具体实施方式
为了更好地理解本发明的技术方案，特以具体的实施例作进一步详细说明，但方案不限于此。
实施例
(一)制备方法
1、电沉积溶液的制备
量取150ml去离子水，用硝酸调节其pH到1.7。加入2.91g硝酸铋和9.96g碘化钾，充分溶解后，加入20ml溶有1.49g对苯醌的乙醇溶液，充分搅拌，形成电沉积溶液。
2、钒酸铋基底的制备
采用三电极体系，外加-0.1V vs Ag/AgCl的偏压沉积5分钟，于导电载体FTO上沉积一层BiOI膜，用水清洗BiOI膜，氮气吹干。最后在BiOI膜上均匀滴加50微升的含有1.06g乙酰丙酮氧矾的DMSO溶液，于450℃保持2h。待其冷却到室温后，将其放入0.1M的氢氧化钠溶液中，大约浸泡30min后取出，用水冲洗，氮气吹干，得到淡黄色的多孔的钒酸铋基底。用氢氧化钠水溶液浸泡的目的是溶掉基底表面的五氧化钒等杂质。
3、块状氮化钽的合成
在氨气的条件下，将氧化钽于500℃下高温煅烧4h，升温速率为2℃/min，形成淡黄色的粉末，即为氮化钽。
4、氮化钽水溶胶的制备
取0.04g氮化钽溶解于50mL水中，超声，形成氮化钽水溶胶。
5、TaN/BiVO4异质结复合材料
将钒酸铋基底浸入氮化钽水溶胶中，60℃保持30-60min后，置于马弗炉中500℃煅烧2h。
(二)检测
1、图1为钒酸铋的扫描电镜图。由图1可见，钒酸铋是多孔状的均匀的结构，其孔道可以为氮化钽的负载提供适当的位置。
2、图2为氮化钽的X射线衍射图(XRD)。由图2可见，可以看到TaN的衍射峰，进一步证明氮化钽成功负载到钒酸铋上。
3、图3为TaN/BiVO4异质结复合材料的扫描电镜图(SEM)，从图中可以清楚地看到块状的氮化钽均匀地负载在多孔状的钒酸铋中。进一步证明本发明的可行性。
4、图4为TaN/BiVO4异质结复合材料在含有亚硫酸钠的线性扫描图(LSV)。从图中的 Linear Sweep Voltammetry(LSV)curves可以看到复合材料在含有亚硫酸钠的电解液中的光电流比单独的钒酸铋有明显的提高，进一步证明异质结的形成。
5、图5为TaN/BiVO4异质结复合材料在磷酸缓冲液中的线性扫描图(LSV)，从图中的 Linear Sweep Voltammetry(LSV)curves可以看出，在pH 7的磷酸缓冲溶液中，单独的钒酸铋的光催化性能较低，而TaN/BiVO4异质结复合材料其催化性能明显的提高，说明异质结能提高光解水的催化性能。
Claims (8)
1.TaN/BiVO4异质结复合材料的制备方法，其特征在于，包括如下步骤：
1）制备钒酸铋基底：于含有硝酸铋、碘化钾和对苯醌的电沉积溶液中，采用三电极体系，在导电载体FTO上沉积一层BiOI膜，水洗，氮气吹干后，于BiOI膜上均匀滴加乙酰丙酮氧矾的DMSO溶液后，于450℃保温2h，冷却至室温后，放入无机碱溶液中浸泡30min，取出，用水冲洗，氮气吹干，得钒酸铋基底；
2）制备TaN/BiVO4异质结复合材料：将钒酸铋基底浸入氮化钽水溶胶中，60℃ 保持30-60min后，置于马弗炉中500 ℃ 煅烧2h。
2.根据权利要求1所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤1）中，所述的电沉积溶液的制备方法是：取适量去离子水，用硝酸调节其pH到1.7，加入硝酸铋和碘化钾，充分溶解后，加入对苯醌的乙醇溶液，充分搅拌，制成电沉积溶液。
3.根据权利要求1所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤1）中，采用三电极体系，沉积条件为：外加-0.1 V vs Ag/AgCl 的偏压沉积5分钟。
4.根据权利要求1所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤1）中，所述的无机碱为氢氧化钠或氢氧化钾。
5.根据权利要求1所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤2）中，所述的氮化钽的制备方法是：在氨气的条件下，将氧化钽于500℃下煅烧4h，形成氮化钽。
6.根据权利要求1所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，步骤2）中，所述的氮化钽水溶胶的制备方法是：取氮化钽溶解于水中，超声，形成氮化钽水溶胶。
7.根据权利要求6所述的TaN/BiVO4异质结复合材料的制备方法，其特征在于，氮化钽与水的料液比为：1g：（10-15）mL。
8.按照权利要求1所述的方法制备的TaN/BiVO4异质结复合材料作为修饰电极在光催化分解水制氢中的应用。
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