CN106268804A - 一步水热技术制备Ag2O/Ag2WO4纳米棒的方法 - Google Patents
一步水热技术制备Ag2O/Ag2WO4纳米棒的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 238000013019 agitation Methods 0.000 claims abstract description 3
- 239000002131 composite material Substances 0.000 claims abstract description 3
- 239000012153 distilled water Substances 0.000 claims abstract description 3
- 238000012856 packing Methods 0.000 claims abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 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 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
本发明属于一步水热法制备Ag2WO4/Ag2O纳米棒的方法。将摩尔比为2:1的硝酸银和钨酸钠加入蒸馏水中，搅拌30 min，在搅拌下将硝酸银溶液滴加入钨酸钠溶液中，此悬浊液呈黄色，再搅拌30 min，用1 mol/L NaOH调节溶液pH等于14，此时悬浊液呈黑色，搅拌30 min，再次测量pH值，超声分散30 min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中，充填度为75 %，于160 oC加热24 h。反应结束后，将此悬浊液用去离子水超声洗涤2次，无水乙醇洗涤一次，将洗涤后的沉淀放入真空干燥箱50 oC烘干，得Ag2O/Ag2WO4复合材料。此方法简单易行，可重复性高。可按比例扩大批量生产；在低维纳米材料的制备及应用方面有广阔的前景。
Description
技术领域
本发明属于纳米材料制备的技术领域，特别涉及了一种一步水热法制备Ag2WO4/Ag2O纳米棒的方法。
背景技术
半导体光催化技术由于对环境污染物具有降解彻底、节约能源和无二次污染等优点而成为在诸多环境污染治理技术方面最有前途的方法之一。半导体光催化是由光催化剂通过吸收光能在导带和价带分别产生具有极强还原能力的光生电子和氧化能力的光生空穴，在催化剂表面发生直接或间接的还原或氧化反应。然而，该技术广泛使用的TiO2光催化剂具有光生电子－空穴对复合几率较高、太阳光利用率低而且成本较高等缺点，大大制约了光催化技术在废水处理中的应用。因此，人们在对TiO2进行改性研究的同时不断寻找开发新型光催化材料。近年来，高活性光催化剂的开发已成为光催化领域研究的主要内容。目前报道的新型光催化剂有钨酸盐、铌酸盐、钽酸盐、钒酸盐等。目前，人们对于钨酸银的研究比较少，是因为钨酸盐在微酸性溶液中可聚合成同多酸盐，控制不同的条件可得聚合程度不同的同多酸盐，所以制备钨酸银有Ag2WO4、二聚体Ag4W2O8、 三聚体Ag6W3O12、四聚体Ag8W4O16等。
Ag2O作为另一种重要的P型窄带隙半导体材料，已在感光材料、光记忆材料、光电转换器件等方面获得了广泛的应用。但是，单一的Ag2O半导体对光子利用率低，且易发生光腐蚀生成单质Ag。
发明内容
本发明的目的是要提供一种一步水热技术制备Ag2O/Ag2WO4纳米棒的方法，克服了单一Ag2O不稳定的特点，并得到了没有多聚的Ag2WO4，而且由于形成了Ag2O/Ag2WO4异质结，使得光生电子-空穴对更容易分离，有利于提高催化剂的光催化效率。
本发明的技术方案是：
Ag2O/Ag2WO4的一步制备方法，先取硝酸银和钨酸钠，摩尔比为2:1，所采用原料均为分析纯，分别将硝酸银和钨酸钠加入蒸馏水中，搅拌30 min，在搅拌下将硝酸银溶液滴加入钨酸钠溶液中，此悬浊液呈黄色，再搅拌30 min，用1 mol/L NaOH调节溶液pH等于14，此时悬浊液呈黑色，搅拌30 min，再次测量pH是否仍为14，超声分散30 min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中进行水热反应。反应结束后，将此悬浊液用去离子水超声洗涤2次，无水乙醇洗涤一次，将洗涤后的沉淀放入真空干燥箱50 oC烘干，得到黑色粉末，即为Ag2O/Ag2WO4复合材料。
本发明的有益效果是：
1、本发明要解决的技术问题是，公开一种水热法的Ag2O/Ag2WO4一步制备方法；此方法简单易行，可重复性高。可按比例扩大批量生产；在低维纳米材料的制备及应用方面有广阔的前景。
2、本发明在Ag2O/Ag2WO4纳米棒的制备中，所用的原料，只是钨酸钠和硝酸银，不需要任何助剂及模版剂。
3、Ag2O/Ag2WO4纳米棒克服了单一Ag2O不稳定的特点，并得到了没有多聚的Ag2WO4，而且由于形成了Ag2O/Ag2WO4异质结，使得光生电子-空穴对更容易分离，有利于提高催化剂的光催化效率。
附图说明
图1 Ag2O/Ag2WO4纳米棒制备流程示意图
图2 所制备Ag2O/Ag2WO4纳米棒的XRD图
图3 所制备Ag2O/Ag2WO4纳米棒的SEM照片。
具体实施方式
2 mmol硝酸银加入5mL水中，1 mmol钨酸钠加入10mL水中，分别搅拌30 min，将硝酸银溶液滴加入钨酸钠溶液中，此悬浊液呈黄色，再搅拌30 min，用1 mol/L NaOH调节溶液pH等于14，此时悬浊液呈黑色，搅拌30 min，再次测量pH是否仍为14，超声分散30 min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中，充填度为75 %，于160 oC加热24 h。反应结束后，将此悬浊液用去离子水超声洗涤2次，无水乙醇洗涤一次，将洗涤后的沉淀放入真空干燥箱50 oC烘干，得到黑色粉末，即为Ag2O/Ag2WO4纳米棒。
图1为所制备Ag2O/Ag2WO4纳米棒的XRD图。从图中可以观察到Ag2O（JCPDS No. 41-1104）和Ag2WO4（JCPDS No. 34-0061）的衍射峰。说明所制备样品为Ag2O/Ag2WO4复合物。没有观察到任何杂相的衍射峰，且衍射峰尖锐，说明样品的结晶程度较高。
图2为所制备Ag2O/Ag2WO4纳米棒的SEM图。从图中可以看出所制备样品的形貌为棒状，直径约为100 nm，长度可达几微米。
Claims (2)
1.一种Ag2O/Ag2WO4的一步制备方法，其特征在于：先取硝酸银和钨酸钠，摩尔比为2:1，所采用原料均为分析纯，分别将硝酸银和钨酸钠加入蒸馏水中，搅拌30 min，在搅拌下将硝酸银溶液滴加入钨酸钠溶液中，此悬浊液呈黄色，再搅拌30 min，用1 mol/L NaOH调节溶液pH等于14，此时悬浊液呈黑色，搅拌30 min，再次测量pH是否仍为14，超声分散30 min后将悬浊液加入聚四氟乙烯内衬的不锈钢反应釜中进行水热反应；反应结束后，将此悬浊液用去离子水超声洗涤2次，无水乙醇洗涤一次，将洗涤后的沉淀放入真空干燥箱50 oC烘干，得到黑色粉末，即为Ag2O/Ag2WO4复合材料。
2.根据权利要求1所述的一种Ag2O/Ag2WO4的一步制备方法，其特征在于：所述水热反应条件是充填度为75 %，于160 oC加热24 h。
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Cited By (6)
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| CN107051558A (zh) * | 2017-03-30 | 2017-08-18 | 常州大学 | 一种钨酸银复合磷酸银光催化剂的制备方法 |
| CN107096549A (zh) * | 2017-03-30 | 2017-08-29 | 常州大学 | 一种钨酸银复合溴化银光催化剂的制备方法 |
| CN107884446A (zh) * | 2017-11-07 | 2018-04-06 | 钟永松 | 一种基于多元金属氧化物敏感材料的乙醇气体传感器 |
| CN107884445A (zh) * | 2017-11-07 | 2018-04-06 | 潘柏霖 | 一种用于车辆的安全监测系统 |
| CN108558230A (zh) * | 2018-03-12 | 2018-09-21 | 华南理工大学 | 具有高可见光光催化性能的氧化银钨青铜复合隔热材料及其制备方法 |
| CN115646514A (zh) * | 2022-10-26 | 2023-01-31 | 洛阳理工学院 | 一种富含氧空位钨酸银/溴氧化铋纳米光催化剂制备方法 |
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| CN108558230A (zh) * | 2018-03-12 | 2018-09-21 | 华南理工大学 | 具有高可见光光催化性能的氧化银钨青铜复合隔热材料及其制备方法 |
| CN115646514A (zh) * | 2022-10-26 | 2023-01-31 | 洛阳理工学院 | 一种富含氧空位钨酸银/溴氧化铋纳米光催化剂制备方法 |
| CN115646514B (zh) * | 2022-10-26 | 2024-01-26 | 洛阳理工学院 | 一种富含氧空位钨酸银/溴氧化铋纳米光催化剂制备方法 |
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