CN107376928A - 一种一步法合成α‑Fe2O3/Bi复合物的方法 - Google Patents
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 7
- 238000001308 synthesis method Methods 0.000 title claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 235000011187 glycerol Nutrition 0.000 claims abstract description 4
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims abstract description 4
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 14
- 229910002651 NO3 Inorganic materials 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
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- 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 2
- 238000006243 chemical reaction Methods 0.000 claims 2
- 239000006194 liquid suspension Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 11
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052797 bismuth Inorganic materials 0.000 abstract description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 2
- 239000002994 raw material Substances 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
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- 230000000737 periodic effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
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- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
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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
- 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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Abstract
本发明公开了一种一步法合成α相氧化铁(α‑Fe2O3)/单质铋(Bi)复合物的方法，属于功能材料制备工艺技术领域。本发明采用Fe(NO3)3·9H2O和Bi(NO3)3·5H2O为原料，称取适量比例的原料溶于乙二醇，再加入KOH溶液获得前驱沉淀物，并加入适量十二烷基苯磺酸钠(SDBS)和丙三醇，充分搅拌均匀后移入水热反应釜，在170摄氏度反应50小时。待反应结束后，自然冷却至室温，离心清洗后，即可获得α‑Fe2O3/Bi复合物。本发明具有制备成本低，一步合成，工艺简单等优点。
Description
技术领域
本发明具体是一种一步法合成α-Fe2O3/Bi复合物的方法，属于功能材料制备工艺技术领域。
背景技术
α相氧化铁(α-Fe2O3)是一种典型的n型半导体金属氧化物，是最为稳定的铁氧化物，其带隙窄，大约为2.1eV，在可见光区域具有很强的光吸收能力，而且具有较强的光生空穴能力，因此，已被广泛用作可见光催化剂。而且，比表面积大的α-Fe2O3纳米材料是也可用作传感、气敏材料，具有较好的稳定性和较强的附着力强，可用于检测多种气体以及生物传感。另外，作为典型的铁氧化物，α-Fe2O3纳米材料具有矫顽力高、超顺磁性等特点，可以应用于各种磁性元件和磁性仪器方面。
虽然光电分解水制氢和光催化降解有机物都是α-Fe2O3重要应用，但是α-Fe2O3导带位置太低，不能够分解水制氧，而且光催化性能也不够理想。近些年的研究发现，通过引入贵金属材料如Ag，Au和Pt等可以作为增敏剂来构建复合材料，不仅可以提高半导体金属氧化物的光催化活性，而且可以提高气敏性能。不过贵金属材料成本较高，因此探索低成本的复合材料成为研究的重点。铋(Bi)元素位于元素周期表第6周期，第5主族，原子序数为83，Bi是一个不具有明显放射性的重元素，是所有已知稳定元素中原子质量最高的，而且，Bi元素处于周期表中金属区与半导体区之间，因此具有典型的半金属特征。大量的研究发现很多Bi基氧化物(如：Bi2WO6、Bi2MoO6、BiVO4等)都具有较高的光催化活性，这主要由于Bi的6s轨道于周围氧的2p轨道杂化形成的价带，能够使带隙变窄，同时可以増强光生空穴在价带上的迁移率。作为Bi基氧化物的重要组成，Bi单质也具有光催化活性，研究发现，Bi单质不仅对液相污染物有较好的光催化降解活性，对气体污染物也有一定的降解效果。因此，制备高质量的α-Fe2O3/Bi复合物具有极大的应用潜力。
发明内容
技术问题：本发明要解决的问题在于提供一种一步法合成α-Fe2O3/Bi复合物的方法，本制备工艺简单、结晶度较高，便于获得性能良好的α-Fe2O3/Bi复合物。
技术方案：本发明合成α-Fe2O3/Bi复合物的制备方法具体为：
称取适量比例的硝酸铁Fe(NO3)3·9H2O和硝酸铋Bi(NO3)3·5H2O，加入到20mL乙二醇中，搅拌至澄清前驱液。将氢氧化钾(KOH)溶液，缓慢逐滴滴入前驱液中，再加入表面活性剂，常温下搅拌12小时。将溶液配成37mL移入45mL的水热反应釜中，170摄氏度水热反应50小时，自然冷却后，经多次离心清洗，即可获得。
附图说明
图1是本发明的α-Fe2O3/Bi复合物的XRD图谱；
图2是本发明的α-Fe2O3/Bi复合物的SEM图谱，其中(a)为Fe(NO3)3·9H2O和Bi(NO3)3·5H2O的摩尔比1:1，(b)为Fe(NO3)3·9H2O和Bi(NO3)3·5H2O的摩尔比1:2，(c)为Fe(NO3)3·9H2O和Bi(NO3)3·5H2O的摩尔比2:1。
具体实施方式
下面结合实施实例和有关图表对本发明进行详细阐述，但本发明不限于所给实例：
实例1：
(1)Fe(NO3)3·9H2O和Bi(NO3)3·5H2O的摩尔比选用1:1，分别称取1.2093g的Fe(NO3)3·9H2O和2.4255g的Bi(NO3)3·5H2O加入到20mL乙二醇中，在磁力搅拌器上搅拌1小时，获得澄清前驱液。
(2)称取6.5g的KOH，超声溶于8mL去离子水中。在搅拌的情况下，将KOH溶液缓慢逐滴滴入上一步配置的前驱液中。
(3)在获得的悬浮液中加入0.2g十二烷基苯磺酸钠(SDBS)和0.5mL丙三醇，继续搅拌12个小时。
(4)将搅拌均匀的悬浮液添加适量去离子水，配置成37mL，移入45mL的水热反应釜中。将反应釜置入干燥箱中，170摄氏度温度下反应50个小时后，自然冷却至室温。将反应釜中的沉淀物离心清洗，即获得所需的α-Fe2O3/Bi复合物。
图1为所制备的α-Fe2O3/Bi复合物的XRD图谱，从图中可以看出样品的结晶度良好，基本没有杂相。其中“●”符号标出的α-Fe2O3，PDF标准卡为：89-0597；“◆”符号标出的Bi单质，PDF标准卡为：85-1329。图2(a)为样品的SEM图谱，图中尺寸较大的多边形为Bi单质，其上附着的絮状多空纳米颗粒为α-Fe2O3，其尺寸较小，附着的并不均匀。
实例2：
(1)Fe(NO3)3·9H2O和Bi(NO3)3·5H2O的摩尔比选用2:1，分别称取2.4186g的Fe(NO3)3·9H2O和2.4255g的Bi(NO3)3·5H2O加入到20mL乙二醇中，在磁力搅拌器上搅拌1小时，获得澄清前驱液。
(2)称取6.5g的KOH，超声溶于8mL去离子水中。在搅拌的情况下，将KOH溶液缓慢逐滴滴入上一步配置的前驱液中。
(3)在获得的悬浮液中加入0.2g十二烷基苯磺酸钠(SDBS)和0.5mL丙三醇，继续搅拌12个小时。
(4)将搅拌均匀的悬浮液添加适量去离子水，配置成37mL，移入45mL的水热反应釜中。将反应釜置入干燥箱中，170摄氏度温度下反应50个小时后，自然冷却至室温。将反应釜中的沉淀物离心清洗，即获得所需的α-Fe2O3/Bi复合物。
图2(c)为样品的SEM图谱，图中尺寸较大的多边形为Bi单质表面完全附着的絮状多空纳米颗粒为α-Fe2O3，附着的相对均匀。
Claims (1)
1.一种一步法合成α-Fe2O3/Bi复合物的方法，其特征在于，包括以下步骤：
1）称取适量比例的硝酸铁Fe(NO3)3·9H2O和硝酸铋Bi(NO3)3·5H2O，加入到20mL乙二醇中，搅拌至澄清前驱液；
2）称取6.5g的KOH，超声溶于8mL去离子水中，在搅拌的情况下，将KOH溶液缓慢逐滴滴入上一步配置的前驱液中，获得的沉淀物为反应的前驱体；
3）在上述获得的悬浮液中加入0.2g十二烷基苯磺酸钠（SDBS）和0.5mL丙三醇，搅拌12个小时；
4）将搅拌均匀的前驱体悬浮液添加适量去离子水，配置成37mL，移入45mL的水热反应釜中；将反应釜置入干燥箱中，170摄氏度温度下反应50个小时后，自然冷却至室温；将反应釜中的沉淀物离心清洗，即获得所需的α-Fe2O3/Bi复合物。
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| CN112156768A (zh) * | 2020-09-29 | 2021-01-01 | 重庆工商大学 | 复合光催化剂的制备方法及其应用 |
| CN114655992A (zh) * | 2020-12-23 | 2022-06-24 | 哈尔滨工业大学（深圳） | 一种铁酸铋纳米片材料及其制备方法及用途 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110034286A (zh) * | 2019-03-25 | 2019-07-19 | 天津大学 | 制备三氧化二铁-铋金属碳纤维复合材料及方法 |
| CN110034286B (zh) * | 2019-03-25 | 2022-03-15 | 天津大学 | 制备三氧化二铁-铋金属碳纤维复合材料及方法 |
| CN112156768A (zh) * | 2020-09-29 | 2021-01-01 | 重庆工商大学 | 复合光催化剂的制备方法及其应用 |
| CN112156768B (zh) * | 2020-09-29 | 2022-06-14 | 重庆工商大学 | 复合光催化剂的制备方法及其应用 |
| CN114655992A (zh) * | 2020-12-23 | 2022-06-24 | 哈尔滨工业大学（深圳） | 一种铁酸铋纳米片材料及其制备方法及用途 |
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