CN106111114B - 一种In2O3/Bi2Sn2O7复合可见光催化剂及其制备方法 - Google Patents
一种In2O3/Bi2Sn2O7复合可见光催化剂及其制备方法 Download PDFInfo
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 31
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 20
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 10
- 239000003643 water by type Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000011941 photocatalyst Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000001802 infusion Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
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- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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Abstract
本发明公开了一种型In2O3/Bi2Sn2O7复合可见光催化剂及其制备方法,该复合可见光催化剂包括Bi2Sn2O7颗粒及立方型In2O3块体;本发明使用水热法和浸渍法,即利用Bi2Sn2O7作为基体与In(NO)3混合物来制备In2O3/Bi2Sn2O7复合光催化剂;这种复合光催化剂可以减少电子空穴对的复合,能够有效提高太阳光的利用率;本发明的优点是:工艺简单,可控性好,协调性高。
Description
技术领域
本发明涉及复合可见光催化剂及其制备方法,特别涉及一种In2O3/Bi2Sn2O7复合可见光催化剂及其制备方法。
背景技术
随着环境污染问题越来越严重,人们也正面临着巨大的能源危机,解决当前严重的环境污染问题和能源短缺问题已迫在眉睫。其中,半导体光催化技术能够降解有机污染物和还原二氧化碳,已经被认为解决当前环境污染问题的重要手段。目前关于光催化性能及其光电转换效率优异的材料主要集中在TiO2、ZnO、SnO2以及铌酸盐等宽禁带半导体,通常这些半导体的带隙能在3eV以上,因此只能吸收紫外光部分,这极大地影响了光催化材料的催化性能。关于半导体材料的研究主要有两种方法:一是通过掺杂缩小带隙能的间距;二是通过制备复合材料,促进电子-空穴对的有效分离。
近年来由于部分铋基氧化物及其复合物(锡酸铋)因有层状结构且Bi 6s和02p 轨道的杂化使价带发生上移,从而使其具有较小的带隙和价带离散的特点,这将有利于光生电子从价带向导带迁移,在可见光下能分解水和有效降解有机污染物,成为一类有发展潜力的光催化材料。而In2O3作为一种光敏剂,常用来和宽带隙半导体复合,以提高材料的可见光催化性能。
在光催化剂应用中,将N型半导体材料制成复合材料主要是将能带相匹配的两种物质相结合,从而起减少电子和空穴复合率的作用,材料主要有TiO2,ZnO,ZrO2, SnO2和SiO2等。Bi2Sn2O7纳米颗粒虽然可以吸收可见光,但受光激发所形成的电子和空穴对的复合率较高。
发明内容
本发明的目的在于提供一种利用N型半导体In2O3与N型半导体Bi2Sn2O7制备成In2O3/Bi2Sn2O7复合可见光催化剂及其制备方法。
为达到上述目的,本发明In2O3/Bi2Sn2O7复合可见光催化剂由粒径为10-20nm的Bi2Sn2O7纳米颗粒附着在0.1μm的立方型In2O3块体上构成。
本发明的制备方法如下:
1)Bi2Sn2O7前驱物的制备
将3~5mol的Bi(NO3)3溶于30~60mL浓度为1mol/L的硝酸溶液里,搅拌得溶液 A;
将3~5mol的K2Sn2O3溶于30~60mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加1~3mol/L 的NaOH溶液至pH为10~12后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.2~0.6g的CTAB(十六烷基三甲基溴化铵)溶于15~30mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.1~0.3mol/L的NaOH 至pH为10~12得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗, 75℃烘干得Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将0.1~1.4g的In(NO3)3溶于10~50mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,400-500 ℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
本发明的In2O3/Bi2Sn2O7复合可见光催化剂是将Bi2Sn2O7纳米颗粒分散到In(NO3)3的乙醇溶液中,然后通过退火使得Bi2Sn2O7纳米颗粒附着在立方型In2O3块体表面上,从而形成复合材料,光催化反应进行时可以达到电子-空穴的有效分离。
由于在光催化剂应用中,将N型半导体材料制成复合材料主要是将能带相匹配的两种物质相结合,从而起减少电子和空穴复合率的作用。Bi2Sn2O7纳米颗粒虽然可以吸收可见光,但受光激发所形成的电子和空穴对的复合率较高,因此为增加对太阳光更大范围内的有效利用并促进电子和空穴的有效分离,本发明通过使用立方型In2O3与Bi2Sn2O7纳米颗粒进行复合,即利用退火法将Bi2Sn2O7纳米颗粒附着在立方型In2O3块体上来制备能带结构相匹配的In2O3/Bi2Sn2O7复合可见光催化剂。所述能带结构相匹配是指Bi2Sn2O7的价带和导带位置与In2O3的导带和价带位置可以形成典型的Ⅱ型异质结结构,通过将Bi2Sn2O7纳米颗粒附着在立方型In2O3块体上,在Bi2Sn2O7与In2O3的接触面上形成活性中心,Bi2Sn2O7纳米颗粒受光激发后,导带上电子会转移到In2O3的导带上,而In2O3受光激发在价带上生成的空穴会转移到Bi2Sn2O7的价带上,这些活性物质经过不同的反应过程可实现对水中污染物的有效降解,即实现电子和空穴的有效分离,提高半导体材料的光催化效率。在保证Bi2Sn2O7对可见光仍有吸收的情况下,还能够使可见光吸收范围变宽且电子和空穴能有效分离的复合催化剂。
本发明均采用湿化学方法制备In2O3/Bi2Sn2O7复合可见光催化剂,工艺简单,可控性好,协调性高。
附图说明
图1是本发明制备的In2O3/Bi2Sn2O7复合可见光催化剂结构示意图;其中分散的黑点是Bi2Sn2O7纳米颗粒,立方型块体为In2O3。
图2是在可见光照下,0.1In2O3/Bi2Sn2O7复合可见光催化剂和0.1In2O3/Bi2Sn2O7混合光催化剂对罗丹明B的降解曲线。
具体实施方式
实施例1:
1)Bi2Sn2O7前驱物的制备
将5mol的Bi(NO3)3溶于50mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将5mol的K2Sn2O3溶于50mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加2mol/L的 NaOH溶液至pH为12后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得 Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.5g的CTAB(十六烷基三甲基溴化铵)溶于25mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.1mol/L的NaOH至pH为10 得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得 Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将0.1g的In(NO3)3溶于10mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,400℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
由图1可看出所制备的In2O3/Bi2Sn2O7复合可见光催化剂由粒径为10-20nm的Bi2Sn2O7纳米颗粒附着在0.1μm左右的立方型In2O3块体上构成。
对比例1
1)Bi2Sn2O7的制备
将5mol Bi(NO3)3溶于50mL1mol/L的硝酸溶液里,搅拌1h,溶液A;将5mol 的K2Sn2O3溶于50mL5℃的超纯水中,溶液B;将溶液B逐滴加到A中得混合物A;搅拌0.5h后,滴加2mol/LNaOH溶液,至混合物A的pH为12,将混合物A转移到 50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用200mL超纯水和 200mL无水乙醇分别清洗三次,75℃烘干5h,得产物B。
2)In2O3的制备
将5mmol的In(NO3)3溶于50mL无水乙醇中,搅拌1h,溶液C;在80℃下加热,蒸干溶剂,产物C,将产物C置于马弗炉中,400-500℃退火3h。降至室温后,备用。
3)In2O3/Bi2Sn2O7的制备
将0.15g的In2O3和1g的Bi2Sn2O7加到10mL乙醇中得混合物D;超声0.5h,然后搅拌3h,在80℃下加热,蒸干溶剂,产物E。
将产物E在400-500℃退火3h,降至室温得In2O3-Bi2Sn2O7混合光催化剂。
将实施例1与对比例进行光催化性能测试,由图2可以看出对比In2O3-Bi2Sn2O7机械共混、In2O3和Bi2Sn2O7材料,0.1In2O3/Bi2Sn2O7复合材料表现出最好的光催化性能。
实施例2:
1)Bi2Sn2O7前驱物的制备
将3mol的Bi(NO3)3溶于30mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将4mol的K2Sn2O3溶于40mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加1mol/L的 NaOH溶液至pH为11后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得 Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.3g的CTAB(十六烷基三甲基溴化铵)溶于18mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.2mol/L的NaOH至pH为12 得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得 Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将0.5g的In(NO3)3溶于20mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,450℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
实施例3:
1)Bi2Sn2O7前驱物的制备
将4mol的Bi(NO3)3溶于40mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将3.5mol的K2Sn2O3溶于35mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加3mol/L的 NaOH溶液至pH为10后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得 Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.6g的CTAB(十六烷基三甲基溴化铵)溶于30mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.3mol/L的NaOH至pH为11 得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得 Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将0.8g的In(NO3)3溶于30mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,500℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
实施例4:
1)Bi2Sn2O7前驱物的制备
将3.5mol的Bi(NO3)3溶于45mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将3mol的K2Sn2O3溶于30mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加1.5mol/L 的NaOH溶液至pH为11后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得 Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.2g的CTAB(十六烷基三甲基溴化铵)溶于15mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.3mol/L的NaOH至pH为10 得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得 Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将1.0g的In(NO3)3溶于40mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,480℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
实施例5:
1)Bi2Sn2O7前驱物的制备
将4.5mol的Bi(NO3)3溶于60mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将4.5mol的K2Sn2O3溶于60mL5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加2.5mol/L 的NaOH溶液至pH为12后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得 Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.4g的CTAB(十六烷基三甲基溴化铵)溶于20mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.1mol/L的NaOH至pH为12 得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得 Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将1.4g的In(NO3)3溶于50mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,420℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
Claims (1)
1.一种In2O3/Bi2Sn2O7复合可见光催化剂的制备方法,其特征在于:
1)Bi2Sn2O7前驱物的制备
将3~5mol的Bi(NO3)3溶于30~60mL浓度为1mol/L的硝酸溶液里,搅拌得溶液A;
将3~5mol的K2Sn2O3溶于30~60mL 5℃的超纯水中得溶液B;
将溶液B逐滴加到溶液A中搅拌均匀得混合物C;向混合物C中滴加1~3mol/L的NaOH溶液至pH为10~12后离心,并用超纯水和无水乙醇分别清洗,在75℃烘干得Bi2Sn2O7前驱物;
2)Bi2Sn2O7的制备
将0.2~0.6g的CTAB溶于15~30mL超纯水中搅拌均匀得溶液D;将Bi2Sn2O7前驱物分散到溶液D中搅拌均匀后,滴加0.1~0.3mol/L的NaOH至pH为10~12得混合物E;将混合物E转移到50mL的聚四氟乙烯内胆中,180℃下保持24h,冷却至室温后,用100~200mL超纯水和200~400mL无水乙醇分别清洗,75℃烘干得Bi2Sn2O7;
3)In2O3/Bi2Sn2O7的制备
将0.1~1.4g的In(NO3)3溶于10~50mL无水乙醇中,搅拌均匀得溶液F;将Bi2Sn2O7分散到溶液F中,搅拌5h,在80℃下加热,蒸干溶剂后的产物置于马弗炉中,400-500℃退火3h,降至室温后得In2O3/Bi2Sn2O7复合可见光催化剂。
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