CN106914236A - 高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶 - Google Patents
高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶 Download PDFInfo
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- CN106914236A CN106914236A CN201710164082.7A CN201710164082A CN106914236A CN 106914236 A CN106914236 A CN 106914236A CN 201710164082 A CN201710164082 A CN 201710164082A CN 106914236 A CN106914236 A CN 106914236A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 76
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000004065 semiconductor Substances 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000010970 precious metal Substances 0.000 claims description 9
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 238000006722 reduction reaction Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910010252 TiO3 Inorganic materials 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 229910011011 Ti(OH)4 Inorganic materials 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000011260 aqueous acid Substances 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 238000005034 decoration Methods 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910001510 metal chloride Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 14
- 230000000844 anti-bacterial effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229960002163 hydrogen peroxide Drugs 0.000 description 3
- 230000004298 light response Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000002546 antimould Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种具有高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶及其制备方法与应用,其是以贵金属与纳米TiO2,或其它半导体‑贵金属与纳米TiO2之间通过化学连接形成的异质结结构体为纳米微粒组成单元构成,可利用贵金属与纳米TiO2或其他半导体‑贵金属与纳米TiO2之间协同产生的肖特基结与局域表面等离子体共振效应获得优异的可见光光催化效果,解决了常规TiO2光催化剂可见光利用率低的问题。
Description
技术领域
本发明属于光催化材料制备领域,具体涉及一种具有高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶及其制备方法与应用。
背景技术
随着社会发展和人们生活水平的提高,环境污染日益影响到人们的健康,而半导体TiO2光催化材料对环境中各种污染物的明显去除效果已引起世界的广泛关注。在大于其带隙能光照条件下,TiO2光催化剂能完全降解环境中的有害有机物,还可氧化去除大气中的氮氧化物和硫化物等有毒气体。另外,TiO2光催化材料还具有杀菌、除臭、表面自清洁等功能,可进一步净化、改善我们的生活环境。然而,TiO2可见光利用率低的缺点限制了其应用范围。为促进TiO2光催化材料的实用化,必须提高其光催化性能,扩宽其光响应范围。已报道的解决方法包括:表面光敏化、离子掺杂、贵金属沉积、复合半导体等,但受各种因素限制,以上方法各自有其不足之处,使现有市场上还未出现相应实用性产品。
本发明制备的纳米TiO2是一种具有高效可见光响应型的非晶态等离子体异质结纳米TiO2溶胶,该溶胶的纳米微粒组成单元是以贵金属-纳米TiO2、其它半导体-贵金属-纳米TiO2之间通过化学连接形成的异质结结构体,其利用贵金属与TiO2半导体或半导体-贵金属与纳米TiO2之间协同产生的肖特基结与局域表面等离子体共振效应获得优异的可见光光催化效果,解决了常规TiO2光催化剂可见光利用率低的问题。
发明内容
本发明的目的是提供一种具有高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶及其制备方法与应用,其合成工艺简单,制备的纳米溶胶中二氧化钛粒子为非晶态,分散性良好,具有高效的可见光光催化活性及良好的贮存稳定性,并具有良好抗菌、防霉作用。
为实现上述目的,本发明采用如下技术方案:
一种高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶,其是以贵金属与纳米TiO2,或其它半导体-贵金属与纳米TiO2之间通过化学连接形成的异质结结构体为纳米微粒组成单元构成的;
所述纳米TiO2为非晶态纳米TiO2;
所述贵金属包括金、银、铂、钌、铑、钯、锇、铱或其氧化物中的任意一种;
所述其它半导体包括SiO2、SnO2、ZnO、Fe2O3、WO3、Sr(TiO3)中的任意一种或几种。
所述溶胶中贵金属或其它半导体-贵金属所占质量为0.01~2‰;纳米TiO2所占质量为0.5~3%。
所述非晶态等离子体异质结纳米TiO2溶胶的方法包括以下步骤:
1)液相法制备过氧化钛水溶液:将钛酸酯或钛酸盐在激烈搅拌条件下溶于酸性水溶液中,加碱经水解反应得Ti(OH)4沉淀;所得Ti(OH)4沉淀经离心、洗涤去除杂质后,搅拌分散于双氧水中,制得质量浓度为0.5~6%的过氧化钛水溶液;
2)非晶态纳米TiO2溶胶的制备:在步骤1)所得过氧化钛水溶液中加入晶型转换控制剂,在搅拌条件下加热回流,制备非晶态纳米TiO2溶胶;
3)非晶态等离子体异质结纳米TiO2溶胶的制备:在步骤2)制备的非晶态纳米TiO2溶胶中加入贵金属盐水溶液或其它半导体纳米溶胶与贵金属盐水溶液的混合物,超声分散后,在超声条件下利用光化学还原反应,对非晶态纳米TiO2溶胶进行等离子体异质结结构改性。
其中,步骤1)中所述酸性水溶液为pH=1的盐酸、硝酸或硫酸的水溶液;
所述钛酸酯为有机钛酸酯,如钛酸四丁酯,钛酸异丙酯等,所述钛酸盐为钛的无机盐,如四氯化钛、硫酸氧钛等;钛酸酯或钛酸盐在酸性水溶液中的摩尔浓度为0.1~2mol/L;
所述水解反应的条件为:温度0~20℃,pH值6~10,反应时间为0.5~2小时;
Ti(OH)4与双氧水的摩尔比为1:20~4。
步骤2)中晶型转换控制剂的用量与过氧化钛的摩尔比为0.05~2:1;
所述晶型转换控制剂为纳米SiO2、SnO2、ZnO、Fe2O3、WO3、Sr(TiO3)中的任意一种或几种;
所述加热回流的温度为60~100℃,回流时间为1~12小时。
步骤3)中所述贵金属盐水溶液中贵金属离子的浓度为1~3000ppm;所述贵金属盐为贵金属氯化物或贵金属硝酸盐,如氯化铁、硝酸银、硝酸铜、氯金酸、氯铂酸等;
所述超声分散的条件为:超声功率400~1000W,时间为5~30min;
所述光化学还原反应的条件为:光照波长245~400nm,光照强度1~20mw/cm2,反应温度20~60℃,反应时间0.5~2小时。
所述非晶态等离子体异质结纳米TiO2溶胶在可见光下能有效去除室内有毒、有害及异味气体,净化室内空气,可直接涂覆于室内墙壁、天花板、家具、家居饰品表面,以改善生活环境,并具有抗菌、防霉的作用,。
本发明所制备的纳米溶胶是一种非晶态纳米TiO2溶胶。光催化材料的光学吸收特性在一定程度上决定其光吸收能力的强弱,而材料的光吸收特性取决于其所具有的能带结构,由于非晶态纳米TiO2具有“短程有序,长程无序”的结构特点,使其具有与晶态纳米TiO2不同的能带结构:价带和导带之间有电子态的存在,使电子跃迁能够在价带和导带之间的电子态之间发生,从而使非晶态纳米TiO2可以吸收利用能量较低、波长较长的可见光,激发电子在价带和导带之间的电子态之间发生跃迁,由此形成的电子-空穴对也会参与到光催化反应过程中。
本发明所制备的纳米溶胶也是一种等离子体异质结构纳米TiO2溶胶。等离子体光催化剂是近年来发展迅速的一种在可见光下可以高效响应的光催化剂,其组成单元为贵金属(及其化合物)与半导体材料之间通过化学连接形成的异质结结构,金属与半导体之间形成的肖特基接触不但可以促进光生电子-空穴对的有效分离,并且可以提供有益于电子转移的快速电荷转移通道,利用二者之间协同产生的肖特基接触与局域表面等离子体共振(LSPR)效应可以获得优异的可见光光催化效果,包括A、良好的可见光响应;B、有效的增强光吸收;C、减小光生电子-空穴对的扩散距离;D、增强局域电场效应;E、LSPR直接诱导的电子-空穴分离;F、局域加热效应;G、分子极化效应。
本发明的另一技术特点在于,在采用溶胶-凝胶法制备纳米二氧化钛光催化剂溶胶的过程中,通过引入贵金属离子进行改性,在TiO2晶格内引入缺陷位、改变其结晶度或提高其表面羟基位,从而影响其电子-空穴对的复合和表面氧化还原反应,提高其光催化性能;同时,由于贵金属离子的掺杂,使纳米TiO2的光谱吸收产生一定的红移,实现了扩宽其光响应范围的目的;且利用部分贵金属离子(银、铜等)本身具有较好的抗菌性能,可使所得溶胶具备双重抗菌、防霉性能。
本发明所制备的纳米溶胶具有以下优点和积极效果:
1)本发明所用原料价格便宜、易得,特别是钛的无机盐。
2)本发明制备过程简单、易行,无需高温、高压。
3)本发明制备的纳米溶胶中二氧化钛粒子为非晶态、分散性良好。
4)本发明所制备的溶胶可在室温下贮存二年以上,其各种性能仍保持不变,与常规的溶胶-凝胶法制备的光催化剂溶胶相比更稳定。
5)本发明制备的纳米溶胶可见光响应明显,在可见光下光催化效果显著。
6)按GB/T 30706-2014《可见光照射下光催化抗菌材料及制品抗菌性能测试方法及评价》标准试验条件进行测试,本发明所制备的纳米溶胶抗菌、防霉性能优异。
附图说明
图1为实施例3制得的非晶态等离子异质结纳米TiO2溶胶的TEM图。
图2为实施例3制得的非晶态等离子异质结纳米TiO2溶胶经50℃烘干后的XRD衍射图。
图3为实施例3制得的非晶态等离子异质结纳米TiO2溶胶与市售常规TiO2溶胶的UV-Vis图。
图4为实施例3制得的非晶态等离子异质结纳米TiO2溶胶与市售常规TiO2溶胶的可见光响应效果图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1:水性过氧化钛溶液的制备
1)在冰水浴条件下将0.1mol的TiOSO4以1滴/s的速度滴入强烈搅拌的1000mL pH=1的硫酸水溶液中,制得0.1mol/L的TiOSO4溶液;
2)用氨水调节溶液的pH值至8,离心得到Ti(OH)4沉淀;
3)将所得Ti(OH)4沉淀用去离子水洗涤10遍;
4)将洗涤后的Ti(OH)4沉淀分散于400mL质量浓度为10%的过氧化氢溶液中,制备得到质量浓度为2%的水性过氧化钛溶液。
实施例2:非晶态纳米TiO2溶胶的制备:
将0.5克30wt%的纳米SiO2水分散液(晶型转换控制剂)加入实施例1制备的400mL水性过氧化钛溶液中,常温下搅拌30分钟,然后将溶液升温至80℃,并保温回流8小时,制得非晶态纳米TiO2溶胶。
实施例3:非晶态等离子异质结构纳米TiO2溶胶的制备:
在实施例2制备的非晶态纳米TiO2溶胶中加入4克的硝酸银溶液(银粒子浓度为1000ppm),600W超声分散10min后,在超声条件下,于温度20℃、400nm光照波长、10mw/cm2光照强度下光化学还原反应0.5小时,得到非晶态等离子异质结构纳米TiO2溶胶。
图1为所得非晶态等离子异质结构纳米TiO2溶胶的TEM图。由图1可见,所得溶胶样品的异质结结构体纳米微粒单元是由内部相互连接的更为微小的纳米银(黑体)与纳米TiO2(阴隐体)组成的。
图2为所得非晶态等离子异质结构纳米TiO2溶胶的XRD图。由图2可见,所得溶胶样品中纳米TiO2为非晶态。
图3为所得非晶态等离子异质结构纳米TiO2溶胶与常规TiO2溶胶的UV-Vis图,其中A为常规TiO2溶胶,B为非晶态等离子异质结纳米TiO2溶胶。图3表明,与常规TiO2相比,本发明所得溶胶在可见光范围内的吸收强度明显增强。
1. 可见光响应试验:
1.1光降解空白
准备250 mL 10 mg/L的罗丹明B溶液,在可见光(反应液面的光强为500 Lux)下进行搅拌反应120 min,每隔20 min进行取样,以水为对照(起始吸光度A0),测试溶液在554 nm波长处的吸光度值,得到不同时间光降解空白反应溶液的吸光度Ap;
1.2 暗反应
准备250 mL含有10 mg/L的罗丹明B以及0.1 g有效固体成分TiO2溶胶的反应液,在暗条件下搅拌反应120 min,每隔20 min取样测试,得到不同时间暗条件下反应溶液的吸光度Ad;
1.3 光降解反应
准备250 mL含有10 mg/L的罗丹明B以及0.1 g有效固体成分TiO2溶胶的反应液,在可见光(反应液面的光强为500 Lux)下搅拌120 min进行光解实验,每隔20 min取样测试,得到的不同时间光降解溶液的吸光度Ac;
1.4 数据处理:降解率=(Ap+Ad-Ac-A0)/A0。
按上述方法将实施例3制备的溶胶与常规市售的不同知名品牌TiO2溶胶进行可见光响应试验。
图4为实施例3制得的非晶态等离子异质结纳米TiO2溶胶与市售常规TiO2溶胶的可见光响应效果图。由图4可见,本发明非晶态等离子异质结纳米TiO2溶胶在20分钟内对罗丹明B的降解率即可达到70%以上,在80分钟内对罗丹明B的降解率可达到97%以上,明显高于常规TiO2溶胶。
2. 抗菌效果试验:
将实施例3所制备的溶胶及常规TiO2溶胶直接涂覆于玻璃片表面,按GB/T 30706-2014《可见光照射下光催化抗菌材料及制品抗菌性能测试方法及评价》标准试验条件分别进行测试,结果如表2。
表2 抗菌试验结果
由表2可见,在可见光条件下,本发明溶胶具有较强的抗菌作用。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (9)
1.一种高效可见光响应的非晶态等离子体异质结纳米TiO2溶胶,其特征在于:所述非晶态等离子体异质结纳米TiO2溶胶是以贵金属与纳米TiO2,或其它半导体-贵金属与纳米TiO2之间通过化学连接形成的异质结结构体为纳米微粒组成单元构成的;
所述纳米TiO2为非晶态纳米TiO2;
所述贵金属包括金、银、铂、钌、铑、钯、锇、铱或其氧化物中的任意一种;
所述其它半导体包括SiO2、SnO2、ZnO、Fe2O3、WO3、Sr(TiO3)中的任意一种或几种。
2.如权利要求1所述的非晶态等离子体异质结纳米TiO2溶胶,其特征在于:所述溶胶中贵金属或其它半导体-贵金属所占质量为0.01~2‰;纳米TiO2所占质量为0.5~3%。
3.一种制备如权利要求1所述非晶态等离子体异质结纳米TiO2溶胶的方法,其特征在于:包括以下步骤:
1)使用液相法制备质量浓度为0.5~6%的过氧化钛水溶液;
2)在步骤1)所得过氧化钛水溶液中加入晶型转换控制剂,在搅拌条件下加热回流,制备非晶态纳米TiO2溶胶;
3)在步骤2)制备的非晶态纳米TiO2溶胶中加入贵金属盐水溶液或其它半导体纳米溶胶与贵金属盐水溶液的混合物,超声分散后,在超声条件下利用光化学还原反应,对非晶态纳米TiO2溶胶进行等离子体异质结结构改性。
4.根据权利要求3所述非晶态等离子体异质结纳米TiO2溶胶的制备方法,其特征在于:步骤1)中液相法制备过氧化钛水溶液的具体操作包括:将钛酸酯或钛酸盐在激烈搅拌条件下溶于酸性水溶液中,加碱经水解反应得Ti(OH)4沉淀,再将Ti(OH)4沉淀搅拌分散于双氧水中制得;
所述酸性水溶液为pH=1的盐酸、硝酸或硫酸的水溶液;
所述钛酸酯为有机钛酸酯,所述钛酸盐为钛的无机盐;其在酸性水溶液中的摩尔浓度为0.1~2mol/L;
所述水解反应的条件为:温度0~20℃,pH值6~10,反应时间为0.5~2小时;
Ti(OH)4与双氧水的摩尔比为1:20~4。
5.根据权利要求3所述非晶态等离子体异质结纳米TiO2溶胶的制备方法,其特征在于:步骤2)中晶型转换控制剂的用量与过氧化钛的摩尔比为0.05~2:1;
所述晶型转换控制剂为纳米SiO2、SnO2、ZnO、Fe2O3、WO3、Sr(TiO3)中的任意一种或几种。
6.根据权利要求3所述非晶态等离子体异质结纳米TiO2溶胶的制备方法,其特征在于:步骤2)中加热回流的温度为60~100℃,回流时间为1~12小时。
7.根据权利要求3所述非晶态等离子体异质结纳米TiO2溶胶的制备方法,其特征在于:步骤3)中所述贵金属盐水溶液中贵金属离子的浓度为1~3000ppm;
所述贵金属盐为贵金属氯化物或贵金属硝酸盐。
8.根据权利要求3所述非晶态等离子体异质结纳米TiO2溶胶的制备方法,其特征在于:步骤3)中超声分散的条件为:超声功率400~1000W,时间为5~30min;
光化学还原反应的条件为:光照波长245~400nm,光照强度1~20mw/cm2,反应温度20~60℃,反应时间0.5~2小时。
9.一种如权利要求1所述非晶态等离子体异质结纳米TiO2溶胶的应用,其特征在于:将所述非晶态等离子体异质结纳米TiO2溶胶直接涂覆于室内墙壁、天花板、家具、家居饰品表面。
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