不銹鋼網(wǎng)負(fù)載氫鈦酸納米線薄膜及其結(jié)構(gòu)、光催化性能優(yōu)化
發(fā)布時(shí)間:2018-05-23 23:19
本文選題:氫鈦酸 + 納米線薄膜; 參考:《浙江大學(xué)》2015年碩士論文
【摘要】:一維氫鈦酸及鈦酸鹽納米材料在光催化、染料敏化太陽(yáng)能電池、鋰電池電極、氣體傳感器、儲(chǔ)氫材料等領(lǐng)域具有廣泛的應(yīng)用前景。研發(fā)一種設(shè)備要求低、反應(yīng)溫和、操作簡(jiǎn)單且能夠適應(yīng)多襯底材料的氫鈦酸納米材料通用制備方法具有十分重要的意義。本文成功地在覆蓋TiO2籽晶層的不銹鋼網(wǎng)表面負(fù)載氫鈦酸納米線薄膜,研究了不同工藝參數(shù)對(duì)其形貌的影響,初步探索了“一鍋”制備大面積(-960cm2)不銹鋼網(wǎng)負(fù)載氫鈦酸納米線薄膜的放大實(shí)驗(yàn)。測(cè)試了薄膜的光催化降解染料羅丹明B性能,以及雙氧水、硫酸添加等對(duì)光催化效率的改善作用。采用熱水處理、熱處理等方法對(duì)制備的氫鈦酸納米線薄膜進(jìn)行結(jié)構(gòu)性能調(diào)控。最后,測(cè)試了大片樣品光催化降解羅丹明B、磺基水楊酸、苯酚等有機(jī)物的循環(huán)性能,以及市政自來(lái)水溶液體系中有機(jī)物的降解特性。論文獲得主要結(jié)論如下:1.氫鈦酸納米線薄膜的制備:在Ti-H2O2溶液體系中,以海綿鈦為鈦源,溶液中添加三聚胺和硝酸,80℃低溫環(huán)境下在覆蓋溶膠-凝膠TiO2籽晶層的不銹鋼網(wǎng)表面制備了均勻稠密的氫鈦酸納米線薄膜。系列工藝參數(shù)優(yōu)化試驗(yàn)結(jié)果表明,當(dāng)反應(yīng)時(shí)間6-48 h、雙氧水濃度20~30wt.%、硝酸量11.5~19.2 mL/L、三聚氰胺量0.385~1.93 g/L均可獲得稠密的氫鈦酸納米線薄膜,工藝穩(wěn)定性較好。放大實(shí)驗(yàn)顯示,通過(guò)兩次溶膠-凝膠浸漬提拉干燥熱處理制備TiO2籽晶層,可以在直徑35 em不銹鋼網(wǎng)基底上負(fù)載氫鈦酸納米線薄膜。2.氫鈦酸納米線薄膜光催化性能測(cè)試及改善:2.5×2.5 cm2不銹鋼網(wǎng)負(fù)載的氫鈦酸納米線薄膜光催化降解50 mL、初始濃度為0.005 mM的羅丹明B溶液,2 h降解率為82.1%,但循環(huán)穩(wěn)定性不理想。硫酸添加有利于光催化降解性能的提高,添加5×10-2M硫酸降解率提高18.9%。雙氧水的添加也有利于光催化降解性能的提高,添加20 ppm雙氧水,降解率提高17.3%,過(guò)高濃度的雙氧水則不利于光催化降解性能提高。3.氫鈦酸納米線薄膜的結(jié)構(gòu)和光催化性能調(diào)控:不銹鋼網(wǎng)負(fù)載氫鈦酸納米線薄膜經(jīng)80℃熱水處理48 h后,其光催化降解性能最優(yōu),此時(shí),氫鈦酸納米線分解轉(zhuǎn)化為納米顆粒堆積呈線狀的銳鈦礦TiO2;90℃熱水處理顯著加快氫鈦酸納米線轉(zhuǎn)化進(jìn)程。200℃爐熱處理1h后,氫鈦酸納米線形貌和結(jié)構(gòu)均未發(fā)生變化,但其光催化性能大幅下降;550℃爐熱處理1 h氫鈦酸納米線完全分解轉(zhuǎn)化為細(xì)小晶粒堆積的線狀銳鈦礦TiO2。大片樣品550℃爐熱處理1 h,添加20ppm雙氧水光催化降解初始濃度0.01 mM羅丹明B溶液循環(huán)降解10次仍能保持100%降解率,光催化降解10 mg/L磺基水楊酸溶液循環(huán)10次仍能保持90%降解率。添加20 ppm和未添加雙氧水光催化降解60 mg/L苯酚溶液2 h降解率分別為80.8%和48.5%。以杭州市政自來(lái)水配制的羅丹明B溶液和磺基水楊酸溶液為降解對(duì)象時(shí),光催化性能較去離子水配置的溶液均出現(xiàn)明顯下降現(xiàn)象。
[Abstract]:One-dimensional hydrotitanic acid and titanate nanomaterials have been widely used in photocatalysis, dye sensitized solar cells, lithium battery electrodes, gas sensors, hydrogen storage materials and so on. It is of great significance to develop a universal preparation method for hydrotitanic acid nanomaterials with low equipment requirements, mild reaction, simple operation and adaptability to multi-substrate materials. In this paper, the surface of stainless steel mesh coated with TiO2 seed layer has been successfully loaded with nanowires of hydrotitanate, and the influence of different process parameters on the morphology of the film has been studied. In this paper, the amplification experiment of a large area of stainless steel netted hydrogen titanate nanowire film prepared by "one pot" has been studied. The photocatalytic degradation of Rhodamine B and the improvement of photocatalytic efficiency by adding hydrogen peroxide and sulfuric acid were tested. The structure and properties of hydrotitanate nanowires were controlled by hot water treatment and heat treatment. At last, the cycling performance of Rhodamine B, sulfosalicylic acid, phenol and organic compounds in municipal tap water solution were tested by photocatalytic degradation of Rhodamine B, sulfosalicylic acid, phenol and so on. The main conclusions are as follows: 1: 1. Preparation of nanowire hydrotitanate thin films: in Ti-H2O2 solution system, sponge titanium was used as titanium source, Homogeneous and dense thin films of hydrogen titanate nanowires were prepared on the surface of stainless steel mesh coated with sol-gel TiO2 seed layer at 80 鈩,
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