ZnS基納米復(fù)合材料的制備及光催化性能研究
發(fā)布時(shí)間：2018-09-12 13:44
【摘要】：半導(dǎo)體光催化劑因環(huán)保節(jié)能等優(yōu)點(diǎn)在環(huán)境治理,特別是在水體有機(jī)污染物降解方面發(fā)揮了巨大的作用。在眾多半導(dǎo)體光催化劑中,ZnS因具有優(yōu)異的性能備受人們的關(guān)注。但ZnS半導(dǎo)體材料因具有較寬的禁帶,只對(duì)紫外光有響應(yīng),致使ZnS對(duì)太陽光的利用率較低。近年來,通過摻雜或復(fù)合來提高半導(dǎo)體光催化劑對(duì)污染物的降解效率已成為催化領(lǐng)域研究的熱點(diǎn)之一。在本文中,我們以硫化物半導(dǎo)體材料為主體進(jìn)行研究,采用水熱法、高溫煅燒、離子交換等方法,結(jié)合材料本身的容度積等物理化學(xué)性質(zhì),制備了CdS/ZnS納米片,Co、Mn共摻雜ZnS納米球,ZnO/CdS/ZnS納米球等納米復(fù)合材料,并對(duì)制備的產(chǎn)物進(jìn)行光催化活性研究。主要包括以下3個(gè)方面：(1) CdS/ZnS納米片的制備及光催化活性研究：通過水熱法制備ZnS(en)0.5前驅(qū)體,以ZnS(en)0.5前驅(qū)體和氯化鎘為原料,利用離子交換法和水熱法成功制備了CdS/ZnS納米片。利用SEM、XRD、XPS、UV-Vis、TEM等對(duì)樣品的組成、結(jié)構(gòu)及形貌進(jìn)行表征。XRD結(jié)果表明,隨著鎘摻雜量的增加,CdS/ZnS納米片的衍射峰依次向小角度方向移動(dòng),說明我們所制備的樣品是ZnS和CdS的復(fù)合材料,而不是ZnS和CdS的物理混合；從SEM圖像可清楚的觀察到ZnS(en)0.5前驅(qū)體和CdS/ZnS納米片是由厚度均勻的納米片組成。之后,以CdS/ZnS納米片為光催化劑,甲基橙為模擬污染物進(jìn)行光催化降解實(shí)驗(yàn)。實(shí)驗(yàn)結(jié)果表明,當(dāng)Cd/Zn的摩爾比等于0.8時(shí)(即CZ0.8),片狀CdS/ZnS納米復(fù)合材料具有最好的催化活性,將10mg樣品CZ0.8加入到50ml甲基橙水溶液(濃度為10mg/L)中,在可見光下照射60min,甲基橙溶液的降解率為99%。(2) Co、Mn共摻雜ZnS納米球的制備及光催化活性研究：首先利用水熱法制備Mn摻雜ZnS納米球,然后通過離子交換法摻雜第三種金屬離子Co,制備Co、Mn共摻雜ZnS納米球復(fù)合材料。利用XRD、UV-Vis及SEM等對(duì)所得樣品進(jìn)行表征。SEM圖表明樣品是由許多直徑在400nm左右的球形顆粒組成。之后,分別以ZnS,Co摻雜ZnS, Mn摻雜ZnS和Co、Mn共摻雜ZnS納米球?yàn)楣獯呋瘎?甲基橙水溶液為模擬污染物,進(jìn)行光催化降解實(shí)驗(yàn)。實(shí)驗(yàn)結(jié)果證明,Co、Mn共摻雜ZnS納米球具有最好的催化活性,當(dāng)向50ml甲基橙水溶液(濃度為3mg/L)中加入20mmg此催化劑,可見光照射下,90min的降解率為96.7%。(3) ZnO/CdS/ZnS納米球的制備及光催化活性研究：通過水熱法制備ZnS納米球,以ZnS為基礎(chǔ),分別利用高溫煅燒、離子交換等方法制備CdS/ZnS納米球、ZnO/CdS/ZnS納米球。利用SEM、XRD、XPS、UV-Vis等對(duì)其組成、形貌和性能進(jìn)行表征。SEM圖顯示樣品ZnO/CdS/ZnS是由許多粒徑均一、表面粗糙的納米球組成。之后以甲基橙為模擬污染物,對(duì)四種樣品的光催化性能進(jìn)行研究。結(jié)果表明,ZnO/CdS/ZnS納米球具有最好的催化活性,將20mg ZnO/CdS/ZnS納米球分散到50ml 10mg/L的甲基橙溶液中,可見光照射下,60min的降解率為96.8%。
[Abstract]:Semiconductor photocatalysts play an important role in environmental control, especially in the degradation of organic pollutants in water because of the advantages of environmental protection and energy saving. Among many semiconductor photocatalysts, ZnS has attracted much attention because of its excellent properties. However, the ZnS semiconductor material has a wide band gap and only responds to ultraviolet light, which results in a low utilization rate of solar light for ZnS. In recent years, improving the degradation efficiency of semiconductor photocatalyst by doping or recombination has become one of the hot spots in the field of catalysis. In this paper, we take sulfide semiconductor materials as the main body of research, adopt hydrothermal method, high temperature calcination, ion exchange and other physical and chemical properties, such as volume product of materials, etc. Co-doped CdS/ZnS nanospheres, ZnS nanospheres and ZnS / ZnS nanospheres were prepared and their photocatalytic activity was studied. The main contents are as follows: (1) the preparation and photocatalytic activity of CdS/ZnS nanoparticles: ZnS (en) 0.5 precursors were prepared by hydrothermal method, and CdS/ZnS nanoparticles were successfully prepared by ion exchange method and hydrothermal method using ZnS (en) 0.5 precursor and cadmium chloride as raw materials. SEM,XRD,XPS,UV-Vis,TEM was used to characterize the composition, structure and morphology of the samples. The results showed that the diffraction peaks of CDs / ZnS nanocrystals shifted to small angles with the increase of CD doping content, indicating that the samples we prepared were composites of ZnS and CdS. Instead of the physical mixing of ZnS and CdS, it can be clearly observed from the SEM images that the ZnS (en) 0.5 precursor and CdS/ZnS nanocrystals are composed of uniform thickness nanocrystals. After that, the photocatalytic degradation of methyl orange was carried out using CdS/ZnS nanoparticles as photocatalyst and methyl orange as simulated pollutant. The experimental results show that when the molar ratio of Cd/Zn is equal to 0.8 (that is, CZ0.8), the flake CdS/ZnS nanocomposites have the best catalytic activity. The 10mg sample CZ0.8 is added to the 50ml methyl orange aqueous solution (the concentration is 10mg/L). Under visible light irradiation for 60 min, the degradation rate of methyl orange solution was 99%. (2) preparation and photocatalytic activity of Co,Mn co-doped ZnS nanospheres: firstly, Mn doped ZnS nanospheres were prepared by hydrothermal method. Then Co,Mn co-doped ZnS nanospheres were prepared by doping a third metal ion Co, by ion exchange method. XRD,UV-Vis and SEM were used to characterize the samples. The results showed that the samples were made up of many spherical particles about the diameter of 400nm. Then the photocatalytic degradation experiments were carried out using ZnS and Co,Mn co-doped ZnS nanospheres doped with ZnS,Co and ZnS, Mn as photocatalysts and methyl orange aqueous solution as simulated pollutants respectively. The experimental results show that the codoped ZnS nanospheres have the best catalytic activity. 20mmg is added to the 50ml methyl orange aqueous solution (concentration of 3mg/L). (3) preparation and photocatalytic activity of ZnO/CdS/ZnS nanospheres: ZnS nanospheres were prepared by hydrothermal method. Based on ZnS, CdS/ZnS nanospheres were prepared by high temperature calcination and ion exchange respectively. SEM,XRD,XPS,UV-Vis was used to characterize its composition, morphology and properties. The results showed that the ZnO/CdS/ZnS was composed of many nanospheres with uniform particle size and rough surface. The photocatalytic properties of four kinds of samples were studied with methyl orange as the simulated pollutant. The results show that ZnO / CDs / ZnS nanospheres have the best catalytic activity. When 20mg ZnO/CdS/ZnS nanospheres are dispersed into 50ml 10mg/L methyl orange solution, the degradation rate of 50ml 10mg/L nanospheres is 96.8g under visible light irradiation for 60min.
【學(xué)位授予單位】：河南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB33;O643.36
[Abstract]:Semiconductor photocatalysts play an important role in environmental control, especially in the degradation of organic pollutants in water because of the advantages of environmental protection and energy saving. Among many semiconductor photocatalysts, ZnS has attracted much attention because of its excellent properties. However, the ZnS semiconductor material has a wide band gap and only responds to ultraviolet light, which results in a low utilization rate of solar light for ZnS. In recent years, improving the degradation efficiency of semiconductor photocatalyst by doping or recombination has become one of the hot spots in the field of catalysis. In this paper, we take sulfide semiconductor materials as the main body of research, adopt hydrothermal method, high temperature calcination, ion exchange and other physical and chemical properties, such as volume product of materials, etc. Co-doped CdS/ZnS nanospheres, ZnS nanospheres and ZnS / ZnS nanospheres were prepared and their photocatalytic activity was studied. The main contents are as follows: (1) the preparation and photocatalytic activity of CdS/ZnS nanoparticles: ZnS (en) 0.5 precursors were prepared by hydrothermal method, and CdS/ZnS nanoparticles were successfully prepared by ion exchange method and hydrothermal method using ZnS (en) 0.5 precursor and cadmium chloride as raw materials. SEM,XRD,XPS,UV-Vis,TEM was used to characterize the composition, structure and morphology of the samples. The results showed that the diffraction peaks of CDs / ZnS nanocrystals shifted to small angles with the increase of CD doping content, indicating that the samples we prepared were composites of ZnS and CdS. Instead of the physical mixing of ZnS and CdS, it can be clearly observed from the SEM images that the ZnS (en) 0.5 precursor and CdS/ZnS nanocrystals are composed of uniform thickness nanocrystals. After that, the photocatalytic degradation of methyl orange was carried out using CdS/ZnS nanoparticles as photocatalyst and methyl orange as simulated pollutant. The experimental results show that when the molar ratio of Cd/Zn is equal to 0.8 (that is, CZ0.8), the flake CdS/ZnS nanocomposites have the best catalytic activity. The 10mg sample CZ0.8 is added to the 50ml methyl orange aqueous solution (the concentration is 10mg/L). Under visible light irradiation for 60 min, the degradation rate of methyl orange solution was 99%. (2) preparation and photocatalytic activity of Co,Mn co-doped ZnS nanospheres: firstly, Mn doped ZnS nanospheres were prepared by hydrothermal method. Then Co,Mn co-doped ZnS nanospheres were prepared by doping a third metal ion Co, by ion exchange method. XRD,UV-Vis and SEM were used to characterize the samples. The results showed that the samples were made up of many spherical particles about the diameter of 400nm. Then the photocatalytic degradation experiments were carried out using ZnS and Co,Mn co-doped ZnS nanospheres doped with ZnS,Co and ZnS, Mn as photocatalysts and methyl orange aqueous solution as simulated pollutants respectively. The experimental results show that the codoped ZnS nanospheres have the best catalytic activity. 20mmg is added to the 50ml methyl orange aqueous solution (concentration of 3mg/L). (3) preparation and photocatalytic activity of ZnO/CdS/ZnS nanospheres: ZnS nanospheres were prepared by hydrothermal method. Based on ZnS, CdS/ZnS nanospheres were prepared by high temperature calcination and ion exchange respectively. SEM,XRD,XPS,UV-Vis was used to characterize its composition, morphology and properties. The results showed that the ZnO/CdS/ZnS was composed of many nanospheres with uniform particle size and rough surface. The photocatalytic properties of four kinds of samples were studied with methyl orange as the simulated pollutant. The results show that ZnO / CDs / ZnS nanospheres have the best catalytic activity. When 20mg ZnO/CdS/ZnS nanospheres are dispersed into 50ml 10mg/L methyl orange solution, the degradation rate of 50ml 10mg/L nanospheres is 96.8g under visible light irradiation for 60min.
【學(xué)位授予單位】：河南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB33;O643.36
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