ZnS和ZnO纳米材料的制备及其光致发光性能的研究
摘要
纳米ZnS和ZnO是宽禁带半导体材料,由于具有量子限域效应、尺寸效应和优越的荧光特性等优点而吸引了众多研究者的目光。因此,在近十几年里,ZnS和ZnO纳米材料已经在光催化、传感器、透明电极、荧光探针、二极管、太阳能电池和激光器等领域的研究中显示出了巨大的发展潜力。通过在ZnS和ZnO基质中掺杂不同离子可以调节这些宽禁带纳米半导体材料的电学、光学和磁学特性,从而使它们得到更广泛的应用。由于发光特性是纳米半导体材料的一个重要特性,对ZnS和ZnO及其掺杂型纳米粒子发光特性进行研究不仅有科研方面的意义,而且在实际应用方面也有潜在的价值。因此,本论文针对ZnS和ZnO及其掺杂型纳米粒子的制备和光谱性能展开研究,主要的研究内容和结果如下：
(1)分别采用沉淀法和固相法合成了不同粒径的ZnS纳米粒子,X射线衍射分析,透射和扫描电镜测试表明所有样品均为闪锌矿结构,平均粒径分别约为6.40nm和9.48nm。与沉淀法相比,固相法制备的ZnS纳米粒子的结晶度更好,发光强度更强。
(2)采用沉淀法制备了ZnS：Mg2+纳米粒子,实验结果表明：在Znl-xMgxS(0≤x≤0.55)纳米粒子中,随着Mg2+浓度由0mol%增加到55mol%时,虽然样品的发光强度随Mg2+浓度的增加而降低,但其带隙由3.70eV增加至3.98eV,这说明Mg2+的掺杂能调节ZnS纳米粒子的带隙宽度。
(3)采用低温固相法制备了ZnS：O2-纳米粒子,研究了O2-的掺杂浓度、反应条件和退火条件对样品荧光特性的影响,讨论了ZnS：O2-纳米粒子的荧光发射机理,研究结果表明：与ZnS纳米粒子相比,O2-掺杂后的样品室温下蓝色发光强度相对增强,这表明掺杂后的样品具有良好的光学性质。当初始原料中Zn和O的摩尔比为10：5.3时,样品的发射强度最强,其强度为未掺杂ZnS样品的9倍。研究反应条件对ZnS：O2-(Zn/O=10：5.3)样品荧光特性影响时,发现反应时间由1h延长至5h和反应温度由120℃升高至160℃时,样品的粒径由7.93nm增大到19.10nm,最佳反应时间和反应温度分别为3h和130℃。同时,通过研究退火条件的影响时,发现：退火能使ZnS：O2-(Zn/O=10：5.3)样品粒径和发光强度增加,最佳退火条件为：空气中退火时,最佳退火时间和退火温度分别为0.5h和100℃；而在真空中退火时,最佳退火时间和退火温度则分别为3h和150℃。
(4)采用固相法制备了卤素掺杂的ZnS纳米粒子,光谱测试结果表明：卤素离子的掺杂,能提高样品的发光强度,最佳的反应摩尔比分别为：F/Zn=0.3,Cl/Zn=0.35,Br/Zn=0.4,I/Zn=0.45。同时,研究表面活性剂(聚乙烯醇,PVA)对样品荧光性能影响时,发现：PVA能有效减少卤素掺杂的ZnS纳米粒子的表面悬挂键,提高样品的发光强度。
(5)分别采用溶胶-凝胶法和低温固相法合成了ZnO纳米粒子,测试结果表明所有样品均为六角纤锌矿结构,平均粒径分别为17.42nm和20.28nm。与溶胶-凝胶法相比,固相法制备的ZnO纳米粒子的结晶度好,发光强度较强。通过探讨反应条件对溶胶-凝胶法制备的ZnO纳米粒子的晶体结构和发光性能的影响,发现：当反应温度为60℃,反应时间由6h增加至10h时,ZnO纳米粒子的粒径由16.0nm增大到30.2nm,反应时间为7h的样品的发光强度最强；当反应时间为7h,反应温度由50℃增加到90℃时,ZnO纳米粒子的粒径由17.3nm增大到32.2nm,反应温度为60℃的样品的发光强度最强。不同退火条件对样品性能影响的研究结果表明：退火处理能改善样品的结晶度,增大粒径,提高发光强度。最佳退火温度和退火时间分别为100℃和0.5h。另外,在该退火条件下,真空退火样品的荧光强度高于空气退火的样品,这是由于真空退火能更有效的使样品表面吸附的氧原子发生脱附反应。
(6)采用低温固相法制备ZnO：S2-纳米粒子和ZnS/ZnO：S2-纳米异质结材料,研究发现：当S2-的掺杂量低于S2-在ZnO中的固溶度时,产物为ZnO：S2-纳米粒子；当S2-的掺杂量高于ZnS和ZnO的固溶度时,除了生成ZnO：S2-纳米粒子外,还存在ZnS纳米颗粒,形成ZnS/ZnO：S2-纳米异质结。荧光光谱表明：ZnO：S2-纳米粒子的发光强度高于ZnO样品的,但是却低于ZnS/ZnO：S2-纳米异质结材料的荧光强度,而且ZnS/ZnO：S2-纳米异质结的发光强度约为ZnO样品的25倍。其原因是：对ZnO：S2-纳米粒子而言,S2-掺杂能有效提高样品的辐射复合发光几率,增强样品的荧光强度,而ZnS/ZnO：S2-纳米异质结材料中,表面层的ZnS纳米粒子能起到修饰ZnO：S2-纳米粒子表面的作用,从而降低表面缺陷态浓度,提高样品的荧光强度。
(7)采用低温固相法制备了ZnO：Mg2+纳米粒子,研究结果表明：Mg2+的掺杂能引起锌空位,镁间隙等新缺陷的产生,使样品的辐射跃迁增强,导致样品的荧光强度增强。
As wide band-gap semiconductor materials, zinc sulfide (ZnS) and Zinc oxide (ZnO) nanoparticles have attracted considerable interest because of their quantum confinement effects, size effects, and superior luminescence characteristics. In the last two decades, ZnS and ZnO nanoparticles have been found broad applications in many different technological areas, including photo-catalysis, sensors, transparent electrodes, fluorescent probes, light-emitting diodes, solar cells, and lasers. Moreover, the electrical, optical, and magnetic properties of the wide band-gap nano-semiconductors can be conveniently adjusted by impurity doping for different applications. One of the important properties of ZnS and ZnO nanoparticles is the luminescence property. The investigation on the luminescent properties of ZnX (X=S and O) and ZnX:M (M is the doping ion) is significative for both scientific research and practical applications. So, the preparation and photoluminescence properties of ZnS and ZnO nano-luminescence materials were studied in this thesis.
In this thesis, the following work has been finished:
(1) ZnS nanoparticles were successfully prepared using a facile chemical solution method and solid state reaction method at low temperature, respectively. The size, the crystal structure and luminescent properties of ZnS nanoparticles were characterized by X-ray diffraction (XRD), transmission electronic microscope (TEM) and scanning electron microscopy (SEM). The result showed that the product had a cubic crystal structure and the average crystallite size was6.40and9.48nm, respectively. As compared with chemical solution method, ZnS nanoparticles, which were obtained by solid state reaction method, had better crystallinity and higher emission intensity.
(2) Zn1-xMgxS nanoparticles were synthesized using a chemical solution method. The result showed that the energy band gap of the Zn1-xMgxS nanoparticles increased from3.70eV at x=0to3.98eV at x=0.55, which indicated that Mg2+-doped can adjust the energy band gap of the Zn1-xMgxS nanoparticles. However, the PL intensity of the Zn1-xMgxS nanoparticles was found to decrease with x due to an increase in the number of non-radiative deep traps.
(3) ZnS:O2-nanoparticles were synthesized using a solid state reaction method at low temperature. The effect of O2-contents, reaction condition and anneal condition on the PL properties of samples was studied in detail. The result showed that O2-doping remarkably increased the luminescence intensity of ZnS nanoparticles, and a maximum emission was reached when Zn/O=10:5.3in the starting materials. The emission intensity of the ZnS:O2-(Zn/O=10:5.3) nanoparticles was about9times as high as that of the undoped ZnS sample. The average diameter of ZnS:O2-(Zn/O=10:5.3) nanoparticles increased from7.93to19.10nm with the increase of reaction time (from1to5h) and temperature (from120to160℃). A maximum emission of the ZnS:O2-(Zn/O=10:5.3) nanoparticles was observed when the reaction time and temperature were3h and130℃, respectively. The result also indicated that after annealing all samples showed larger radius and stronger visible emission for ZnS:O2-(Zn/O=10:5.3) nanoparticles. In this work, the optimal anneal temperature and anneal time were found to be100℃and0.5h for air annealed, and150℃and3h for vacuum annealed, respectively.
(4) ZnS:X'(X=F, Cl, Br and I) nanoparticles was prepared by solid state reaction method and researched their PL properties. The result showed that after doping with halogen ion, all samples showed stronger visible emission for ZnS:X-(X=F, Cl, Br and I) nanoparticles, and the optimal molar ratio of X/Zn was found to be0.3,0.35,0.4and0.45for F, Cl, Br and I, respectively. It was also observed that PVA can decrease the number of the surface dangling bonds and then resulted in an increase in PL intensity of ZnS:X-(X=F, Cl, Br and I) nanoparticles.
(5) ZnO nanoparticles were successfully prepared using sol-gel method and solid state reaction method at low temperature, respectively. The result showed that the product had a hexagonal wurtzite crystal structure and the average crystallite size was17.42and20.28nm, respectively. As compared with sol-gel method, ZnO nanoparticles, which were obtained by solid state reaction method, had better crystallinity and higher emission intensity. The effects of the reaction time and temperature on the microstructures and photoluminescence properties of ZnO nanoparticles were studied in detail. The result indicated that with the reaction time increasing (from6to10h), the diameter of ZnO nanoparticles was increased from16.0to30.2nm and the maximum intensity of emission was obtained while the reaction time was7h, under the same reaction temperature60℃. And under the same reaction time7h, with the reaction temperature increasing (from50to90℃), the diameter of ZnO nanoparticles was augmented from17.3to32.2nm and the maximum emission was attained when the reaction temperature was60℃. The effects of annealing conditions on the crystallinity, diameter, and PL properties of ZnO nanoparticles prepared by sol-gel method were investigated. All annealed ZnO nanoparticles showed stronger UV-visible emission and crystallinity than the as-grown ZnO nanoparticles. In this work, the optimal anneal temperature and anneal time were found to be100C and0.5h, respectively. Under the optimal anneal conditions, the vacuum annealed ZnO nanoparticles showed stronger emission intensity than the air annealed ZnO nanoparticles.
(6) ZnO:S2-nanoparticles and ZnS/ZnO:S2-nanoheterostructure were obtained by solid state reaction method. The result showed that when S2-content was less than the solid solubility of ZnS and ZnO, S2-replaced O2-and formed ZnO1-xSx nanoparticles, and when S2-content was higher than the solid solubility of ZnS and ZnO, some parts of S2-had replaced O2-and form ZnO1-y-Sy (y is the maximum of the solid solubility between ZnS and ZnO) nanoparticles, others could not incorporate into ZnO1-+ySy nanoparticles and would react with Zn2+formed ZnS, which resulted in forming ZnS/ZnO1-ySy, nanoheterostructure. It can be seen that the emission intensity of samples follows the order ZnS/ZnO:S2->ZnO:S2->ZnO. And the photoluminescence intensity of ZnS/ZnO:S2-nanoheterostructure is much stronger than ZnO nanoparticles by25times. This may suggest that S2-dopants increase the number of radiative recombination sites in ZnO:S2-nanoparticles, but when ZnO:S2-nanoparticles were caped by ZnS nanoparticles, hackly surface was modified to some extent, which can decrease the number of the surface dangling bonds and then resulted in an increase in PL intensity.
(7) Mg2+--doped ZnO nanoparticles were prepared by solid state reaction method. The result showed that doped with Mg2+can induce defect states in the ZnO nanocrystals such as VZn (zinc vacancy) and Mgi (interstitial magnesium), which resulted in enhance radiative recombination and PL intensity.
(1)分别采用沉淀法和固相法合成了不同粒径的ZnS纳米粒子,X射线衍射分析,透射和扫描电镜测试表明所有样品均为闪锌矿结构,平均粒径分别约为6.40nm和9.48nm。与沉淀法相比,固相法制备的ZnS纳米粒子的结晶度更好,发光强度更强。
(2)采用沉淀法制备了ZnS：Mg2+纳米粒子,实验结果表明：在Znl-xMgxS(0≤x≤0.55)纳米粒子中,随着Mg2+浓度由0mol%增加到55mol%时,虽然样品的发光强度随Mg2+浓度的增加而降低,但其带隙由3.70eV增加至3.98eV,这说明Mg2+的掺杂能调节ZnS纳米粒子的带隙宽度。
(3)采用低温固相法制备了ZnS：O2-纳米粒子,研究了O2-的掺杂浓度、反应条件和退火条件对样品荧光特性的影响,讨论了ZnS：O2-纳米粒子的荧光发射机理,研究结果表明：与ZnS纳米粒子相比,O2-掺杂后的样品室温下蓝色发光强度相对增强,这表明掺杂后的样品具有良好的光学性质。当初始原料中Zn和O的摩尔比为10：5.3时,样品的发射强度最强,其强度为未掺杂ZnS样品的9倍。研究反应条件对ZnS：O2-(Zn/O=10：5.3)样品荧光特性影响时,发现反应时间由1h延长至5h和反应温度由120℃升高至160℃时,样品的粒径由7.93nm增大到19.10nm,最佳反应时间和反应温度分别为3h和130℃。同时,通过研究退火条件的影响时,发现：退火能使ZnS：O2-(Zn/O=10：5.3)样品粒径和发光强度增加,最佳退火条件为：空气中退火时,最佳退火时间和退火温度分别为0.5h和100℃；而在真空中退火时,最佳退火时间和退火温度则分别为3h和150℃。
(4)采用固相法制备了卤素掺杂的ZnS纳米粒子,光谱测试结果表明：卤素离子的掺杂,能提高样品的发光强度,最佳的反应摩尔比分别为：F/Zn=0.3,Cl/Zn=0.35,Br/Zn=0.4,I/Zn=0.45。同时,研究表面活性剂(聚乙烯醇,PVA)对样品荧光性能影响时,发现：PVA能有效减少卤素掺杂的ZnS纳米粒子的表面悬挂键,提高样品的发光强度。
(5)分别采用溶胶-凝胶法和低温固相法合成了ZnO纳米粒子,测试结果表明所有样品均为六角纤锌矿结构,平均粒径分别为17.42nm和20.28nm。与溶胶-凝胶法相比,固相法制备的ZnO纳米粒子的结晶度好,发光强度较强。通过探讨反应条件对溶胶-凝胶法制备的ZnO纳米粒子的晶体结构和发光性能的影响,发现：当反应温度为60℃,反应时间由6h增加至10h时,ZnO纳米粒子的粒径由16.0nm增大到30.2nm,反应时间为7h的样品的发光强度最强；当反应时间为7h,反应温度由50℃增加到90℃时,ZnO纳米粒子的粒径由17.3nm增大到32.2nm,反应温度为60℃的样品的发光强度最强。不同退火条件对样品性能影响的研究结果表明：退火处理能改善样品的结晶度,增大粒径,提高发光强度。最佳退火温度和退火时间分别为100℃和0.5h。另外,在该退火条件下,真空退火样品的荧光强度高于空气退火的样品,这是由于真空退火能更有效的使样品表面吸附的氧原子发生脱附反应。
(6)采用低温固相法制备ZnO：S2-纳米粒子和ZnS/ZnO：S2-纳米异质结材料,研究发现：当S2-的掺杂量低于S2-在ZnO中的固溶度时,产物为ZnO：S2-纳米粒子；当S2-的掺杂量高于ZnS和ZnO的固溶度时,除了生成ZnO：S2-纳米粒子外,还存在ZnS纳米颗粒,形成ZnS/ZnO：S2-纳米异质结。荧光光谱表明：ZnO：S2-纳米粒子的发光强度高于ZnO样品的,但是却低于ZnS/ZnO：S2-纳米异质结材料的荧光强度,而且ZnS/ZnO：S2-纳米异质结的发光强度约为ZnO样品的25倍。其原因是：对ZnO：S2-纳米粒子而言,S2-掺杂能有效提高样品的辐射复合发光几率,增强样品的荧光强度,而ZnS/ZnO：S2-纳米异质结材料中,表面层的ZnS纳米粒子能起到修饰ZnO：S2-纳米粒子表面的作用,从而降低表面缺陷态浓度,提高样品的荧光强度。
(7)采用低温固相法制备了ZnO：Mg2+纳米粒子,研究结果表明：Mg2+的掺杂能引起锌空位,镁间隙等新缺陷的产生,使样品的辐射跃迁增强,导致样品的荧光强度增强。
As wide band-gap semiconductor materials, zinc sulfide (ZnS) and Zinc oxide (ZnO) nanoparticles have attracted considerable interest because of their quantum confinement effects, size effects, and superior luminescence characteristics. In the last two decades, ZnS and ZnO nanoparticles have been found broad applications in many different technological areas, including photo-catalysis, sensors, transparent electrodes, fluorescent probes, light-emitting diodes, solar cells, and lasers. Moreover, the electrical, optical, and magnetic properties of the wide band-gap nano-semiconductors can be conveniently adjusted by impurity doping for different applications. One of the important properties of ZnS and ZnO nanoparticles is the luminescence property. The investigation on the luminescent properties of ZnX (X=S and O) and ZnX:M (M is the doping ion) is significative for both scientific research and practical applications. So, the preparation and photoluminescence properties of ZnS and ZnO nano-luminescence materials were studied in this thesis.
In this thesis, the following work has been finished:
(1) ZnS nanoparticles were successfully prepared using a facile chemical solution method and solid state reaction method at low temperature, respectively. The size, the crystal structure and luminescent properties of ZnS nanoparticles were characterized by X-ray diffraction (XRD), transmission electronic microscope (TEM) and scanning electron microscopy (SEM). The result showed that the product had a cubic crystal structure and the average crystallite size was6.40and9.48nm, respectively. As compared with chemical solution method, ZnS nanoparticles, which were obtained by solid state reaction method, had better crystallinity and higher emission intensity.
(2) Zn1-xMgxS nanoparticles were synthesized using a chemical solution method. The result showed that the energy band gap of the Zn1-xMgxS nanoparticles increased from3.70eV at x=0to3.98eV at x=0.55, which indicated that Mg2+-doped can adjust the energy band gap of the Zn1-xMgxS nanoparticles. However, the PL intensity of the Zn1-xMgxS nanoparticles was found to decrease with x due to an increase in the number of non-radiative deep traps.
(3) ZnS:O2-nanoparticles were synthesized using a solid state reaction method at low temperature. The effect of O2-contents, reaction condition and anneal condition on the PL properties of samples was studied in detail. The result showed that O2-doping remarkably increased the luminescence intensity of ZnS nanoparticles, and a maximum emission was reached when Zn/O=10:5.3in the starting materials. The emission intensity of the ZnS:O2-(Zn/O=10:5.3) nanoparticles was about9times as high as that of the undoped ZnS sample. The average diameter of ZnS:O2-(Zn/O=10:5.3) nanoparticles increased from7.93to19.10nm with the increase of reaction time (from1to5h) and temperature (from120to160℃). A maximum emission of the ZnS:O2-(Zn/O=10:5.3) nanoparticles was observed when the reaction time and temperature were3h and130℃, respectively. The result also indicated that after annealing all samples showed larger radius and stronger visible emission for ZnS:O2-(Zn/O=10:5.3) nanoparticles. In this work, the optimal anneal temperature and anneal time were found to be100℃and0.5h for air annealed, and150℃and3h for vacuum annealed, respectively.
(4) ZnS:X'(X=F, Cl, Br and I) nanoparticles was prepared by solid state reaction method and researched their PL properties. The result showed that after doping with halogen ion, all samples showed stronger visible emission for ZnS:X-(X=F, Cl, Br and I) nanoparticles, and the optimal molar ratio of X/Zn was found to be0.3,0.35,0.4and0.45for F, Cl, Br and I, respectively. It was also observed that PVA can decrease the number of the surface dangling bonds and then resulted in an increase in PL intensity of ZnS:X-(X=F, Cl, Br and I) nanoparticles.
(5) ZnO nanoparticles were successfully prepared using sol-gel method and solid state reaction method at low temperature, respectively. The result showed that the product had a hexagonal wurtzite crystal structure and the average crystallite size was17.42and20.28nm, respectively. As compared with sol-gel method, ZnO nanoparticles, which were obtained by solid state reaction method, had better crystallinity and higher emission intensity. The effects of the reaction time and temperature on the microstructures and photoluminescence properties of ZnO nanoparticles were studied in detail. The result indicated that with the reaction time increasing (from6to10h), the diameter of ZnO nanoparticles was increased from16.0to30.2nm and the maximum intensity of emission was obtained while the reaction time was7h, under the same reaction temperature60℃. And under the same reaction time7h, with the reaction temperature increasing (from50to90℃), the diameter of ZnO nanoparticles was augmented from17.3to32.2nm and the maximum emission was attained when the reaction temperature was60℃. The effects of annealing conditions on the crystallinity, diameter, and PL properties of ZnO nanoparticles prepared by sol-gel method were investigated. All annealed ZnO nanoparticles showed stronger UV-visible emission and crystallinity than the as-grown ZnO nanoparticles. In this work, the optimal anneal temperature and anneal time were found to be100C and0.5h, respectively. Under the optimal anneal conditions, the vacuum annealed ZnO nanoparticles showed stronger emission intensity than the air annealed ZnO nanoparticles.
(6) ZnO:S2-nanoparticles and ZnS/ZnO:S2-nanoheterostructure were obtained by solid state reaction method. The result showed that when S2-content was less than the solid solubility of ZnS and ZnO, S2-replaced O2-and formed ZnO1-xSx nanoparticles, and when S2-content was higher than the solid solubility of ZnS and ZnO, some parts of S2-had replaced O2-and form ZnO1-y-Sy (y is the maximum of the solid solubility between ZnS and ZnO) nanoparticles, others could not incorporate into ZnO1-+ySy nanoparticles and would react with Zn2+formed ZnS, which resulted in forming ZnS/ZnO1-ySy, nanoheterostructure. It can be seen that the emission intensity of samples follows the order ZnS/ZnO:S2->ZnO:S2->ZnO. And the photoluminescence intensity of ZnS/ZnO:S2-nanoheterostructure is much stronger than ZnO nanoparticles by25times. This may suggest that S2-dopants increase the number of radiative recombination sites in ZnO:S2-nanoparticles, but when ZnO:S2-nanoparticles were caped by ZnS nanoparticles, hackly surface was modified to some extent, which can decrease the number of the surface dangling bonds and then resulted in an increase in PL intensity.
(7) Mg2+--doped ZnO nanoparticles were prepared by solid state reaction method. The result showed that doped with Mg2+can induce defect states in the ZnO nanocrystals such as VZn (zinc vacancy) and Mgi (interstitial magnesium), which resulted in enhance radiative recombination and PL intensity.
引文
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