水热合成ZnS超细材料的白光及X射线发光研究
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摘要
针对目前对近紫外(n-UV)LED用白光发光材料和高发光效率纳米X射线发光材料的迫切需求,本论文进行了掺杂型硫化锌白光发光材料、X射线激发材料的合成和发光特性研究。主要工作包括：
采用水热法直接合成了高发光强度的类球形ZnS:Cu,Al纳米荧光粉。制备的纳米晶为纯立方相结构,其粒子尺寸约为15nm,且分散性较好。系统研究了在343nm激发下,不同摩尔比的ns/nZn、nCu/nAl及表面活性剂对清洗样品和未清洗样品的光致发光(PL)光谱的影响。实验结果表明,激活剂浓度不变而改变ns/nZn摩尔比时发光强度显著增强,同时未清洗样品的PL强度均比清洗样品的强,且未清洗样品的PL强度增强的比值在低的ns/nZn时更显著。另外,PL强度还与是否添加表面活性剂有关,说明其PL强度与纳米材料的表面态有很大的关系。在我们的实验中,用343nm紫外光激发时,nCu/nZn, ns/nZn, nCu/nAl分别为0.0003,3和0.5时未清洗样品的发光最强,此时于室内照明条件下可观察到明亮的绿光。
借助X射线能谱(EDX)和原子吸收光谱仪,研究了样品中S，Zn和Cu的含量并详细研究了在ns/nZn=3时改变nCu/nZn,nCu/nAl摩尔比对ZnS:Cu,Al样品在375nm紫外光激发下PL光谱的特性。结果证明存在大量Zn空缺,Cu离子经过水热处理后已掺入到ZnS基体中。PL光谱特性为：样品的激发谱为宽带谱,利用370-410nm之间任意波长的光激发时,发射谱均为宽带谱,且它们基本重合。表明此材料作为近紫外(370-410nm)发光二极管·[(n)-UV(370-410nm)LED)用荧光粉及全色荧光粉具有很大的应用潜力。样品在375nm激发下全色宽带发射谱是460,510和576nm带光谱的高斯叠加。当nCu/nZn,nCu/nAl分别为3×10-4和2时,于室内照明条件下肉眼可观察到白色发光。
采用低温水热法结合热处理工艺成功制备了ZnS:Cu,Al、ZnS:Au,Cu和ZnS:Cu,Tm三种超细X射线发光粉材料。研究结果表明：1)水热法直接制备的ZnS:Cu,Al的PL和X射线激发发光(XEL)光谱均为宽带谱,在nCu/nZn,nCn/nAl分别为3×10-4和0.5时PL和XEL光谱强度最大,XEL峰值在470nm处。在此条件下,水热处理3h直接合成的纳米晶在氩气保护下于800℃退火1h后样品的XEL发光进一步增强。XEL光谱强度约是退火前样品的8倍,此时峰值波长在520nm,团聚后粒径为200-500nm的类球形六方相结构。发光强度增强,但粒径很小,对提高成像系统分辨率非常有意义。通过比较样品的XEL和PL光谱,讨论了XEL和PL光谱的发光机理和激发机制及退火对其特性的影响；2)水热法直接制备的ZnS:Au,Cu的PL和XEL光谱均为宽带谱,在nCu/nZn,nCu/nAl分别为3×10-5和0.5时PL和XEL光谱强度最大,XEL峰值在459nm处。在此条件下,水热处理12h直接合成的纳米晶在氩气保护下于1000℃退火1h后样品的XEL发光最强,此时其两个峰值分别位于445和513nm,且与未退火前相比XEL强度增强了10倍左右。团聚后尺寸为1-2μm的类球形六方相结构。另外,在未经退火的ZnS:Cu,Al和ZnS:Au,Cu纳米材料中,均观察到随着Cu2+离子摩尔比的增大,XEL光谱峰值的红移现象;3)通过研究水热处理时间对ZnS:Cu,Tm纳米晶的结构、形貌、XEL光谱的影响,发现随着水热处理时间的延长,样品的尺寸增大且结晶性增强,但是其XEL发光强度却降低。分析认为这一异常现象可归因于表面态的影响。因此,水热合成ZnS:Cu,Tm纳米晶的反应时间不宜过长,最佳时间为12小时。ZnS:Cu,Tm在nCu/nZn,nCu/nTm分别为3×10-4和0.5时PL和XEL光谱强度最大,900℃为最佳退火温度,此时所得样品的粒子尺寸为200～600nm的类球形六方相结构,且与未退火前相比XEL发光增强了11倍,其两个发射峰值分别位于453nm和525nm。
Based on the urgent requirement of white light emission (n) UV LEDs phosphors and X-ray nano-phosphors with high luminescent efficiency, this paper focuses on the syntheses and study on luminescence properties of ZnS white light and X-ray phosphors activated with different dopants. The major works are shown as follows:
Spherical ZnS:Cu,Al nanocrystals with high luminescence intensity were synthesized by a hydrothermal method. The synthesized nanocrystals show single cubic structure and well dispersity with average grain size of about 15nm. The effects of the molar ratio of ns/nZn、nCu/nAland surfactant on the photoluminescence (PL) spectra of rinsed and unrinsed samples under 343nm excitation were investigated systematically. The results indicate that with the increase of ns/nZn the PL intensity increases remarkably, and the PL intensites of unrinsed samples are stronger than that of rinsed ones. Moreover, the PL intensities of unrinsed samples are increased more significantly under a low ratio of nS/nZn. The PL intensity has a relation to the surfactants, this suggests that surface state of nanomaterials can also affect the PL intensity. In our experiment, the optimal condition is the unrinsed sample under n(Cu/Zn)=0.0003, nS/nZn=3, n(Cu/Al)=0.5, and the bright green light can be observed with the naked eye in the daytime.
The energy dispersive X-ray spectroscopy (EDX) and atomic absorption spectrometry were applied to the analysis of S, Zn and Cu content in the sample. The results proved that a large number of zinc vacancies exist and Cu is incorporation into the sample lattice. The excitation spectrum is broad. Under 370-410nm excitation the sample emits white light. The broad emission spectra are almost coincident with any excitation wavelength of between 370-410nm making them attractive as conversion phosphors for LED application and full-color fluorescent display devices. The emitted white light under 375nm excitation was found to be the result of blue, green, and orange emission bands. For nCu/nZn, nCu/nAl and nS/nZn molar ratios of 0.0003,2 and 3, respectively, the near blue white light can be observed with the naked eye in daylight.
ZnS:Cu,Al, ZnS:Au,Cu and ZnS:Cu,Tm fine X-Ray phosphors were successfully synthesized using a hydrothermal method combined with heat treatment technology. The experimental results are shown as follows:1) For ZnS:Cu,Al, the PL and XEL spectra of all of the samples show a broad emission band. The maximum PL and X-ray excited luminescence (XEL) intensities are observed for sample with nCu/nZn=0.0003 and nCu/nAl=0.5. The XEL peak center is at about 470nm. In this condition, the XEL intensity of the sample which was hydrothermally treated at 200℃for 3h then annealed in Ar at 800℃for 1h is enhanced and the peak is located at 520nm. In the mean time, the XEL intensity is about eight times by comparison with that of the samples without annealing. The particles agglomerate size is about 200-500nm and roughly spherical particles show pure hexagonal structure. The Samples with highly luminescence efficiencies and the smaller size could enhance the resolution of imaging systems. By comparing the PL and XEL spectra, the luminescence mechanism and different excitation mechanism of PL and XEL and effect of annealing on XEL have been discussed.2) For ZnS:Au,Cu, the PL and XEL spectra of all of samples show a broad emission band. The maximum XEL intensity of sample directly synthesized by hydrothermal treatment is observed for sample with nCu/nZn=0.00003 and n(Cu/Au)=0.5. The XEL peak center is at about 459nm. In this condition, the strongest XEL emission is observed for the direct synthesized sample further annealing in Argon at 1000℃for 1h sample and the XEL peak was centered at about 445 and 513nm, respectively. In the meantime, the XEL intensity increased about ten times by comparison with directly synthesized without annealing. The particles agglomerate size is about 1-2μm and roughly spherical particles show pure hexagonal structure. In addition, with the increase of Cu2+ content, we observe the red shift of XEL spectra both in ZnS:Cu,Al and ZnS:Au,Cu without annealing samples.3) For ZnS:Cu,Tm, the effects of hydrothermal treatment time on the structure, morphology and XEL spectrum of ZnS:Cu,Tm nanocrystals were studied. It is found that with the prolonging of hydrothermal treatment time the particle size and crystallization are increased, while the intensity of XEL is decreased. The analyzed results show that the decrease of XEL intensity can be attributed to the surface state. Based on the above results, it is suggested that the long hydrothermal treatment time is not beneficial to the XEL intensity of ZnS:Cu,Tm nanocrystals, and the optimal treatment time is 12h. The maximum XEL intensity of sample directly synthesized by hydrothermal treatment is observed for nCu/nZn=0.0003 and nCu/nTm=0.5. the optimal annealing temperature is 900℃. After annealing at this temperature, the particle size is 200-600nm. the sample with pure hexagonal structure shows the stronger XEL spectrum with emission peaks at 453nm and 525nm, the XEL intensity increased about eleven times by comparison with directly synthesized without annealing.
采用水热法直接合成了高发光强度的类球形ZnS:Cu,Al纳米荧光粉。制备的纳米晶为纯立方相结构,其粒子尺寸约为15nm,且分散性较好。系统研究了在343nm激发下,不同摩尔比的ns/nZn、nCu/nAl及表面活性剂对清洗样品和未清洗样品的光致发光(PL)光谱的影响。实验结果表明,激活剂浓度不变而改变ns/nZn摩尔比时发光强度显著增强,同时未清洗样品的PL强度均比清洗样品的强,且未清洗样品的PL强度增强的比值在低的ns/nZn时更显著。另外,PL强度还与是否添加表面活性剂有关,说明其PL强度与纳米材料的表面态有很大的关系。在我们的实验中,用343nm紫外光激发时,nCu/nZn, ns/nZn, nCu/nAl分别为0.0003,3和0.5时未清洗样品的发光最强,此时于室内照明条件下可观察到明亮的绿光。
借助X射线能谱(EDX)和原子吸收光谱仪,研究了样品中S，Zn和Cu的含量并详细研究了在ns/nZn=3时改变nCu/nZn,nCu/nAl摩尔比对ZnS:Cu,Al样品在375nm紫外光激发下PL光谱的特性。结果证明存在大量Zn空缺,Cu离子经过水热处理后已掺入到ZnS基体中。PL光谱特性为：样品的激发谱为宽带谱,利用370-410nm之间任意波长的光激发时,发射谱均为宽带谱,且它们基本重合。表明此材料作为近紫外(370-410nm)发光二极管·[(n)-UV(370-410nm)LED)用荧光粉及全色荧光粉具有很大的应用潜力。样品在375nm激发下全色宽带发射谱是460,510和576nm带光谱的高斯叠加。当nCu/nZn,nCu/nAl分别为3×10-4和2时,于室内照明条件下肉眼可观察到白色发光。
采用低温水热法结合热处理工艺成功制备了ZnS:Cu,Al、ZnS:Au,Cu和ZnS:Cu,Tm三种超细X射线发光粉材料。研究结果表明：1)水热法直接制备的ZnS:Cu,Al的PL和X射线激发发光(XEL)光谱均为宽带谱,在nCu/nZn,nCn/nAl分别为3×10-4和0.5时PL和XEL光谱强度最大,XEL峰值在470nm处。在此条件下,水热处理3h直接合成的纳米晶在氩气保护下于800℃退火1h后样品的XEL发光进一步增强。XEL光谱强度约是退火前样品的8倍,此时峰值波长在520nm,团聚后粒径为200-500nm的类球形六方相结构。发光强度增强,但粒径很小,对提高成像系统分辨率非常有意义。通过比较样品的XEL和PL光谱,讨论了XEL和PL光谱的发光机理和激发机制及退火对其特性的影响；2)水热法直接制备的ZnS:Au,Cu的PL和XEL光谱均为宽带谱,在nCu/nZn,nCu/nAl分别为3×10-5和0.5时PL和XEL光谱强度最大,XEL峰值在459nm处。在此条件下,水热处理12h直接合成的纳米晶在氩气保护下于1000℃退火1h后样品的XEL发光最强,此时其两个峰值分别位于445和513nm,且与未退火前相比XEL强度增强了10倍左右。团聚后尺寸为1-2μm的类球形六方相结构。另外,在未经退火的ZnS:Cu,Al和ZnS:Au,Cu纳米材料中,均观察到随着Cu2+离子摩尔比的增大,XEL光谱峰值的红移现象;3)通过研究水热处理时间对ZnS:Cu,Tm纳米晶的结构、形貌、XEL光谱的影响,发现随着水热处理时间的延长,样品的尺寸增大且结晶性增强,但是其XEL发光强度却降低。分析认为这一异常现象可归因于表面态的影响。因此,水热合成ZnS:Cu,Tm纳米晶的反应时间不宜过长,最佳时间为12小时。ZnS:Cu,Tm在nCu/nZn,nCu/nTm分别为3×10-4和0.5时PL和XEL光谱强度最大,900℃为最佳退火温度,此时所得样品的粒子尺寸为200～600nm的类球形六方相结构,且与未退火前相比XEL发光增强了11倍,其两个发射峰值分别位于453nm和525nm。
Based on the urgent requirement of white light emission (n) UV LEDs phosphors and X-ray nano-phosphors with high luminescent efficiency, this paper focuses on the syntheses and study on luminescence properties of ZnS white light and X-ray phosphors activated with different dopants. The major works are shown as follows:
Spherical ZnS:Cu,Al nanocrystals with high luminescence intensity were synthesized by a hydrothermal method. The synthesized nanocrystals show single cubic structure and well dispersity with average grain size of about 15nm. The effects of the molar ratio of ns/nZn、nCu/nAland surfactant on the photoluminescence (PL) spectra of rinsed and unrinsed samples under 343nm excitation were investigated systematically. The results indicate that with the increase of ns/nZn the PL intensity increases remarkably, and the PL intensites of unrinsed samples are stronger than that of rinsed ones. Moreover, the PL intensities of unrinsed samples are increased more significantly under a low ratio of nS/nZn. The PL intensity has a relation to the surfactants, this suggests that surface state of nanomaterials can also affect the PL intensity. In our experiment, the optimal condition is the unrinsed sample under n(Cu/Zn)=0.0003, nS/nZn=3, n(Cu/Al)=0.5, and the bright green light can be observed with the naked eye in the daytime.
The energy dispersive X-ray spectroscopy (EDX) and atomic absorption spectrometry were applied to the analysis of S, Zn and Cu content in the sample. The results proved that a large number of zinc vacancies exist and Cu is incorporation into the sample lattice. The excitation spectrum is broad. Under 370-410nm excitation the sample emits white light. The broad emission spectra are almost coincident with any excitation wavelength of between 370-410nm making them attractive as conversion phosphors for LED application and full-color fluorescent display devices. The emitted white light under 375nm excitation was found to be the result of blue, green, and orange emission bands. For nCu/nZn, nCu/nAl and nS/nZn molar ratios of 0.0003,2 and 3, respectively, the near blue white light can be observed with the naked eye in daylight.
ZnS:Cu,Al, ZnS:Au,Cu and ZnS:Cu,Tm fine X-Ray phosphors were successfully synthesized using a hydrothermal method combined with heat treatment technology. The experimental results are shown as follows:1) For ZnS:Cu,Al, the PL and XEL spectra of all of the samples show a broad emission band. The maximum PL and X-ray excited luminescence (XEL) intensities are observed for sample with nCu/nZn=0.0003 and nCu/nAl=0.5. The XEL peak center is at about 470nm. In this condition, the XEL intensity of the sample which was hydrothermally treated at 200℃for 3h then annealed in Ar at 800℃for 1h is enhanced and the peak is located at 520nm. In the mean time, the XEL intensity is about eight times by comparison with that of the samples without annealing. The particles agglomerate size is about 200-500nm and roughly spherical particles show pure hexagonal structure. The Samples with highly luminescence efficiencies and the smaller size could enhance the resolution of imaging systems. By comparing the PL and XEL spectra, the luminescence mechanism and different excitation mechanism of PL and XEL and effect of annealing on XEL have been discussed.2) For ZnS:Au,Cu, the PL and XEL spectra of all of samples show a broad emission band. The maximum XEL intensity of sample directly synthesized by hydrothermal treatment is observed for sample with nCu/nZn=0.00003 and n(Cu/Au)=0.5. The XEL peak center is at about 459nm. In this condition, the strongest XEL emission is observed for the direct synthesized sample further annealing in Argon at 1000℃for 1h sample and the XEL peak was centered at about 445 and 513nm, respectively. In the meantime, the XEL intensity increased about ten times by comparison with directly synthesized without annealing. The particles agglomerate size is about 1-2μm and roughly spherical particles show pure hexagonal structure. In addition, with the increase of Cu2+ content, we observe the red shift of XEL spectra both in ZnS:Cu,Al and ZnS:Au,Cu without annealing samples.3) For ZnS:Cu,Tm, the effects of hydrothermal treatment time on the structure, morphology and XEL spectrum of ZnS:Cu,Tm nanocrystals were studied. It is found that with the prolonging of hydrothermal treatment time the particle size and crystallization are increased, while the intensity of XEL is decreased. The analyzed results show that the decrease of XEL intensity can be attributed to the surface state. Based on the above results, it is suggested that the long hydrothermal treatment time is not beneficial to the XEL intensity of ZnS:Cu,Tm nanocrystals, and the optimal treatment time is 12h. The maximum XEL intensity of sample directly synthesized by hydrothermal treatment is observed for nCu/nZn=0.0003 and nCu/nTm=0.5. the optimal annealing temperature is 900℃. After annealing at this temperature, the particle size is 200-600nm. the sample with pure hexagonal structure shows the stronger XEL spectrum with emission peaks at 453nm and 525nm, the XEL intensity increased about eleven times by comparison with directly synthesized without annealing.
引文
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