机构地区:[1]承德石油高等专科学校数理部,河北承德067000 [2]河北大学物理科学与技术学院,河北保定071002 [3]河北大学电子信息工程学院,河北保定071002 [4]承德石油高等专科学校计算机与信息工程系,河北承德067000
出 处:《光谱学与光谱分析》2019年第3期682-685,共4页Spectroscopy and Spectral Analysis
基 金:国家自然科学基金青年科学基金项目(61205180);河北省重点研发计划自筹项目(17211307)资助
摘 要:荧光纳米材料不但具备纳米材料的优势,同时还具有优异的光学性质,被广泛应用于荧光标记、离子识别、荧光免疫分析、光学成像和医学诊断等方面。因此,荧光纳米材料的制备、结构分析和荧光特性等方面的研究备受人们的关注。为了获得发光强度大、荧光量子效率高和制备过程可控的Si基荧光纳米材料,实验进一步研究了Si纳米线对样品发光特性的影响和样品的光学稳定性。首先,基于固-液-固生长机制,在反应温度为1 100℃、 N_2气流量为1 500 sccm、生长时间为15~60 min等工艺条件下,分别以"抛光"和"金字塔"织构表面的单晶Si(100)为衬底,生长出不同长度和分布的Si纳米线;以Au或Au-Al合金膜层作为金属催化剂,生长出密度分别约为10~8和10^(10) cm^(-2)的Si纳米线;然后,利用L4514自动控温管式加热炉,基于高温固相法,在温度为1 100℃、掺杂时间为60 min和N_2气流量为1 000 sccm等工艺条件下,以高纯Tb_4O_7(99.99%)粉末为稀土掺杂剂对不同Si纳米线衬底进行稀土掺杂,制备一系列的荧光纳米材料SiNWs:Tb^(3+)样品;室温下利用Hitachi F-4600型荧光分光光度计,固定激发光波长为243 nm、激发光狭缝为2.5 nm、发射光狭缝为2.5 nm、扫描波长范围为450~650 nm、光电倍增管(photomultiplier lube, PMT)电压为600 V等参数下,测量了不同样品的光致发光特性;最后,实验测试了该荧光纳米材料的光学稳定性,如时间(0~30 d)、温度(300~500 K)、酸碱(pH 1和11)、抗光漂白(0~120 min)等稳定性以及水溶性和分散性。结果显示,在衬底为"金字塔"织构表面上、生长时间为30 min、以Au为金属催化剂等条件下制备的Si纳米线为Tb^(3+)掺杂衬底时, SiNWs:Tb^(3+)的绿光发射强度较大,其发光强峰值位于554 nm,属于能级~5D_4→~7F_5的跃迁,另外在波长为494, 593和628 nm出现了三条发光谱带,它们分别属于能级~5D_4→~7F_6,~5D_4→~7F_4和~5D_4→~7F_Fluorescent nanomaterials not only have the advantages of nanomaterials,but also have excellent optical properties.They are widely used in fluorescent labels,ion recognition,fluorescence immunoassays,optical imaging and medical diagnostics.Therefore,researches on the preparation,structure analysis and fluorescence characteristics of fluorescent nanomaterials have received much attention.In order to obtain Si-based fluorescent nanomaterial with high luminous intensity,high fluorescent quantum efficiency and better controlling of preparation process,the effects of Si nanowires on the luminescence properties and the optical stabilities of the samples were investigated.First,based on the solid-liquid-solid growth mechanism,Si nanowires were grown under the conditions of reaction temperature of 1 100℃,N2 gas flow rate of 1 500 sccm and growth time of 15~60 min.The Si nanowires with different lengths and distributions were grown on single-crystal Si(100)substrates with"polishing"and"pyramid"texture surfaces respectively.And the Si nanowires with density of about 10^8 and 10^10 cm^-2 were grown with Au or Au-Al alloy film as metal catalyst.Then,a series of fluorescent nanometers SiNWs:Tb^3+samples were prepared using L4514 automatic temperature control tube heating furnace based on high-temperature solid-state method under the temperature 1 100℃,doping time 60 min,N2 gas flow rate 1 000 sccm,different Si nanowire substrates and high-purity Tb 4O 7(99.99%)powder as doping agent.Next,at room temperature,the photoluminescence characteristics of different samples were measured by the Hitachi F-4600 fluorescence spectrophotometer with the fixed excitation light wavelength of 243 nm,the excitation light slit of 2.5 nm,the emission light slit of 2.5 nm,the scanning wavelength range of 450~650 nm and the PMT voltage of 600 V.Finally,the optical stabilities of the fluorescent nanomaterial was experimentally tested,such as time stability(0~30 d),temperature stability(300~500 K),acid and alkali stability(pH 1 and pH 11),anti-p
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