Synthesis and characterization of submicron Co3+-doped LaBO3 powders by combustion method
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摘要: 以La(NO3)3·6H2O、Co(NO3)3·6H2O、H3BO3和C2H5NO2为原料，采用燃烧法合成Co3+掺杂LaBO3粉体，其中原料摩尔比为[La(NO3)3·6H2O+Co(NO3)3·6H2O]:H3BO3:C2H5NO2=3:3:5，研究了目标产物La(1−x)CoxBO3（x=0.01～0.04）在750～950 ℃的合成反应过程及产物结晶形态，分析了合成条件对产物晶体形态的影响，得到了最佳的原料配比、反应温度、反应时间和掺杂量。结果表明，燃烧合成法可用于制备Co3+掺杂LaBO3粉体，且实验条件简单，煅烧温度较低，产率高，易于工业化。最佳反应条件为900 ℃、4 h，改性剂钴的掺杂量为x=0.03，产物为La0.97Co0.03BO3粉体。在该反应条件下，产物颗粒大小均匀，为直径115～185 nm、长度400～600 nm的短棒状粉体。Co3+掺杂LaBO3粉体产物在330～440 nm处出现一个较宽的荧光激发带，说明具有较为均匀粒径和晶体形貌的Co3+掺杂LaBO3粉体可以作为制备发光粉体的基质材料。Abstract: Co3+-doped LaBO3 powders were synthesized by combustion method using La(NO3)3·6H2O, Co(NO3)3·6H2O), H3BO3, and C2H5NO2 as the raw materials with the mole ratio of [La(NO3)3·6H2O+Co(NO3)3·6H2O]:H3BO3:C2H5NO2=3:3:5. The synthesis process and crystal morphology of the target products La(1−x)CoxBO3 (x=0.01~0.04) at 750~950 ℃ were studied. The influence of synthesis conditions on the crystal morphology of the powder products was analyzed. The optimal ratio of the raw materials, reaction temperature, reaction time, and doping dosage were obtained. In the results, the combustion synthesis method can be used to prepare the Co3+-doped LaBO3 powders, and the experimental conditions are simple, the calcination temperature is low, the yield is high, and it is easy to industrialization. The optimal reaction condition is 900 ℃ and 4 h, the doping dosage of cobalt as modifier is x=0.03, and the products are La0.97Co0.03BO3 powders. Under the optimal reaction condition, the products are the short rod-like powders in the uniform particle size distribution with the diameter of 115~185 nm and the length of 400~600 nm. The fluorescence excitation band appears at 330~440 nm for the Co3+-doped LaBO3 powders, indicating that the Co3+-doped LaBO3 powders with the uniform particle size and crystal morphology can be used as the substrate material for preparing the luminescent powders.
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Key words:
- LaBO3 powders /
- combustion method /
- rare earth metals /
- Co3+ doping
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图 1 不同煅烧温度下Co3+掺杂LaBO3粉体X射线衍射图谱
Figure 1. XRD patterns of the Co3+-doped LaBO3 powders synthesized at different calcination temperatures
图 2 不同保温时间下Co3+掺杂LaBO3粉体X射线衍射图谱
Figure 2. XRD pattern of the Co3+-doped LaBO3 powders synthesized at different holding times
图 3 900 ℃、4 h制备的Co3+掺杂LaBO3粉体显微形貌
Figure 3. SEM images of the Co3+-doped LaBO3 powders prepared at 900 ℃ for 4 h
图 4 950 ℃、4 h制备的Co3+掺杂LaBO3粉体显微形貌
Figure 4. SEM images of the Co3+-doped LaBO3 powders prepared at 950 ℃ for 4 h
图 5 900 ℃、4 h制备的纯相LaBO3粉体透射电镜显微形貌
Figure 5. TEM images of the pure phase LaBO3 powders prepared at 900 ℃ for 4 h
图 6 900 ℃、4 h制备的Co3+掺杂LaBO3粉体透射电镜显微形貌
Figure 6. TEM images of the Co3+-doped LaBO3 powders prepared at 900 ℃ for 4 h
图 7 不同改性剂剂量下Co3+掺杂LaBO3粉体X射线衍射图谱
Figure 7. XRD patterns of the Co3+-doped LaBO3 powders with the different dosage of modifier
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[1] Zhou Y, Jia H Y, Li D X, et al. Low-temperature preparation and characterization of LaBO3 flurescent matrix materials. China Powder Sci Technol, 2019, 25(1): 35周宇, 贾涵月, 李冬霞, 等. LaBO3荧光基质材料的低温制备与表征. 中国粉体技术, 2019, 25(1): 35 [2] Wang D, Chen P, Ji L X, et al. Preparation and characterization of CaSiO3: Eu2+, Dy3+ storage luminescent materials by sol-gel method. J Liaoning Petrochem Univ, 2014, 34(1): 23王德, 陈鹏, 纪灵娴, 等. 溶胶-凝胶法制备CaSiO3: Eu2+, Dy3+蓄能发光材料及性能研究. 辽宁石油化工大学学报, 2014, 34(1): 23 [3] Yang G B, Jin F J, Guo M, et al. Preparation of oil-soluble lanthanum borate nanoparticles and investigation on their tribological properties in different base oils. Lubr Eng, 2019, 44(4): 8杨广彬, 金凤杰, 郭淼, 等. 油溶性硼酸镧纳米微粒的制备及其在不同基础油中的摩擦学性能研究. 润滑与密封, 2019, 44(4): 8 [4] Gu K C, Chen B S, Wang X M, et al. Preparation, friction and wear properties of hydrophobic lanthanum borate nanorods in rapeseed oil. Trans Nonferrous Met Soc China, 2014, 24(11): 3578 doi: 10.1016/S1003-6326(14)63504-4 [5] Wang Y, Zhou Y K, Huang D K, et al. The tribology performance of La2[B4O5(OH)4]3/In composite nanoparticles in rapeseed oil. Non-Met Min, 2016, 39(6): 82王玥, 周元康, 黄代宽. 硼酸镧/铟复合纳米微粒在菜籽油中的摩擦学性能. 非金属矿, 2016, 39(6): 82 [6] Ramesh P, Jagannath G, Eraiah B, et al. Optical and physical investigations of lanthanum bismuth borate glasses doped with Ho2O3. IOP Conf Ser Mater Sci Eng, 2018, 310(1): 012032 [7] Zheng F K, Zhang G N, Chen X J, et al. A new method of preparing high-performance high-entropy alloys through high-gravity combustion synthesis. Int J Miner Metall Mater, 2020, 27(10): 1347 doi: 10.1007/s12613-020-2028-x [8] Wang Y W, Wu X J, Cai Y F, et al. Research progress of rare earth doped Sr2MgSi2O7 long afterglow luminescent materials. Powder Metall Technol, 2020, 38(2): 143王岳武, 武鑫江, 蔡永丰, 等. 稀土掺杂Sr2MgSi2O7长余辉发光材料的研究进展. 粉末冶金技术, 2020, 38(2): 143 [9] Li S. Study on Electrospinning Synthesis and Structural Characterizations of One-Dimensional Nanostructure of Borate [Dissertation]. Changchun: Jilin University, 2010李霜. 硼酸盐一维纳米结构材料的静电纺丝法制备与结构表征[学位论文]. 长春: 吉林大学, 2010 [10] Selda S, Senberber F T, Yildirim M, et al. Lanthanum borate synthesis via the solid-state method from a La2O3 precursor: Electrical and optical properties. Mater Chem Phys, 2017, 200: 196 doi: 10.1016/j.matchemphys.2017.07.056 [11] Pari G, Jaya S M, Subramoniam G, et al. Density-functional description of the electronic structure of LaMO3 (M=Sc, Ti, Cr, Mn, Fe, Co, Ni). Phys Rev B, 1995, 51(23): 16575 doi: 10.1103/PhysRevB.51.16575 [12] Li X P, Yuan Z, Gong X J, et al. Preparation of nickel ferrite composite oxide with combustion and its photocatalytic application. J Liaoning Petrochem Univ, 2016, 36(2): 9李秀萍, 袁哲, 宫晓杰, 等. 燃烧法制备铁酸镍复合氧化物及光催化研究. 辽宁石油化工大学学报, 2016, 36(2): 9 [13] Jiao Z W, Wang R J, Wang X Q, et al. LaZnB5O10, the first lanthanum zinc borate. Acta Crystallogr, Sect E: Struct Rep Online, 2010, 66(1): 11 [14] Zhao X G, Zhou Y, Li D X, et al. Preparation and characterization of LaBO3: Eu, Gd, powders by microwave induced combustion. J Optoelectron Laser, 2019, 30(2): 129赵旭光, 周宇, 李冬霞, 等. 微波诱导燃烧法制备LaBO3: Eu, Gd粉体及其表征. 光电子激光, 2019, 30(2): 129 [15] Jin H B, Zhao X G, Fan H F, et al. Preparation and spectral properties of LaBO3: Yb3+ powders. J Optoelectron Laser, 2019, 30(8): 817金怀宝, 赵旭光, 范华风, 等. LaBO3: Yb3+粉体的制备及光谱性质研究. 光电子激光, 2019, 30(8): 817 [16] Kononets N V, Seminko V V, Maksimchuk P O, et al. Processes of energy migration in mixed europium–lanthanum magnesium borate nanocrystals. Spectrosc Lett, 2017, 50(7): 399 doi: 10.1080/00387010.2017.1345946 [17] Li L. Preparation and properties of Eu: La2CaB10O19 by sol-gel method. Guangdong Chem Ind, 2011, 38(5): 117李岚. 溶胶-凝胶法合成掺铕硼酸镧钙荧光粉及其表征. 广东化工, 2011, 38(5): 117 [18] Jain S R, Adiga K C, Vemeker V R P. A new approach to thermochemical calculations of condensed fuel-oxidizer mixtures. Combust Flame, 1981, 40: 71 doi: 10.1016/0010-2180(81)90111-5 -
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