非水解溶胶–凝胶法低温合成纳米BiVO_4黄色色料
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摘要
以无水三氯化铋(Bi Cl3)和三氯化钒(VCl3)为原料,乙醇为氧供体,通过非水解溶胶–凝胶法(NHSG)制备了钒酸铋(BiVO_4)黄色色料。分别通过X射线衍射和场发射扫描电子显微镜分析了色料的晶体结构和显微形貌,采用Fourier变换红外光谱(FTIR)探究了非水解溶胶–凝胶法制备BiVO_4黄色色料的反应过程。同时系统研究了Bi/V摩尔比和温度对色料色度值的影响。结果表明:该色料为单斜白钨矿型(m-BiVO_4),粒径尺寸约为400 nm。同时,采用非水解溶胶–凝胶法能够实现BiVO_4色料的低温合成,合成温度由传统固相法的650℃降至400℃,且色料呈亮黄色,当Bi/V摩尔比为1.1时,制备出的色料色度值为L*=61.6、a*=2.74、b*=62.9,远高于采用固相法合成BiVO_4色料的色度值。FTIR测试表明,非水解溶胶–凝胶法制备BiVO_4黄色色料的反应过程为钒醇盐和金属卤化物间发生非水解亲核取代反应,缩聚形成BiVO_4,有利于提高样品的均匀性和降低合成温度。
BiVO_4 yellow pigment was prepared by a non-hydrolytic sol–gel(NHSG) method, using bismuth trichloride(BiCl3) and vanadium trichloride(VCl3) as raw materials, ethanol as oxygen donor, respectively. The phase composition and the morphology of the pigment were studied by means of X-ray diffraction patterns and field emission scanning electron microscope, and the NHSG process of BiVO_4 yellow pigment was investigated by Fourier transform infrared(FTIR) spectroscopy. The effects of Bi/V molar ratio and temperature on the chromatic value of the pigment were systematically studied. The results indicate that the resulting products have monoclinic scheelite-structure, and the particle size is about 400 nm. Meanwhile, the BiVO_4 pigment can be synthesized via NHSG method at low-temperature. Compared with the conventional solid state method, its synthesis temperature is decreased from 650 ℃ to 400 ℃, and the pigment exhibits brighter yellow hue. When the molar ratio of Bi/V is 1.1, the BiVO_4 yellow pigment shows excellent chromatic performance, as L*=61.6,a*=2.74,b*=62.9, which is much higher than that of the sample prepared by the conventional solid state method. FTIR spectra results show that the vanadium alkoxide react with metal halide through non-hydrolytic nucleophilic substitution reaction, and BiVO_4 gel is formed via polycondensation process, resulting in the highly homogeneous samples and the low synthesis temperature.
BiVO_4 yellow pigment was prepared by a non-hydrolytic sol–gel(NHSG) method, using bismuth trichloride(BiCl3) and vanadium trichloride(VCl3) as raw materials, ethanol as oxygen donor, respectively. The phase composition and the morphology of the pigment were studied by means of X-ray diffraction patterns and field emission scanning electron microscope, and the NHSG process of BiVO_4 yellow pigment was investigated by Fourier transform infrared(FTIR) spectroscopy. The effects of Bi/V molar ratio and temperature on the chromatic value of the pigment were systematically studied. The results indicate that the resulting products have monoclinic scheelite-structure, and the particle size is about 400 nm. Meanwhile, the BiVO_4 pigment can be synthesized via NHSG method at low-temperature. Compared with the conventional solid state method, its synthesis temperature is decreased from 650 ℃ to 400 ℃, and the pigment exhibits brighter yellow hue. When the molar ratio of Bi/V is 1.1, the BiVO_4 yellow pigment shows excellent chromatic performance, as L*=61.6,a*=2.74,b*=62.9, which is much higher than that of the sample prepared by the conventional solid state method. FTIR spectra results show that the vanadium alkoxide react with metal halide through non-hydrolytic nucleophilic substitution reaction, and BiVO_4 gel is formed via polycondensation process, resulting in the highly homogeneous samples and the low synthesis temperature.
引文
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[32]陈渊,周科朝,黄苏萍,等.BiVO4纳米片的水热合成及可见光催化性能[J].中国有色金属学报,2011,21(7):1570-1579.CHEN Yuan,ZHOU Kechao,HUANG Suping,et al.Chin J Nonferr Met(in Chinese),2011,21(7):1570-1579.
[33]ZHANG A P,ZHANG J Z,CUI N Y,et al.Effects of pH on hydrothermal synthesis and characterization of visible-light-driven BiVO4 photocatalyst[J].J Mol Catal A Chem,2009,304:28-32.
[34]LI G Q,BAI Y,ZHANG W F.Difference in valence band top of BiVO4 with different crystal structure[J].Mater Chem Phys,2012,136:930-934.
[2]PATIL V J,BHOGE Y E,PATIL U D,et al.Room temperature solution spray synthesis of bismuth vanadate nanopigment and its utilization in formulation of industrial OEM coatings[J].Vacuum,2016,127:17-21.
[3]GUAN L,FAN J L,ZHANG Y Y.Facile preparation of highly cost-effective Ba SO4@Bi VO4 core-shell structured brilliant yellow pigment[J].Dyes Pigm,2016,128:49-53.
[4]ZHAO G S,LIU W,DONG M,et al.Synthesis of monoclinic sheet-like BiVO4 with preferentially exposed(040)facets as a new yellow-green pigment[J].Dyes Pigm,2016,134:91-98.
[5]THALLURI S M,HUSSAIN M,SARACCO G,et al.Green-synthesized Bi VO4 oriented along{040}facets for visible-light-driven ethylene degradation[J].Ind Eng Chem Res,2014,53:2640-2646.
[6]PATIL S S,DUBAL D P,TAMBOLI M S,et al.Ag:BiVO4 dendritic hybrid-architecture for high energy density symmetric supercapacitors[J].J Mater Chem A,2016,4:7580-7584.
[7]ZHAO Y,LI R G,MU L C,et al.Significance of crystal morphology controlling in semiconductor-based photocatalysis:A case study on BiVO4 photocatalyst[J].Cryst Growth Des,2017,17(6):2923-2928.
[8]MENG W W,WANG L,LI Y H,et al.Enhanced sensing performance of mixed potential ammonia gas sensor based on Bi0.95Ni0.05VO3.975 by silver[J].Sens Actuators B,2018,259:668-676.
[9]ZHANG Z J,ZHENG Q C,SUN L.Synthesis of 2-D nanostructured Bi VO4:Ag hybrid as an efficient electrode material for supercapacitors[J].Ceram Int,2017,43(18):16217-16224.
[10]ULLAH H,TAHIR A A,MALLICK T K.Structural and electronic properties of oxygen defective and Se-doped p-type BiVO4(001)thin film for the applications of photocatalysis[J].Appl Catal B,2018,224:895-903.
[11]LINDEN E G V D,MALTA L F B,MEDEIROS M E.Evaluation of synthetic routes to pigmentary grade bismuth vanadate[J].Dyes Pigm,2011,90:36-40.
[12]ZHANG L,CHEN D R,JIAO X L.Monoclinic structured BiVO4nanosheets:Hydrothermal preparation,formation mechanism,and coloristic and photocatalytic properties[J].J Phys Chem B,2006,110:2668-2673.
[13]NEVES M C,LEHOCKY M,SOARES R,et al.Chemical bath deposition of cerium doped BiVO4[J].Dyes Pigm,2003,59:181-184.
[14]高善民,乔青安,赵培培,等.沉淀法制备不同形貌和结构的纳米BiVO4[J].无机化学学报,2007,23(7):1153-1158.GAO Shanmin,QIAO Qingan,ZHAO Peipei,et al.Chin J Inorg Chem(in Chinese),2007,23(7):1153-1158.
[15]王敏,刘琼,孙亚杰,等.溶胶-凝胶法制备Eu3+掺杂BiVO4及其可见光光催化性能[J].无机材料学报,2013,28(2):153-158.WANG Min,LIU Qiong,SUN Yajie,et al.J Inorg Mater(in Chinese),2013,28(2):153-158.
[16]SAMEERA S F,PADALA P R,VINEETHA J,et al.Probing structural variation and multifunctionality in niobium doped bismuth banadate materials[J].Dalton T,2014,43(42):15851-15860.
[17]CORRIU R,LECLERCQ D,LEFEVRE P,et al.Preparation of monolithic binary oxide gels by a nonhydrolytic sol-gel process[J].Chem Mater,1992,4(5):961-963.
[18]WEI H Y,LI H,CUI Y,et al.Synthesis of flexible mullite nanofibres by electrospinning based on non-hydrolytic sol-gel method[J].JSol-Gel Sci Technol,2017,82(3):718-727.
[19]ALHENDAL A,MENGIS S,MATTHEWS J,et al.Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coating for samle preparation[J].JChromatogr A,2016,1468:23-32.
[20]SCIANCALEPORE C,BONDIOLI F,MESSORI M.Non-hydrolytic sol-gel synthesis and reactive suspension method:an innovative approach to obtain magnetite-epoxy nanocomposite materials[J].JSol-Gel Sci Technol,2017,81(1):69-83.
[21]JAGDALE P,CASTELLINO M,MARREC F,et al.Nanosized bismuth oxychloride by metal organic chemical vapour deposition[J].Appl Surf Sci,2014,303:250-254.
[22]WANG C H,ZHANG X T,YUAN B,et al.Simple route to self-assembled BiOCl networks photocatalyst from nanosheet with exposed(001)facet[J].Micro Nano Lett,2012,7:152-154.
[23]刘国聪,刘又年,刘素琴,等.锂离子电池正极材料Li3V2-2x/3Mnx(PO4)3的溶胶-凝胶法合成和电化学性能[J].无机材料学报,2012,27(10):1017-1022.LIU Guocong,LIU Younian,LIU Suqing,et al.J Inorg Mater(in Chinese),2012,27(10):1017-1022.
[24]CHANG X F,WANG S B,QI Q,et al.Insights into the growth of bismuth nanoparticles on 2D structured BiOCl photocatalysts:an in situ TEM investigation[J].Dalton Trans,2015,44(36):15888-15896.
[25]SONG J M,MAO C J,NIU HL,et al.Hierarchical structured bismuth oxychlorides:self-assembly from nanoplates to nanoflowers via a solvothermal route and their photocatalytic properties[J].Crystengcomm,2010,12,3875-3881.
[26]魏恒勇,江伟辉,林健,等.非水解和水解溶胶-凝胶法合成钛酸铝粉体的研究对比[J].无机材料学报,2009,24(1):199-203.WEI Hengyong,JIANG Weihui,LIN Jian,et al.J Inorg Mater(in Chinese),2009,24(1):199-203.
[27]LI H Y,ZHU Z L,YANG F L,et al.Structure of V2O5-P2O5-Sb2O3-Bi2O3glass[J].Int J Miner Metall Mater,2012,19(7):628-635.
[28]ALLAF A W.Theoretical and experimental investigations of vanadium(III)oxychloride[J].J Chem Res,2003,9:553-555.
[29]ROSENTHAL E C E,CUI H,LANGE K C H,et al.Synthesis,molecular structure,and olefin polymerization activity of an oxovanadium(V)alkoxide with unprecedented chloride bridging ligands[J].Eur J Inorg Chem,2004,2004(23):4681-4685.
[30]李静,宋伟,窦伯生.丙烷氧化反应中多组分氧化物Bi-V-Mo-O催化作用的红外光谱研究[J].应用化学,1996,13(5):58-60.LI Jing,SONG Wei,DOU Bosheng.Chin J Appl Chem(in Chinese),1996,13(5):58-60.
[31]PASCUTA P,BORODI G,CULEA E,et al.Structural investigation of bismuth borate glass ceramics containing gadolinium ions by X-ray diffraction and FTIR spectroscopy[J].J Mater Sci:Mater Electron,2009,20(4):360-365.
[32]陈渊,周科朝,黄苏萍,等.BiVO4纳米片的水热合成及可见光催化性能[J].中国有色金属学报,2011,21(7):1570-1579.CHEN Yuan,ZHOU Kechao,HUANG Suping,et al.Chin J Nonferr Met(in Chinese),2011,21(7):1570-1579.
[33]ZHANG A P,ZHANG J Z,CUI N Y,et al.Effects of pH on hydrothermal synthesis and characterization of visible-light-driven BiVO4 photocatalyst[J].J Mol Catal A Chem,2009,304:28-32.
[34]LI G Q,BAI Y,ZHANG W F.Difference in valence band top of BiVO4 with different crystal structure[J].Mater Chem Phys,2012,136:930-934.