SnO2/NiO复合半导体纳米纤维的制备及气敏性能研究

采用静电纺丝技术结合化学沉淀法和高温煅烧处理, 制备了具有不同Sn含量的SnO₂/NiO复合半导体纳米纤维。采用扫描电子显微镜(SEM), X射线衍射仪(XRD)和能量色散X射线光谱仪(EDS)对样品的形貌, 结构以及各元素含量进行表征。以乙醇为目标气体, 探究SnO₂/NiO纳米纤维的气体传感性质, 以及Sn含量对复合纳米纤维气敏性能的影响。研究结果表明, SnO₂/NiO复合纳米纤维具有三维网状结构, SnO₂复合对NiO纳米纤维的气敏性能具有明显的增强作用。随着SnO₂含量的增加, 复合纤维对乙醇气体的响应灵敏度增强, 其中响应最高的复合纳米纤维在最佳工作温度160 ℃条件下对体积分数为100×10^-6乙醇气体的响应灵敏度为13.4, 是NiO纳米纤维最大响应灵敏度的8.38倍。与市面常见的乙醇气体传感器MQ-3相比, SnO₂/NiO复合纳米纤维的最佳工作温度更低, 响应灵敏度更高, 具有一定的实际应用价值。     

In2O3纳米孔材料的制备及其甲醛气敏性能研究

以In(NO3)3·4.5H2O为主要原料,采用溶剂热法成功地制备出In2O3纳米孔材料.采用X射线粉末衍射、透射电子显微镜等对样品的物相和形貌进行了表征和分析,并系统研究了其气敏性能.结果表明,成功合成的六方相In2O3纳米孔材料,其孔径小于17nm,孔道形状复杂且相互连通,以该材料制成的气敏元件对甲醛有很好的气敏性能,对50×10-6甲醛的灵敏度高达23.6.     

花状SnO2的制备及其气敏特性的研究

以乙二醇(C2H6O2)为有机溶剂,采用溶剂热法制备了花状SnO2纳米材料,并将制备的SnO2制成旁热式气敏元件.通过XRD,SEM等测试手段对SnO2纳米材料进行了表征,并初步分析了气敏元件对丙酮的敏感机理.制备的SnO2材料是由粒径约为10 nm的颗粒有规则的堆叠而成的直径约为3～4μm的花瓣清晰的多孔分级花状结构.研究发现,气敏元件对丙酮气体有很好的响应灵敏度.在最佳工作温度(350℃)时,检测的丙酮体积分数最低为1×10-6.对100 ppm丙酮的响应及恢复时间分别为40和50 s.且气敏元件对丙酮气体的响应灵敏度远高于对苯、甲苯、甲醇、甲醛、氨等气体的响应灵敏度.     

片状ZnO/ZIF-8异质结的正丁醇气敏性能增强研究

本文利用水热法，以2-甲基咪唑和氧化锌(ZnO)纳米片为原料原位合成了片状ZnO/ZIF-8异质结复合材料。利用X射线衍射(XRD)、红外光谱(IR)和扫描电子显微镜(SEM)对样品进行表征，并通过气敏性能测试仪系统研究了样品的气敏性能，进一步探讨了ZnO/ZIF-8气敏性能增强的可能机理。气敏性能分析结果表明：与纯相ZnO(其最佳工作温度为180℃)相比，ZnO/ZIF-8的最佳工作温度降低为160℃。在最佳工作温度下，ZnO/ZIF-8对正丁醇表现出了优异的选择性，对200 ppm正丁醇的响应达到了76.778。在5～200 ppm正丁醇浓度范围内，ZnO/ZIF-8的灵敏度与浓度的相关性近似呈线性，重复性及稳定性良好，适合检测低浓度的正丁醇气体。     

LaFeO_3纳米纤维的制备及其气敏特性研究

采用静电纺丝方法制备了LaFeO3纳米纤维,利用电子扫描显微镜(SEM)、X-射线衍射(XRD)对其进行表征。所合成的LaFeO3纳米纤维材料作为敏感材料制作烧结型旁热式气敏元件,测试其气敏特性。结果表明,基于LaFeO3纳米纤维的气体传感器对于乙醇气体的最佳工作温度为200℃,对于浓度为500×10-6的乙醇气体,灵敏度为46,LaFeO3纳米纤维材料对乙醇具有快速的响应恢复速度。     

异质复合结构纳米纤维SnO2/ZnO的制备及其气敏特性研究

采用静电纺丝法制备了多级中空结构的SnO₂纳米纤维, 然后将SnO₂纳米纤维置于90℃乙酸锌溶液中, 恒温水浴条件下, 在SnO₂纳米纤维上生长了ZnO纳米球, 形成了异质结构的SnO₂/ZnO复合纳米纤维。分别通过XRD、SEM、EDX和XPS等表征手段对异质复合纳米纤维SnO₂/ZnO材料的结构、形貌及元素含量进行了表征分析。异质结构的SnO₂/ZnO复合纳米纤维保持了SnO₂纳米纤维多级中空的纤维结构, SnO₂纳米纤维长度约为300 nm, 依附于SnO₂纤维表面的SnO₂纳米颗粒生长的ZnO纳米球直径为250~300 nm。采用静态气体测试系统对异质复合纳米纤维SnO₂/ZnO气敏元件的气敏性能进行了测试。测试结果表明: 异质复合纳米纤维SnO₂/ZnO气敏元件在最佳工作温度350℃下, 对(0.5~100)×10^-6丙酮具有优异的响应灵敏度、较好的选择性和长期稳定性。异质复合纳米纤维SnO₂/ZnO中存在于ZnO纳米球与SnO₂纳米颗粒间的N-N同型异质结导致复合材料晶界势垒高度的降低, 改善了电子与空穴的输运特性, 促使SnO₂/ZnO异质复合纳米纤维的吸附能力大大增强, 从而改善了SnO₂/ZnO元件的丙酮敏感特性。     

SnS2纳米片的制备及其对NO2气体的检测

二维金属硫化物材料具有较低的电子噪声以及极大的比表面积, 使其非常适合用作气敏材料, 因此寻求高效可控的方法制备二维金属硫化物材料是目前的研究热点。本研究使用高温化学浴法制备了不同形貌的高结晶二维六方SnS₂纳米片。采用不同手段对制备的SnS₂纳米片进行表征, 并进一步研究了SnS₂纳米片的气敏性能。结果显示: 油酸、油胺用量(体积)相同时, 产物SnS₂的形貌是均一的六角形纳米片, 其直径约150 nm, 厚度约4~6 nm。气敏测试表明该SnS₂纳米片对NO₂气体具有良好响应, 且响应过程可逆, 选择性好。其最佳工作温度为130 ℃, 响应和恢复时间分别为98和680 s。     

sol-gel法制备的SnO_2-TiO_2厚膜及其气敏特性研究

采用sol-gel法,以钛酸丁酯、四氯化锡为前驱体制备了不同掺杂量的Sn O2-Ti O2纳米粉末,样品经300,500,700和900℃退火后,利用浸渍提拉法,在Al2O3陶瓷管表面制备了Sn O2-Ti O2厚膜。通过XRD和SEM对制备的纳米粉末的物相、形貌进行表征,静态配气法对其气敏性能进行测试,并结合分子轨道理论探讨了气敏机理。实验结果表明,经700℃退火的4%(原子分数)掺杂的Sn O2-Ti O2气敏元件,对乙醇气体具有很好的选择性,在工作温度为63℃时,对乙醇气体的灵敏度可达1 903,响应-恢复时间分别为1和3 s,所制备的气敏元件有望用于乙醇气体的实用化检测。     

MWCNTs/多孔ZnO纳米材料的制备及室温NO气敏性研究

为开发室温气敏传感器材料,以Zn(NO3)2.6H2O为锌源、尿素为沉淀剂,在制备水合碱式碳酸锌(Zn4CO3(OH)6.H2O)的过程中加入羧基化的MWCNTs(MWCNT-COOH),焙烧制备了MWCNTs/ZnO复合材料.采用XRD,SEM和TEM等对其进行了分析.结果表明:复合材料中MWCNTs分散均匀,ZnO呈多孔纳米片状,纳米片由多个尺寸在10～20 nm的ZnO颗粒组成;在室温、空气湿度为50%的氛围中测试复合材料对NO的气敏响应发现,复合材料对体积浓度1×10-4的NO气敏响应灵敏度大约是MWCNT-COOH的3倍,明显高于MWCNT-COOH;对比加入不同量MWCNT-COOH制备的3种复合材料对NO的气敏性可知,加入200 mg MWCNT-COOH所制备的复合材料对低浓度(体积浓度≤50×10-6)的NO气体表现出较高的灵敏度.     

溶胶凝胶模板法制备In2O3纳米线及其气敏性能

以InCl3·4H2O和乙二胺为原料,采用溶胶凝胶模板法合成了立方晶系的In2O3纳米线,利用X射线衍射仪、扫描电镜、透射电镜对材料的组成、形貌、晶粒的大小、直径进行了表征,结果表明,产物是直径为80-100nm,晶粒直径为4-10 nm的纳米线。用产物In2O3纳米线制备气敏元件,气敏测试结果显示,合成的In2O3纳米线对NO2具有很高的灵敏度,器件的最佳工作温度为360 ℃。     

NiO/PB复合电致变色薄膜的制备及其性能研

采用水热法制备了垂直生长的氧化镍(NiO)纳米片薄膜, 并利用电沉积法将普鲁士蓝(PB)负载到NiO纳米片薄膜上, 制备了新型的NiO/PB复合电致变色薄膜。利用X射线衍射仪(XRD)、场发射扫描电镜(SEM)对样品的晶型以及微观形貌进行了表征, 采用紫外-可见光光度计以及电化学工作站对NiO/PB复合薄膜的电化学和电致变色性能进行了研究和表征。结果表明: NiO/PB复合电致变色薄膜具有多孔结构和较大的比表面积, 可以增大电解质与电极材料的接触面积。PB成功负载到NiO薄膜表面, 使NiO/PB复合薄膜表现出较大的电流密度。相比于单层NiO薄膜, NiO/PB复合薄膜表现出更好的电致变色性能, 其光调制范围可以达到46%, 着色效率为141 cm²/C, 并且其着色时间可以缩短到5 s, 褪色时间为6 s。     

Ba3V2O8∶Eu3+纳米花的制备及光致发光性能研究

采用复合氢氧化物媒介法制备了Ba3V2O8∶Eu3+纳米花。利用SEM-EDS、XRD、TEM和XPS对晶体的形貌和尺寸、结构和化学组成进行了表征。结果表明产物是由厚度约20nm的纳米片组成的花状Ba3V2O8∶Eu3+纳米晶体。荧光光谱测定发现Ba3V2O8∶Eu3+晶体在紫外光和蓝光激发下都能产生591和612nm 2个强发射峰,表明其具有将紫外光和蓝光转换成红光的能力,可以进一步应用于光转换和光发射领域。探讨了Ba3V2O8∶Eu3+纳米花的发光机理。     

Synthesis of hierarchical Ni(OH)(2) and NiO nanosheets and their adsorption kinetics and isotherms to Congo red in water

Ni(OH)(2) and NiO nanosheets with hierarchical porous structures were synthesized by a simple chemical precipitation method using nickel chloride as precursors and urea as precipitating agent. The as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy and nitrogen adsorption-desorption isotherms. Adsorption of Congo red (CR) onto the as-prepared samples from aqueous solutions was investigated and discussed. The pore structure analyses indicate that Ni(OH)(2) and NiO nanosheets are composed of at least three levels of hierarchical porous organization: small mesopores (ca. 3-5 nm), large mesopores (ca. 10-50 nm) and macropores (100-500 nm). The equilibrium adsorption data of CR on the as-prepared samples were analyzed by Langmuir and Freundlich models, suggesting that the Langmuir model provides the better correlation of the experimental data. The adsorption capacities for removal of CR was determined using the Langmuir equation and found to be 82.9, 151.7 and 39.7 mg/g for Ni(OH)(2) nanosheets, NiO nanosheets and NiO nanoparticles, respectively. Adsorption data were modeled using the pseudo-first-order, pseudo-second-order and intra-particle diffusion kinetics equations. The results indicate that pseudo-second-order kinetic equation and intra-particle diffusion model can better describe the adsorption kinetics. The as-prepared Ni(OH)(2) and NiO nanosheets are found to be effective adsorbents for the removal of Congo red pollutant from wastewater as a result of their unique hierarchical porous structures and high specific surface areas.     

水热合成一维α-MoO3纳米棒及其湿敏性能研究

采用水热法,以钼酸铵和硝酸为原料合成了一维纳米α-MoO_3棒状材料,并利用X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)对其物相及形貌进行了表征。一维α-MoO_3纳米棒直径为200~300nm,长度为5~10μm。一维α-MoO_3纳米棒表现出良好的湿敏性能,所制得的传感器在100Hz、11%~95%湿度范围内,其复阻抗-相对湿度关系在半对数坐标下有5个数量级的变化,线性度好。元件的恢复和响应时间较短,分别为3s和35s,元件的湿滞约为4%RH。利用器件在不同湿度下的阻抗图谱建立了相应的等效电路,分析其电导过程。结果表明,在低湿度范围内,器件传导主要依靠一维α-MoO_3材料内少量的自由电子传导以及材料本身束缚电荷的极化;在高湿度范围内,吸附水分子的分解和极化所引起的离子导电占主导地位。     

γ-Bi2O3/TiO2复合纤维的制备及光催化性能

采用静电纺丝技术与溶剂热法相结合制备了γ-Bi2O3/TiO2复合纤维光催化材料.利用X射线衍射(XRD)、扫描电镜(SEM)、电子能谱(EDS)、透射电镜(TEM)、高分辨透射电镜(HRTEM)和紫外–可见吸收光谱(UV-Vis)等分析测试手段对材料进行了表征,并以罗丹明B(RB)的脱色降解为模式反应,考察了材料的可见光催化性能.结果表明:γ-Bi2O3纳米片均匀地生长在TiO2纤维上,形成了具有异质结构的γ-Bi2O3/TiO2复合纤维光催化材料,其光谱响应范围拓宽至可见光区,有利于TiO2光生电子和空穴的分离,增强了体系的量子效率.与纯TiO2纤维相比可见光催化活性明显提高,对RB的脱色率达87.8%.     

Optical Absorption Characterizations of Porous Al_2O_3Host/NiO Nanocomposites

Porous Al2O3 host/NiO nanocomposites have been prepared by pyrolysis of Ni2(OH)2CO3 inthe nanostructured Al2O3 hosts. Diffuse reflection spectra in the wavelength range of 200 to800 nm were measured. Results show that (1) in each spectrum exist several absorption bandsof nano-NiO. With increasing the pyrolysis temperature from 550 to 1000℃, the numbers ofabsorption bands of NiO increase from 2 to 6 (P1-P6), (2) comparing with optical absorptionbands of single crystal NiO, for porous nanocomposites the P1, P2 and P4 present "blue shift"and the P3, P5 and P6 exhibit "red shift"; (3) when the pyrolysis temperature, Tp, is 550℃, theabsorption bands become so weak that only two bands (P1 and P6) can be observed and inverselywhen Tp=1000℃ all six absorption bands of NiO are strong, (4) for porous Al2O3/NiOnanocomposites prepared by pyrolysis at 1000℃ the PF+ caused by the F+ centers in theAl2O3 host moves towards the short wavelength at first with increasing the doping amount ofNiO from 5 to 50 wt pct and then shifts to the long wavelength with further increasing NiO. Inthis paper, the above phenomena and mechanism of the absorption bands of NiO are discussedin detail.     

Green synthesis of nickel oxide nanoparticles and studies of their photocatalytic activity in degradation of polyethylene films

Nickel oxide nanoparticles (NiO NPs) were synthesized using Ananas comosus leaf extract, and were characterized by UV–Vis spectroscopy, Fourier transform infrared (FTIR) spectroscopy, high resolution transmission electron microscopy (HRTEM), Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) techniques. The FTIR analysis confirms the formation of the NiO with appearance of NiO band at 468 cm⁻¹. The HRTEM analysis reveals that the NiO NPs size was in the range of 0.63–5.75 nm, with an average particle size of 1.42 ± 1.76 nm. The EDX analysis shows clear peaks of Ni (2.7%) and O (5.74%) in the spectrum. The peaks of XRD analysis at (2θ) 30°, 43.89°, 60.16°, 77.95° and 82.94° were assigned to (1 1 1), (2 0 0), (2 2 0), (3 1 1) and (2 2 2) planes of the face-centered cubic (fcc) lattice of NiO. The photocatalytic properties of the NiO NPs were studied through the solid phase degradation of low-density polyethylene (LDPE) film. We observed that polymeric nanocomposites (NCs) showed a significant weight loss of 33 ± 1.6% compared with the pure LDPE (8.6 ± 0.7%) after exposure to solar light irradiation for 240 h, while the nanocomposites under the dark condition gave a weight reduction of 1.90 ± 0.05 at the end of 240 h. The FTIR analysis also confirms the presence of carbonyl group, a degradation product of LDPE, with carbonyl index of 0.4. All these important factors showed that NiO is an effective photocatalyst. The study therefore suggests the incorporation of NiO NPs into the polymer matrix so as to enhance its photodegradation.     

分级介孔结构组成的ZnO微球及光催化性能

以硝酸锌、脲素及酒石酸为反应物, 采用水热法制备碱式碳酸锌前驱体微球, 通过煅烧前驱体制备了介孔氧化锌微球。通过扫描电子显微镜(SEM)可以观察到, 氧化锌微球的直径约为2~4 μm, 由大量厚度约为10 nm的介孔纳米片组装而成。X 射线衍射(XRD)和透射电镜(TEM)结果表明: ZnO微球为六方纤锌矿结构, 并结晶较好。比表面积测试(BET)表明ZnO微球为介孔材料, 孔径为20~50 nm, ZnO微球比表面积约为29.8 m²/g。以亚甲基蓝为目标降解物, 对介孔氧化锌微球进行了光催化降解实验。实验结果表明, 所合成的介孔ZnO微球对亚甲基蓝的光催化性能较好。     

Gas sensing study of hydrothermal reflux synthesized NiO/graphene foam electrode for CO sensing

Nickel oxide nanosheets have been successfully synthesized on the graphene foam (GF) using hydrothermal reflux process for their application as carbon monoxide (CO) gas sensor. X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, energy dispersive spectroscopy, and gas sorption analysis were used to characterize the structure and morphology of the samples. The morphology (SEM), crystal structure (XRD and Raman), and elemental composition (EDS) analysis of NiO/GF composite confirmed the cubic crystal structure of NiO and elemental composition (i.e., Ni, O, and C) of NiO/GF composite. The results reveal that the incorporation of graphene into NiO nanosheets not only improved the surface area of NiO/GF composite, but also enhanced the performance of the composite on CO sensing by improving its conductivity. These results indicate that NiO/GF has potential as electrode material for CO gas sensor.     

异质结型NiO/ZnO复合纳米纤维的制备及光催化性能

采用静电纺丝技术, 以聚乙烯醇(PVA)和醋酸锌[Zn(CH₃COO)₂]为前驱体, 制备纯ZnO纳米纤维, 并以其为基质, 醋酸镍为镍源, 通过溶剂热法制备了NiO/ZnO复合纳米纤维. 利用X射线衍射(XRD)、扫描电镜(SEM)、高分辨透射电镜(HRTEM)和荧光光谱(PL)等分析测试手段对样品的结构和形貌进行表征。以罗丹明Ｂ的脱色降解为模式反应, 考察了样品的光催化性能。结果表明: NiO粒子均匀地负载到ZnO纳米纤维上, 得到了异质结型NiO/ZnO复合纳米纤维光催化材料, 与纯ZnO纳米纤维相比光催化活性明显提高, 且易于分离、回收和再利用。循环使用3次, RB的脱色率仍保持在89%以上。