Calcination-temperature-dependent gas-sensing properties of mesoporous α-Fe2O3 nanowires as ethanol sensors

The mesoporous α-Fe₂O₃ nanowires (NWs) were successfully synthesized by changing the calcination temperature from 550 to 750 °C (marked NWs-550, NWs-650 and NWs-750) via using SBA-15 silica as the hard templates with the nanocasting method. The characterization results indicated that the bandgap of the as-prepared samples hardly changed and the high BET surface areas changed a little with the calcination temperature from 550 to 750 °C. Mesoporous α-Fe₂O₃ NWs had been found to possess the remarkable gas-sensing performance to ethanol gas. The gas-sensing behavior indicated that α-Fe₂O₃ NWs-650 exhibited the higher response than that of α-Fe₂O₃ NWs-550 and α-Fe₂O₃ NWs-750. The calcination-temperature-dependent gas-sensing properties were mainly attributed to the competition of surface defects and body defects by the crystallization temperature. The lower calcination temperature could create more surface defects to improve the gas-sensing response, while the higher temperature would reduce the body defect and make the charge carriers transport easily. As the result, the suitable calcination temperature was desired to optimize the defects of nanostructures to improve the gas sensitivity.     

Synthesis,characterization, and biosensing application of ZnO/SnO2 heterostructured nanomaterials

In this work, zinc oxide/tin oxide (ZnO/SnO₂) heterostructured nanomaterials were synthesized by hydrothermal method. Transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction measurements revealed that the product was composed of ZnO nanowires and SnO₂ nanobranches. The novel ZnO/SnO₂ heterostructured nanocrystals were for the first time used as a supporting matrix to explore a novel immobilization and biosensing platform of redox proteins. UV–visible absorption investigation indicated that hemoglobin (Hb) intercalated well in the ZnO/SnO₂ heterostructured nanocrystals retained its native structure. Comparative experiments have confirmed that the ZnO/SnO₂-based biosensor not only had enhanced direct electron transfer capacity but also displayed excellent electrocatalytic properties such as higher sensitivity and wider linear range to the detection of hydrogen peroxide in comparison with the ZnO- and SnO₂-based biosensors.     

SnO2 quantum dots and quantum wires: controllable synthesis, self-assembled 2D architectures, and gas-sensing properties

SnO2 quantum dots (QDs) and ultrathin nanowires (NWs) with diameters of approximately 0.5-2.5 and approximately 1.5-4.5 nm, respectively, were controllably synthesized in a simple solution system. They are supposed to be ideal models for studying the continuous evolution of the quantum-confinement effect in SnO2 1D --> 0D systems. The observed transition from strong to weak quantum confinement in SnO2 QDs and ultrathin NWs is interpreted through the use of the Brus effective-mass approximation and the Nosaka finite-depth well model. Photoluminescence properties that were coinfluenced by size effects, defects (oxygen vacancies), and surface capping are discussed in detail. With the SnO2 QDs as building blocks, various 2D porous structures with ordered hexagonal, distorted hexagonal, and square patterns were prepared on silicon-wafer surfaces and exhibited optical features of 2D photonic crystals and enhanced gas sensitivity.     

Formation of SnO2 hollow nanospheres inside mesoporous silica nanoreactors

We report an interesting approach for efficient synthesis of SnO(2) hollow spheres inside mesoporous silica "nanoreactors". The as-prepared products are shown to have a uniform size distribution and good structural stability. When evaluated for their lithium storage properties, these SnO(2) hollow spheres manifest improved capacity retention.     

Synthesis of hierarchical shell-core SnO2 microspheres and their gas sensing properties

Using SnSO₄, d-glucose, urea and water, hierarchical shell-core SnO₂ microspheres were successfully synthesized via a simple hydrothermal method. The characterization results showed that the sizes of as-prepared SnO₂ microspheres were 0.6–1 μm, with shell thicknesses of 40−60 nm. The shell and large core of the SnO₂ microspheres were all comprised of the same basic rice-like nanoparticles with diameters of 16−25 nm and lengths of 16−45 nm. Further investigaton showed that the glucose and urea served as structural guiding agents, and urea facilitated the formation of the hierarchical structure. The as-prepared SnO₂ nanomaterials were used to fabricate a gas sensor with an electrode blade used for the gas sensitivity tests. The hierarchical shell-core SnO₂ microspheres exhibited high sensitivity and selectivity toward ethanol, with a responsivity of 63.8 for 50 ppm ethanol at 250 °C, while the response and recovery time were 7 s and 28 s respectively. Moreover, the responsivity of the materials showed good linearity at ethanol concentrations from 500 ppb to 10 ppm. The simple synthetic method, environmentally-friendly raw materials, and excellent gas sensitivity demonstrate that the as-prepared SnO₂ nanomaterial has great potential applications for the sensing of ethanol gas.     

Synthesis of ZnO nanomaterials with controlled morphology and their photoelectrochemical properties

Three morphologies of ZnO nanomaterials (ZnO-hand grenade, ZnO-rod and ZnO-particle) were synthesized via a facile hydrothermal method. The as prepared ZnO nanomaterials were used as photoelectrodes to fabricate dye sensitized solar cells (DSSCs). Of the three samples, ZnO-particle displays the highest photovoltaic conversion efficiency which can be attributed to the high surface area to absorb light more efficiently. Intensity modulated photocurrent spectroscopy (IMPS), and intensity-modulated voltage spectroscopy (IMVS) indicate that ZnO-rod provides superior electron transfer kinetics: fast electron transfer and long electron lifetimes with suppressed recombination.     

溶剂热合成具有海绵状结构的介孔SnO2

采用溶剂热方法, 以SnCl4·5H2O/尿素/乙醇三元体系合成了具有特定结构的前驱体, 该前驱体经焙烧后得到了具有海绵状结构的介孔SnO2. 利用X射线粉末衍射(XRD)、傅立叶红外吸收光谱(FT-IR)、透射电镜(TEM)、热分析(TG-DTA)和氮气等温吸附鄄脱附等方法对产物的结构、形貌和热稳定性进行表征. 结果表明, 300 ℃焙烧处理后的样品由粒径约为5 nm的纳米粒子堆积而形成海绵状结构, 其中孔的尺寸范围在2-8 nm, 样品比表面积达到了134 m2·g-1.     

Development of reproducible thiourea sensor with binary SnO2/V2O5 nanomaterials by electrochemical method

In this methodology, the thiourea (TU) sensor was made-up by means of glassy carbon electrode (GCE) layered by the wet-chemically prepared binary SnO₂/V₂O₅ nanomaterials (NMs). The existence of SnO₂ and V₂O₅ in prepared spherical NPs were categorized by X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM), Energy-dispersive X-ray spectroscopy and X-ray Powder Diffraction (XRD). The TU sensor was displayed the linear responses in concentration range (LDR) of 0.1 nM ~ 0.01 mM. The calibration curve of TU sensor was made by plotting current verses concentration of TU, which was measured by electrochemical technique. The sensitivity and lower limit of detection (DL) for TU sensor were calculated from calibration curve, which are found as 17.0918 µAµM^-1cm⁻² and 95.40 ± 4.77 pM respectively. The analytical parameters of TU sensor such as reproducibility, response time and stability were measured and found efficient results. It also was validated in the detection of TU in presence of real bio-samples. Thus, this unique and prospective method is introduced to develop the selective biosensor by electrochemical approach, which might be a pioneer sensor probe for its simple and reliable approach for the safety of healthcare and biomedical fields in a large scales.     

Hydrothermal synthesis of hierarchical SnO2 nanomaterials for high-efficiency detection of pesticide residue

Acephate pesticide contamination in agricultural production has caused serious human health problems. Metal oxide semiconductor (MOS) gas sensor can be used as a portable and promising alternative tool for efficiently detection of acephate. In this study, hierarchical assembled SnO₂ nanosphere, SnO₂ hollow nanosphere and SnO₂ nanoflower were synthesized respectively as high efficiency sensing materials to build rapid and selective acephate pesticide residues sensors. The morphologies of different SnO₂ 3D nanostructures were characterized by various material characterization technology. The sensitive performance test results of the 3D SnO₂ nanomaterials towards acephate show that hollow nanosphere SnO₂ based sensor displayed preferable sensitivity, selectivity, and rapid response (9 s) properties toward acephate at the optimal working temperature (300 °C). This SnO₂ hollow nanosphere based gas sensor represents a useful tool for simple and highly effective monitoring of acephate pesticide residues in food and environment. According to the characterization results, particularly Brunauer-Emmett-Teller (BET) and Ultraviolet-Visible Spectroscopy (UV–vis), the obvious and fast response can be attributed to the mesoporous hollow nanosphere structure and appropriate band gap of SnO₂ hollow nanosphere.     

不同形态SnO2纳米晶的制备

In this paper, we report our research on morphologically selective synthesis of nanocrystalline SnO2 by the combination of hydrothermal preparation and calcinated process. We firstly prepared SnO2 nanocrystals by the hydrothermal method at 140 ℃ for 3 h, using SnCI4 as the reactant. With the initial pH of 1.8 or 1.34, we prepared uniform and well-dispersed SnO2(tetragonal) nanocrystals, with similar size of about 3 nm, as determined by TEM. However, after being calcinated at 500 ℃ for 2 h, specimen 1 prepared at pH＝1.8 showed the rod-like shape with an average size of 5 nm×20 nm, while the other one(specimen 2)prepaed at pH＝1.34 showed a granular shape with an average size of 10 nm. XRD experiments showed that specimen 1 had a new diffraction peak after calcination, which was contributed by the (023) face of orthorhombic SnO2. The experiment results indicated that the morpholgy of SnO2 nanocrystals after calcination was closely related to the initial acidity of the reaction solution, possibly due to the difference in surface properties, e.g. the difference in crystalline faces exposed to the surface of particals, under different hydrothermal conditions.     

Physicochemical aspects of novel surfactantless, self-templated mesoporous SnO2 thin films

A novel method of synthesis consisting of the production of ordered arrangements of tubular pores distributed inside SnO2 annealed thin films, which are prepared from a rotating disk process carried out at 2000-3500 rpm, is herein described. The main novelty is that no surfactant molecules are required in order to create these ordered pore structures; the templating entities are supramolecular assemblies of oligomeric chains formed during the extra-long aging allowed to the sol-gel processing of tin(IV) tetra-tert-amiloxide, Sn(OAm(t))4, chelated with acetylacetone molecules. Low angle X-ray diffraction peaks of SnO2 thin films calcined at 500 degrees C clearly certify the existence of ordered mesostructures when employing the right H2O/Sn(OAm(t))4 molar ratio during the SnO2 sol-gel synthesis. The final SnO2 ordered mesostructures are reminiscent of those linked to MCM-41 and SBA-15 substrates. Pore-size distribution analyses proceeding from N2 sorption isotherms at 76 K on the SnO2 thin films calcined at 500 degrees C unequivocally confirm the presence of tubular mesopores (mode pore sizes ranging from 5 to 7 nm). The thicknesses of the SnO2 films range from 80 to 150 nm after performing a drying process at 100 degrees C and from 70 to 125 nm after calcining in air at 500 degrees C; these film thicknesses show, in general, decreasing trends when either the spinning rate or the H2O/(Sn(OAm(t))4 ratio is increased.     

Influence of mechanochemical and microwave treatment of tin dioxide on porous structure and gas-sensitive properties of SnO2-based sensor nanomaterials

Research on Chemical Intermediates - Microwave and mechanochemical treatments were used to obtain mesoporous or meso-macroporous structure of tin nanomaterials based on tin dioxide, including with...     

Synthesis and characterization of porous WO3–SnO2 nanomaterials: An infrared study of adsorbed pyridine and dimethyl methylphosphonate

High surface area porous W/Sn oxide nanomaterials were prepared via water/oil based (W/O) emulsion. Tungstic acid solution was generated by cation exchange of sodium tungstate in acidic Dowex resin. The acid was then mixed with a clear homogeneous aqueous N-cetyl trimethyl ammonium bromide (CTAB) solution followed by a slow addition of 0.2 M SnCl₄ solution. The mixture was stirred for 24 h and then subjected to slow calcination at 500 °C. The prepared materials were characterized using SEM-EDX, BET surface area, and sorption of nitrogen and water. Fourier transform infrared spectroscopy (FTIR) was used to characterize the surface acidic properties using pyridine vapor as a probe. The materials were then tested toward the Dimethyl methylphosphonate (DMMP) adsorption at various temperatures using infrared spectroscopy. At elevated temperatures, the desorption of DMMP from WO₃ and SnO₂ surfaces results in forming methyl phosphonate that strongly bounds on the metal oxide surfaces. In contrast, the FTIR spectra showed that the adsorbed dimethyl methylphosphonate (DMMP) on the mixed W/Sn oxide powders can be molecularly desorbed without any decomposition.     

Sensitive detection of Penicillin-G chemical using SnO2.YbO nanomaterials by electrochemical approach

In this approach, binary tin oxide doped ytterbium oxide nanosheets (SnO₂.YbO NSs) were synthesized in an alkaline phase using under low-temperature facile hydrothermal technique. Traditional methods such as UV–Visible spectroscopy, Fourier Transform Infra-Red Spectroscopy (FTIR), Powder X-ray diffraction (XRD), Field Emission Scanning Microscopy (FESEM) equipped with X-ray electron dispersive spectroscopy (XEDS), and X-ray photoelectron spectroscopy (XPS) were used to fully characterize the prepared SnO₂.YbO NSs. Fabrication of a thin-coating with doped NSs onto GCE by using 5% nafion conducting binder resulted in development of a selective and enzyme-free penicillin-G sensor probe. A reliable I-V technique was used to perform electrochemical performances of good sensitivity, large LDR, and long-term stability of the desired Penicillin-G sensor (SnO₂.YbO NSs/GCE/Nf). With a wide range of Penicillin-G concentration, the proposed calibration plot is noticed good linearity (R² = 0.9830). Sensitivity and LOD of the sensor were calculated as 24.75 μAμM^-1cm^?2 and 30.0 pM, respectively based on S/N = 3 formula. Real samples (Human and rabbit serum, milk, and red-sea water) were analyzed with the fabricated SnO₂.YbO NSs/GCE/Nf sensor probe and the findings results were acceptable and satisfactory. This approach could be a noble development of in-situ Penicillin-G sensor based on binary SnO₂.YbO NSs/GCE/Nf by reliable I-V technique for important sensing applications including beneficial doped nanomaterials and nano-technological system.     

Synthesis and gas-sensing properties of phenylhydrazine-functionalized single wall carbon nanotubes in polymer matrix

Gas sensor material was prepared by encapsulation of functionalized single-walled carbon nanotubes (SWCNT) into a gas-permeable polymer poly(1-trimethylsilyl-1-propyne) (PTMSP). A phenylhydrazino group was used for the functionalization of SWCNTs to improve their solubility and compatibility with polymers. Syntheses were carried out in aqueous surfactant solutions and in pure phenylhydrazine without surfactant. Two different temperatures (24 and 50°C) and two surfactants (sodium dodecyl sulfate and tricaprylmethylammonium chloride — Aliquat®336) were compared. Functionalized SWCNTs were characterized by X-ray photoelectron (XPS), Raman and Fourier transform infrared (FTIR) spectroscopy. Analyses showed that the synthesis at higher temperature in pure phenylhydrazine resulted in the highest functionalization yield. Phenylhydrazine itself proved to be a good solvent for SWCNTs. The functionalized nanotubes were soluble in organic solvents that under the same conditions were appropriate solvents for polymers. The sensitivity of functionalized SWCNT-PTMSP thin film composite to NO₂ gas at room temperature was significantly higher than that of the similar sensor material containing the pristine SWCNTs.      

Hydrothermal routes to prepare nanocrystalline mesoporous SnO2 having high thermal stability

We report simple hydrothermal routes to prepare thermally stable SnO2 particles having high specific surface areas and mesoporosity. The preparation method includes a new combination of synthetic processes: hydrolysis of tin(IV) chloride at 95 degrees C in the absence of alkaline solutions (aqueous NH3 or NaOH), formation of nanocrystalline SnO2, and subsequent hydrothermal treatments at temperatures between 100 and 200 degrees C. After annealing treatments of the hydrothermally treated SnO2 particles at 400 or 500 degrees C, their crystallite sizes remained smaller than 7.7 nm and their specific surface areas were still higher than 110 m2/g, indicative of the high thermal stability against particle growth and sintering. Furthermore, mesoporosity evolved with a relatively narrow pore size distribution typically in the range of 3.0-4.3 nm. The effects of the hydrothermal treatment were explained by uniformization of the particle size that was beneficial to the suppression of particle growth.     

Synthesis of mesoporous maghemite with high surface area and its adsorptive properties

Mesoporous maghemite (γ-Fe₂O₃) with high surface area was prepared by the thermal decomposition of Fe–urea complex ([Fe(CON₂H₄)₆](NO₃)₃) with the aid of cetyltrimethyl ammonium bromide (CTAB), and its adsorption ability for the removal of fluoride was investigated. X-ray diffraction (XRD), nitrogen adsorption–desorption measurements, transmission electron micrograph (TEM) observations, and magnetic measurements show that the γ-Fe₂O₃ has a mesoporous structure and its crystallite size, specific surface area, and magnetic properties can be controlled by varying the content of CTAB in [Fe(CON₂H₄)₆](NO₃)₃. The maximum adsorption capacity of the mesoporous γ-Fe₂O₃ for fluoride is estimated to be 7.9 mg/g, which suggests that the mesoporous γ-Fe₂O₃ is an excellent adsorbent for fluoride.     

功能化介孔硅材料的合成及其对富含裸露组氨酸蛋白质的选择性吸附

通过自由基聚合反应合成了具有高比表面积的介孔硅(PPOSS),并对其表面进行修饰和铜离子(Cu~(2+))的固定,最终得到功能化介孔硅材料(PPOSS-IDA-Cu~(2+)),然后利用PPOSS-IDA-Cu~(2+)中的Cu~(2+)与蛋白质裸露组氨酸的螯合作用,选择性吸附富含裸露组氨酸的蛋白质。对牛血红蛋白、牛血清白蛋白、肌红蛋白和溶菌酶的吸附结果表明,所合成的PPOSS-IDA-Cu~(2+)材料对富含组氨酸的牛血红蛋白有较好的吸附选择性和较大的吸附容量(3 150mg/g),并且有望与其他材料联合使用,以检测到更多相对丰度较低的蛋白质,丰富人类蛋白质组学信息,为疾病的临床诊断及病理研究提供帮助。     

Synthesis and Gas-sensing Performance of Nanosized SnO2

Nanosized tin dioxide particles were prepared by sol-gel dialytic processes with tin(Ⅳ) chloride and alcohol as start materials. The nanoparticles of tin dioxide were charactered by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and BET. The results show that the average diameter of tin dioxide particles dried at 353 K was about 2nm. Even if the tin dioxide particles were calcined at 873 K, the average diameter of particles was less than 10 nm. The removal of Cl^- was solved by using this kind of method. The mechanism of the formation of tin dioxide nanosized particles was proposed and analyzed in this paper. We also measured the sensitivity of the sensor based on the tin oxide powder calcined at 673K to NH3, alcohol, acetone, hexane and CO. The gas-sensing performance results indicate that this sensor has a higher sensitivity to alcohol and acetone, and selectivity for NH3, hexane and CO at an operating temperature of 343 K.     

Microstructural control and selective C2H5OH sensing properties of Zn2SnO4 nanofibers prepared by electrospinning

Microstructural evolution of spinel Zn(2)SnO(4) nanofibers was manipulated via an in situ phase separation process of inorganic precursors and a matrix polymer during electrospinning and calcination. Chemiresistive gas sensors using porous Zn(2)SnO(4) fibers exhibited superior C(2)H(5)OH sensing response.