Rapid synthesis of MoSi2-Si3N4 nanocomposite via reaction milling of Si and Mo powder mixture

The nanocomposite of MoSi2-SiaN4 （molybdenum disilicide-silicon nitride） was synthesized by reaction milling of the Mo and Si powder mixture. Changing the processing parameters led to the formation of different products such as a- and B-MoSi2, SiaN4, Mo2N, and M05Si3 at various milling times. A thermodynamic appraisal showed that the milling of Moa2Siss powder mixture was associated with highly exothermic mechanically induced self-sustaining reaction （MSR） between Mo and Si. The MSR took place around 5 h of milling led to the formation of a-MoSi2 and the reaction between Si and N2 to produce Si3N4 under a nitrogen pressure of 1 MPa. By increasing the nitrogen pressure to 5 MPa, more heat is released, resulting in the dissociation of Si3N4 and the transformation of a-MoSi2 to β-MoSi2. Heat treatment was also performed on the milled samples and led to the formation of Mo2N and the transformation of a-MoSi2 to β-MoSi2 at the milling times of 10 and 40 h, respectively.     

Fabrication of an r-Al2Ti intermetallic matrix composite reinforced with α-Al2O3 ceramic by discontinuous mechanical milling for thermite reaction

In this study, a powder mixture with an Al/TiO2 molar ratio of 10/3 was used to form an r-Al2Ti intermetallic matrix composite (IMC) reinforced withα-Al2O3 ceramic by a novel milling technique, called ...     

Structure evolution of Y2O3 nanoparticle/Fe composite during mechanical milling and annealing

Fe-25 wt% Y2O3composite powders have been fabricated by mechanical milling(MM) Fe powders of 100 μm in diameter and Y2O3nanoparticles in an argon atmosphere for the milling periods of4,8,12,24,36,and 48 h,respectively.The features of these powders were characterized by using X-ray diffraction(XRD),scanning electron microscopy(SEM),electron probe micro analyzer(EPMA) and transmission electron microscopy(TEM).The experimental results showed that the mean particle size and crystalline size of MM powders decreased with the milling time increasing.All the elements distributed homogenously inside the powders after 48 h of MM.The lattice constant of the matrix α-Fe kept constant with the milling time,and no solid solution took place during MM process.After 8 h of MM,the α-Fe in each powder became nanocrystalline.After 48 h of MM,Y2O3changes from nanostructure into amorphous structure,and the crystalline size of α-Fe further decreased to 10 nm.The Y2O3in the powders mechanically milled for 48 h kept the amorphous structure after being annealed at 400 1C,and starts to crystallize when the powders are annealed at 600 1C.The amorphous Y2O3contains a small amount of Fe,and crystalline FeYO3appears at 800 1C.     

Synthesis of Mg2B2O5 whiskers via coprecipitation and sintering process

Mg₂B₂O₅ whiskers with high aspect ratio were synthesized by coprecipitation and sintering process using MgCl₂·6H₂O, H₃BO₃, and NaOH as raw materials and KCl as a flux. Their formation process was investigated by thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), and scanning electron microcopy (SEM). It is found that the products synthesized at 832°C are monoclinic Mg₂B₂O₅ whiskers with a diameter of 200?C400 nm and a length of 50?C80 ??m. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) analyses show that the whiskers obtained at 832°C are single crystalline and grow along with the [010] direction. The growth mechanism of Mg₂B₂O₅ whiskers was also presented.     

Mineral-phase evolution and sintering behavior of MO-SiO2-Al2O3-B2O3 (M=Ca,Ba) glass-ceramics by low-temperature liquid-phase sintering

In this work, network former SiO₂ and network intermediate Al₂O₃ were introduced into typical low-melting binary compositions CaO·B₂O₃, CaO·2B₂O₃, and BaO·B₂O₃ via an aqueous solid-state suspension milling route. Accordingly, multiple-phase aluminosilicate glass-ceramics were directly obtained via liquid-phase sintering at temperatures below 950℃. On the basis of liquid-phase sintering theory, mineral-phase evolutions and glass-phase formations were systematically investigated in a wide MO-SiO₂-Al₂O₃-B₂O₃ (M=Ca, Ba) composition range. The results indicate that major mineral phases of the aluminosilicate glass-ceramics are Al₂₀B₄O₃₆, CaAl₂Si₂O₈, and BaAl₂Si₂O₈ and that the glass-ceramic materials are characterized by dense microstructures and excellent dielectric properties.     

Effect of B2O3 on the aqueous tape casting and microwave properties of Li2O–Nb2O5–TiO2 ceramics

The effect of B2O3 addition on the aqueous tape casting, sintering, microstructure and microwave dielectric properties of Li2O-Nb2O5-TiO2 ceramics has been investigated. The tape casting slurries exhibit a typical shear-thinning behavior without thixotropy, but the addition of B2O3 increases the viscosity of the slurries significantly. It was found that doping of B2O3 can decrease the tensile strength, strain to failure and density of the green tapes. The sintering temperature could be lowed down to 900℃ with the addition of 2 wt% B2O3 due to the liquid phase effect. No secondary phase is observed. The addition of B2O3 does not induce much degradation on the microwave dielectric properties. Optimum microwave dielectric properties of εr 67, Q×f 6560 GHz are obtained for Li2O-Nb2O5-TiO2 ceramics containing 2 wt% B2O3 sintered at 900 1C. It represents that the ceramics could be promising for multilayer low-temperature co-fired ceramics (LTCC) application.     

Preparation of NiO nanoparticles from Ni（OH）2-NiCO3-4H2O precursor by mechanical activation

A mechanical activation process was introduced as a facile method for producing nickel oxide nanopowders. The precursor compound Ni（OH）2-NiCO3-4H2O was synthesized by chemical precipitation. The precursor was milled with NaCl diluent. A high-energy ball milling process led to decomposition of the precursor and subsequent dispersal in NaCl media. Nickel oxide nanocrystalline powders were produced by subsequent heat treatment and water washing. Milling rotation speed, milling time, ball-to-powder ratio （BPR）, and nickel chlo-ride-to-precursor ratio were introduced as influential parameters on the wavelength of maximum absorption （λmax）. The effects of these pa-rameters were investigated by the Taguchi method. The optimum conditions for this study were a milling rotation speed of 150 r/min, a mill-ing time of 20 h, a BPR of 15/1, and a NaCl-to-powder weight ratio （NPR） of 6/1. In these conditions,λmax was predicted to be 292 nm. The structural properties of the samples were determined by field emission scanning electron microscopy, X-ray diffraction, and energy dispersive spectrometry.     

Effects of the hierarchical pyrolysis polyaniline on reversible hydrogen storage of LiBH4

In this work,LiBH_4–20 wt%PP composite was prepared by ball-milling with as-synthesized hierarchical pyrolysis polyaniline(PP)and LiBH_4,and the hydrogen sorption performance as well as catalytic mechanism of the composite was studied.It is found that the onset desorption temperature of the composite decreases to 75°C,almost 235°C lower than that of the milled LiBH_4.Moreover,the composite could release 4.1 wt%H_2and rehydrogenate a total of 4.4 wt%H_2when the temperature raiseds up to 400°C,showing an outstanding reversibility,which even 3.9 wt%H_2can be kept after five cycles.Through scanning electron microscopy(SEM)observation and X-ray diffraction(XRD)analysis,we found that the PP surface forms some nanoholes after hydrogenation-dehydrogenation cycles,which leads to the confinement of some LiBH_4in the PP nanoporous structure,therefore,the hydrogen sorption kinetics and reversibility are significantly enhanced.In addition,we also found the oxygenic groups of the PP can react with LiBH_4forming LiBO_2and Li_3BO_3,where the containing Li–B–O bonds loaded in the porous structure of the PP catalyze the hydrogenation reaction of LiBH_4.     

Preparation of narrow band gap V2O5/TiO2 composite films by micro-arc oxidation

V₂O₅/TiO₂ composite films were prepared on pure titanium substrates via micro-arc oxidation (MAO) in electrolytes consisting of NaVO₃. Their morphology and elements were characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) analysis. Phase composition and valence states of species in the films were characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Ultraviolet-visible diffuse reflectance spectra (UV-Vis DRS) were also employed to evaluate the photophysical property of the films. The V₂O₅/TiO₂ composite films show a sheet-like morphology. Not only V₂O₅ phase appears in the films when the NaVO₃ concentration of the electrolyte is higher than 6.10 g/L and is loaded at the surface of anatase, but also V⁴⁺ is incorporated into the crystal lattice of anatase. In comparison with pure TiO₂ films the V₂O₅/TiO₂ composite films exhibit significantly narrow band gap energy. The film prepared in an electrolyte consisting of NaVO₃ with a concentration of 8.54 g/L exhibits the narrowest band gap energy, which is approximately 1.89 eV. The V₂O₅/TiO₂ composite films also have the significantly enhanced visible light photocatalytic activity. The film prepared in an electrolyte consisting of NaVO₃ with a concentration of 8.54 g/L exhibits the best photocatalytic activity and about 93% of rhodamine is degraded after 14 h visible light radiation.     

Rational construction of NiCo_2O_4@Fe_2O_3 core-shell nanowire arrays for high-performance supercapacitors

Fe_2O_3 electrode materials exhibit excellent electrochemical performance in electrochemical energy storage system. However, its poor electrical conductivity limits its future practical application. The binder-free Ni Co_2O_4@Fe_2O_3 composites was reasonably designed and fabricated on carbon fiber paper with NiCo_2 O_4 nanowires as conductive scaffold in the present investigation. The three-dimensional nanostructure of the porous Fe_2O_3 nanorods coated the Ni Co2 O4 nanowire arrays showed the fascinating electrochemical performance, including high specific capacitance of 262 m F/cm2 at a current density of 1 m A/cm2, and remarkable cycle stability with～74.2% capacitance retention after 4000 cycles. The excellent pseudocapacitance performance of NiCo_2O_4@Fe_2O_3 composite materials is due to synergistic effect between NiCo_2O_4 and Fe_2O_3. The results of the present work show that NiCo_2O_4@Fe_2O_3 core-shell composite electrode is expected to exhibit excellent performance in the field of supercapacitors.     

Highly sensitive ZnO nanoparticles-loaded In2O3 hollow microsphere for detecting ppb-level NO2 at low working temperature

This paper presents a NO₂ sensor operating at low temperature, which was fabricated by ZnO nanoparticles-loaded In₂O₃ hollow microspheres composites. SEM, XRD, XPS and HRTEM were executed to determine the morphology and microstructure of ZnO–In₂O₃. The sensing performance of pure In₂O₃ and ZnO–In₂O₃ composite sensors was tested. The NO₂ sensing properties of the composite were greatly improved in contrast with the pure In₂O₃ sensor at the optimized operating temperature (75 °C). ZnO–In₂O₃ composite sensor exhibited an obviously higher response (805.2 for 100 ppb NO₂) than that of the pure In₂O₃ sensor (14 for 100 ppb NO₂). In particular, the response/recovery rate of ZnO–In₂O₃ composite sensor was greatly improved in contrast with the pure In₂O₃ sensor. The n-n heterojunctions created at ZnO–In₂O₃ interfaces improved the sensing performance.     

Improved dehydriding property of polyvinylpyrrolidone coated Mg-Ni hydrogen storage nano-composite prepared by hydriding combustion synthesis and wet mechanical milling

In this work, polyvinylpyrrolidone(PVP) coated Mg_(95)Ni_5 nano-composites were prepared by hydriding combustion synthesis(HCS) plus wet mechanical milling(WM) with tetrahydrofuran(THF) and donated as WM-x wt% PVP(x = 1, 3, 5 and 7) respectively. The phase compositions, microstructures and dehydriding property, as well as the co-effect of PVP and THF were investigated in detail. XRD results showed that the average crystal size of MgH_2 in the milled Mg_(95)Ni_5 decreased from 23 nm without PVP to 18 nm with 1 wt% PVP. The peak temperature of dehydrogenation of MgH_2 in the milled Mg_(95)Ni_5 decreased from 293.0 ℃ without THF to 250.4 ℃ with THF. The apparent activation energy for decomposition of MgH_2 in WM-7 wt% PVP was estimated to be 66.94 kJ/mol, which is 37.70 kJ/mol lower than that of milled Mg_(95)Ni_5 without THF and PVP. PVP and THF can facilitate the refinement of particle size during mechanical milling process. Attributed to small particle sizes and synergistic effect of PVP and THF, the composites exhibit markedly improved dehydriding properties.     

Integrated Bi2O3 nanostructure modified with Au nanoparticles for enhanced photocatalytic activity under visible light irradiation

An integrated Bi_2O_3(i-Bi_2O_3) nanostructure with a particle size 10 nm inducing agglomerated structure were synthesized by dissolving bismuth nitrate pentahydrate in diethylene glycol at 180 ℃ with post heat treatment.The prepared i-Bi_2O_3 nanostructures were employed for the construction of Au/i-Bi_2O_3 composite system and characterized by X-ray diffraction pattern,UV-visible diffuse reflectance spectroscopy(DRS),and transmission electron microscopy,X-ray photoemission spectroscopy(XPS) and Energy dispersive X-ray spectroscopy(EDS).The i-Bi_2O_3 nanostructure and Au/i-Bi_2O_3 composite system were found to exhibit high photocatalytic activity than commercial Bi_2O_3 in decomposing salicylic acid under visible light irradiation.The high catalytic activity of i-Bi_2O_3 nanostructure was deduced to be caused by charge separation facilitated by electron hopping between the particles within the integrated structure and space-charge separation between i-Bi_2O_3 and Au.The charge separation behavior in i-Bi_2O_3 nanostructure was further bolstered by comparing the measured.OH radical produced in the solution with i-Bi_2O_3 nanostructure,commercial Bi_2O_3 and Au/i-Bi_2O_3 composite which readily react with 1,4-terephthalic acid(TA) inducing 2-hydroxy terephthalic acid(TAOH) that shows unique fluorescence peak at 426 nm.The space-charge separation between i-Bi_2O_3 and An was confirmed by measuring the electron spin resonance(ESR) spectra.     

Structural characterization of AA 2024-MoSi2 nanocomposite powders produced by mechanical milling

Nano-sized MoSi₂ powder was produced successfully from commercially available MoSi₂ by a mechanical milling process carried out for 100 h, and mechanical alloying was employed to synthesize AA 2024-MoSi₂ nanocomposites. The effects of MoSi2 reinforcement and mechanical milling on the structure, morphology, and iron contamination of the produced materials were investigated using X-ray diffraction, scanning electron microscopy, and atomic absorption spectrometry. It is revealed that the morphology of the aluminum alloy changes continuously during milling from spherical to plate-like, irregular, and finally equiaxed. The presence of MoSi₂ reinforcement accelerates the milling process and results in a smaller average particle size. The Williamson-Hall method determined that the crystallite size of the aluminum alloy in the composite powder is smaller than that of the unreinforced alloy at the same milling time and this size reaches 45 nm after 16 h milling time. The Fe contamination content is higher for the nanocomposite in comparison with the unreinforced alloy because of the wearing role of MoSi₂ hard particles.     

Preparation and magnetic properties of CoFe2O4/TiO2 composite films

Using （Ti（OC4H9）4） and metal chlorates as starting materials, CoFe2O4/TiO2 composite films were prepared by sol-gel method. The effects of heat treatment temperature and pH of the precursor on microstructure and magnetic properties were studied. The phase structure of the samples was examined by X-ray diffraction. The microstructure was examined by scanning electron microscope, atomic force microscope and polarized microscope. The magnetic property was measured by vibrating sample magnetometer. The results show that the crystals of different phases grow up independently. CoFe2O4 is uniformly embedded into the TiO2 matrix in the prepared composite films, and the growth of composite films is dependent on the heat treatment temperatures and PH of the precursor. The average size of CoFe2O4 crystal is 19 nm in Nanocomposite film prepared when the heat treatment temperature is 800℃ and the pH of the precursor is between 2 and 3. The magnetism of the composite films is enhanced as the heat treatment temperature increases.     

Mn_2O_3/CRF复合材料的制备及其在超级电容器中的应用

通过采用沉淀法在碳气凝胶表面负载金属氧化物三氧化二锰,制备得到Mn_2O_3/CRF复合材料。采用X射线衍射及电镜扫描等技术对所制备的复合材料进行结构形貌表征。实验结果发现碳气凝胶具有多重片层结构且孔隙发达。通过调节锰盐的含量考察三氧化二锰负载量对复合材料电化学性能的影响作用。采用循环伏安法及充放电测试对材料的电化学性能进行测试,结果表明Mn_2O_3/CRF复合材料具有良好的电容性及较好的可逆性。当Mn_2O_3含量达15%时复合材料的比电容最大,可达118.5 F/g。通过充放电测试1000次后发现该电极的比电容依然能够保持在一稳定值上,具有较好的稳定性。     

高能球磨法制备铁与聚四氟乙烯纳米复合材料

该文介绍了用高能球磨法制备铁与聚四氟乙烯纳米复合材料,研究预磨聚四氟乙烯的时间对所制备纳米复合材料组分的影响。材料的组分采用穆斯堡尔谱学方法研究分析,穆斯堡尔谱结果表明有界面谱登加在原来的,Fe谱上,这说明a-Fe的颗粒已达到纳米级,除此之外还有Fe²⁺和Fe³⁺的子谱,分别对应于FeF₂和FeF₃,随着球磨时间的延长,界面谱消失,出现物相Fe₃C实验结果还表明预磨聚四氟乙烯有利于FeF₃的产生。     

THz spectra of five borates crystals

Terahertz spectral responses have been studied for five borate crystals Nas[B2P3O13] （NBP）, Zn3BPO （ZBP）, SrB407 （SBO）, Na3LagO3（BO 3）8 （NLBO） and PbB407 （PBO）. It is found that the samples had good transmission in 0.25--1.5 THz region. Both SBO and NLBO have an absorption coefficient less than 10 cm^-1. Among them, SBO has not only the smallest absorption coefficient but also a very flat dispersion in the frequency region under investigation. Distinct resonance absorption peaks are observed for ZBP at v1 = 1.4 THz, v2 = 2.0 THz and SBO at v = 2.4 THz. In the spectrum of PBO, two abnormal dispersions appear in the frequency regions 1.44--1.74 and 2.2--2.5 THz. The absorption coefficients and refraction indices of the five crystals are extracted from the THz time-domain （THz-TDS） spectra in 0.25--2.5 THz region. The properties and origins of the spectral responses are addressed.     

MnO_2@NiCo_2O_4核-壳异质结构的构筑及电化学性能和催化性能

采用2步水热法制备出1种以NiCo_2O_4纳米线为核,MnO_2纳米颗粒为壳的三维结构MnO_2@NiCo_2O_4@Ni-foam复合材料。通过X射线衍射(XRD),扫描电子显微镜(SEM)对复合催化剂的结构和形貌进行表征;通过循环伏安法(CV),恒流充放电性能(GCD)和电化学阻抗谱(EIS)来进行表征复合材料的电化学性能;通过O_3催化降解装置对复合材料的催化性能进行研究。结果表明:MnO_2@NiCo_2O_4@Ni-foam复合材料在频率范围为0.1～10 000 Hz时阻抗较低;通过降解实验发现,MnO_2@NiCo_2O_4@Ni-foam对O_3的降解率高于50%,表现出良好的催化效果。这表明MnO_2@NiCo_2O_4@Ni-foam复合材料在降解O_3,净化空气方面有广阔的应用前景。     

Nb_2O_5/CdS纳米粒子的制备及其光催化性能研究

通过简单的沉淀法合成了Nb2O5/Cd S纳米粒子,利用XRD、TEM、XPS对其进行了表征,采用制备的Nb2O5/Cd S纳米粒子在可见光照射下对罗丹明B进行了降解实验.结果表明:负载在Nb2O5表面上的Cd S粒径大小较均一,约为35 nm,在可见光照射下,Cd S质量比为20%的Nb2O5/Cd S纳米粒子光催化活性最佳,可见光照射下3 h对罗丹明B降解率为98%,经过3次循环利用,发现其具有良好的光催化稳定性.