High-performance liquid-phase catalytic purification of phosphine in tail gas using Pd(Ⅱ)/Cu(Ⅱ)composite

Pd/Cu liquid-phase composite was utilized as the catalyst in this study to remove PH_(3) at low temperatures.The anti-heterotoxicity of catalysts in the PH_(3) catalytic oxidation purification process was carefully explored and pioneered.The catalytic performance,thermodynamics,kinetics,and catalytic oxidation mechanism of Pd/Cu liquid-phase catalyst catalytic oxidation of PH_(3) were thoroughly investigated.The results showed that Pd/Cu has a superior catalytic effect on the removal of PH_(3) in the gas mixture under low temperature.With CO as the carrier gas,the removal efficiency of PH_(3) could be maintained at 100%for nearly 450 min,indicating that the Pd/Cu liquid phase catalyst has good resistance to heterotoxicity.According to the thermodynamic,kinetic,and related characterization results of the PH_(3) purification process,the kinetic region of the gas–liquid reaction of PH_(3) absorption by Pd/Cu solution was an interfacial reaction.Pd was the primary catalyst and Cu was the secondary catalyst,and the adsorption of PH_(3)was a primary reaction.PH_(3) was spontaneously oxidized to H_(3)PO_(4) in the Pd/Cu catalytic system during the removal process.Pd was regenerated by O_(2) and Cu,increasing the activity and stability of the Pd/Cu catalyst in the sustain and efficient purification of PH_(3) in tail gas.

Kinetics of Liquid-Phase Hydrogenation of Toluene Catalyzed by Hydrogen Storage Alloy MlNi_5

The kinetics of liquid-phase hydrogenation of toluene catalyzed by MlNi_5 was studied by investigating the influences of the reaction temperature and pressure on the mass transfer-reaction processes inside the slurry. The results show that the reaction rate accelerates when the reaction temperature increases, and reaches its maximum at about 490 K, but if temperature is higher than 510 K, the reaction rate decreases rapidly. The whole reaction process is controlled by the reaction at the surface of the catalyst particles. The mass transfer resistance at gas-liquid interface and that from the bulk liquid phase to the surface of the catalyst particle can be neglected. The apparent reaction rate is zero order for toluene concentration and first order for hydrogen concentration in the liquid phase. The kinetic model is obtained. The kinetic model fits the experimental data very well. The apparent activation energy of the hydrogen absorption reaction of MlNi_5-toluene slurry system is 41.01 kJ·mol^(-1).

Studies on the structure and catalytic performance of Cu-Zn-Al catalyst prepared by liquid-phase preparation technology under different heat treatment atmosphere

Cu-Zn-Al slurry catalysts were prepared using a complete liquid-phase preparation technology under different heat treatment atmospheres.The catalysts were characterized using X-ray diffraction,X-ray photoelectron spectroscope,and N2 adsorption-desorption.Their application in the single-step synthesis of dimethyl ether from syngas was also investigated.The results indicate that the type of heat treatment atmosphere has an influence on the Cu species and the Cu0/Cu＋ ratio on the catalyst surface.Moreover,the final Cu/Zn ratio on the catalyst surface is mainly dependent on the composition and reaction environment of the catalyst and less on the type of heat treatment atmosphere.The prepared catalysts can suppress sintering of active sites at high temperatures,and the type of heat treatment atmosphere mainly affects the capability of the catalyst for methanol synthesis.The catalysts perform best using N2 as the heat treatment atmosphere.

On the liquid-phase technology of carbon fiber/aluminum matrix composites

The main problems with the liquid-phase technology of carbon fiber/aluminum matrix composites include poor wetting of the fiber with liquid aluminum and formation of aluminum carbide on the fibers’surface.This paper aims to solve these problems.The theoretical and experimental dependence of porosity on the applied pressure were determined.The possibility of obtaining a carbon fiber/aluminum matrix composite wire with a strength value of about 1500 MPa was shown.The correlation among the strength of the carbon fiber reinforced aluminum matrix composite,the fracture surface,and the degradation of the carbon fiber surface was discussed.

Interfacial reactions and diffusion path in partial transient liquid-phase bonding of Si_3N_4/Ti/Ni/Ti/Si_3N_4

The interfacial reactions in partial transient liquid-phase bonding of Si3N4 ceramics with Ti/Ni/Ti interlayers were studied by means of scanning electron microscopy （SEM）, energy dispersive spectrometry （EDS） and X-ray diffractometry （XRD）. It was shown that the interfacial structure of Si3N4/TiN/Ti5Si3+Ti5Si4 + Ni3Si/ （NiTi ） /Ni3Ti/ Ni was formed after bonding. The activation energies for TiN layer and the mixed reaction layer of Ti5Si3 + Ti5Si4 + Ni3Si are 546. 8 kJ/mol and 543. 9 kJ/mol, respectively. The formation and transition processes of interface layer sequence in the joint were clarified by diffusion path. An important characteristic, which is different from the conventional brazing and soid-state diffusion bonding, has been found, i. e., during the partial transient liquid-phase bonding, not only the reaction layers which have formed grow, but also the diffusion path in the subsequent reaction changes because of the remarkable variation of the concentration on the metal side.

Poly(ethylene glycol)-supported Liquid-phase Parallel Synthesis of Di(aryloxyacetyl)thiosemicarbazides

An efficient poly(ethylene glycol) (PEG)-supported liquid-phase parallel approach to di(aryloxyacetyl)thiosemicarbazides is described. PEG-bound phenol reacted with chloroacetic acid to afford PEG-bound phenyloxyacetic acid, which was readily converted into corresponding phenyloxyacetyl chloride. Subsequent nucleophilic substitution with ammonium thiocyanate followed by addition of aryloxyacetic acid hydrazides gave PEG-bound di(aryloxyacetyl)thiosemi-carbazides, which were easily cleaved to give the resulting library of 1-aryloxyacetyl-4-(4'-methoxylcarbonylphenyloxyacetyl)thiosemicarbazides in good to high yield and high purity.

Liquid-phase and solid-phase microwave irradiations for reduction of graphite oxide

In this paper, two microwave irradiation methods：（i） liquid-phase microwave irradiation（MWI） reduction of graphite oxide suspension dissolved in de-ionized water and N, N-dimethylformamide, respectively, and（ii） solid-phase MWI reduction of graphite oxide powder have been successfully carried out to reduce graphite oxide. The reduced graphene oxide products are thoroughly characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectral analysis, Raman spectroscopy, UV-Vis absorption spectral analysis,and four-point probe conductivity measurements. The results show that both methods can efficiently remove the oxygencontaining functional groups attached to the graphite layers, though the solid-phase MWI reduction method can obtain far more efficiently a higher quality-reduced graphene oxide with fewer defects. The I（D）/I（G） ratio of the solid-phase MWI sample is as low as 0.46, which is only half of that of the liquid-phase MWI samples. The electrical conductivity of the reduced graphene oxide by the solid method reaches 747.9 S/m, which is about 25 times higher than that made by the liquid-phase method.

Mineral-phase evolution and sintering behavior of MO–SiO_2–Al_2O_3–B_2O_3 (M = Ca,Ba) glass-ceramics by low-temperature liquid-phase sintering

In this work, network former SiO_2 and network intermediate Al_2O_3 were introduced into typical low-melting binary compositions CaO·B_2O_3, CaO·2B_2O_3, and BaO·B_2O_3 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°C. On the basis of liquid-phase sintering theory, mineral-phase evolutions and glass-phase formations were systematically investigated in a wide MO–SiO_2–Al_2O_3–B_2O_3(M = Ca, Ba) composition range. The results indicate that major mineral phases of the aluminosilicate glass-ceramics are Al_(20)B_4O_(36), CaAl_2Si_2O_8, and BaAl_2Si_2O_8 and that the glass-ceramic materials are characterized by dense microstructures and excellent dielectric properties.

Two-dimensional polyaniline nanosheets via liquid-phase exfoliation

Two-dimensional（2D） organic nanomaterials are fascinating because of their unique properties and pentential applications in future optoelectronic devices.Polyaniline（PANI） has attracted much attention for its high conductivity,good environmental stability and unusual doping chemistry.We report on liquid-phase exfoliation of layered PANI films grown by electrochemical polymerization.Atomic force microscopy images demonstrate that few-or even mono-layer PANI nanosheets can be fabricated.The PANI nanosheets can be transferred onto a variety of surfaces,providing a promising route to their incorporation into a variety of devices for further studies and various applications.

Nanobubble Dynamics in Aqueous Surfactant Solutions Studied by Liquid-Phase Transmission Electron Microscopy

Nanobubbles have attracted considerable attention in various industrial applications due to their exceptionally long lifetime and their potential as carriers at the nanoscale.The stability and physiochemical properties of nanobubbles are highly sensitive to the presence of surfactants that can lower their surface tension or improve their electrostatic stabilization.Herein,we report real-time observations of the dynamic behaviors of nanobubbles in the presence of soluble surfactants.Using liquid-phase transmission electron microscopy(TEM)with multi-chamber graphene liquid cells,bulk nanobubbles and surface nanobubbles were observed in the same imaging condition.Our direct observations of nanobubbles indicate that stable gas transport frequently occurs without interfaces merging,while a narrow distance is maintained between the interfaces of interacting surfactant-laden nanobubbles.Our results also elucidate that the interface curvature of nanobubbles is an important factor that determines their interfacial stability.

Combination of hollow fiber-based liquid-phase microextraction with sweeping techniques in micellar electrokinetic chromatography for the determination of Strychnos alkaloids in human urine

A new method for the enrichment of Strychnos alkaloids in biological samples via liquid-phase microextxaodon （LPME） based on porous polypropylene hollow fibers in combination with on-line sweeping in micellar electrokinodc chromatography was developed. The calibration curve was linear over the range of 20-200 ng mL^-1 for both strychnine and brucine in human urine sample. The detection limits （S/N = 3：1） for strychnine and brucine were 1 ng mL^-1 and 2 ng mL^-1, respectively. The LPME-sweeping method has been successfully applied to the analysis of strychnine and brucine in real urine samples.

Direct MALDI-MS Analysis of Proteins Isolated by Liquid-phase Isoelectric Focusing Electrophoresis

A liquid-phase isoelectric focusing electrophoresis system(Rotofor) was used as the prefractionation tool for the sample preparation in the MALDI-MS analysis of a protein mixture. Each fraction collected was then directly subjected to MALDI-TOF-MS analysis. By this approach, we are able to resolve two types of hemoglobins, A and C, which cannot be successfully separated by means of the traditional SDS-PAGE method.

Trace Determination of Tamoxifen in Biological Fluids Using Hollow Fiber Liquid-Phase Microextraction Followed by High-Performance Liquid Chromatography-Ultraviolet Detection

The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase;SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase;MP) followed by the back-extraction into a second aqueous solution (receiving phase;RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 - 500 ng?mL–1 and the limit of detection was found to be 0.5 ng?mL–1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% - 4.2%, n = 3) and inter-assay (7.5% - 7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.

Ultraviolet Photodetector based on Sr_(2)Nb_(3)O_(10) Perovskite Nanosheets

Liquid-phase exfoliation was employed to synthesize Sr_(2)Nb_(3)O_(10) perovskite nanosheets with thicknesses down to 1.76 nm.Transmission electron microscopy(TEM),atomic force microscope(AFM),X-ray photoelectron spectrometer(XPS),and other characterization techniques were used to evaluate the atomic structure and chemical composition of the exfoliated nanosheets.A UV photodetector based on individual Sr_(2)Nb_(3)O_(10) nanosheets was prepared to demonstrate the application of an ultraviolet(UV) photodetector.The UV photodetector exhibited outstanding photocurrent and responsivity with a responsivity of 3×10^(5) A·W^(-1) at 5 V bias under 280 nm illumination,a photocurrent of 60 nA,and an on/off ratio of 3×10^(2).

Properties and microstructure of oxide dispersion strengthened tungsten alloy prepared by liquid-phase method:a review

The addition of the second phase into tungsten can significantly refine the grain size of tungsten alloys,and also play a role in dispersion strengthening,thus improving the properties of tungsten alloy.As a preparation method of tungsten alloy powder,liquid-phase method avoids the disadvantage of mechanical alloying,and the obtained powder composition is accurate and controllable,with high purity and excellent uniformity.At present,the second phase particles used for dispersion strengthening tungsten alloys are mainly composed of oxides.Oxide particles can be synthesized and precipitated in nitrate solution through in situ chemical reaction,and are uniformly distributed in composite powder by mixing and stirring.Finally,the oxide dispersion strengthened tungsten alloy(ODS-W)was obtained by reduction and sintering.Liquid-phase methods for preparing ODS-W alloys include azeotropic distillation,sol-gel methods,freeze-drying,hydrothermal synthesis,spray-drying,etc.In this paper,several liquid-phase methods for preparing tungsten alloy composite powder precursors are reviewed,and their latest research progresses are discussed.In addition,the morphologies and properties of tungsten alloys prepared by different methods are compared,which provides guidance for preparing high-performance tungsten alloys.

Activation of 2D MoS_(2) electrodes induced by high-rate lithiation processes

MoS_(2) is a highly promising material for application in lithium-ion battery anodes due to its high theoretical capacity and low cost.However,problems with a fast capacity decay over cycling,especially at the first cycles,and poor rate performance have deterred its practical implementation.Herein,electrodes comprised solely of few-layers 2D MoS_(2) nanosheets have been manufactured by scalable liquid-phase exfoliation and spray deposition methods.The long-standing controversy questioning the reversibility of conversion processes of MoS_(2)-based electrodes was addressed.Raman studies revealed that,in 2D MoS_(2) electrodes,conversion processes are indeed reversible,where nanostructure played a key role.Cycling of the electrodes at high current rates revealed an intriguing phenomenon consisting of a continuously increasing capacity after ca.100-200 cycles.This phenomenon was comprehensively addressed by a variety of electrochemical and microscopy methods that revealed underlying physical activation mechanisms that involved a range of profound electrode structural changes.Activation mechanisms delivered a capacitive electrode of a superior rate performance and cycling stability,as compared to the corresponding pristine electrodes,and to MoS_(2) electrodes previously reported.Herein,we have devised a methodology to overcome the problem of cycling stability of 2D MoS_(2) electrodes.Moreover,activation of electrodes constitutes a methodology that could be applied to enhance the energy storage performance of electrodes based on other 2D nanomaterials,or combinations thereof,strategically combining chemistries to engineer electrodes of superior energy storage properties.

Intercalation assisted liquid phase production of disulfide zirconium nanosheets for efficient electrocatalytic dinitrogen reduction to ammonia

Disulfide zirconium(ZrS_(2)) is a two-dimensional(2D) transition metal disulfide and has given rise to extensive attention because of its distinctive electronic structure and properties.However,mass production of high quality of ZrS_(2)nanosheets to realize their practical application remains a challenge.Here,we have successfully exfoliated the bulk ZrS_(2)powder with the thickness of micron into single and few-layer nanosheets through liquid-phase exfoliation in N-methylpyrrolidone(NMP) assisted via aliphatic amines as intercalators.It is found that the exfoliation yield is as high as 27.3%,which is the record value for the exfoliation of ZrS_(2)nanosheets from bulk ZrS_(2)powder,and 77.1% of ZrS_(2)nanosheets are 2-3 layers.The molecular geometric size and aliphatic amine basicity have important impact on the exfoliation.Furthermore,the ZrS_(2)nanosheets have been used as catalyst in the electrocatalytic dinitrogen reduction with the NH3yield of 57.75 μg h^(-1)mg_(cat.)^(-1),which is twice that by ZrS_(2)nanofibers reported in literature and three times that by the bulk ZrS_(2)powder.Therefore,the liquid phase exfoliation strategy reported here has great potential in mass production of ZrS_(2)nanosheets for high activity electrocatalysis.

Real-Time and Spatial Electroanalysis of Biomolecules in One Living Cell Using Liquid-Phase Modified Nanopipette

The well-developed solid-phase modified strategy at the electrode has enabled the preparation of biosensors for the detection of multiple analytes,even in single living cells.However,limited assay elements can be modified at the solid surface,restricting the types of molecules that can be analyzed and the sensitivity of detection.Here,a novel liquid-phase modified strategy at the tip of a nanopipette is designed to realize real-time and local analysis of biomolecules inside the cell that are barely detectable using solid-phase modified nanoelectrodes.This design utilizes the nanotip structure at a platinized carbon open nanopipette to stably retain a nanodroplet that contains the required reagents with high reactivity for the assay of the target analyte.The generated hydrogen peroxide is electrochemically quantified at the Pt layer to carry out the real-time measurement in a living cell with a spatial resolution of 70 nm.Taking advantage of highly spatial and real-time detection,uneven distribution of sphingomyelinase(SMase)in the living CT26 cell is unprecedentedly shown to exhibit the significance in the establishment of liquid-phase modified nanopipette.This new modification strategy opens up a new direction for sensor design and consequently advances the development of biosensors in the chemical and biological research.

MoS_(2)core-shell nanoparticles prepared through liquid-phase ablation and light exfoliation of femtosecond laser for chemical sensing

Molybdenum disulfide(MoS_(2))-based nanostructures are highly desirable for applications such as chemical and biological sensing,photo/electrochemical catalysis,and energy storage due to their unique physical and chemical properties.In this work,MoS_(2)core-shell nanoparticles were first prepared through the liquid-phase processing of bulk MoS2by a femtosecond laser.The core of prepared nanoparticles was incompletely and weakly crystalline MoS_(2);the shell of prepared nanoparticles was highly crystalline MoS_(2),which wrapped around the core layer by layer.The femtosecond laser simultaneously achieved liquid-phase ablation and light exfoliation.The formation mechanism of the core-shell nanoparticles is to prepare the nanonuclei first by laser liquid-phase ablation and then the nanosheets by light exfoliation;the nanosheets will wrap the nanonuclei layer by layer through van der Waals forces to form core-shell nanoparticles.The MoS_(2)core-shell nanoparticles,because of Mo-S bond breakage and recombination,have high chemical activity for chemical catalysis.Afterward,the nanoparticles were used as a reducing agent to directly prepare three-dimensional(3D)Au-MoS_(2)micro/nanostructures,which were applied as surface-enhanced Raman spectroscopy(SERS)substrates to explore chemical sensing activity.The ultrahigh enhancement factor(1.06×10^(11)),ultralow detection limit(10-13M),and good SERS adaptability demonstrate highly sensitive SERS activity,great ability of ultralow concentration detection,and ability to detect diverse analytes,respectively.This work reveals the tremendous potential of 3D Au-MoS_(2)composite structures as excellent SERS substrates for chemical and biological sensing.