In situ investigation of tensile behavior of Cf/SiC mini composites

This study presents an in depth analysis over the in situ tensile behavior of C_f/SiC mini composites. As part of the process, the matrix crack spacing at saturation was determined by the in situ x-ray microtomography tensile test and the test results were compared with others obtained by in situ optical microscope tensile test and scanning electron microscopy scan. Moreover, elastic modulus of fiber and matrix as well as interface shear stress were identified by the indirect method and in situ modulus of C fibers and SiC matrix were also measured by the nanoindentation test, showing outcomes much lower than those identified by indirect method. The in situ property parameters measured by in situ XCT tensile test and identified by the indirect method were substituted into the shear-lag model to predict the stress-strain responses of C_f/SiC mini composites and the predicted results agrees well with the experimental data, while there exists large deviation between the stress-strain response predicted by using the in situ modulus of C fibers tested by nanoindentation and the experimental data, which indicates that in situ modulus of C fibers tested by nanoindentation tests cannot be utilized to model the tensile stress-strain responses due to the possible asymmetry of tension and compression of C fibers.     

In vivo biocompatibility and bioactivity of in situ synthesized hydroxyapatite/polyetheretherketone composite materials

Hydroxyapatite/polyetheretherketone (HA/PEEK) composite materials were prepared via an in situ synthesis process in order to achieve strong bonding between PEEK matrix and hydroxyapatite fillers, and ultimately to improve the mechanical properties of the composites. In the study, the biocompatibility of the synthesized HA/PEEK materials was investigated by acute toxicity test, hemolytic test, sensitization test, pyrogen test, intradermal test, and toxicity assay test on animal tissue and cells for the purpose of examining the possible adverse effects of the residue organic chemicals from the in situ synthesis process. In vivo bioactivity of both lab‐synthesized PEEK and HA/PEEK composites with various HA content was also studied. It is found that the in situ synthesized composite materials possess good biocompability without toxicity. Although the bioactivity of the material increases with HA content, the composite material with 5.6 vol % HA exhibits satisfactory bioactivity without compromising its excellent mechanical performance, which hints to a potential use as load‐bearing orthopedic material. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Insights into arc-assisted self-propagating high temperature synthesis of TiB2-TiC ceramic coating via wire-arc deposition

TiB₂-TiC ceramic coating was fabricated by wire-arc deposition of Ti-B₄C cored wire in conjunction with self-propagating high temperature synthesis (SHS) technology, to enhance the hardness and wear resistance of Ti. Results showed that a periodic combustion reaction, triggered by the capillary infiltration of molten Ti sheath into the inside B₄C particles, occurred as the wire entered the arc zone. During combustion reaction, B₄C experienced the course of dissolution as well as the transformation of decarbonization expressed as B₄C→B₁₃C₂→B₁₃C_{x(1.27<x<2.00)}. In particular, the loss of C was more notable at combustion front region. The as-synthesized coating exhibited ultralow porosity thanks to the elevated adiabatic temperature, and possessed gradient microstructures formed due to the dissolution-precipitation mechanism. Mechanical and tribological tests showed that the coating had ultrahigh microhardness (2140 HV_0.5, close to theorical value) and low wear rate (5.5×10⁻³ mm⁻³ min^-1·N^-1). The superior performance was attributed to ultralow porosity and high-strength coherent TiB₂/TiC interface.     

高压氢环境奥氏体不锈钢焊件氢脆研究进展

奥氏体不锈钢焊件是高压氢系统中重要的承载结构,其长期服役在高压高纯氢气环境中会出现塑性损减、疲劳裂纹扩展速率加快等氢脆现象,导致高压氢系统存在安全隐患。因此,为保障高压氢系统的安全运行,研究高压氢环境奥氏体不锈钢焊件的氢脆具有重要意义。本文首先介绍奥氏体不锈钢焊件中氢的两种来源,随后讨论评价材料氢脆敏感性的静态实验方法和动态实验方法,其次概述当前主流的氢脆机理,然后着重分析内部因素及外部因素对奥氏体不锈钢焊件氢脆敏感性的影响,最后归纳并总结五种典型的奥氏体不锈钢焊接工艺对焊件微观组织的影响,并进一步探讨相应焊件的氢脆敏感性。基于上述分析,针对奥氏体不锈钢焊件氢脆性能研究现状及发展趋势提出了若干建议。     

In situ synthesis,structure, and properties of a dendritic branched nano-thickening agent for high temperature fracturing fluid

The aim of this work was to prepare a novel dendritic branched nano-thickening agent by free radical polymerization of acrylamide (AM), acrylic acid (AA), sodium p-styrene sulfonate, dimethyl diallyl ammonium chloride, and multiwalled carbon nanotubes. The as-synthesized nano-thickening agent was characterized by Fourier transform infrared, Raman spectra, transmission electron microscope, ¹H-NMR, and thermogravimetric analysis (TGA). Compared with the pristine polymer and partially hydrolyzed polyacrylamide (HPAM), thickening capacity, temperature resistance, and salt tolerance properties of the nano-thickening agent considerably improved, and the viscosity of 0.5% nano-polymer solution was 126.5 mPa·s. Additionally, the properties of the nano-gel prepared by nano-thickener, such as temperature and shear tolerance, viscoelasticity, sand carrying capacity, and gel breaking performance, were evaluated showing the satisfactory performance of the nano-gel under high temperature condition. The results indicated that the nano-thickener has potential applications in the field of oil and gas production. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48446.     

Synthesis by in situ chemical oxidative polymerization and characterization of polyaniline/iron oxide nanoparticle composite

Polyaniline (PANI) is a well‐studied material and is the pre‐eminent electrically conducting organic polymer with the potential for a variety of applications such as in batteries, microelectronics displays, antistatic coatings, electromagnetic shielding materials, sensors and actuators. Its good environmental as well as thermal stability and electrical conductivity tunable by appropriate doping make PANI an ideal active material for several applications. In this paper, we report the synthesis of water‐dispersible colloidal PANI/iron oxide composite nanoparticles using an in situ chemical oxidation polymerization method in a micellar medium of sodium dodecylsulfate, where the cores (iron oxide) are embedded in a PANI matrix layer. Transmission electron micrographs showed evidence of the formation of an iron oxide core/PANI shell composite with a thin layer of PANI over the iron oxide cores. The results of thermogravimetric, Fourier transform infrared and UV‐visible analysis indicated that the iron oxide nanoparticles could improve the composite thermal stability possibly due to the interaction between iron oxide particles and PANI backbone. We believe that the synthetic route described can also be adapted for the assembly of hierarchical structures of other metal oxides or hydroxides onto various cores. Copyright © 2010 Society of Chemical Industry     

In situ high temperature FTIR studies of NOx reduction with propylene over Cu/ZSM-5 catalysts

High temperature in situ FTIR has been used to investigate the surface species present on Cu/ZSM-5 during the reduction of NO_x with propylene in a lean environment. Parallels have been observed between adsorbed surface species and catalytic activity for this reaction. Species detected at low temperatures are not representative of those detected at high temperatures where the catalyst is active. An oxidized nitrogen-containing species has been observed at 2580 cm^–1 on Cu during reaction conditions (400°C). In contrast, at low temperatures, where the catalyst is less active, coke and Cu⁺-CO predominated. The effects of Cu weight loading, C/NO ratio, reaction temperature, and catalyst deactivation by steaming have been investigated with IR.     

In situ synthesis and thermal shock resistance of a cordierite-mullite composite for solar thermal storage

Cordierite-mullite composite ceramic was synthesized in situ by semidry pressing and pressureless sintering from andalusite, kaolin, γ-Al₂O₃, talc, potassium feldspar, and albite in air. The effects of composition and sintering temperature on the density, bending strength, thermal shock stability, crystal phases, and microstructure of the specimens were studied. The results show that specimen B2 (the theoretical content of cordierite was 20 wt%) has excellent performance, that is, a bending strength of 104.59 MPa, 30 cycles of thermal shock resistance without cracking, and a loss rate of 13.12%. X-ray diffractometer (XRD) analysis and scanning electron microscope (SEM) micrographs showed that spherical cordierite crystals were grown on the surface of the mullite, therefore, the specimen possessed a superior bending strength and thermal shock resistance, where a great number of granules combined to restrain crack initiation as well as propagation over time during the thermal shock test. The thermal conductivity of specimen B2 was determined to be 3.83 W/(m·K) (36°C), and the sensible heat storage density was 1136 kJ/kg, with the temperature difference (ΔT) ranging from 0 to 800°C. Consequently, the cordierite-mullite composite is a potentially applicable material for solar thermal storage.     

镁热剂/铝热剂体系SHS法固化处理无钙焙烧铬渣

采用Al-Fe₂O₃（铝热剂）和Mg-Fe₂O₃（镁热剂）2种自蔓延高温合成体系（SHS）对无钙焙烧铬渣（COPR）进行固化处理,并通过浸出毒性试验对自蔓延产物的无害化效果进行评估。研究结果表明：2种反应体系均可实现铬渣的高效无害化,其中铝热剂体系和镁热剂体系铬渣含量分别高达80%和85%,其自蔓延产物浸取浓度ρ（总铬）和ρ（六价铬）分别低于4.5、1.5 mg·L^-1,符合生活垃圾填埋场污染控制标准GB 16889-2008,可进行填埋处置。在SHS反应过程中,六价铬还原率均高于90%,还原后的六价铬主要以非晶形式弥散分布于自蔓延产物中,且部分铬离子参与MgAlCrO₄尖晶石等矿物的形成,铬元素同时以物理和化学固定化的形式存在于自蔓延产物中。     

In situ synthesis of Pt nanoparticles in hyperbranched thin film for electrocatalytic reduction of dioxygen

Hyperbranched thin film (HTF) with amino and imino groups, which can accommodate PtCl₆²⁻, was synthesized with small organic molecules on gold substrate based on SN₂ displacement reaction. Platinum nanoparticles (Pt_NPs) were in situ synthesized by electrochemically reduction of precursors, PtCl₆²⁻, within HTF. The prepared films were characterized by X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS) and atomic force microscopy (AFM). It was confirmed that densely packed Pt_NPs were prepared with a narrow size distribution. EIS indicated that HTF inhibits electron transfer slightly while Pt nanoparticles in the HTF enhanced the electron-transfer ability greatly. Cyclic voltammetry (CV) indicated that HTF containing Pt_NPs exhibited a remarkable electrocatalytic activity for the electrochemical reduction of dioxygen. The quantity of Pt_NPs could be expediently controlled by the thickness of HTF. So the catalytic ability can be tailored correspondingly.     

In situ electrochemical impedance and noise measurements of corroding stainless steel in high temperature water

An in situ corrosion study of austenitic stainless steel 08CH18N10T in high temperature water was performed. The material under study is used in the construction of steam generator of PWR (pressurized water reactor) nuclear power stations and is similar to AISI 321 stainless steel.In situ 300-h tests were performed under autoclave conditions at 280 °C and 8 MPa and consisted of impedance measurements, polarization measurements and electrochemical noise measurements. The experiments were performed in deionised water with the pH adjusted to 9.5, in the presence/absence of chlorides. An additional modification of corrosivity was achieved by changing oxygen concentration.A detailed analysis of the impedance data is presented identifying in the impedance spectra contributions of oxide, corrosion reaction, double layer and diffusion process. A good agreement was found between corrosion data from electrochemical impedance spectroscopy (EIS) and that from electrochemical noise (EN) measurements. It was confirmed that the oxide response cannot be attributed to the overall oxide layer but only to the part corresponding to the space charge layer, thus indicating the semi-conductive character of the oxide.     

Preparation of polyimide/siloxane‐functionalized graphene oxide composite films with high mechanical properties and thermal stability via in situ polymerization

An effective approach to prepare polyimide/siloxane‐functionalized graphene oxide composite films is reported. The siloxane‐functionalized graphene oxide was obtained by treating graphene oxide (GO) with 1,3‐bis(3‐aminopropyl)‐1,1,3,3‐tetra‐methyldisiloxane (DSX) to obtain DSX‐GO nanosheets, which provided a starting platform for in situ fabrication of the composites by grafting polyimide (PI) chains at the reactive sites of functional DSX‐GO nanosheets. DSX‐GO bonded with the PI matrix through amide linkage to form PI‐DSX‐GO films, in which DSX‐GO exhibited excellent dispersibility and compatibility. It is demonstrated that the obvious reinforcing effect of GO to PI in mechanical properties and thermal stability for PI‐DSX‐GO is obtained. The tensile strength of a composite film containing 1.0 wt% DSX‐GO was 2.8 times greater than that of neat PI films, and Young's modulus was 6.3 times than that of neat PI films. Furthermore, the decomposition temperature of the composite for 5% weight loss was approximately 30 °C higher than that of neat PI films. © 2015 Society of Chemical Industry     

In situ hybridization and characterization of fibrous hydroxyapatite/chitosan nanocomposite

Nano‐fibrous hydroxyapatite/chitosan (HA/CS) composites with HA contents of 0–70 wt % were prepared by in situ hybridization with a preprepared chitosan film as semipermeable membrane to slow down the hybridization process. The phase composition, microstructure, and morphology of the composites were characterized by means of Fourier transform infrared spectroscopy, X‐ray diffraction, and high‐resolution transmission electron microscopy. It was found that the in situ prepared inorganic phase was hydroxyapatite nano‐fibers that were uniformly dispersed in the chitosan matrix. The average diameter of the fibers were about 3 nm, while the length of the fibers increases from 20 to 60 nm when the hydroxyapatite content increased from 10 to 70 wt %. The compressive strength and Young's modulus of these nano‐fibrous HA/CS composites increased with the increasing HA content and reached the highest values of 170 and 1.7 GPa, respectively, at the HA content of 50–70 wt %, which were much higher than the values of samples prepared by coprecipitation. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Low‐temperature synthesis of uranium monocarbide by a Pechini‐type in situ polymerizable complex method

Uranium monocarbide (UC) was successfully synthesized by the Pechini‐type in situ polymerizable complex technique (IPC) with the organic matter as the only carbon source. In the aqueous process, a mixture of citric acid (CA) and mannitol with was polymerized to form a spongy‐like organic polymeric precursor without any precipitations. The structural evolution and formation mechanism of the precursor were investigated using XRD, DSC‐TG, SEM (EDX), TEM, and FT‐IR. XRD results demonstrated that UC was obtained with the /mannitol/CA molar ratios of 1.0/0.3/1.0 at a low temperature of 1400°C. SEM and TEM analyses revealed that the UO₂ nanoparticles were uniformly distributed in the carbon matrix to form UO₂/C nanocomposites, and submicrometer‐sized ellipsoidal UC particles cemented together. FT‐IR showed that a ‐CA chelated structure was firstly obtained, achieving the molecular scale mixing of uranium and C. Then the in situ charring guaranteed the intimate contact of UO₂ and C, leading to a low reaction temperature in carbothermal reduction owing to a short diffusion distance.     

In situ modulus and strength of carbon fibers in C/SiC composites

The in situ elastic modulus and strength distribution of carbon fibers in C/SiC composites were studied. To obtain the in situ property data, fibers were heat treated according to the fabrication process of C/SiC composites. Tensile tests were performed on the single fibers and fiber bundles. The equivalent in situ modulus and strength were proposed considering the loose and unparallel fibers in the composites. The experimental and numerical results showed that the equivalent elastic modulus and average strength of in situ fibers are much lower than that of the original fibers. In addition, the equivalent strength distribution of in situ fibers is more dispersive.     

In situ synthesis of polyamide 6/MWNTs nanocomposites by anionic ring opening polymerization

In situ anionic ring opening polymerization is used to prepare monomer casting polyamide 6 (MCPA6)/carbon nanotubes (CNTs) nanocomposites, whereby water is used as auxiliary dispersing agent of hydroxyl functionalized multiwalled carbon nanotubes (MWNTs‐OH) and ε‐caprolactam (CL) monomer. The MWNTs‐OH were dispersed homogenously in MCPA6 matrix when being observed through transmission electron microcopy. The well dispersed MWNTs‐OH existed at the center of many radial texture phases in MCPA6 matrix. Polarizing microscope analysis showed that these radial texture phases were MCPA6 spherulitic crystallities. Differential scanning calorimetry analysis revealed that the crystallization temperature of the MCPA6/MWNTs‐OH nanocomposites had been improved by adding only 0.2 wt % MWNTs‐OH when compared with pure MCPA6. The influence of MWNTs‐OH on the thermal stability of MCPA6 under nitrogen and air environments was also investigated by thermal gravimetric analysis (TGA). © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

微通道中原位分散技术可控制备氧化铜纳米流体及复合薄膜前体

疏水纳米颗粒分散于有机体系中形成的纳米分散体,具有独特的理化性质和重要的应用价值。其中,纳米颗粒的单分散性、均匀性和稳定性是决定纳米分散体性能的关键。以CuO纳米分散体作为纳米流体和复合薄膜前体这一典型体系为研究对象,通过设计平板型微通道实现了CuO纳米分散体制备过程中的液滴聚并和改性CuO纳米颗粒的原位分散。制备了颗粒体积分数达2%、平均粒径约30 nm的CuO-基础油纳米流体,该纳米流体具有良好的稳定性和达到0.184 W·m^-1·K^-1的较高热导率;制备的CuO-PDMS（聚二甲基硅氧烷）复合薄膜具有较强的抗菌性能和颗粒复合层稳定性。通过系统性实验研究,证明了原位分散方法在强化改性颗粒高效分散中的重要作用,确定了颗粒性能及分散行为对分散体性能的影响规律。     

In situ solvothermal synthesis and characterization of transparent epoxy/TiO2 nanocomposites

A solvothermal process was developed to in situ prepare epoxy (EP)/TiO₂ hybrid precursors. The chemical structure of samples was confirmed by X-ray and Fourier transformed infrared spectroscopy. Field emission scanning electron microscope micrographs of cured EP/TiO₂ hybrid composites showed that well-dispersed TiO₂ nanoparticles were successfully in situ formed in epoxy matrix through the solvothermal process. The thermogravimetic analysis, DSC, and gel content measurements showed that EP/TiO₂ hybrid precursors were fully cured with the glass transition temperature decreasing gradually. The effect of TiO₂ contents on optical and surface properties was investigated in detail. The results indicated that epoxy/TiO₂ nanocomposites exhibited excellent UV shielding effect and high visible light transparency. The contact angle of EP/TiO₂ nanocomposites, when the content of silane-coupling agent (KH560) was 5 g and the content of tetrabutyl titanate (TBT) was 3 g, can reach as high as 101°, which was 36° higher than that of pure EP, representing for the increase of hydrophobicity. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

In situ reactive synthesis and plasma-activated sintering of binderless WC ceramics

Binderless micrometre tungsten carbide ceramics (～1.1?μm) were in situ synthesised and densified by plasma-activated sintering (PAS) from mixed powders of tungsten trioxide and carbon black. The influence of sintering process and powders’ composition ratio on the phase composition, microstructure and mechanical properties of as-prepared samples was clarified in detail. The phase evolution was ascertained by X-ray diffraction to be WO₃→WO_2.72→WO₂→W₂C→WC, with the formation of CO and CO₂ gases. The sample with nearly single WC phase, dense structure and excellent mechanical properties was fabricated under the optimised process with the proper composition ratio. Owing to the micrograin size, the fracture toughness (8.88?MPa?m^1/2) was enhanced while high hardness (2159 HV10) was maintained, in the absence of any ceramic toughening phase.     

In situ synthesis of bone‐like hydroxyapatite/polyamide 6 nanocomposites

BACKGROUND: Polymer/hydroxyapatite (HA) nanocomposites have emerged in recent years as a new class of biomaterials that can be used as artificial bone. Compared to pure HA or HA‐based bioceramics, and metallic implants, they exhibit good plasticity, improved toughness and good mechanical compatibility with natural bone. Compared to their microcomposite counterparts and the pristine polymer matrix, they show increased tensile strength and modulus, and enhanced bioactivity. RESULTS: In this study, polyamide 6 (PA6)/nanoscale HA (n‐HA) nanocomposites were prepared via in situ hydrolytic ring‐opening polymerization of ε‐caprolactam in the presence of newly synthesized n‐HA aqueous slurry. The synthesized n‐HA, which is similar to bone apatite in chemical composition, microscopic morphology and phase composition, dispersed uniformly in the composites even if its loading was up to 60 wt%. The PA6/n‐HA composites show a similarity to natural bone in chemical composition to a certain extent. Mechanical tests show that the composites are reinforced considerably by the incorporation of needle‐like n‐HA, and the composites have mechanical properties near to those of natural bone. CONCLUSION: The PA6/n‐HA nanocomposite with high n‐HA content shows a similarity to natural bone in terms of chemistry and mechanical properties. This makes it a possible candidate for biomaterials suitable for bone repair or fixation. Copyright © 2008 Society of Chemical Industry