Through-the-thickness residual stress analysis by neutron diffraction in inoxidizable martensitic steel samples with and without tungsten carbide coating

The residual stress (RS) induced in the substrate by thermal spray-coating plays a significant role in the behaviour of coated materials. The characterisation of High-Velocity Oxy-Fuel (HVOF) coatings through RS determination justifies various cases of failure or bad performance due to the delamination of coating which is not easily interpretable through more traditional microstructural analyses and mechanical tests.Two 13Cr4Ni inoxidizable martensitic steel samples, one having a thermal spray (WC–12% Co) HVOF coated surface, the other a shoot peened surface, were analyzed by neutron diffraction (ND) in order to determine the real RS depth-profile and investigate the effects of the thermal process on the considered materials.The stresses resulted in the range from − 80 to 50 MPa for the uncoated sample, while for the coated sample they increased gradually from a slight compressive status in correspondence of the uncoated surface, to greatest values of ~ 250 MPa in correspondence of the coating. A traditional X-ray investigation on the coated surface measured compressive RS values σ = − 550 ± 40 MPa, showing that ND investigation is very suitable for critical applications, where a much greater stress situation could be present at a diverse depth.The results achieved yielded trends that can be used in monitoring of the coating characteristics, in particular adhesion, thereby confirming the relevance of thermal stresses induced by HVOF coating processes.     

Microstructure and tribological characteristics of nitrided layer on 2Cr13 steel in air and vacuum

A 2Cr13 steel was gas nitrided in pure NH₃ gas atmosphere at 793 K for 20 h. The microstructure, composition and microhardness of the nitrided samples were examined. The tribological behaviour of the nitrided 2Cr13 steel in air and vacuum was investigated in order to analyse effects of the nitriding on wear resistance of the 2Cr13 steel. The results show that the nitrided layer consists of a compound layer and diffusion zone. The nitriding increases both the surface hardness and wear resistance of 2Cr13 steel in air and vacuum, and the anti-wear characteristic of the nitrided 2Cr13 steel in vacuum is much higher than that in air. The nitrided layer exhibits a mild wear in air, and avoids the severe wear that happens on the unnitrided steel. While the adhesion dominates the wear process in vacuum. The material transfer between the wear couples helps to improve the tribological characteristics of the nitrided layer in vacuum.     

Characterization and tribological properties of composite 3Cr13/FeS layer

The 3Cr13 coating was prepared on the surface of 1045 steel by high velocity arc spraying method, and then treated by low temperature ion sulfuration to obtain the solid lubrication composite 3Cr13/FeS layer. SEM was used to observe the surface, cross-section and worn scar morphologies. XRD was utilized to analyze the phase structure. X-ray stress determinator was utilized to measure its residual stress. The nano-hardness and elastic modulus of composite 3Cr13/FeS layer were surveyed by the nano-indentation tester. The tribological properties were investigated on a ball-on-disk wear tester under dry and oil lubrication conditions. The results showed that the friction coefficient and wear scar depth of the composite 3Cr13/FeS layer were always lower than those of FeS film and 1045 steel under dry and oil lubrication conditions. Therefore the composite 3Cr13/FeS layer had excellent Friction-reduction and anti-wear properties.     

Excimer laser surface treatment of plasma sprayed alumina-13% titania coatings

Surface modification of engineering materials allows the production of far superior products in terms of reduced wear, increased corrosion resistance, better biocompatibility, and improved optical and altered electrical/electronic properties. Excimer laser annealing provides a rapid and efficient means for surface alloying and modification of ceramic materials. In this study, alumina-13% titania (AT-13) coatings were sprayed with a water-stabilized plasma spray gun. The coated surface was treated by excimer laser having a wavelength of 248 nm and pulse duration of 24 ns. The surface structure of the treated coating was examined by field emission scanning electron microscope and X-ray diffraction (XRD). A detailed parametric study was performed to investigate the effects of different parameters such as laser energy density (fluence), pulse repetition rate (PRR), and number of pulses on the mechanical properties, surface morphology, and microstructure of the coatings. The study reveals that the laser fluence plays a major role in modifying the surface morphology of the coating, followed by the pulse repetition rate.     

橙汁中总糖和果肉的δ13C测定及应用

稳定碳同位素分析是食品质量鉴别和产地溯源的有效手段。本工作结合分离技术,建立了元素分析-稳定同位素比值质谱（EA-IRMS）测定橙汁中总糖和果肉δ¹³C的方法,并研究了天然橙汁与模拟造假橙汁中总糖和果肉的碳同位素特征差异。实验结果表明,本方法不会导致同位素分馏,且标准偏差仅为0.1‰;初步研究证明,橙汁总糖与果肉的δ¹³C相近,而与甘蔗糖的δ¹³C差异明显,因此,以橙汁果肉作为内标物质鉴别橙汁中的C4植物糖是可行的。     

饲料对牛乳的碳稳定同位素比值的影响

通过等电点沉淀与离心分离牛乳中的酪蛋白和脂肪,采用元素分析 串联稳定同位素比值质谱法（EA-IRMS）测定牛乳组分的δ¹³C值。经验证,该方法具有良好的准确性和重复性,牛乳及其各组分δ¹³C值测定精度标准偏差（SD）均小于0.1‰（n=5）。对不同牛乳中δ¹³C值进行比较表明,饲料组成直接影响牛乳中的碳稳定同位素组成。以玉米为主要饲料的奶源地牛乳中δ¹³C值均高于-17.6‰,若饲料中含有羊草和苜蓿会使牛乳的δ¹³C值相对偏负。购自不同地区的市售乳样品δ¹³C值具有不同特点,中国市售乳样品的δ¹³C值与一些发达国家样品的δ¹³C值具有显著差异。研究结论验证了牛乳δ¹³C值在牛乳溯源中的作用,为稳定同位素分析技术在牛乳真实性溯源的应用积累了数据与理论基础。     

Conformation transition and molecular mobility of isolated poly(ethylene oxide) chains confined in urea nanochannels

Inclusion compounds formed from host small molecules and guest polymers have provided a novel platform to study the behavior of isolated polymer chains confined in nanochannels. In this article, the PEO chain conformation in the metastable poly(ethylene oxide) (PEO)-urea inclusion compound (IC) and its transition was characterized via a combination of different analytical methods. Based on the FTIR and Raman spectroscopy results, PEO chains in the metastable tetragonal IC are tentatively assigned to the tgg′ conformation. The structural changes of the metastable tetragonal IC to the stable trigonal form were observed via in situ FTIR and ex situ WAXD. The transformation is a kinetic solid-solid process and can even occur at room temperature. The activation energy of about 222 kJ/mol indicates that the transition occurred via cooperative disruption of several hydrogen bonds. Measurement of the laboratory frame spin-lattice relaxation time T₁ (¹³C) shows that molecular motions of the nanoconfined PEO chains are more intensive than the neat crystalline PEO but weaker than those of the neat amorphous PEO. Second harmonic generation microscopy demonstrates that the trigonal IC exhibits stronger nonlinear optical activity than the tetragonal IC. The intermolecular hydrogen bonding is attributed to the driving force for the transformation of the metastable tetragonal IC into the stable trigonal form.     

NMR study of temperature-induced phase separation and polymer-solvent interactions in poly(vinyl methyl ether)/D2O/ethanol solutions

The changes in the dynamic structure during temperature-induced phase transition in D₂O/ethanol solutions of poly(vinyl methyl ether) (PVME) were studied using NMR methods. The effect of polymer concentration and ethanol (EtOH) content in D₂O/EtOH mixtures on the appearance and extent of the phase separation was determined. Measurements of ¹H and ¹³C spin-spin and spin-lattice relaxations showed the presence of two kinds of EtOH molecules: besides the free EtOH expelled from the PVME mesoglobules there are also EtOH molecules bound in PVME mesoglobules. The existence of two different types of EtOH molecules at temperatures above the phase transition was in solutions with polymer concentration 20 wt% manifested by two well-resolved NMR signals (corresponding to free and bound EtOH) in ¹³C and ¹H NMR spectra. With time the originally bound EtOH is slowly released from globular-like structures. From the point of view of polymer-solvent interactions in the phase-separated PVME solutions both EtOH and water (HDO) molecules show a similar behaviour so indicating that the decisive factor in this behaviour is a polar character of these molecules and hydrogen bonding.     

Carbon‐13 NMR,GPC, and DSC study on a propylene‐1‐butene copolymer fractionated by temperature rising elution fractionation

A random copolymer of propylene with small amounts of 1‐butene comonomer, synthesized with a Ziegler–Natta catalyst, was fractionated by temperature rising elution fractionation (TREF) to systemically investigate the fraction samples' molecular microstructure, as well as their relationship to the melting and crystallization behavior. First, TREF was employed to fractionate the sample, and then crystallization analysis fractionation (Crystaf) was used to check the effect of the TREF experiment. In the characterization of the molecular microstructure, carbon‐13 NMR spectroscopy (¹³C NMR) and gel permeation chromatography (GPC) experiments gave the following results: the fraction samples have relatively uniform molecular microstructure; with an increase in elution temperature, the 1‐butene content in the fraction samples decreases, but the molecular weight (M_n) and number average sequence length of propylene (n?_P) increase. In the study on melting and crystallization behavior, differential scanning calorimetry (DSC) experimental results show that the melting temperature increasingly decreases with an increase in 1‐butene content; however, dependence of the melting temperature on molecular weight becomes weaker and weaker with an increase in the number average molecular weight in the range of number average molecular weight below 1.82 × 10⁵ g/mol. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 845–851, 2006     

Cellulose derivatives with adamantoyl groups

A new synthesis pattern of adamantoyl esters of cellulose (AdTMSC) is described. The process was approached by two steps. The first one consists in the obtaining of trimethylsilylcellulose (TMSC), by reacting cellulose in N,N‐dimethylacetamide/lithium chloride (DMA/LiCl) solution with chlorotrimethylsilane and hexamethyldisilazane. The AdTMSC was synthesized by reacting trimethylsilylcellulose with 1‐adamantanecarbonyl chloride, at 130°C. The obtained compounds were characterized by elemental analysis, ¹H and ¹³C NMR, FTIR spectroscopy, thermogravimetry method, and X‐ray diffraction. From ¹H NMR spectroscopy and elemental analyses, the degree of substitution (DS) of the cellulose derivatives was established. The AdTMSC is soluble in common organic solvent like chloroform, THF, and DMSO. As revealed by ¹³C NMR spectroscopy, a faster reaction takes place at the O (6)H group from AGU compared with O (2)H or O(3)H groups. Furthermore, other important properties were established by X‐ray diffraction and thermogravimetry method. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 105–112, 2006