酸化缓蚀剂含羟基双季铵盐的合成及性能评价

根据季铵化反应原理,以喹啉和1,3-二氯-2-丙醇合成了一种含羟基双季铵盐酸化缓蚀剂(BQ-1)。用红外光谱对其结构进行了表征,采用静态失重法和电化学测试研究了该缓蚀剂在15%HCl溶液中对N80钢的缓蚀性能。结果表明,该缓蚀剂具有明显的腐蚀抑制能力,在15%HCl、90℃下,5mmol/L该缓蚀剂对N80钢片的缓蚀率达96%以上,缓蚀性能优良;此外,该缓蚀剂是一种混合型缓蚀剂,在N80钢片表面的吸附作用符合Langmuir等温吸附规律。表面分析试验(SEM和EDS)验证了缓蚀剂分子在N80钢片表面确实形成了一层保护膜。     

一种增强型曼尼希碱酸化缓蚀剂的合成及其性能

以乙二胺、多聚甲醛和苯乙酮为原料经曼尼希反应合成了乙二胺双曼尼希碱盐酸盐,并合成了2-苯甲酰基-3-羟基-1-丙烯(BAA)和3-羟基苯丙酮,使用核磁共振氢谱分别对其结构进行了表征。三者复配得到增强型酸化缓蚀剂,采用静态失重法,电化学方法和SEM观察等研究了复配缓蚀剂在15%HCl溶液中对N80钢的缓蚀性能。结果表明:在90℃、15%HCl溶液中加入0.1%复配缓蚀剂,N80钢片的腐蚀速率为2.316 2g·m~(-2)·h~(-1),即达到一级标准(SY/T 5405-1996)。此外,该缓蚀剂是一种混合型缓蚀剂,在N80钢片表面的吸附作用符合Langmuir等温吸附规律。表面分析试验(SEM和EDS)验证了缓蚀剂分子在N80钢片表面形成了一层保护膜。     

乌洛托品季铵盐缓蚀剂的合成与复配研究

以乌洛托品、溴己烷为主要原料,甲醇为溶剂,合成了一种乌洛托品季铵盐缓蚀剂,采用失重法研究了季铵盐缓蚀剂在15%(质量分数) HCl溶液中的缓蚀性能及复配性能,并采用量子化学计算对缓蚀剂机理进行分析,通过红外光谱、SEM对腐蚀后表面进行分析。结果表明,季铵盐缓蚀剂具有良好的缓蚀性能,在15%HCl、90℃下,加量0.5%(质量分数)时,缓蚀率达98.41%,并且与聚乙二醇、KI、丙炔醇复配后协同增效效果较好;量子化学计算表明该季铵盐缓蚀剂分子活性主要分布在分子环上,与乌洛托品相比具有更小的能隙,在Fe表面也具有更大吸附能,因此乌洛托品季铵盐活性更高。表面分析实验进一步验证了该缓蚀剂分子在QT-800钢片表面形成一层吸附膜。     

喹啉季铵盐中氯和溴对其缓蚀性能的影响

以喹啉为母体,以氯化苄、溴化苄为季铵化试剂,制得两种喹啉季铵盐缓蚀剂。采用失重法、电化学方法、扫描电镜(SEM)及能谱分析(EDS)法考察两种缓蚀剂单独使用以及不同复配条件下的缓蚀性能。结果表明:溴化苄基喹啉(BQB)与增效剂复配后,其缓蚀率可以达到98.73%;在相同条件下BQB的缓蚀性能优于氯化苄基喹啉(BQC)的;两种喹啉季铵盐在碳钢表面的吸附符合Langmuir吸附等温式,是一个自发、放热的混合吸附过程;BQC的吉布斯吸附自由能和活化能均大于BQB的。     

高温高压H2S/CO2环境缓蚀剂分子结构与缓蚀性能关系的研究

用静态和动态腐蚀失重法研究喹啉季铵盐、吡啶季铵盐、曼尼希碱和咪唑啉季铵盐四种不同主体类型缓蚀剂在高温高压H₂S/CO₂环境中N80钢的缓蚀性能,并结合扫描电子显微镜（SEM）和X射线光电子能谱（XPS）表面分析技术研究了不同缓蚀剂主体分子结构与缓蚀性能的关系。结果表明,四类缓蚀剂的缓蚀效率的大小顺序是：喹啉季铵盐>吡啶季铵盐>曼尼希碱>咪唑啉季铵盐。喹啉季铵盐与其他三种缓蚀剂主体分子结构相比具有更好的抗硫性能,其对N80钢具有良好的吸附性能,可形成抗腐蚀性介质渗透能力强的致密均匀和稳定不易分解的有机膜。其缓蚀剂用量为0.15%时,缓蚀率可达97%。     

一种新型高温酸化缓蚀剂的制备及性能评价

目的改善缓蚀剂在高温酸液中的缓蚀性能,满足油田高温井酸化施工的要求。方法在合成一种新型吡啶季铵盐的基础上,添加炔醇、碘化钾等助剂进行复配,得到一种新型高温酸化缓蚀剂HTCI-1。使用HK-1高温高压动态腐蚀仪对其缓蚀性能进行测试,通过电化学测试、SEM、EDS等实验对其缓蚀机理进行分析。结果该酸化缓蚀剂在160℃、16 MPa、20%HCl或者土酸(12%HCl+3%HF)、质量分数3.0%的条件下,使N80试片的腐蚀速率分别为24.53 g/(m~2·h)和23.72 g/(m~2·h),达到了SY/T 5405—1996中的一级指标。结论在高温酸液中,N80钢片腐蚀速率降低,主要是由于缓蚀剂分子吸附到碳钢表面形成了一层致密的疏水性吸附膜,从而降低了侵蚀性离子与钢铁表面接触的几率,腐蚀电极反应过程受到抑制,达到了高温条件下防护金属的目的。     

一种复合型咪唑啉缓蚀剂

以油酸和二乙烯三胺为原料合成咪唑啉季铵盐缓蚀剂后,在50℃、5%的盐酸溶液中用静态失重法对咪唑啉季铵盐与阴离子表面活性剂和无机阴离子进行研究,得到了一个与咪唑啉季铵盐有最佳复配效果的复配体,咪唑啉季铵盐与I-复配比为1∶1(质量比)时,缓蚀剂的缓蚀效果最佳。在不同时间和不同温度下对复合型缓蚀剂的缓蚀效率进行了测量。这种缓蚀剂对A3钢的缓蚀率达到99%以上,比单独用咪唑啉季铵盐缓蚀效率提高了0.7%。     

丙二胺型双曼尼希碱酸化缓蚀剂的缓蚀性能

将1,2-丙二胺和1,3-丙二胺分别与多聚甲醛和苯乙酮反应,制备出1,2-丙二胺型双曼尼希碱(BTM-2)和1,3-丙二胺型双曼尼希碱(BTM-3)两种缓蚀剂。采用常压静态挂片失重试验和电化学测试,分析了缓蚀剂添加量对15%HCl溶液中N80钢缓蚀效果的影响,并采用量子计算方法,进一步探讨了其缓蚀机理。结果表明：BTM-2和BTM-3均具有明显的缓蚀效果,BTM-2的缓蚀效果优于BTM-3的;BTM-2与BTM-3缓蚀剂分子均在N80钢表面产生了物理吸附和化学吸附的组合吸附作用,形成了一层吸附膜,其吸附作用符合Langmuir吸附等温模型,量子化学计算结果与试验结果一致。     

曼尼希碱缓蚀剂的合成及其缓蚀效果

以甲醛、苄叉丙酮、对甲基苯胺为原料,通过曼尼希反应,制备了一种新型的曼尼希碱缓蚀剂(MHX),并采用正交试验优化了制备条件。采用静态失重法、电化学测试及分子动力学模拟的方法,研究了MHX添加量对N80钢片在HCl溶液中缓蚀效果的影响。结果表明：在90℃、添加1%MHX的20%HCl溶液中,N80钢片的腐蚀速率为2.6 g·m^-2·h^-1,缓蚀率为99.63%;该缓蚀剂是一种以抑制阳极为主的混合型缓蚀剂,可以大幅降低腐蚀电流密度,提高电极阻抗;MHX能够在N80钢表面吸附成膜,降低钢表面Fe的损耗,使其表面粗糙度降至93.81 nm; MHX分子在N80钢表面的吸附能为-7.59 eV,能有效取代H₂O分子吸附在金属表面,从而起到缓蚀作用。     

两种曼尼希碱缓蚀剂的缓蚀性能

采用甲醛/苯甲醛、苯乙酮和水合肼为原料分别合成了AJ和BJ两种曼尼希碱缓蚀剂。通过静态挂片失重法、电化学测试法等方法研究了在15%HCl(质量分数)溶液中,这两种缓蚀剂对N80钢的缓蚀性能。结果表明:在15%的HCl溶液中,AJ和BJ缓蚀剂对N80钢具有良好的缓蚀作用,且BJ缓蚀剂的缓蚀效果要优于AJ缓蚀剂的;两种缓蚀剂均为阳极型缓蚀剂,都能自发吸附在N80钢表面,其行为均符合Langmuir吸附等温式。     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Thermodynamics Study on the Decomposition of Chromite with KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

Influence of Heat Treatment on Damping Behaviour of the Magnesium Wrought Alloy AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.     

Quantitative Analysis of the Crystallographic Orientation Relationship Between the Martensite and Austenite in Quenching–Partitioning–Tempering Steels

The orientation relationships(ORs)between the martensite and the retained austenite in low-and medium-carbon steels after quenching–partitioning–tempering process were studied in this work.The ORs in the studied steels are identified by selected-area electron diffraction(SAED)as either K–S or N–W ORs.Meanwhile,the ORs were also studied based on numerical fitting of electron backscatter diffraction data method suggested by Miyamoto.The simulated K–S and N–W ORs in the low-index directions generally do not well coincide with the experimental pole figure,which may be attributed to both the orientation spread from the ideal variant orientations and high symmetry of the low-index directions.However,the simulated results coincide well with experimental pole figures in the high-index directions{123}_(bcc).A modified method with simplicity based on Miyamoto’s work was proposed.The results indicate that the ORs determined by modified method are similar to those determined by Miyamoto’method,that is,the OR is near K–S OR for the low-carbon Q–P–T steel,and with the increase of carbon content,the OR is closer to N–W OR in medium-carbon Q–P–T steel.     

电化学噪声数据处理方法概述

综述了常见的电化学噪声数据处理方法,介绍了直流趋势剔除、统计分析、快速傅立叶变换(FFT)法计算功率谱密度(PSD)以及小波变换处理电化学噪声信号的基本过程,并阐释了各种数学处理及所得参数的物理意义。