Ti/Ir0.4Sn0.6O2电极材料的电容性能

为了得到高比电容的电极材料,采用热分解法制备了不同温度下Ti/Ir0.4Sn0.6O2电极材料。运用X射线衍射(XRD)、差热分析、扫描电镜(SEM)和循环伏安法(CV)分别测试了该材料的晶体结构、表面形貌和电化学特性。结果表明:涂层的晶化温度高于360℃。320℃退火的电极表面有很多白色小颗粒析出,其活性氧化物较多。比电容受热处理影响较大,在280℃时电容值很小,可逆性低,320℃退火的电极比电容为454 F/g。该电极随着充放电循环次数的增加,比电容增加,经过9000次循环后,比电容才开始下降,经历10000次循环充放电后的比电容为493 F/g,比未经循环时还大10%。     

退火温度对Ti/IrO_2-Ta_2O_5电极的结构和电容性能的影响

采用热分解法在Ti基体上制备了Ti/IrO_2-Ta_2O_5氧化物电极涂层。采用X射线衍射、循环伏安、恒流充放电、交流阻抗等方法对其组织结构和电化学性能之间的关系进行了详细研究。结果表明:温度低于350℃的电极以非晶态的形式存在,当温度为370℃时,金红石衍射峰出现,说明在350~370℃范围为电极的临界结晶温度区间。370℃下制备的电极具有最大的积分电量,电量损失率最小,比电容达到最大值,为239.2 F/g。随温度升高,电荷转移电阻R_(ct)总体呈下降趋势。     

电弧复合磁控溅射结合热退火制备Ti2AlC涂层

利用电弧复合磁控溅射技术制备不同Ti/Al比的Ti-Al-C涂层,结合后续的退火处理制备Ti_2AlC相涂层。利用SEM、EDS、XRD、Raman光谱仪和TEM等研究了Ti/Al比及退火温度对退火后Ti-Al-C涂层的相和微观结构的影响。结果表明,Ti-Al-C沉积态涂层为富Al层和TiCx层交替堆垛的多层结构,涂层表面大颗粒较少且结构致密。Ti/Al比对退火后涂层中的相结构有重要的影响:当Ti/Al比为2.04时,退火后涂层中Ti_2AlC的纯度和结晶度最高;Ti/Al比过高(3.06)时,退火后涂层中形成TiC和Ti_3AlC杂质相,而低Ti/Al比(0.54)则大幅度降低Ti_2AlC相的纯度和结晶度。同时,退火温度很大程度影响Ti_2AlC相的形成,当沉积态涂层中Ti/Al比为2.38时,Ti_2AlC相涂层形成的最佳退火温度为750℃,偏低的退火温度(600℃)下,原子不能充分扩散,难以形成211结构的Ti_2AlC相,而退火温度过高时(900℃)涂层中存在较多的TiC、TiAlx等杂质相。     

RuO2-SiO2二元氧化物被覆钛涂层的制备

采用Pechini法，通过涂覆、烧结和退火，制备成系列含硅的RuO2-SiO2／Ti样品。二元涂层的摩尔成分为X％RuO2-Y％SiO2（以下简写为RuxSiyO2）。采用SEM和XRD方法分析了该阳极涂层材料的组织结构特征。结果表明所制备的涂层的相结构主要由金红石相的RuO2所组成，高温处理出现金红石相TiO2，加入的硅以非晶态SiO2的形式存在。经450℃处理的含硅样品的平均晶粒尺寸均小于10nm，明显低于不含硅的样品。同时具有很强的尺寸稳定性，即使经800℃退火处理后，涂层的平均晶粒尺寸仍在45nm以下。这表明掺杂适量的非晶态SiO2组元，可以明显细化晶粒，稳定相结构，同时可粘连分散的活性组元颗粒，起到“支架”的作用。     

Zr-2.5Nb合金中β-Nb相的氧化过程

Zr-2.5Nb合金经β相水淬、冷轧变形及580℃,50 h退火处理,在静态高压釜中进行500℃/10.3 MPa的过热蒸汽腐蚀实验.HRTEM观测表明,580℃,50 h退火处理的锆合金析出了颗粒细小(<100 nm)的β-Nb第二相,其数量较多,分布较均匀.β-Nb相的氧化速率比锆合金基体缓慢,在氧化过程中首先生成NbO_2,呈现晶态和非晶态的混合组织,然后转变成非晶态占主导的氧化物,最后流失到腐蚀介质中.     

磁控溅射-热处理两步法制备Cr_2AlC涂层及力学性能

Cr_2AlC属于三元层状化合物MAX相,其兼具金属和陶瓷的综合性能,如金属的导热、导电、可加工性,陶瓷的抗氧化、耐腐蚀等性能。利用直流磁控溅射技术和后续退火工艺在高速钢基体上制备了Cr_2AlC涂层,采用XRD、SEM等研究了气体流量及热处理工艺对涂层成分和物相组成的影响。结果表明:气体流量和退火温度对Cr_2AlC相的形成至关重要,气体流量比过大和退火温度过高均不利于Cr_2AlC的形成。不同气体流量下沉积态涂层主要由Cr-C化合物、非晶或者纳米晶等组成,均没有发现Cr_2AlC相;涂层经750℃退火后不同气体流量比涂层均有一定量Cr_2AlC相形成;且Cr_2AlC相形成的温度范围随CH_4/Ar气体流量比增加而变窄。含Cr_2AlC MAX相涂层的硬度为10.6~17.6GPa,弹性模量为255.3~323.4GPa。     

RuO2-SiO2二元氧化物被覆钛涂层的制备

采用Pechini法,通过涂覆、烧结和退火,制备成系列含硅的RuO2-SiO2/Ti样品.二元涂层的摩尔成分为X%RuO2-Y%SiO2(以下简写为RuxSiyO2).采用SEM和XRD方法分析了该阳极涂层材料的组织结构特征.结果表明所制备的涂层的相结构主要由金红石相的RuO2所组成,高温处理出现金红石相TiO2,加入的硅以非晶态SiO2的形式存在.经450℃处理的含硅样品的平均晶粒尺寸均小于10nm,明显低于不含硅的样品.同时具有很强的尺寸稳定性,即使经800℃退火处理后,涂层的平均晶粒尺寸仍在45mm以下.这表明掺杂适量的非晶态SiO2组元,可以明显细化晶粒,稳定相结构,同时可粘连分散的活性组元颗粒,起到"支架"的作用.     

高比能量Ti/(Ir_(0.3)Sn_(0.7-x)Ce_x)O_2电极材料的制备及其电化学性能

采用热分解法在360℃制备Ti/(Ir0.3Sn(0.7-x)Cex)O2三元氧化物电极材料(0x0.5)。采用X射线衍射(XRD)、交流阻抗和循环伏安法分析成分对Ti/(Ir0.3Sn(0.7-x)Cex)O2电极材料的晶体结构和电化学性能的影响。结果表明:适量的Ce可降低氧化物涂层中金红石相的晶化程度,优化氧化物涂层的结构,并提高Ti/(Ir0.3Sn(0.7-x)Cex)O2电极材料的电容性能。当x=0.2时,Ti/(Ir0.3Sn0.5Ce0.2)O2电极的比电容达到414 F/g,约为Ti/Ir O2-Sn O2二元氧化物电极的3倍;该电容材料表现出很高的比能量特性,在4.97 k W/kg的高功率密度放电时,对应的能量密度达到82.88 W·h/kg。当x≥0.3时,随着Ce含量增大,氧化物涂层的导电性能和频率响应特性会遭到恶化,对电极的电容性能不利。因此,Ce的含量控制在0.2(摩尔分数)以内为宜。     

La掺杂的SnO2-Sb中间层对钛基IrO2+Ta2O5电极性能的影响

目的改善Ti/IrO_2+Ta_2O_5涂层电极的析氧电催化性能。方法用热分解法在钛基材上制备了La掺杂的SnO_2-Sb中间层,并以此作为基体涂覆IrO_2+Ta_2O_5活性层,制备了Ti/SnO_2-Sb-La/IrO_2+Ta_2O_5涂层电极。采用扫描电子显微镜(SEM)、能量散射能谱(EDS)及X-射线衍射光谱(XRD)技术分别分析了中间层和活性层的表面形貌、元素组成及晶相结构。采用线性扫描伏安曲线(LSV)和强化寿命测试方法在硫酸溶液中分别研究了Ti/SnO_2-Sb-La/IrO_2+Ta_2O_5涂层电极的析氧电催化活性和使用稳定性。同时,考察了La的掺杂比例对Ti/SnO_2-Sb-La/IrO_2+Ta_2O_5电极强化寿命的影响。结果相对未掺杂La的中间层,掺杂La后的中间层表面裂纹减少,有更高的析氧过电位和更低的析氧电流密度。La掺杂对活性层的表面形貌和晶相结构基本没有影响,但电极的析氧电流密度有所提高。通过测试不同La掺杂比例涂层电极的强化寿命,发现La最佳掺杂比例为nLa:nSn=0.5:100。和未掺杂La涂层相比,La最佳掺杂比例涂层电极的强化寿命提高了22.8%。结论相对于未掺杂的Ti/SnO_2-Sb/IrO_2+Ta_2O_5电极,La掺杂后的Ti/SnO_2-Sb-La/IrO_2+Ta_2O_5涂层电极析氧电催化活性和强化寿命都得到改善。     

添加SnO_2组元对RuO_2 SnO_2 TiO_2/Ti钛阳极组织形貌的影响

通过溶胶凝胶 (Sol gel)法经涂刷、烧结、退火等工艺制备了添加不同含量SnO2 的RuO2 SnO2 TiO2 /Ti三元涂层钛阳极。并通过X射线衍射 (XRD)、差热分析 (DTA)、透射电子显微 (TEM )分析了SnO2 组元对RuO2 TiO2 SnO2 /Ti阳极涂层组织、晶粒尺寸和外观形貌的影响。结果表明 ,所获三元涂层颗粒尺寸细小 ,均为纳米结构 ,且添加SnO2 组元后有显著细化涂层晶粒的效果。在不同退火温度下 ,随SnO2 含量的增加 ,涂层晶粒均能发生一定程度的细化。所获三元阳极涂层主要组成物相为金红石 (Ru ,Sn ,Ti)O2 固溶体 ,SnO2 组元含量较高的涂层出现不同成分金红石相共存的现象 ;当涂层退火温度由 45 0℃升高至 6 0 0℃后 ,SnO2 组元不能阻止 (Ru ,Sn ,Ti)O2 固溶体脱溶分解 ,并析出六方晶系Ru单质 ;添加SnO2 组元的RuO2 SnO2 TiO2 涂层晶粒外观呈较理想等轴状特征     

Effect of Different Shapes of the Titanium Based IrO2-Ta2O5 Coatings Anode on Electrochemical Properties

钛基IrO2-Ta2O5涂层阳极的形状分别是板状和扩张网。采用涂覆了H2IrCl6.H2O的盐酸溶液和TaCl5乙醇溶液的混合溶液再进行热分解制备得到IrO2-Ta2O5涂层。分别采用SEM,EDX,CV和加速寿命测试对电极的微观结构和电化学性能进行分析。相对板状电极而言,由于较少的活性物质IrO2在电极表面结晶析出,扩张网状电极具有更低的电化学催化活性。但是由于表面的裂纹较为细密、表面活性元素分布也较为均匀,并且其纵截面的形状更有利于电解析出的气泡排出,扩张网状电极具有更长的加速寿命。     

Morphology,Structure, Microhardness and Corrosion Resistance of Ni-W Coating Annealed in Hydrogen and Argon Atmosphere

In this paper, an amorphous Ni-W coating was electrodeposited on the low-carbon steel and then annealed in hydrogen and argon atmosphere. Their characterization was carried out using scanning electron microscopy and x-ray diffraction. The corrosion characterization was carried out using the potentiodynamic polarization (Tafel) and electrochemical impedance spectroscopy. The results show that microcracks inevitably exist on the surface of Ni-W coating when annealed at 750 °C or higher temperature. After annealing treatment, amorphous structure transforms to crystalline and some new phases are precipitated, which is significantly affected by the annealing temperature and atmosphere. The microhardness of annealed Ni-W coatings is much higher than that of as-deposited coating, while an adverse corrosion performance is observed for the annealed Ni-W coatings. The coating annealed in hydrogen at 500 °C shows a huge improvement in hardness and a fairly acceptable corrosion resistance compared with the as-deposited Ni-W coating.     

IrO2-SnO2涂层电极材料的电容性能研究

通过热分解法在Ti基体上制备了不同Sn含量的IrO2-SnO2涂层。采用循环伏安(CV),恒流充放电和透射电镜(TEM)等测试方法分析了涂层的电容性能和组织结构的关系。结果表明,所制备的IrO2-SnO2涂层电极的比电容随Sn含量的增加呈先增后减的变化,电极材料的可逆性和快速充放电性能逐渐得到改善。在Sn含量为70mol%时,有最大的比电容值485.07F/g。该涂层以非晶态结构为主,其中含有尺寸分布均匀,大小约1nm的微晶,增大了活性点的面积,比纯IrO2电极的比电容提高了7.5倍。     

Effect of Vacuum Annealing on the Characteristics of Plasma Sprayed Al2O3-13wt.%TiO2 Coatings

Adhesion strength is one of the critical properties for plasma-sprayed coating. In this study, the plasma-sprayed Al₂O₃-13wt.%TiO₂/NiCrAl coatings were annealed at 300-900?°C for 6?h in vacuum. The tensile bond strength and porosity of the coatings were investigated. The microstructure and the fracture were studied using optical microscopy, scanning electron spectroscopy, and x-ray diffraction. It was found that the tensile bond strength of coatings increased with the increase of annealing temperature until 500?°C, reaching the maximum value of 41.2?MPa, and then decreased as the annealing temperature continues to increase. All coatings presented a brittle fracture and the fracture occurred inside the ceramic coatings except for the coating annealed at 500?°C, which had a brittle-ductile mixed fracture and the fracture occurred at the interface of bond coating and the substrate.     

Effect of Thermal Annealing on Tribological and Corrosion Properties of DLC Coatings

In this study, the mechanical, tribological, and corrosion properties of annealed diamond-like carbon (DLC) coatings on M2 steel with various annealing temperatures were investigated. The results indicated that DLC coating on M2 steel annealed at 500 °C had the worst performance. Both corrosion polarization resistance and wear resistance against ceramic alumina counterface of DLC coatings decreased with increasing annealing temperature, which can be due to the decline of the coating hardness after the thermal treatment. When sliding against aluminum counterface material, the DLC annealed at 600 °C had the lowest coefficient of friction (cof) and wear resistance due to its high graphitic structure and low hardness. Compared with the original coating, cofs increased for coatings treated at below 300 °C; however, further increasing the annealing temperature led to the decrease of the cofs. Little material attachment occurred between DLC coatings (original and annealed) and counterface materials (both alumina and aluminum balls) except for the DLC annealed at 600 °C, in which coating material transferred to the surface of counterface ball.     

Annealing temperature effect on the corrosion parameters of autocatalytically produced Ni-P and Ni-P-Al2O3 coatings in artificial seawater

Ni-P and Ni-P-Al₂O₃ amorphous alloy coatings with 9.3 and 8.3 wt.% P respectively were obtained by autocatalytic deposition at 90 °C on carbon steel substrates. The effect of annealing temperature (100, 200, 300, 400 and 500 °C) upon the corrosion parameters of the coatings in artificial seawater with pH 5.0 and 8.1 at room temperature was evaluated by potentiodynamic polarisation and electrochemical impedance spectroscopy. It was found that deposits annealed at 400 and 500 °C presented an increase of the charge transfer resistance and negligible changes on samples annealed at lower temperature. Polarisation tests showed a charge transfer controlled anodic kinetics on both Ni-P and Ni-P-Al₂O₃ deposits and diffusion controlled cathodic reaction in artificial seawater at pH 5.0 and 8.1. The coatings did not present passive behaviour in the electrolytes and impedance measurements showed a single time constant for all cases with the lowest double layer capacitance (C_dl) for samples annealed at 400 and 500 °C. The best corrosion parameters were observed on Ni-P and Ni-P-Al₂O₃ coatings annealed at temperatures higher than 400 °C, which is the temperature where crystallisation of this kind of coatings takes place.     

氧化铱薄膜的制备及其导电机理研究

采用脉冲激光沉积技术在Si(100)衬底上制备了高导电的IrO2薄膜,重点研究了退火前后其电学性能和微观结构的变化规律。采用X射线衍射(XRD)、原子力显微镜(AFM)、光电子能谱(XPS)和四探针法对退火前后IrO2薄膜的结构和电性能进行了表征,并利用霍尔效应研究了IrO2薄膜的导电机理。结果表明:IrO2薄膜在空气中退火后,导电性能得到提高,其中在750℃退火的电阻率达到最小值37μΩ.cm。在25～500℃范围内,IrO2薄膜的高温电阻率随着温度的升高呈线性关系逐渐增大,呈现出类似金属的导电特征。在250～400℃沉积的IrO2薄膜载流子的类型为p型;沉积温度较高(500℃)或在更高温度退火处理后,IrO2薄膜载流子的类型为n型,其导电机理以电子导电为主。     

Plasma Spraying of Silica-Rich Calcined Clay Shale

Silica-rich clay shale is a viable candidate for replacement of mullite in many applications, especially when outstanding refractoriness and chemical resistance to various agents are desirable. In this contribution, instead of the commonly used synthetic mullite feedstock, the thermal stability of inexpensive calcined natural raw clay shale sprayed using water stabilized plasma system is reviewed. Phase stability and phase changes at elevated temperatures up to 1500 °C were studied by an array of experimental techniques ranging from measurements of thermal conductivity and the heat flow as functions of temperature, scanning electron microscopy, x-ray diffraction (XRD) of the annealed samples, and in situ high temperature XRD. The mostly amorphous as-sprayed coatings with less than 10 wt.% of mullite are temperature stable up to 800 °C and rapid crystallization occurs between 920 and 940 °C. Performed analyses gave evidence about the increase of mullite grain sizes for temperatures higher than 1200 °C and, moreover, certain saturation of crystallinity, not surpassing the threshold of 60 wt.% even for 1500 °C, is observed. The microstructure after annealing at 1500 °C is notable by clusters of fine needle-like mullite crystallites with sizes within the range of tens of nanometers in Si-rich amorphous matrix.     

INVESTIGATION OF SURFACE MORPHOLOGY, STRUCTURE AND ELECTROCATALYTIC PROPERTIES FOR O_2 EVOLUTION OF TITANIUM BASED IrO_2+Ta_2O_5 COATINGS

1.IntroductionTitaniumbasednoblemetalokidecoatingshavebeenwidelyinvestigatedsincethepast3oyears[l':].Inthisperiod,variousmirtures,compositiollswerepreparedanddifferentmulti-coatingprocessesweredevelopedaselectrodematerialsinelectrochemicalfieId.Inbinaxysystems,thecoatingsof7Omol%IrO2 3Omol%Ta2O5wereverifiedtopossessthemaximumactivityanddurabilityforoxygenevolutio.[3'4],Iroz Taosdepositshavebeenstudiedentensively;ThehighstabilityofthisbinarymixturecouldbeattributedtotheformationofIro2baseds…