Transmission electron microscopy observation of microstructure of plasma-sprayed nanostructured zirconia coating

Nanostructured zirconia coatings deposited by plasma spraying technique were observed using transmission electron microscopy (TEM). It was found that the as-sprayed nanostructured zirconia coating had bimodal microstructures in terms of grain size distribution in the direction parallel to substrate surface. One was in the range 30–120 nm, which was the dominative structure of the coating, and the other was about 150–400 nm. The cross-section micrograph of the plasma sprayed nanostructured zirconia coating revealed that the coating still exhibited lamellar structure with columnar grains extending through its thickness. In conjunction with partially molten zirconia grains, amorphous regions were found. Domain structure and superlattice structure were observed in the plasma-sprayed nanostructured zirconia coating. The formations of the domain and superlattice structures are discussed in this paper.     

Thermal and mechanical properties of ZrO2-CeO2 plasma-sprayed coatings

The thermal and mechanical properties of ZrC₂-C_{eO 2}plasma-sprayed coatings were evaluated to examine their potential as a thermal barrier coating. ZrO₂-CeO₂ solid-solution powders containing up to 70 mol % CeO₂ are successfully plasma sprayed, but cerium content decreases during spraying due to the vaporization of cerium oxide. Hardness is greatest at 30 mol% CeO₂. With increased CeO₂ content, the thermal conductivity decreases to 0.5 W/m K and the thermal expansion coefficient increases to 12.5 x 10_-6 /K. Increased torch input power causes both the relative density and the hardness to increase monotonically, while the thermal conductivity and the thermal expansion coefficient are not significantly affected. When heated above 1300 K, the coating shrinks considerably due to sintering and its thermal conductivity increases abruptly.     

Study on porosity of plasma-sprayed coatings by digital image analysis method

The porosities of plasma-sprayed Al₂O₃, ZrO₂, and TiO₂ coatings deposited on 304 stainless steel plates were evaluated by the digital image analysis method. As the accuracy of this method depends significantly on metallographic preparation and metallography procedure for coating specimens, the effects of cross-surface roughness, magnification, and number of fields of view on the porosity were studied. The results indicate that the porosity value from polished specimen with cross-surface roughness no more than 0.1 μm is acceptable. The porosity value obtained at higher magnification is a little bit higher, especially when the real porosity is higher; more fields of view have to be considered in this case. Both experimental results and statistic analysis suggest that 15 fields of view at 1000× magnification can be implemented to evaluate porosity of plasma-sprayed coating considering both the domain size and the resolution at the same time. The original version of this paper was published as part of the DVS Proceedings: “Thermal Spray Solutions: Advances in Technology and Applications,” International Thermal Spray Conference, Osaka, Japan, 10–12 May 2004, CD-Rom, DVS-Verlag GmbH, Düsseldorf, Germany.     

液相脉冲放电制备Cr-C涂层的性能

以铬/石墨半烧结体电极为工具电极,利用液相脉冲放电涂层（EDC）技术,在普通中碳钢表面制备出以Cr₇C₃为主相的耐磨涂层。对涂层的硬度、结合力、摩擦性能进行了检测与分析,并考察了峰值电流、脉冲宽度对涂层性能的影响。结果表明,涂层与基体呈冶金结合,结合力达83.5 N。涂层厚度随峰值电流及脉冲宽度的增加而增加。当峰值电流小于10 A时,涂层硬度逐渐增加,而当脉冲宽度大于8 μs时,涂层硬度逐渐减小。硬度从涂层表面至基体呈逐渐减小的梯度分布,涂层表面硬度最高达1820 HV0.2。与H13热作模具钢相比,在相同的载荷下,涂层的摩擦因数较小,仅为0.12左右,展现出良好的减摩耐磨特性。     

脉冲电化学沉积制备n-HA/ZrO2复合涂层

用脉冲电化学沉积法在生物医用钛金属表面成功制备了纳米RA/ZrO2复合涂层,涂层中的成分均以离子形式沉积到基材上,得到ZrO2均匀分布的HA/ZrO2复合涂层.脉冲电位为-3.5 V时有利于离子的沉积结晶,有利于复合涂层的沉积.复合涂层的成分、结构、形貌及生物活性等的研究结果表明:复合涂层烧结前成分为HA、OCP及碱式硝酸锫,高温烧结后得到均匀致密HA/ZtO2复合涂层.检测表明HA/ZrO2复合涂层能够诱导磷灰石生成,具有较好的生物活性.     

Effects of zincate treatment on adhesion of electroless Ni-P coating onto various aluminum alloys

The effects of alloying elements on zincate treatment and adhesion of electroless Ni-P coating onto various aluminum alloy substrates were examined. Surface morphology of zinc deposits in the 1st zincate treatment and its adhesion were changed depending on the alloying element. The zinc deposits in the 2nd zincate treatment became thinly uniform, and the adhesion between aluminum alloy substrate and Ni-P coating was improved irrespective of the alloying element. XPS analysis revealed the existence of zinc on the surface of each aluminum alloy substrate after the pickling in 5% nitric acid. This zinc on the surface should be an important factor influencing the morphology of zinc deposit at the 2nd zincate treatment and its adhesion.     

钛合金表面等离子喷涂Y2O3稳定的ZrO2涂层的 扫描热显微镜分析

以纳米结构Y2O3稳定的ZrO2热喷涂粉末为原料,采用等离子喷涂法在Ti-6Al-4V合金上制备了纳米结构的热障涂层。利用扫描电镜(SEM)及扫描热显微镜(SThM)对涂层的微观组织及热性能进行了分析。在实验基础上建立了理论模型,并对涂层及基体的热导率进行了估算。结果表明:采用SThM分析方法估算的涂层厚度及涂层上的缺陷尺寸与采用其它分析方法测得的结果一致;虽然热导率的估算结果与采用其它方法得出的结果差异较大,但显示出扫描热显微镜分析是估算材料热导率潜在的方法。     

等离子喷涂ZrO2-NiCoCrAlY梯度涂层的界面强化热处理工艺

在大气条件下经高温长时间保温后,ＺｒＯ２ＮｉＣｏＣｒＡｌＹ 梯度涂层中的ＮｉＣｏＣｒＡｌＹ 组元发生严重氧化, 形成大量的ＮｉＯ, Ａｌ２Ｏ３ 和Ｃｒ２Ｏ３ 等氧化物, 导致ＺｒＯ２ 表面层中产生粗大网状裂纹, 并最终导致ＺｒＯ２ 表面层碎裂而失效。对梯度涂层进行（９００ ℃） 保温（８ ｈ） 的真空热处理后, 涂层完好无损, ＮｉＣｏＣｒＡｌＹ 底层与ＴＣ４ 基体发生了冶金化学反应, 在涂层与基体界面形成了含ＮｉＴｉ, ＮｉＴｉ２ 和ＴｉＡｌ３ 等化合物的反应层, 涂层的抗热震性能得以显著地提高     

Spark plasma sintering of high-toughness ZrO2 materials doped with yttrium

Zirconia powders doped with yttrium prepared by special liquid-phase precipitation method were sintered by spark plasma sintering (SPS) to obtain high performance samples.The microstructure,phase composition,and mechanical properties of the samples were studied.The results of X-ray diffraction (XRD),Raman spectrum,and transmission electron microscope (TEM) show that the phase is tetragonal.The powders with large surface area and high sintering activity,due to small crystallite size,could be densified at 1100℃.The highest relative density of the sample obtained at 1300℃ is higher than 99% (the tetragonal phase is 6.08 g/cm3).The Hv and Kic are 13.76 GPa and 15.4 MPa.m1/2,respectively.     

Influence of heat treatment on nanocrystalline zirconia powder and plasma-sprayed thermal barrier coatings

Nanostructured zirconia top coat was deposited by air plasma spray and NiCoCrAlTaY bond coat was deposited on Ni substrate by low pressure plasma spray.Nanostructured and conventional thermal barrier coatings were heat-treated at temperature varying from 1050 to 1 250oC for 2-20 h.The results show that obvious grain growth was found in both nanostructured and conventional thermal barrier coatings(TBCs)after high temperature heat treatment.Monoclinic/tetragonal phases were transformed into cubic phase in the agglomerated nano-powder after calcination.The cubic phase content increased with increasing calcination temperature.Calcination of the powder made the yttria distributed on the surface of the nanocrystalline particles dissolve in zirconia when grains grew.Different from the phase constituent of the as-sprayed conventional TBC which consisted of diffusionlesstransformed tetragonal,the as-sprayed nanostructured TBC consisted of cubic phase.     

Correlation between liquid structure and γ2-phase precipitation of Cu-Al-Ni shape memory alloys

1　ＩＮＴＲＯＤＵＣＴＩＯＮＣｕ ｂａｓｅｓｈａｐｅｍｅｍｏｒｙａｌｌｏｙｓ (ＳＭＡ)ａｒｅｃｏｍ ｍｅｒｃｉａｌｌｙａｔｔｒａｃｔｉｖｅｓｙｓｔｅｍｓｆｏｒｔｈｅｐｒａｃｔｉｃａｌｅｘｐｌｏｉｔａ ｔｉｏｎｏｆｔｈｅｓｈａｐｅｍｅｍｏｒｙｅｆｆｅｃｔ (ＳＭＥ     

Mechanical wet-milling and subsequent consolidation of ultra-fine Al2O3-（ZrO2＋3%Y2O3） bioceramics by using high-frequency induction heat sintering

Alumina/zirconia composites were synthesized by wet-milling technique and rapid consolidation with high frequency induction heat sintering(HFIHS). The starting materials were a mixture of alumina micro-powder (80%, volume fraction) and 3YSZ nano-powders (20%). The mixtures were optimized for good sintering behaviors and mechanical properties. Nano-crystalline grains are obtained after 24 h milling. The nano-structured powder compacts are then processed to full density at different temperatures by HFIHS. Effects of temperature on the mechanical and microstructure properties were studied. Al2O3-3YSZ composites with higher mechanical properties and small grain size are successfully developed at relatively low temperatures through this technique.     

Mn对Al-Ti-B、Al-Ti-C中间合金细化铝晶粒效果的影响

试验研究了Mn元素对Al-5Ti-1B和Al-5Ti-0.2C两种铝用中间合金晶粒细化效果的影响,分析了Mn元素影响两种中间合金晶粒细化效果的机制。结果表明,总体来讲,Mn对Al-5Ti-1B和Al-5Ti-0.2C的晶粒细化效果有不同程度的破坏作用。微量Mn元素不会影响铝熔体中形核基底的活性,Mn元素加入铝熔体后的生长限制因子很小,不能有效阻止小尺寸晶粒的长大和相互融合,添加Mn元素所导致的熔体过热对晶粒细化的破坏作用占主导地位,最终导致中间合金的晶粒细化效果被削弱。     

液体中脉冲放电制备(Ti,Al)C陶瓷涂层的研究

用粉末模压成型工艺和无压烧结方法制备了Ti-Al混合烧结工具电极,采用所制备的电极在煤油中对45钢表面进行脉冲放电沉积(Ti,Al)C陶瓷涂层。探讨了粉体配比对工具电极致密度和相组成以及对液相放电所制备的涂层组织与表面形貌的影响。结果表明,随着Al含量的提高,工具电极密度和相对密度先下降后升高,当Al含量为60%时,电极密度达到最小;XRD结果显示制备出涂层的物相主要为(Ti,Al)C,而制备出的涂层表面形貌明显不同,随着电极中Al元素的升高,熔滴状的熔池尺寸越来越大,宏观上越来越粗糙,截面涂层厚度约为20μm。     

Liquid Penetration Phenomenon of Gas Atomized Powders during Semi-solid Rolling

在氢气保护性气氛下,采用半固态轧制工艺将Al-5.8Zn-1.63Mg-2.22Cu-0.12Zr(wt%)粉末制备出生带材。研究了加热相同温度610℃(i.e.液相分数f s≈53%)时,不同的加热时间对生带材显微组织的影响,重点研究了液相渗透现象。结果表明:液相渗透程度越高,颗粒在接触界面的边界加速消失,颗粒边界发生了较大的变化。当在610℃下加热,保温时间由10 min延长至30 min时,η(Mg Zn2)相的数量减少,且在晶界处析出了更多的Al2Cu颗粒。Al-5.8Zn-1.63Mg-2.22Cu-0.12Zr(wt%)粉末在610℃下半固态轧制,其最优的保温时间为20~30 min。研究结果表明通过优化半固态轧制工艺可以制备出性能优异的带材。     

Density of liquid NiCoAlCr quartemary alloys measured by modified sessile drop method

The densities of liquid NiCoAlCr quaternary alloys with a fixed molar ratio of Ni to Co to Al （x（Ni）：x（Co）：x（Al）≈ 73：12：15） which is close to the average value of the commercial Ni-based superalloys TMS75, INCO713, CM247LC and CMSX-4, and the mass fraction of chromium changes from 0 to 9% were measured by a modified sessile drop method. It is found that with increasing temperature and chromium concentration in the alloys, the densities of the liquid NiCoAICr quaternary alloys decrease, whereas the molar volume of the liquid NiCoAICr quaternary alloys increases. And the liquid densities of NiCoAICr quaternary alloys calculated from the partial molar volumes of nickel, cobalt, aluminum and chromium in the corresponding Ni-bases binary alloys are in good agreement with the experimental ones, i.e. within the error tolerance range the densities of the liquid Ni-based multi-component alloys can be predicted from the partial volumes of elements in Ni-based binary alloys in liquid state. The molar volume of liquid NiCoAICr binary alloy shows a negative deviation from the ideal linear mixing and the deviation changes small with the increase of chromium concentration at the same temperature.     

送粉激光熔覆ZrO2/Ni60复合涂层组织结构与性能

采用送粉激光熔覆工艺分别制备了含1％和3％氧化锆陶瓷的强韧化镍基自熔合金涂层，考察了氧化锆含量，以及工艺参数对熔覆层组织结构与性能的关系。结果表明，氧化锆掺杂涂层的组织特征取决于熔池的流动性，由于氧化锆的密度较镍基自熔合金要小许多，因此在激光束提供的能量超过一定值之后，会出现分层的组织结构，反之可获得均匀的两相复合组织结构。最后给出了获得均匀组织结构的工艺方案。