Damage law identification of a quasi brittle ceramic from a bending test using Digital Image Correlation

Although ceramics are generally considered to be elastic brittle solids, some of them are quasi brittle. These ceramics show a non-linear mechanical behaviour resulting most of the time in a difference between their tensile and compressive stress–strain laws. The characterization of their fracture strengths might be biased if linear elastic formulae are used to analyze classical tests like bending tests. Based on Digital Image Correlation (DIC), an efficient technique to measure full field displacements, a methodology is proposed to characterize and model materials with dissymmetric behaviours between tension and compression. Applying specific basis functions for DIC displacement decompositions for bending, compressive and tensile tests, a stress–strain model and its damage law are identified and then validated for aluminium titanate, a damageable micro-cracked ceramic at room temperature. This identification method using DIC can obviously be applied to other quasi brittle materials.     

Approximate Theory of Thermal Stress Resistance of Brittle Ceramics Involving Creep

The effect of stress relaxation by creep on the thermal stress fracture of brittle ceramics at high temperature under conditions of quasi-static heat flow is discussed. It is shown that, to a good approximation, thermal stress relaxation rates can be calculated on the basis of creep rates which correspond to the minimum temperature of the ceramic workpiece. For materials exhibiting linear stress-creep rate dependence, expressions for the relaxation time and maximum temperature difference or heat flux to which ceramic bodies can be subjected are derived in terms of the material variables affecting thermal stress fracture and stress relaxation by creep. A numerical example shows that high-temperature creep can materially affect the thermal stress behavior of brittle ceramics. Appropriate thermal stress parameters are proposed to form the basis of proper material selection for high-temperature environments involving thermal stress and stress relaxation by creep. Conditions for which thermal stress calculations should be based on an elastic or viscoelastic analysis are outlined.     

高温结构陶瓷的高温蠕变

高温蠕变是高温结构陶瓷材料一项非常重要的性能指标。现代耐高温结构材料要求有很高的抗蠕变性能。本文从理论上描述了蠕变及其机理，分析了影响高温结构陶瓷蠕变的因素，并结合实际提出了提高高温结构陶瓷抗蠕变性的措施。     

High-temperature compressive creep behavior and mechanism of Hf6Ta2O17 ceramic as a candidate for thermal barrier coatings

A novel Hf₆Ta₂O₁₇ ceramics is prepared by a solid-state reaction method. High-temperature creep behavior of Hf₆Ta₂O₁₇ and 8YSZ ceramics are investigated by compressive creep test combined with a digital image correlation (DIC) method. It is found that the creep mechanism of Hf₆Ta₂O₁₇ ceramics is controlled by grain boundary sliding associated with dislocation movement (stress exponent ∼2-3, and activation energy of 600–620 kJ/mol). Grain boundary sliding accommodated to the interface reaction is the main creep mechanism of 8YSZ ceramics (stress exponent ∼2, and activation energy of 425∼465 kJ/mol). Hf₆Ta₂O₁₇ ceramics have higher creep resistance than 8YSZ ceramics under the same conditions.     

Application of Hertzian Tests to Measure Stress–Strain Characteristics of Ceramics at Elevated Temperatures

A new method for evaluating the elastic–plastic properties of ceramics from room temperature up to the onset of creep based on Hertzian indentation testing is proposed. Indentation stress–strain curves are compiled for representative alumina and zirconia ceramics at prescribed temperatures. Deconvolution of the indentation stress–strain curves for each material provides a measure of Young's modulus, yield stress, and work-hardening coefficient as a function of temperature, enabling construction of true stress–strain curves. The stress–strain curves flatten out with increasing temperature, in accordance with an expected increased plastic response at elevated temperatures.     

Frequency sensitivity of fatigue processes in polymeric solids

One is faced with an interesting challenge when trying to explain the effect of test frequency on polymer fatigue performance. While hysteretic heating arguments appear sufficient to explain a diminution of fatigue resistance with increasing cyclic frequency in unnotched test samples, the enhancement of fatigue resistance in many polymers with increasing cyclic frequency in notched samples is still not clearly understood. In large measure, this is due to contradictory trends in fre-quency-sensitive material properties which affect the fatigue process. In this paper, a number of proposed fatigue models dealing with the time and strain rate dependence of elastic modulus, yield strength, creep and localized crack tip heating are examined and confronted with available data from the literature. Additional fatigue crack propagation data for poly(methyl methacrylate), poly (vinyl chloride), polystyrene, poly-carbonate, nylon 66, poly(vinylidene fluoride) and poly(2,6-dimethylphenylene oxide) were obtained and are reported herein. These data were obtained over a maximum frequency range of 0.1 to 100 Hz and, for selected polymers, with various waveforms. Frequency sensitivity is shown to be greatest in those polymers that show a high tendency for crazing. Relative fatigue behavior is found to reflect a competition between strain rate and creep effects. Where creep effects dominate, the total crack growth rate may be viewed as consisting of the summation of pure fatigue and creep components, respectively. Finally, the β transition appears to have a role, with frequency sensitivity being at a maximum for polymers where the β transition at room temperature occurs in the range of the experimental test frequency.     

Thermal exposure effects on the long‐term behavior of a mullite fiber at high temperature

The behavior of an oxide fiber at elevated temperatures was analyzed before and after thermal exposures. The material studied was a mullite fiber developed for high‐temperature applications, CeraFib 75. Heat treatments were performed at temperatures ranging from 1200°C to 1400°C for 25 hours. Quantitative high‐temperature X‐ray analysis and creep tests at 1200°C were carried out to analyze the effect of previous heat treatment on the thermal stability of the fibers. The as‐received fibers presented a metastable microstructure of mullite grains with traces of alumina. Starting at 1200°C, grain growth and phase transformations occurred, including the initial formation of mullite, followed by the dissociation of the previous alumina‐rich mullite phase. The observed transformations are continuous and occur until the mullite phase reaches a state near the stoichiometric 3/2 mullite. Only the fibers previously heat treated at 1400°C did not show further changes when exposed again to 1200°C. Overall, the heat treatments increased the fiber stability and creep resistance but reduced the tensile strength. Changes observed in the creep strain vs. time curves of the fibers were related to the observed microstructural transformations. Based on these results, the chemical composition of the stable mullite fiber is suggested.     

Creep behavior of PLA‐based biodegradable plastic exposed to a hydrocarbon liquid

This study explores the effect of hydrocarbon liquid on creep behavior of polylactic acid (PLA)‐based plastic. Evolution of the mechanical properties of the material was investigated experimentally by measurement of creep under tensile load. Tensile creep behavior was studied with a constant load over a temperature range from 30 to 50°C using specimens containing different levels of liquid. It was shown that the hydrocarbon liquid diffusion obeys the Fickian law of diffusion. The viscoelastic properties vary with temperature and these properties dramatically decrease above the glass transition temperature (T_g). Significant decreases in modulus and in the peak of tan δ were observed with an increase in liquid concentration at low temperatures. In contrast, at high temperatures, drier material recorded lower storage modulus. However, only small changes of T_g were recorded. Dependence of compliance on temperature was observed in the creep test at all levels of liquid content. With respect to drier samples, it was noted that the high liquid content material had a lower rate of increasing creep strain with temperature. Therefore, at elevated temperatures, higher creep strain of dry specimens was observed compared to those with a higher liquid content. The improvement of creep resistance and stiffening of material at high temperatures can be attributed to the significant increase of crystallinity fraction induced by liquid absorption. Understanding the effect of liquid diffusion in conjunction with temperature provides useful information for assessment of the potential use of this biodegradable plastic in load‐bearing applications exposed to an organic liquid. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Cavitational Strain Contribution to Tensile Creep in Vitreous Bonded Ceramics

Analysis of the role of cavitation during uniaxial creep deformation in vitreous bonded ceramics reveals that the cavity volume contributes only to the strain in the direction parallel to the tensile stress regardless of the shape and orientation of cavities. Creep asymmetry results from the fact that cavitation preferentially contributes to axial tensile strain while the strain observed under the same conditions in compression is produced only by volume-conserving mechanisms. The contribution of cavitational strain in the axial tensile strain is equal to the volume fraction of cavities and proportional to the difference between tensile and compressive strains in the axial direction. The density change method and a newly proposed method based on the difference in the axial strains were used for separating the cavitational from the true tensile strain in self-reinforced silicon nitride. Both methods consistently revealed more than 90% contribution of cavitation to the total tensile strain. Cavitation is concluded to be the dominant mechanism of tensile creep deformation in vitreous bonded ceramics because the reported volume fractions of cavities during their deformation are usually in the range of 70–90% of tensile strain.     

Creep characterization of vapor‐grown carbon nanofiber/vinyl ester nanocomposites using a response surface methodology

The effects of selected factors such as vapor‐grown carbon nanofiber (VGCNF) weight fraction, applied stress, and temperature on the viscoelastic responses (creep strain and creep compliance) of VGCNF/vinyl ester (VE) nanocomposites were studied using a central composite design (CCD). Nanocomposite test articles were fabricated by high‐shear mixing, casting, curing, and post curing in an open‐face mold under a nitrogen environment. Short‐term creep/creep recovery experiments were conducted at prescribed combinations of temperature (23.8–69.2°C), applied stress (30.2–49.8 MPa), and VGCNF weight fraction (0.00–1.00 parts of VGCNF per hundred parts of resin) determined from the CCD. Response surface models (RSMs) for predicting these viscoelastic responses were developed using the least squares method and an analysis of variance procedure. The response surface estimates indicate that increasing the VGCNF weight fraction marginally increases the creep resistance of the VGCNF/VE nanocomposite at low temperatures (i.e., 23.8–46.5°C). However, increasing the VGCNF weight fraction decreased the creep resistance of these nanocomposites for temperatures greater than 50°C. The latter response may be due to a decrease in the nanofiber‐to‐matrix adhesion as the temperature is increased. The RSMs for creep strain and creep compliance revealed the interactions between the VGCNF weight fraction, stress, and temperature on the creep behavior of thermoset polymer nanocomposites. The design of experiments approach is useful in revealing interactions between selected factors, and thus can facilitate the development of more physics‐based models. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42162.     

基于数字图像相关法的铝镁质耐火材料抗侵蚀性能研究

钢渣侵蚀是耐火材料在服役过程中的主要损毁形式之一,实际侵蚀过程难以直接观察。传统上采用蚀后分析方法来评价耐火材料的抗侵蚀能力和了解侵蚀机理,但易缺少过程信息,导致结果存在偏差。因此,本文在高温可视化系统基础上,结合数字图像相关法,选取三种典型钢渣,开展铝镁质耐火材料的渣蚀行为研究,并探讨了不同钢渣及热处理温度对材料抗侵蚀能力的影响。结果表明：碱度越低的熔渣对铝镁质耐火材料的侵蚀越严重;对铝镁质耐火材料进行1 000℃以上的热处理,可有效提高材料的抗侵蚀能力;通过数字图像相关法可以获得随时间变化的平均应变曲线和侵蚀应变云图,其中平均应变曲线可以对比铝镁质耐火材料对不同钢渣的抗侵蚀能力,侵蚀应变云图可以反映侵蚀的演变过程,两者为耐火材料渣蚀过程的表征提供了量化指标。     

Tensile Stress Relaxation of Alumina at High Temperature

The development of a tensile testing methodology for ceramics which enables a stress vs strain-rate response to be measured at high temperature is described. The test involves a carefully controled stress relaxation test at constant total strain using an experimental procedure and phenomenological analysis previously developed for metallic materials. It is demonstrated here with preliminary tests on alumina at 1050° and 1150°C. This offers, with further development, the possibility of establishing design stresses associated with low strain-rate behavior for structural applications. The results demonstrate that data covering four decades of strain rate may be generated in tests lasting a few hours. The inelastic strain consists of substantial anelastic recoverable strain in addition to a permanent creep strain.     

Grain-Boundary Sliding and Grain Interlocking in the Creep Deformation of Two-Phase Ceramics

Grain-boundary sliding and grain interlocking of two-phase ceramics during creep are examined on the basis of the Dryden–Kucerovsky–Wilkinson–Watt theory. That theory is extended to the plane–strain creep deformation of model arrays of square and hexagonal grains embedded in a continuous grain-boundary melt phase to develop consti-tutive equations for their universal creep. Superposition is derived for the "time-applied stress" and the "time–temperature" relations during creep. The "shift factor" for the time–temperature superposition characterizes the temperature dependence of the apparent viscosity of the ceramic. A two-phase ceramic during creep acts as a non-Newtonian fluid, the viscosity of which is dependent on the creep strain. The constitutive relation between the creep strain rate and the creep strain is then utilized to estimate the viscosity and the volume fraction of the intergranular melt phase. The equilibrium creep strain to achieve grain interlocking is considered through the rotational motion of grains. Creep tests for a β-spodumene glass-ceramic are conducted under simple shear to generate experimental results for scrutinizing the theoretical predictions. Satisfactory agreement is observed, giving important rheological information on the creep process.     

Effects of molecular weight and molecular weight distribution on creep properties of polypropylene homopolymer

The molecular weights of the industrial-grade isotactic polypropylene (i-PP) homopolymers samples were determined by the melt-state rheological method and effects of molecular weight and molecular weight distribution on solid and melt state creep properties were investigated in detail. The melt-state creep test results showed that the creep resistance of the samples increased by M_w due to the increased chain entanglements, while variations in the polydispersity index (PDI) values did not cause a considerable change in the creep strain values. Moreover, the solid-state creep test results showed that creep strain values increased by M_w and PDI due to the decreasing amount of crystalline structure in the polymer. The results also showed that the amount of crystalline segment was more effective than chain entanglements that were caused by long polymer chains on the creep resistance of the polymers. Modeling the solid-state viscoelastic structure of the samples by the Burger model revealed that the weight of the viscous strain in the total creep strain increased with M_w and PDI, which meant that the differences in the creep strain values of the samples would be more pronounced at extended periods of time.     

冻融循环作用下盐浓度对温拌胶粉改性沥青混合料开裂特性影响

为科学分析冻融循环作用下除冰盐侵蚀对温拌胶粉改性沥青混合料(CR-WMA)和热拌胶粉改性沥青混合料(CR-HMA)路面开裂特性的影响,运用数字图像(DIC)技术对三点弯曲重复加载试验下两种半圆试件产生的水平应变进行分析,定量描述沥青混合料的损伤开裂特性。采用半圆弯拉试验(SCB)分析两种试件的蠕变应变能(DCSE),并与基于DIC技术下的损伤开裂指标进行相关性分析。试验结果表明:水平应变场中数值较大的点与试件损伤开裂的演化有密切关系;CR-WMA和CR-HMA的抗损伤开裂性能随着盐浓度的增加先降低后升高,且在盐浓度为8%时最差;无论是水冻还是盐冻条件下,CR-WMA的损伤累积密度D_E值和D_CSE值较CR-HMA高,说明CR-WMA抗开裂性能及抗盐侵蚀能力均优于CR-HMA;发现D_E和D_CSE具有较好的相关性,验证了DIC技术评价沥青混合料损伤开裂特性的合理性。     

Effect of heat treatment on the creep behavior of α/β SiAlON sintered with multication oxide sintering additives

SiAlONs are important materials for high-temperature applications and creep properties of SiAlONs are largely controlled by the amount and type of sintering additives. It has been established that heat treatment can reduce the amount of amorphous intergranular phase through crystallization. However, there is no study on the creep behavior of heat-treated SiAlON ceramics containing multication sintering additives. Therefore, the aim of the study was to investigate the effect of heat treatment on the creep properties of multication containing (Y-Sm-Ca oxides) α/β-SiAlON ceramics. The heat treatments of the sintered samples were carried out at 1600°C for 2 hours. The creep tests were carried out in the range 1300-1400°C under different loads (50-150 MPa). The existing phases and the microstructures of samples before and after creep were investigated using XRD and SEM techniques. It was found that heat treatment resulted in a better creep performance compared to as-sintered samples. The activation energy and stress exponent for heat-treated SiAlONs were also calculated as 708 ± 45 kJ/mol and 1.4, respectively. Compared to the sintered sample values, the results suggested that the acting creep mechanism of grain-boundary sliding and cavitation was reduced with the heat treatment.     

高温结构陶瓷材料的设计准则

针对航空发动机对热结构材料的性能要求，从以下五个方面论述了高温结构陶瓷材料的设计准则，抗氧化性和挥发性，抗蠕变性，显微结构的设计，断裂韧性和抗热震性，抗氧化性和挥发性是由材料的本质特性所决定，脆性是限制结构陶瓷实用的关键，通过对显两重结构和成分的合理设计能有效提高其断裂韧性和抗蠕变性能，而抗热震性则是由构件的材质，结构和环境条件所共同决定的参数。     

Mechanical Properties of Polycrystalline Lithium Orthosilicate

Room-temperature mechanical properties and high-temperature creep deformation of lithium orthosilicate (Li₄SiO₄) were studied. Elastic constants, flexural strength, and fracture toughness were determined for specimens with densities between 68% and 98% of theoretical. Critical quenching temperature and thermal-shock resistance parameters for 90% dense specimens were also measured. High-temperature creep deformation was investigated by a constant-strain-rate test in an argon atmosphere at temperatures between 750° and 1025°C and strain rates ranging from about 10⁻⁶ to 10⁻³ s⁻¹. At 950°C and above, the stress exponent, n , was determined to be 3.6, with a creep activation energy of 715 kJ/mol. Selected results obtained for Li₄SiO₄ are compared with results obtained for other Li-containing ceramics that are under consideration as candidates for fusion reactor breeder blankets.     

Fracture toughness,strength and creep of transparent ceramics at high temperature

Fracture toughness, four-point bending strength of transparent spinel, Y₂O₃ and YAG ceramics in function of temperature (from room temperature up to 1500° C) were measured. Creep resistance at 1500–1550° C was studied too. Grain size distribution was determined on polished and etched surfaces of samples. Fracture surfaces after tests were examined by scanning electron microscopy. The obtained results showed that: in the case of spinel ceramics fracture toughness and strength decreased from 20 to 800° C, increased from 800 to 1200° C and decreased at higher temperature; in the case of Y₂O₃ ceramics they increased from 400 to 800° C, and next kept constant up to 1500° C; in the case of YAG ceramics they kept constant from 20 to 1200° C and then decreased. The creep strain rate was measured for spinel and YAG but not for Y₂O₃ ceramics which appeared creep resistant. The hypotheses concerning toughening and creep mechanisms were proposed.