Miniature Specimens Research Articles

Multiaxial creep deformation investigation of miniature cruciform specimen for type 304 stainless steel at 923 K using non-contact displacement-measuring method

Abstract Multiaxial creep investigations at high temperatures are required to guarantee the integrity of structural materials such as boiler pipes for power generation and turbine blades for aviation and industrial applications. The multiaxial creep testing method using a cruciform specimen has several advantages, and the authors successfully downsized the specimen. The authors also developed a technique for the in situ observation of the specimen in an electric furnace and the non-contact displacement measurement in the development of a biaxial tensile creep testing machine for the miniature cruciform specimen. By observing the specimen at a target mark during the creep testing through an observation window installed at the bottom of the furnace, it was possible to visualize the specimen surface variations and obtain the axial strain from the locus of the target marks. The Mises-type equivalent strain was calculated from the axial strains obtained in the equi-biaxial tensile multiaxial creep testing and was compared with the strains obtained in the uniaxial creep testing. The Mises-type equivalent strain can be expressed using a unified method up to approximately 5% of the initial strain in the test, even in the multiaxial stress state.

Utilization of High-Temperature miniaturized testing to Assist in life management for gas turbine Blades: An Overview

Safely operating gas turbine blades in aero-engines or industrial gas turbines under severe thermo-mechanical conditions always poses a continuous challenge. There is an urgent need for more reliable life prediction tools, necessitating earlier and more rigorous assessments of in-service damage. This paper introduces a systematic examination of high-temperature miniature specimen testing method within a practical life management framework. To improve current practices in assessing the condition of service-aged gas turbine blades, a proactive utilization of miniature specimen testing is recommended for early in-service assessment within the component lifecycle and integrated into a comprehensive life assessment/management framework. The paper outlines a structured approach to life management, combining miniature specimen sampling and creep and fatigue testing methods. This forms the basis for a novel, holistic life assessment methodology, which is proposed in this paper, incorporating the innovative use of high-temperature miniature specimen testing.

Size Effect on the Ductile Fracture of the Aluminium Alloy 2024-T351

BackgroundReliably calibrated criteria are needed for an accurate prediction of fracture of various components. However, there is not always a sufficient amount of material available. Therefore, miniature testing provides an alternative that is researched together with the following calibration of the ductile fracture criteria and investigating the size effect.ObjectiveThe aim is to design miniature testing equipment and specimens for tensile testing, which covers various stress states. This is supplemented by the small punch test, which has the same specimen thickness, taken from the literature to broaden the portfolio for calibration. The second part deals with conducting the finite element analysis, which provided a basis for the calibration of the phenomenological ductile fracture criterion applicable to crack-free bodies to indicate the crack initiation.MethodsThe steel frame to test thin specimens is designed with optical measurement of deformations. The finite element method is used, within Abaqus and user subroutines, to simulate the tests to obtain the variables needed for the calibration. In addition, the calibration of the criterion using machine learning is explored.ResultsThe feasibility of the proposed experimental program is tested on the aluminium alloy 2024-T351. Moreover, the numerical simulations, which showed a good match with experiments in terms of force responses, adds to the knowledge of modelling in the scope of continuum damage mechanics.ConclusionsThe presented results provide a material basis for the aluminium alloy studied on a lower scale, while they broaden the testing possibilities and analyses the calibration strategies for the best failure predictability possible.

On the correlation between fatigue behaviour and the multiphase microstructure of a super duplex stainless steel

This work investigates the relationship between the multiphase microstructure and the macroscale fatigue behaviour of a cast super duplex stainless steel (SDSS). The microstructure of a cast SDSS is typically composed of a FCC γ-phase and a BCC δ-phase. However, deleterious secondary phases (SP), such as sigma and chi, may precipitate when SDSS is exposed to high-temperature ranges, jeopardising its mechanical properties, namely fatigue performance. The purpose of this investigation was to quantify the correlation between SP amounts and fatigue life of a cast SDSS (CD3MWCuN, ASTM A890). Fatigue tests were conducted using miniature specimens taken from a cast C-Ring with different SP amounts. A numerical model was proposed to calibrate the fatigue test parameters. After the tests, SEM and EBSD techniques were used to quantify the SP and analyse the fatigue-crack propagation. The microstructural analysis was complemented with hardness and tensile tests. Regression models were developed to correlate the percentage of SP, the fatigue resistance and the number of cycles to failure, and to predict the microstructural stress concentration from the amount of SP. In addition, a methodology is proposed for predicting S-N curves as a function of the amount of SP, showing a high correspondence in the increase of the percentage of SP with the decrease in fatigue life. Furthermore, the fatigue strength, for a given number of cycles to failure, tends to decrease linearly with increasing the SP, while the microstructural stress concentration factor tends to increase with an increase in SP. These findings contribute to further knowledge on predicting the behaviour of cast SDSS under different cyclic conditions, which can be valuable for optimizing design and performance in various applications.

On comparison of fracture toughness of irradiated and thermally aged decommissioned nuclear weld metals with miniature specimen test technique

This paper investigates the fracture toughness of thermally aged and irradiated weld metals extracted from head and beltline regions of a decommissioned nuclear reactor pressure vessel. Miniature compact tension specimens are fabricated from the thermally aged reactor pressure vessel head weld as well from the circumferential and axial beltline welds having fluences of 2.90 × 1016n/cm2 and 7.94 × 1017n/cm2, respectively. Master curve approach in accordance with the ASTM E1921 is applied to determine the reference temperature T0 and it is found to be − 113.5 °C, −104.4 °C, and − 89.3 °C for the reactor pressure vessel head, axial beltline, and circumferential beltline welds, respectively. In addition, the multimodal reference temperature Tm to assess the homogeneity of welds as well as key curve analysis for the quality assurance of testing are also provided. Fractographic analysis identified variations in crack initiation sites and microstructural inhomogeneities, particularly in the irradiated beltline welds. Overall, fracture mechanical testing of the materials demonstrated that miniature compact tension specimens are effective for characterizing the fracture toughness of limited surveillance weld materials, revealing differences due to irradiation and weld location.

Validity of Toughness Measurements From Miniature Specimens Failing in Different Fracture Modes

Abstract Using miniature compact tension (mini-C(T)) (4 mm thick, 0.16T) specimens to determine toughness in reactor pressure vessel (RPV) steels permits the ductile-to-brittle transition temperature to be derived from small amounts of material and allows more effective use of surveillance specimens. However, questions have been raised as to whether the failure mechanisms are the same in miniature and large specimens, something that must be ensured when transferring fracture results obtained in mini-C(T) specimens to larger components. This work, performed within the FRACTESUS project, presents toughness measurements and detailed fractography on both a homogeneously brittle base metal and a relatively ductile, inhomogeneous weld to assess the transferability of fracture data. The fractography shows that brittle fracture initiates within the part of specimen experiencing small-scale yielding (SSY), so long as the toughness measurement is valid. Similarly, although the precrack front asymmetry appears more marked in smaller specimens, as long as the deviation from planarity is within the American Society for Testing and Materials (ASTM) E1921 limits, the asymmetry does not affect the location of the initiation site. For materials showing a variety of fracture modes, the fracture modes observed at the initiation sites are consistent with those observed in larger specimens. Where data are available, the stress and strain conditions at the initiation sites are also found to be consistent in mini-C(T) and larger specimens. These observations support the thesis that toughness measurements made on mini-C(T) specimens reflect the same material characteristics and failure mechanisms as those made on larger specimens.

Elastic–plastic strain conversion of a thin-plate miniaturized tensile test based on crosshead measurement via an analytical method

This paper underscores the significance of accurate strain measurement in unconventional miniature thin plate specimen (MTPS) tests and proposes a data conversion approach involving an equivalent gauge length (EGL) and a gauge factor (GF). An analytical method is presented to determine EGL for converting elastic–plastic strain data based on the total cross-head deformation of the specimen. The GF values obtained, accounting for various initial geometries of the sample and strain-hardening exponents of the test material, show that, by neglecting elastic elongation, GF only depends on specimen geometries and strain-hardening exponents of the test material, being independent of the applied load, strain rate, and temperature. Validation through Finite Element (FE) simulation and miniaturized tensile tests (MTTs) with digital image correlation (DIC) has demonstrated the sound accuracy of the data conversion method, with the maximum GF errors below 4.82% for selected geometries. The proposed method holds significant implications for the design of MTPS, ductility correction, and comparative analysis of mechanical properties across samples with different dimensions.

Using miniature experiments to reveal strength gradients in battery casings

Complex metallic structures are often manufactured through multi-step forming or casting processes that induce severe mechanical property variations within the final part. Instead of using the virgin material properties to predict the final part performance, the local material properties after manufacturing need to be known. A novel comprehensive testing methodology is presented allowing the resolution of spatial gradients in the plasticity and fracture properties in metallic structures. It involves using a recently-developed miniature linear-motion system that probes the material within 2 mm wide gage sections (uniaxial, notched and central hole tension, in-plane shear). Additionally, a novel mini-bulge testing system is presented along with a mini-punch system to provide further insight into the local material response for biaxial loading conditions. A full testing campaign comprising 60 miniature samples is performed on all sides of a prismatic aluminum casing for Li-ion battery cells. The results demonstrate significant property variations with more than 30 % higher yield stresses for the side walls as compared to the bottom section. The miniature specimens allow identifying a location-dependent anisotropy, which would otherwise be missed by standard-sized samples. Furthermore, it is shown that the anisotropic Yld2000 plasticity model and the stress-state dependent Hosford-Coulomb fracture initiation model can be fully identified using results from experiments on miniature specimens only.

ASTM interlaboratory study on tensile testing of AM deposited and wrought steel using miniature specimens

An interlaboratory study, involving eigth international laboratories and coordinated by COMTES FHT (Czech Republic), was conducted to validate tensile measurements obtained using miniature specimens on additively manufactured (AM) components and artifacts. In addition to AM 316L stainless steel (316L SS), a wrought high-strength steel (34CrNiMo6V, equivalent to AISI 4340) was also used. Based on the results, a precision statement in accordance with ASTM E691 standard practice was developed, intended for inclusion in a proposed annex to the ASTM E8/E8M tension testing method. The primary outcomes of the study highlighted the agreement between yield and tensile strength measured from miniature and standard-sized tensile specimens. Furthermore, most tensile properties exhibited similar standard deviations, offering users insight into the efficacy of miniature specimen applications.

Incorporating surface roughness into numerical modeling for predicting fatigue properties of L-PBF AlSi10Mg specimens

Laser-powder bed fusion (L-PBF) is a popular additive manufacturing method for fabricating metal parts with complex geometries. However, one of the primary setbacks lies in the surface quality of the as-built components. Poor surface quality influences the dynamic fatigue properties of L-PBF parts. Experimental investigation of fatigue properties is time-intensive and expensive. Hence, computational modeling can be implemented to critically evaluate the impact of surface roughness on fatigue. In this work, a numerical modeling framework is developed that considers the influence of part-scale surface roughness on fatigue properties. To calibrate and validate the numerical modeling framework, mechanical investigations of miniature AlSi10Mg specimens are conducted in a custom-built tensile-fatigue testing apparatus. First, the tensile properties are evaluated to find out the reliability of the apparatus. Thereafter, the fatigue investigations of two sets of specimens are conducted: five specimens (FS1-FS5) for calibrating the numerical model and three specimens (VFS1-VFS3) for model validation. The numerical modeling framework involves the 3D reconstructed specimen geometries from computed tomography (CT) imaging of the VFS1-VFS3 specimens. The resultant 3D geometries are discretized using Ansys finite element software and analyzed to simulate the fatigue behavior. The numerical results of fatigue life and failure locations of the VFS1-VFS3 specimens are compared with the experimental observations. The comparison shows that the numerical results are within 5 % of the experimental observations. Additionally, the location of maximum strain localization in numerical modeling matches the crack initiation location. In conclusion, the numerical modeling can predict low cycle fatigue life and failure location of L-PBF AM specimens.

Modelling of crack propagation in miniaturized and normal SENB specimens based on local failure criterion

The use of miniaturized specimen testing methods is a promising way to solve the problem of limited materials in RPV monitoring programs. The use of miniature specimens allows the evaluation of fracture toughness from other specimen materials used. In particular, the small-size compact tensile test specimen (0.16T CT) is promising for the determination of fracture toughness, as it can be produced from the standard size Charpy specimen that has already been tested. However, if we have only 0.16T CT test, we cannot investigate the dimensional response and also have only one restricted deformation state, which may pose problems in verifying geometry independence and determining local parameters for state-of-the-art analyses. It is therefore recommended to prepare at least two tests with two different restricted deformation specimens. Therefore, the testing of mini single edge notched bending (SENB) is also required and can be worked out from the Charpy specimens. The paper presents the determination of fracture toughness for these miniaturized specimens by modifying the virtual crack closure technique (VCCT) simulation method using GTN parameters instead of energy release as the driving force. This allows the calculation of the J-integral to proceed in parallel with the crack propagation.

Identification of creep damage properties of coating via a compound miniaturized testing method and an inverse approach

A systematic analytical approach has been developed to comprehensively characterize the creep damage material properties of coatings on thin-layer substrates. This involves conducting creep tests using a compound, two-material, miniaturized thin plate specimen (MTPS) with an inverse approach. For demonstration, independent creep tests were performed on miniature specimens of the substrate (P91 steel) and the coating (CoNiCrAlY) at 650 °C, as well as on compound substrate-coating specimens. The reference stress method, coupled with finite element analysis, was utilized to obtain conversion parameters for strain data from the miniature specimen tests. Analytical solutions for the Kachanov creep damage model specific to the two-material substrate-coating system were adopted for inverse optimization. The MTPS testing method and the associated inverse approach have proven effective in accurately determining the complete three-stage creep constants within the coating-substrate system. Results obtained for the P91–CoNiCrAlY coated system have shown a clear demonstration of the accuracy and capability of the method in identifying the full sets of uniaxial creep damage properties, i.e. A, n, m, B, χ, and φ, provided the feasible experimental data are available.

Impact of titanium and silicon metal oxide nanoparticles on surface coatings for marine vehicles to mitigate biofouling

This work aimed to develop antifouling coatings for maritime structures and sailing vessels by the integration of nanoparticles as very effective biocidal agents. The paint compositions were created by combining several components with a binder known as linseed alkyd resin. The preparation of TiO2 and SiO2 nanoparticles was conducted by the ball milling technique, followed by their application as pigments in nano paints. The corrosion characteristics of these coatings were examined after the incorporation of the nano paint, to diminish fouling and enhance antibacterial efficacy on maritime vessels. The enhancement of antifouling paint efficacy is expected to be substantial as a result of the advancement in nanoparticle-based compositions that exhibit biocidal capabilities. To evaluate the efficacy of nanocoatings, miniature specimens were submerged in a marine environment for 120 days. The coated samples underwent analysis by various techniques including scanning electron microscopy, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction. Furthermore, an assessment was conducted to determine the efficacy of the protective characteristics exhibited by the coated tiny mild-steel samples. This evaluation involved subjecting the samples to a 120-day immersion in the ocean environment. The inclusion of SiO2 and TiO2 nanoparticles in the paints yields significant corrosion protection for the coated samples, in contrast to those lacking nanoparticles. Additionally, the latter exhibits superior anti-fouling properties.

Semi-automatic miniature specimen testing method to characterize the plasticity and fracture properties of metals

Miniature-testing is essential to characterize the plastic response of materials for which the extraction of conventional full-size specimens is impossible. Examples are weld regions with high property gradients or electronic circuit components. Here, we present the design of a novel testing system for miniature specimens. After inserting the specimens with wedge-shaped shoulders, the system carries out the clamping, initial geometry scanning, and mechanical testing with digital image correlation in an automated manner. The automation prevents the accidental damaging of the miniature specimens during manual handling and adds to the robustness of the overall procedure. It is shown that the experiments with miniature specimens extracted from DP600 steel and aluminum 7075-T6 are highly reproduceable. More importantly, they lead to the same plasticity and fracture properties as experiments on conventional ten-times larger full-size specimens. A correction procedure accounting for the surface roughness, white layer and heat affect zone induced through wire EDM is provided. In addition to developing and validating the new experimental technique, it is applied to characterize a 22MnB4 rod material and stainless steel 316 L foil.

Effects of crystallographic orientation and lamellar configuration on fatigue crack propagation in single-colony structures of Ti–6Al–4V alloy: Alternating shear crack growth vs. damage accumulation crack propagation

In this study, the fatigue crack propagation mechanisms in lamellar colonies of Ti–6Al–4V alloy were examined using miniature compact-tension specimens with a single-colony structure at the crack tip. Fatigue tests were performed on colonies with different α-phase crystallographic orientations and lamellar configurations with respect to the notch plane and direction, followed by post-fatigue metallographic analysis. Crack propagation occurs by three main mechanisms: 1) alternating shear due to in-plane prismatic slip, 2) damage accumulation via dislocation–dislocation interaction due to out-of-plane slip, and 3) interlamellar decohesion due to damage accumulation via lamellar interphase boundary–dislocation interaction. The slope of da/dN vs. ΔK is higher for alternating shear crack growth than for damage accumulation crack propagation via dislocation–dislocation interaction. This is due to an incubation period before substantive crack extension in the latter case, which is dominated by degree of strain accommodation associated with the activated slip systems. When the lamellar interphase boundaries are nearly perpendicular to the loading axis, the crack growth rates drastically increase by interlamellar decohesion. This is attributed to the reduced incubation period due to slip incompatibility at the interphase boundary where numerous crack nuclei were formed during damage accumulation process.

Influence of welding thermal cycles on properties of TMCP and Q&T steels evaluated by thermo-physical simulation

The welding process represents an unintentional, but unavoidable, heat treatment in the form of soft annealing or tempering, but also hardening during the cooling of the melt. Particularly in the case of high-strength fine-grained structural steels, this leads to critical states of the mechanical-technological properties of the base material. In order to investigate the influence of the heat input during welding on the resulting properties of the heat-affected areas, a thermo-physical simulation was carried out on a quenching and forming dilatometer Bähr DIL 805 A/D, considering low-alloyed quenched and tempered (Q&T) and low-alloyed thermo-mechanically controlled processed steels (TMCP) with yield strengths in the range of 500 to 960 MPa (S500MC, S700MC, S770QL, and S960QL). For this purpose, time–temperature cycles based on gas metal arc welding (GMAW) were simulated with different maximum temperatures (1200 °C; 1000 °C; 800 °C), representing the typical microstructural regions of the heat-affected zones (HAZ), and cooling times t8/5 (5 s; 12 s; 20 s; 25 s) on miniature tensile specimens. To evaluate the property changes of the characteristic HAZ, tensile tests, hardness measurements, and microstructural investigations were analyzed. The investigations illustrate the significant influence of heat input during the welding process on the resulting mechanical-technological properties and microstructure for both kinds of steel. It was demonstrated that all the steels investigated tend to soften with increasing cooling times. The investigated Q&T steels have a lower risk of falling below the strength of the untreated base material than the investigated TMCP fine-grained structural steels. The considerably pronounced softening also resulted in the minimum strength values not being achieved for certain cooling time ranges.

Miniature spatial transcriptomics for studying parasite-endosymbiont relationships at the micro scale

Several important human infectious diseases are caused by microscale-sized parasitic nematodes like filarial worms. Filarial worms have their own spatial tissue organization; to uncover this tissue structure, we need methods that can spatially resolve these miniature specimens. Most filarial worms evolved a mutualistic association with endosymbiotic bacteria Wolbachia. However, the mechanisms underlying the dependency of filarial worms on the fitness of these bacteria remain unknown. As Wolbachia is essential for the development, reproduction, and survival of filarial worms, we spatially explored how Wolbachia interacts with the worm’s reproductive system by performing a spatial characterization using Spatial Transcriptomics (ST) across a posterior region containing reproductive tissue and developing embryos of adult female Brugia malayi worms. We provide a proof-of-concept for miniature-ST to explore spatial gene expression patterns in small sample types, demonstrating the method’s ability to uncover nuanced tissue region expression patterns, observe the spatial localization of key B. malayi - Wolbachia pathway genes, and co-localize the B. malayi spatial transcriptome in Wolbachia tissue regions, also under antibiotic treatment. We envision our approach will open up new avenues for the study of infectious diseases caused by micro-scale parasitic worms.

A Comparative Investigation of Machine Learning Algorithms for Pore-Influenced Fatigue Life Prediction of Additively Manufactured Inconel 718 Based on a Small Dataset.

Fatigue life prediction of Inconel 718 fabricated by laser powder bed fusion was investigated using a miniature specimen tests method and machine learning algorithms. A small dataset-based machine learning framework integrating thirteen kinds of algorithms was constructed to predict the pore-influenced fatigue life. The method of selecting random seeds was employed to evaluate the performance of the algorithms, and then the ranking of various machine learning algorithms for predicting pore-influenced fatigue life on small datasets was obtained by verifying the prediction model twenty or thirty times. The results showed that among the thirteen popular machine learning algorithms investigated, the adaptive boosting algorithm from the boosting category exhibited the best fitting accuracy for fatigue life prediction of the additively manufactured Inconel 718 using the small dataset, followed by the decision tree algorithm in the nonlinear category. The investigation also found that DT, RF, GBDT, and XGBOOST algorithms could effectively predict the fatigue life of the additively manufactured Inconel 718 within the range of 1 × 105 cycles on a small dataset compared to others. These results not only demonstrate the capability of using small dataset-based machine learning techniques to predict fatigue life but also may guide the selection of algorithms that minimize performance evaluation costs when predicting fatigue life.

The high-throughput bridge to the rapid evaluation of fatigue reliability of structural engineering materials

A high-throughput strategy using miniature specimens to evaluate the ASTM-defined fatigue endurance limits of some engineering materials through a high-throughput symmetry bending cantilever beam fatigue testing system is proposed. Employing such a high-throughput testing method for examining some typical engineering materials, we reveal that the fatigue limits obtained by the traditional testing standard can be directly determined by the high-throughput method-obtained fatigue limit multiplied by a suitable conversion factor. Such a high-throughput method was validated theoretically by the proposed crack initiation model and experimentally by the F316 stainless steel specimens subjected to different aging treatments and Gamma-ray irradiation.

Novel miniature in situ hole expansion test coupled with microscopic digital image correlation.

The hole expansion ratio (HER) test is used to determine the stretch-flangeability of materials. Standard HER tests are performed on specimens sized a few tens of centimeters, termed macro-HER tests. This leads to significant material wastage due to the destructive nature of the tests. No information at the microstructure length scale is obtained, and the results suffer from user uncertainty in the identification of the through-thickness crack. This paper presents a novel miniature HER setup (termed micro-HER test), in which miniature specimens are tested inside a scanning electron microscope (SEM). The deformation is imaged from the top using the secondary electron detector installed in the SEM, coupled with the digital image correlation (DIC) technique, allowing for measurement of full field strains at the microstructural scale and identifying their deformation/fracture mechanisms. As a case study, six different steel grades were tested to measure their micro-HER values and compare them with the corresponding macro-HER values. The latter were found to be higher for the more ductile grades of steel. Late detection of through-thickness cracks and thicker samples leading to a higher volume of plastic deformation could contribute to this overestimation of values in macro-HER tests. DIC results from micro-HER tests on a ferrite-martensite (10% volume fraction) dual-phase steel showed high magnitudes of strain localization at the ferrite-martensite interfacial regions, indicating that such interfaces might be hotspots for failure under triaxial stress states. The challenges and errors associated with the measurements are also discussed.