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Paper des Monats
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Alkali-silica reaction (ASR) is a chemical reaction within concrete which can lead over time to cracking and spalling. Due to the complexity of the problem, it still causes damage to concrete constructions worldwide.
The publication aims to illustrate the interdisciplinary research of the German Federal Institute for Materials Research and Testing (BAM) within the last 20 years, considering all aspects of ASR topics from the macro to the micro level. First, methods for characterization and assessment of ASR risks and reaction products used at BAM are explained and classified in the international context. Subsequently the added value of the research approach by combining different, preferably nondestructive, methods across all scales is explained using specific examples from a variety of research projects. Aspects covered range from the development of new test-setups to assess aggregate reactivity, to analysis of microstructure and reaction products using microscopical, spectroscopical and X-ray methods, to the development of a testing methodology for existing concrete pavements including in-depth analysis of the visual damage indicator and the de-icing salt input using innovative testing techniques. Finally, research regarding a novel avoidance strategy that makes use of internal hydrophobization of the concrete mix is presented.
Since the BSE signal depends on many factors, like the chemistry of the phase and the acceleration voltage, the size and position of the detector array is (slightly) different from phase to phase so that an (iterative) post-processing of the stored patterns is highly recommended. The derived BSE signal can be used for phase assignment in high resolution and high speed maps when EBSD fails and/or EDS (energy dispersive spectroscopy) needs too much time for a suitable and parallel signal acquisition.
The understanding of process-microstructure-property-performance (PMPP) relationships in additive manufacturing (AM) of metals is highly necessary to achieve wide-spread industrial application and replace conventionally manufactured parts, especially regarding safety-relevant applications. To achieve this understanding, reliable data and knowledge regarding material’s microstructure-property relationships (e.g. the role of defects) is needed, since it represents the base for future more targeted process optimizations and more reliable calculations of performance. However, producing reliable material data and assessing the AM material behaviour is not an easy task: big challenges are e.g. the actual lack of standard testing methods for AM materials and the occasional difficulties in finding one-to-one comparable material data for the conventional counterpart.
This work aims to contribute to end this lack of reliable material data and knowledge for the low cycle fatigue behaviour of the most used titanium alloy in aerospace applications (Ti-6Al-4V). For this purpose, two sets of test specimens were investigated. The first set was manufactured from cylindrical rods produced by an optimized DED-L process and the second was manufactured from a hot formed round bar. The test specimens were cyclically loaded until failure in the low-cycle-fatigue (LCF) regime. The tests were carried out according to ISO 12106 between 0.3 to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behaviour is described and compared between materials and with literature values based on cyclic deformation curves and strain-based fatigue life curves. Besides, the parameters of Manson-Coffin-Basquin relationship were calculated. The microstructures (initial and after failure) and fracture surfaces were comparative characterized. Thereby, the focus lied on understanding the role of grain morphology and defects on the failure mechanisms and fatigue lifetimes. For this latter characterization, optical microscopy (OM), scanning electron microscopy (SEM) and micro computed tomography (µCT) were used.
In Additive Manufacturing everybody is talking about Free Form, Unconventional Design, Re-thinking Components, “Think out of the box”.
However, there are a few outstanding question: a) What are the material properties ? They certainly differ from literature values for conventional materials; b) How about the microstructure? It is different from conventional materials. Does it stay so with ageing? How does it form? c) Do we properly take residual stress into account? We often blame them for our ignorance about failure scenarios. d) Do we apply tailored heat treatments? Very often, we follow conventional schedules…
This talk describes the summary of the efforts carried out within the BAM Project AGIL.
At BAM, we aimed to thoroughly investigate the microstructure and how it evolves as a function of load and temperature (service), to determine the material properties after different process and service conditions, to properly determine residual stress and the way it impacts mechanical properties and component performance, to properly quantify the impact of (unavoidable?) defects, and to determine heat treatments tailored to the process-specific material (stress relieve, microstructure homogenization etc.).
The Project AGIL was and is intimately coupled with the project ProMoAM, dealing with online monitoring of AM processes.
The roles of microalloying niobium, titanium and vanadium for controlling austenite grain growth, microstructure evolution and hardness were investigated at different simulated heat affected zones (HAZ) for high strength low alloy (HSLA) S690QL steel. High resolution FEG-SEM has been used to characterize fine bainitic ferrite, martensite and nanosized second phases at simulated coarse and fine grain HAZs. It was found that for Ti bearing steel (Ti/N ratio is 2) austenite grain had the slowest growth rate due to the presence of most stable TiN. The fine cuboidal particles promoted intragranular acicular ferrite (IGF) formation. Nb bearing steel exhibited relatively weaker grain growth retardation compared with titanium bearing steels and a mixed microstructure of bainite and martensite was present for all simulated HAZs. IGF existed at coarse grain HAZ of Ti+V bearing steel but it was totally replaced by bainite at fine grain HAZs. Hardness result was closely related to the morphology of bainitic ferrite, intragranular ferrite and second phases within ferrite. The microstructure and hardness results of different simulated HAZs were in good agreement with welded experimental results.
Avoid living dangerously: non-destructive characterization of AM parts from powder to end-of-life
(2019)
The freeform and the revolutionary design possibilities offered by additive manufacturing have skyrocketed the amount of optimization studies in the realm of engineering, and metallic additive manufactured parts are becoming a reality in industry.
Not surprisingly, this has not been paralleled by a similar enthusiastic wave in the realm of materials science, and still very little is known about AM materials properties. This has the consequence that, typically, conventional materials properties are still used in design and even in simulations.
lt is necessary to dig a lot deeper than at present, in order to understand these new materials classes, and in particular their microstructure and their intemal stresses, largely different from their cast or wrought companions.
The goal of the Special Issue “Brittle Materials in Mechanical Extremes” was to spark a discussion of the analogies and the differences between different brittle materials, such as, for instance, ceramics and concrete. Indeed, the contributions to the Issue spanned from construction materials (asphalt and concrete) to structural ceramics, reaching as far as ice. The data shown in the issue were obtained by advanced microstructural techniques (microscopy, 3D imaging, etc.) and linked to mechanical properties (and their changes as a function of aging, composition, etc.). The description of the mechanical behavior of brittle materials under operational loads, for instance, concrete and ceramics under very high temperatures, offered an unconventional viewpoint on the behavior of brittle materials. This is not at all exhaustive, but a way to pave the road for intriguing and enriching comparisons.
Alkali silica reaction (ASR) is a major concrete durability problem resulting in significant maintenance and reconstruction costs for concrete infrastructures all over the world. To determine whether an aggregate is potentially reactive, accelerated concrete tests are used. Aim of this study is the chemical and microstructural characterization of ASR-products formed under the performance conditions of motorway pavements and during subsequent tests on the remaining ASR susceptibility. Samples were taken from concrete motorway pavements. Some of the samples already showed first indications for beginning damages whereas others showed deteriorations only after applying a performance testing procedure for the estimation of future risk of ASR damage. In a first step ASR-products were identified by polarized light microscopy in thin sections. The reaction products where then analyzed by Raman Spectroscopy and finally the chemical composition of the ASR-products was identified by SEM with EDX.
The results indicate that most reaction products show an increasing Ca/Si-ratio with progressive crack length. If an ASR-product develops inside an aggregate and moves through the cement paste, it has a high (Na+K)/Si-ratio at the beginning which decreases with increasing distance from its place of origin. The Raman spectra of the ASR-products are characterized by two broad bands indicating specific Q-species of different amorphous gel networks. Within the scope of the analysis distinctions in the microstructure and the chemical composition of the ASR-gels were detected relating to various conditions of accelerated testing.
Characterization of Ti-6Al-4V fabricated by multilayer laser powder-based directed energy deposition
(2022)
Laser powder-based directed energy deposition (DED-L) is increasingly being used in additive manufacturing (AM). As AM technology, DED-L must consider specific challenges. It must achieve uniform volume growth over hundreds of layers and avoid heat buildup of the deposited material. Herein, Ti–6Al–4V is fabricated using an approach that addresses these challenges and is relevant in terms of transferability to DED–L applications in AM. The assessment of the obtained properties and the discussion of their relationship to the process conditions and resulting microstructure are presented. The quality of the manufacturing process is proven in terms of the reproducibility of properties between individual blanks and with respect to the building height. The characterization demonstrates that excellent mechanical properties are achieved at room temperature and at 400 °C.
A study was made on the effect of creep loading on the precipitate radii evolution of the aluminum alloy 2618A.
The overageing process of the alloy was investigated under load at a temperature of 190 °C with stresses between 79 and 181 MPa and compared to stress free isothermal ageing. The precipitates responsible for strength were characterized using dark-field transmission electron microscopy (DFTEM). This allows the experimental Determination of radii distributions of the rod-shaped Al2CuMg precipitates and the evaluation regarding their mean precipitate radius. It was found that the mean precipitate radius enables the comparison of the different microstructural conditions of crept and uncrept samples. The mean precipitate radii of the samples experiencing creep are significantly higher than those of undeformed samples. It was shown that the acquired radii distributions are viable to determine averaged particle radii for comparison of the aged samples. A ripening process including pipe diffusion along dislocations describes the data on coarsening very well for the creep samples.
Composite Facade Elements with Self-Cleaning Surface made of Ultra-High-Performance Concrete (UHPC)
(2020)
In the framework of the European project H-House various concrete façade elements were developed with the aim to ensure a long service life by combining a very durable material with self-cleaning properties. The façade elements presented are made of a shell of UHPC filled with blocks of aerated autoclaved concrete as insulating material. Self-cleaning properties were realized amongst others by imprinting a microstructure into the surface during casting. The paper focuses on selected technological aspects of the manufacturing process of prototypes which had to be performed in two concreting sections. Furthermore the challenges faced when upscaling the self-cleaning properties are addressed and the strategy to assess the self-cleaning properties by measuring the contact and the roll-off angel is presented. The results show that a successfull upscalaing process requires detailed planning and that the best results can often be achieved with a moderate work effort or material use.
Composite Facade Elements with Self-Cleaning Surface made of Ultra-High-Performance Concrete (UHPC)
(2020)
In the framework of the European project H-House various concrete façade elements were developed with the aim to ensure a long service life by combining a very durable material with self-cleaning properties. The façade elements presented are made of a shell of UHPC filled with blocks of aerated autoclaved concrete as insulating material. Self-cleaning properties were realized amongst others by imprinting a microstructure into the surface during casting. The paper focuses on selected technological aspects of the manufacturing process of prototypes which had to be performed in two concreting sections. Furthermore the challenges faced when upscaling the self-cleaning properties are addressed and the strategy to assess the self-cleaning properties by measuring the contact and the roll-off angel is presented. The results show that a successfull upscalaing process requires detailed planning and that the best results can often be achieved with a moderate work effort or material use.
Copolymer structure elucidation by multidimensional techniques with focus on UPLC x ESI-TOF-MS
(2017)
Structure elucidation of complex synthetic copolymers still represents a challenge. An one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Herein a new approach is demonstrated to provide evidence of different functionalities and short block sequences in statistical EO-PO copolymers. Furthermore silsesquioxane mixtures and Polyglycerols are investigated concerning occurring topology effects.
Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L
(2020)
A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage.
The development of refractory CCAs has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy, which resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. The aim of this work is to evaluate the alloy’s mechanical behavior under tension in the temperature range 800-1000°C, by applying creep tests under vacuum (excluding oxidation effects). Some little temperature influence on minimum creep rate @ 1000 and 1100 °C was found and at a first glance, and Norton plots shows that deformation is probably both diffusion and dislocation controlled. However, further work is needed to stablish deformation and degradation micro mechanisms in the studied creep regime.
Damage tolerance counts as one of the most widespread approach to fatigue assessment and surely as one of the most promising in understanding the process-structure-property-performance relationships in additively manufactured metallic materials. Manufacturing defects, surface roughness, microstructural features, short and long crack fatigue propagation, residual stresses and applied loads can be taken into consideration in a fracture mechanics-based fatigue assessment. Many aspects are crucial to the reliable component life prediction. Among those a prominent role is played by an accurate measurement and modelling of the short crack fatigue behavior, and reliable statistical characterization of defects and residual stresses.
This work aims at addressing the issues related to both experimental testing, fatigue and fatigue crack propagation, and fracture mechanics-based modelling of fatigue lives. Examples will be provided on an additively manufactured AISI 316 L.
Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen.
Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation.
At high temperatures and in harsh environments ceramic springs are often superior to metallic ones and allow for innovative solutions. A further application was proposed by using ceramic springs as capacitive force sensor. Lower and upper coil surfaces are coated by electrically conducting layers. Deformation of such spring results in a change of capacity. Sensor application calls for helical springs with rectangular cross-section, a linear stress-strain characteristic over entire deformation range and low manufacturing tolerances relating to inner and outer diameter, coil cross section and spring pitch. Furthermore, complex spring design with integrated connecting elements has to be realized.
Alumina, zirconia (Y-TZP) and silicon nitride springs were produced by hard machining starting from sintered hollow cylinders. After external and internal cylindrical grinding the hollow cylinders were filled with hard wax, followed by multi-stage cutting of spring coils with custom-made cutting discs. Finally, hard wax was removed by melting and burnout. Best surface and edge qualities of springs were reached using Y-TZP material and hot isostatic pressed alumina. Y-TZP springs produced with material-specifically selected cutting discs and optimized process parameters show sharp coil edges without spallings and mean roughness values of inner surfaces < 0.2 μm. Manufacturing tolerances of spring diameters, spring pitch, height and width of coil cross section are in the range of ± 10 microns. Good reproducibility of spring geometry by optimized hard machining technology allows for production of Y-TZP springs with spring constants differing less than ± 1 % within a series.
According to DIN 2090 spring constant for rectangular coil cross section is proportional to the square of height and width of coil cross section and indirectly proportional to number of active coils and to the cube of the mean spring diameter. Hence, spring constants can be tailored over a range of many orders of magnitude by changing the spring dimensions. Good agreement was reached between calculated target spring constants and measured values on produced springs.
Alumina and zirconia springs were characterized relating to deformation behavior under dynamic compression load with various deformation speeds and under static tensile loads over long periods of time. Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs was proved in both test series. It is supposed, that pseudoelasticity caused by stress-induced transformation of tetragonal to monoclinic phase is responsible for this special feature of TZP springs. Therefore, TZP material cannot be used for capacitive spring sensors.
Additive Manufacturing by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts as compared to the traditional subtractive manufacturing strategies. However, the residual stresses (RS) developed during the processing can reduce the load bearing capacity as well as induce unwanted distortion, limiting the application of SLM parts. In the present work, residual stresses in additivly manufactured IN718 part were analised by means of neutron diffraction and synchrotron X-ray diffraction.
Dissimilar metal TIG weld joints of multiple principal element alloys (MPEA) to austenitic steel 304
(2023)
Multi-element alloys (MPEA - Multiple Principal Element Alloys) represent a new class of materials consisting of at least three alloying elements, each with 5 to 35 atomic %. This material class includes high-entropy alloys (HEA, with n ≥ 4 elements). The underlying alloying concept differs fundamentally from conventional materials such as the Fe-based steel. For this purpose, the alloying elements are specifically selected, and the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. The aim is to identify highly innovative MPEA with individually adjustable properties for industrial applications. In the last 20 years, however, the focus has been on pure material synthesis. With the increase in available material quantities, the focus is on processing issues such as joining and welding processes. In that connection, the weldability of MPEAs has received very little attention so far. Experience with dissimilar metal welds (DMWs) is completely lacking but is essential for the application of these materials if joint to conventional materials. This study presents selected experimental results on the weldability of MPEA-DMWs and the resulting microstructures. For this purpose, the equiatomic CoCrFeMnNi (HEA) was investigated in cold-rolled (CR) and heat-treated (HT) condition and joined by tungsten inert gas (TIG) welding to an austenitic stainless steel 304. The DMWs showed defect-free conditions (no lack of fusion, cracks and so on), whereas the cold-rolling increases the microhardness. The global mechanical properties were obtained by instrumented tensile tests of cross-weld samples and showed sufficient yield and tensile strength comparable to that of the individual base materials (BM). The local strain conditions were determined by digital image correlation and showed the highest local strains to occur in the intermixed weld metal. Indeed, the preferred fracture location of the cross-weld tensile samples was in the weld metal. Finally, the experiments proofed the weldability of the MPEAs to conventional 304. This enables targeted further considerations for example as structural materials.
Pre-Inca civilizations like the coastal cultures Moche and Nazca (Early Intermediate) and the inland culture Wari (Middle Horizon) were agrarian societies which supported indigenous elites of impressive wealth, power, and organization. With the expansion of the Wari Empire, the polychrome style and technique of Nazca propagated to the other cultures. High status burials, most of the Late Moche Fine Line ceramics and a large corpus of ceramics with Wari-derived decoration have been recovered in San José de Moro since 1991. The degree of transfer of procedures in this highly interactive scenario is of special interest: is there a limitation to decoration or is it adopted by the local potters also regarding the formulation of the ceramic bodies? In this context the relative amount, size and type of incorporated non-plastic inclusions as temper are important.
Ni-base superalloy single crystals have been used in turbine blades for hot sections of gas turbines for over four decades. In order to increase the efficiency of the turbines, a continuous increase in the inlet temperature of combustion gases into the turbine has driven the design of turbine blades to complicated shapes and the presence of a complex pattern of cooling channels. These three-dimensional shapes, together with the inhomogeneous distribution of stresses along the blade, induce an also complicated triaxial stress state, which does not compare to uniaxial tests that are performed to characterize high temperature properties such as creep. A round notch on a test piece represents a simple configuration that generates a quasi-isostatic stress state across the notch. In the present contribution, the effect of a sharp round notch on the microstructural micromechanisms within the notched region cylindrical bars, loaded along [001] at 1020 °C and 160 MPa net stress, is studied. To this end, a series of interrupted creep tests is conducted on plain and notched bars and the microstructure is compared. Results are discussed in terms of degree microstructural coarsening, and dislocation activity. The effect of notch generation via grinding is also discussed in these terms. The presence of carbides evolving in from residual carbon is also shown and discussed. .Funding by the German Research Association (DFG) [grant number AG 191/1] is acknowledge
High‐temperature corrosion was studied under multiple chemical loads on ferritic‐austenitic model alloys (Fe–13Cr, Fe–18Cr–12Ni, and Fe‐25Cr–20Ni) with KCl deposit under 0.5% SO2/99.5% Ar gas atmosphere at 560°C. Postexposure characterization was done by X‐ray diffraction and scanning electron microscopy. In a pure SO2/Ar environment a protective Cr2O3 scale was formed by all samples. The introduction of KCl deposits causes the scale to be nonprotective and multilayered, consisting of CrS, FeS, Cr2O3, Fe3O4, and Fe2O3. The impact of the microstructure and alloying elements is discussed.
The present research work encloses results of experimental investigations of the interaction between welding process parameters for laser-beam and hybrid-laser-arc as well as type of the filler metal and the achievable mechanical properties of the weld joints on steel grade X8Ni9+QT640 for cryogenic service containing 9% nickel. The results obtained contribute to the development and conversion in the industrial practice a new laser beam-based welding technology for the automated manufacturing of facilities for the liquefaction, storage and the transport of natural gases (LNG facilities). The results show, that the martensitic microstructure of the laser weld metal including low amount of retained austenite not exceeding 3.5% leads to the relatively low V-notch impact energy. The remarkable heterogeneity in the chemical composition of the weld metal through the weld thickness could be recognized in the case of hybrid-laser-arc welding with ERNiCrMo-3 austenitic filler metal, what also led to insufficient impact toughness of the weld metall. The most promising results could be achieved by using 11%Ni filler wire, which is similar to the base metal and provides a homogeneous microstructure with uniform distribution of Ni through the weld seam. It is remarkable, that a correlation between Charpy impact toughness and wire feeding speed and respectively process heat input exists. The highest toughness values were 134±58 J at -196C. The both laser as well as laser-hybrid welds passed the tensile test. The failure stress of 720±3 MPa with a fracture location in the base material was achieved for all samples tested.
Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation.
A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity.
Evaluation of high spatial resolution imaging of magnetic stray fields for early damage detection
(2017)
The paper discusses the evaluation of elastic and plastic strain states in two low-carbon steels of the same steel group with high spatial resolution GMR (giant magneto resistance) sensors. The residual stress distributions of tungsten inert gas welded plates were determined by means of neutron diffraction as a reference. The normal component of local residual magnetic stray fields arise in the vicinity of the positions of maximum stress. The experiments performed on flat tensile specimen indicate that the boundaries of plastic deformations are a source of stray fields. The spatial variations of magnetic stray fields for both the weld and the tensile samples are in the order of the earths magnetic field.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer wise additive manufacturing process which provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative strain-free reference for the material of interest. In this presentation advancements in the field of diffraction-based residual stress analysis of L-PBF Inconel 718 will be presented. The choice of an appropriate set of diffraction-elastic constants depending on the underlying microstructure will be described.
The influence of heat input and welding speed on the microstructure and mechanical properties of single-pass hybrid laser arc welded 20mm thick plates of high-strength pipeline steel X120 were presented. The heat Input was varied in the range of 1.4 kJ mm−1 to 2.9 kJ mm−1, while the welding speed was changed between 0.5m min−1 and 1.5m min−1. A novel technique of bath support based on external oscillating electromagnetic field was used to compensate the hydrostatic pressure at low welding velocities. A major advantage of this technology is, that the welding speed and thus the cooling time t8/5 can be variated in a wide parameter window without issues regarding the weld root quality. The recommended welding thermal cycles for the pipeline steel X120 can be met by that way. All tested Charpy-V specimens meet the requirements of API 5 L regarding the impact energy. For higher heat inputs the average impact energy was 144 ± 37 J at a testing temperature of −40 °C. High heat Input above 1.6 kJ mm−1 leads to softening in the weld metal and heat-affected-zone resulting in loss of strength. The minimum tensile strength of 915 MPa could be achieved at heat inputs between 1.4 kJ mm−1 and 1.6 kJ mm−1.
Spectacular failure cases of fossil power stations in the recent years exhibited severe cracking in T24 welds. The results show that hydrogen-assisted cracking up to 200 °C cannot be excluded. Hence, it is important to gain a basic understanding on how hydrogen might affect the basic material properties in the respective weld microstructures. The present study focuses on hydrogen degradation of the respective weld microstructures, i.e., the weld metal and the coarse grained heat affected zone, where actually cracking appeared in practice. Tensile tests were carried out for coarse grain heataffected zone (CGHAZ) and the weld metal in uncharged and electrochemically hydrogen-charged condition. It turned out that both microstructures show distinct tendency for gradual degradation of mechanical properties in the presence of increasing hydrogen concentration. Already for a hydrogen concentration about and above 2 ml/100 g Fe, a significant ductility reduction has been observed. SEM investigations revealed that the fracture topography changes from ductile topography in uncharged condition to intergranular topography for the CGHAZ and to ductile-brittle mix for the weld metal (WM) in hydrogen charged condition. Ti-rich inclusions were identified as central regions of quasi-cleavage fracture areas in the WM. An approximation procedure is applied to quantify the degradation intensity.
Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen
concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room
temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments
revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot
be excluded, and hydrogen removal should be done before PWHT.
9 %-Cr steel P91 is widely used in power plants due to the excellent creep-resistance. Components of this steel are typically welded and demand for careful welding fabrication, whereas a so-called post weld heat treatment (PWHT), must be conducted to increase the toughness and decrease the hardness of the martensitic as-welded (AW) microstructure. Before the PWHT, a hydrogen removal (or dehydrogenation) heat treatment is necessary as hardened AW martensitic microstructure is generally prone to delayed hydrogen assisted cracking (HAC). The microstructure and temperature dependent hydrogen diffusion is an important issue as it determines how long a potential crack-critical hydrogen concentration could remain in the microstructure. In this context, reliable hydrogen diffusion coefficients of P91 weld metal are rare. Hence, the diffusion behavior of P91 multi-layer weld metal was investigated in two different microstructure conditions: AW and further PWHT (760 °C for 4 h). Two different experimental techniques were used to cover a wide range of hydrogen diffusion temperatures: the electrochemical permeation technique (PT) at room temperature and the carrier gas hot extraction (CGHE) for a temperature range from 100 to 400 °C. From both techniques typical hydrogen diffusion coefficients were calculated and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences in hydrogen diffusivity. The biggest deviations were identified for room temperature. In this case, the AW condition shows significant hydrogen trapping and up to seven times lower diffusion coefficients. Additionally, PT investigations showed a preferred diffusion direction of hydrogen in the weld metal expressed by the diffusion coefficients and the permeability for both heat treatment conditions. The CGHE generally revealed lower diffusion coefficients for the AW microstructure up to 200 °C. In addition, the AW condition showed hydrogen concentrations up to 50 ml/100 g (considering electrochemical charging). Nonetheless, this hydrogen was not permanently (reversibly) trapped. Nonetheless, this temperature is approximately 100 °C below recommended dehydrogenation heat treatment (DHT). This has two main consequences: (I) in case of welding is interrupted or no DHT is conducted, a HAC susceptibility of hardened martensitic P91 weld metal cannot be excluded and (II) DHT can be conducted at temperatures around 200 °C below the recommended temperatures.
Hydrogen-assisted cracking is a critical combination of local microstructure, mechanical load and hydrogen concentration. Welded microstructures of low-alloyed creep-resistant Cr-Mo-V steels show different hydrogen trapping kinetics. This influences the adsorbed hydrogen concentration as well as the diffusion by moderate or strong trapping. A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens
were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. Finally, realistic temperature assessment is mandatory for calculation of activation energy via TDA.
In general, hydrogen assisted cracking is a result of a critical combination of local microstructure, mechanical load and hydrogen concentration. In that connection, welded microstructures of low-alloyed creep-resistant steels can show different hydrogen trapping kinetics. That influences the adsorbed hydrogen concentration as well as the diffusion itself in terms of moderate or strong trapping. A common approach to describe trapping is by the activation energy that is necessary to release hydrogen from a specific trap site. In the present study, T24 base material and weld metal were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis(TDA) with linear heating using a mass spectrometer. The results showed a microstructure effect on hydrogen trapping kinetics at elevated temperatures. Additionally, it is necessary to monitor the specimen temperature. A comparison between idealized temperature profile and real specimen temperature showed that the calculated activation energy varied up to a factor of two. Thus, the assigned trap character(moderate or strong) changed. In case of high temperature peaks, this effect could be more important compared to the microstructure effect itself.
During their life span, concrete structures interact with many kinds of external mechanical loads. Most of these loads are considered in advance and result in reversible deformations. Nevertheless, some of the loads cause irreversible, sometimes unnoticed changes below the macroscopic scale depending on the type and dimension of the impact. As the functionality of concrete structures is often relevant to safety and society, their condition must be known and, therefore, assessed on a regular basis. Out of the spectrum of non-destructive monitoring methods, Coda Wave Interferometry using embedded ultrasonic sensors is one particularly sensitive technique to evaluate changes to heterogeneous media. However, there are various influences on Coda waves in concrete, and the interpretation of their superimposed effect is ambiguous. In this study, we quantify the relations of uniaxial compression and uniaxial tension on Coda waves propagating in normal concrete. We found that both the signal correlation of ultrasonic signals as well as their velocity variation directly reflect the stress change in concrete structures in a laboratory environment. For the linear elastic range up to 30% of the strength, we calculated a velocity variation of −0.97‰/MPa for compression and 0.33%/MPa for tension using linear regression. In addition, these parameters revealed even weak irreversible changes after removal of the load. Furthermore, we show the time-dependent effects of shrinkage and creep on Coda waves by providing the development of the signal parameters over time during half a year together with creep recovery. Our observations showed that time-dependent material changes must be taken into account for any comparison of ultrasonic signals that are far apart in time. The study’s results demonstrate how Coda Wave Interferometry is capable of monitoring stress changes and detecting even small-size microstructural changes. By indicating the stated relations and their separation from further impacts, e.g., temperature and moisture, we anticipate our study to contribute to the qualification of Coda Wave Interferometry for its application as an early-warning system for concrete structures.
The porosity and the surface roughness are recently discussed problems for SLM parts. The influence of SLM process parameters on porosity is well studied for different materials. Nevertheless, the build angle (i.e. the angle between part orientation and build plate) needs to be understood as an additional SLM process parameter, as it has been shown, that the microstructure and hence the mechanical performance of various materials depend on the build angle. The inherent build angle of each strut as a part of a lattice structure is the motivation to investigate the influence of the build angle on the porosity and roughness on round-shaped (1 mm diameter) struts by means of CT. Conventional Coordinate Measuring Machine (CMM) has the limitation towards small and round shaped samples. The need for Computed Tomography (CT) regarding investigations of SLM parts will increase because no other non-destructive technique allows the assessment of complex geometries with inner laying surfaces. We used CT to assess the pores and the strut surface. Seven struts out of the nickel alloy Inconel 625 with build angles from 30° to 90° were studied. It was found that the number of pores is smaller, and the size of pores is larger for the 90° strut. In case of 30° strut, the number of pores is increased towards down-skin side, additionally, this strut orientation showed to have the largest number of attached powder particles. The elongated pores exist exclusively near the strut surface. While the roughness at the down-skin surface is highly depending of the biud angle, the roughness at the up-skin surface is the same for all struts. The mechanisms of pore and surface roughness formation is not mainly driven by gravity.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2017)
Additive Manufacturing (AM) by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts in comparison to the traditional subtractive manufacturing strategies. Developing during the manufacturing process, residual stresses may limit the application of SLM parts by reducing the load bearing capacity as well as induce unwanted distortion depending on the boundary conditions specified in manufacturing.
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
Due to its matrix/γ′ structure, the compositionally complex alloy (CCA) Al10Co25Cr8Fe15Ni36Ti6 has excellent properties that fulfill the requirements for a high-temperature material. This base alloy is alloyed with small amounts of high melting elements to a further improvement of its properties, which results in different shapes, fractions and sizes of the two phases γ′ and Heusler after various homogenization and annealing steps. By correlating this microstructure with time independent and dependent mechanical properties, conclusions can be drawn about the effects of the individual phases. The needle-shaped Heusler-phase leads to bad mechanical behavior if its phase fraction is too high. A fraction below 3 vol% is not critical in tensile tests, but it reduces the creep resistance compared to a purely two-phase matrix/γ′-alloy. Sharp-edged cubic γ′-particles and a coarse Heusler-phase without sharp edges in case of the base alloy with 0.5 at.% hafnium lead to the best tensile and creep properties in the high temperature range. At 750 °C, the Hf-containing alloy clearly outperforms two commercially used alloys in the targeted area of application when it comes to creep resistance.
Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component.
In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. In parallel, using X-ray computed tomography we also observe that porosity is mainly concentrated in the contour region, except in case where the laser speed is small. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process.
Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is
associated with the primary phases.
Three high strength Nb-, Ti- and Ti+V- bearing S690QL steels were welded to investigate and compare the effects of microalloy addition on HAZ toughness. Charpy V notch impact tests from three microalloyed welds under different cooling rates have been performed. Fractographic examination shows that several factors including large-sized grain, upper bainite or hard second phase, interact to determine the brittle fracture mode and impaired toughness of Nb bearing weld at high heat input. In contrast to this reduced toughness, Ti bearing welds exhibits satisfied toughness regardless of at a fast or slow cooling rate as a result of limited austenite grain and refined favourable intragranular acicular ferrite structure. Moreover, in the case of such refined structure as matrix, TiN particles are found to be irrelevant to the fracture process and crystallographic misorientation results also confirms that high angle boundaries between fine ferrites plates provide much effective barrier for crack propagation and contribute to improved toughness.
This study investigated the effect of incorporating three types of nanosilica (NS), two powders, and one colloidal suspension on the hydration, strength, and microstructure of calcium sulfoaluminate (CSA) cement pastes prepared with and without a superplasticizer (SP). X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy (SEM), and compressive strength tests were performed after 2, 5, and 28 days of hydration. The results showed that both NS powders delayed cement hydration at an early age, which was attributed to particle agglomeration (confirmed by dynamic light scattering). Whereas well-dispersed colloidal NS did not significantly affect the hydration of CSA at the investigated ages. SP incorporation improved the dispersion of CSA cement particles, resulting in a 10% increase in the degree of hydration of ye’elimite at 28 days for the system without NS. Conversely, when the SP was incorporated in NS-containing mixtures, it hindered cement hydration of the systems with powdered NS, but did not significantly affect the cement hydration of the system containing colloidal NS. The SEM images suggested that the SP changed the ettringite morphology, thereby negatively affecting the mechanical strength of the CSA pastes.
AlSi10Mg is one of the most applied alloys for laser powder bed fusion (LPBF) technology, due to its great possibilities for implementing new lightweight concepts such as in automotive industries. For the component design it is necessary to know about the mechanical properties and the mechanical behaviour. The many published strength properties of LPBF processed AlSi10Mg show significant differences up to approximately 225 MPa in ultimate tensile strength (UTS) and 195 MPa in yield strength (YS). To understand these varying properties, a ring trial was carried out manufacturing specimens on 6 LPBF machines with different parameters and build-up strategies. They were studied in the as-built (AB) condition and after heat treatment at 300 °C for 30 min, respectively. For examining the mechanical properties, tensile tests and hardness measurements were carried out. The microstructure was characterized by optical light microscopy (OM), field emission scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). The identified differences in strength properties were discussed based on the 4 strengthening mechanism known for metallic materials and at the background of material defects. It was found that the size of the typical sub-cell structure of LPBF AlSi10Mg affected substantially the mechanical properties in the AB condition, in which with decreasing sub-cell size strength increased. If heat treatment was applied, the strength properties decreased and did not differ anymore. Since annealing led to coarsened sub-cells, whereas the grains itself did not change in size, the influence of sub-cell structure on strength was further confirmed. In addition, acicular precipitates in the AB condition were observed at specimens from one LPBF machine showing the lowest tensile elongation.
This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction.
Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields.
Ultra high performance concrete (UHPC) is characterised by its high compressive strength of more than 120 MPa and its high durability. With thermal treatment at 90°C, hydration is accelerated and a strength comparable to the 28-day strength can be achieved immediately after the treatment. In applying Optimum process conditions, the strength can be even further increased by up to 30%. Previous Research showed that thermal treatment can lead to inhomogeneities in form of a visible zonation within the cross-section, if the UHPC is not protected sufficiently from desiccation. This led to the question, to what extent the related changes in mechanical properties, microstructure and phase composition are of relevance for the performance of the UHPC. First investigations of small specimens thermally treated without protection exhibited a decrease of compressive strength, indicating that the zonation aspect requires further research.
In this study the zonation of UHPC treated thermally at 90°C is investigated after applying four different procedures of treatment and curing in comparison. The samples are characterized with respect to their chemistry, mineral composition and microstructure to allow an assessment on durability and strength development, with focus on potential depth dependent changes associated with the zonation.
The measurements reveal the formation of a visible zonation in case of unprotected treatment, if followed by immersion in water. The compressive strength is not significantly impaired, but a decrease in bending strength gives reason for concern. Further results allow clear correlation with changes in pore structure, whereas the interpretation of relationships with phase distribution, degree of hydration, microchemistry is more complex and therefore, provides only partial clarification.
Ultra high performance concrete (UHPC) is characterised by its high compressive strength of more than 150 MPa and its high durability. Due to thermal treatment at 90°C a strength comparable to the 28-days-strength can be achieved immediately after the treatment and in some cases can be even further increased up to 30 %. The explanations for the increase in strength are the accelerated hydration of the clinker minerals and the intensified pozzolanic reaction contributing to a denser microstructure and hence, a high performance in compressive strength.
Former research shows that thermal treatment can lead to inhomogeneities in form of a visible zonation within the cross-section. The width of the margin increases with shorter pre-storage time before the thermal treatment and with omitting protective measures against desiccation during the treatment. Specimens exhibiting a zonation typically show a lower compressive strength compared to the undisturbed reference whereas changes in chemistry, mineral content and microstructure were not reported in detail.
In this study the zonation of thermally treated UHPC is investigated with respect to its chemistry, mineral composition and microstructure to allow predictions on durability and strength development. Measurements show a change in pore sizes, minerals phase composition and element distribution leading to the visible zonation and weaker bending tensile strength compared to the reference.