5 Werkstofftechnik
Filtern
Dokumenttyp
- Vortrag (122)
- Zeitschriftenartikel (71)
- Beitrag zu einem Tagungsband (24)
- Forschungsdatensatz (21)
- Posterpräsentation (20)
- Buchkapitel (7)
- Dissertation (4)
- Forschungsbericht (4)
- Sammelband (Herausgeberschaft für den kompletten Band) (3)
- Monografie (1)
Sprache
- Englisch (228)
- Deutsch (49)
- Französisch (1)
Schlagworte
- Ontology (34)
- Creep (27)
- Microstructure (23)
- Additive manufacturing (21)
- LCF (16)
- Additive Manufacturing (14)
- Degradation (13)
- Fatigue (13)
- Ti-6Al-4V (13)
- Aluminium (11)
Organisationseinheit der BAM
- 5.2 Metallische Hochtemperaturwerkstoffe (278) (entfernen)
Paper des Monats
- ja (1)
The influence of prestraining on the aging response of an Al-Cu-Li alloy is investigated by preparation of different strain states (3 %, 4 %, 6 %) of the initial aging state. The Brinell hardness of the subsequently aged samples (up to 60 h aging time) was measured and it was found that the increasing dislocation concentration in the 3 different initial states leads to faster hardness increases and slightly higher maximum hardness.
An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies.
In this study an approach for dressing metallic bonded honing stones with hard cutting grains on the basis of electrolysis is investigated. By a combination of concepts from electrochemical machining (ECM) and electropolishing a test rig was designed and put into operation. In general, it can be stated that the Approach investigated in this paper has proved to be a suitable dressing method for honing stones. However, the dressing result is highly dependent on bond components, cutting grain size and concentration which lead to local differences in the material removal and irregular topographies. This could be overcome, for example, by setting the dressing parameters more precisely based on the best results presented in this paper.
Despite of the significant advances in AM process optimization there is still a lack of experimental results and understanding regarding the mechanical behavior and microstructural evolution of AMparts, especially in loading conditions typical for safety-relevant applications e.g. in the aerospace or power engineering. Within the scope of the presented investigations, a characterization of the fatigue behavior of additively manufactured Ti-6Al-4V in the low cycle fatigue regime was carried out in the range of 0.3 to 1.0 % strain amplitude at room temperature, 250°C and 400°C. The Ti-6Al-4V specimens are machined out of lean cylindrical rods, which were fabricated using powder laser metal deposition (LMD) with an improved build-up strategy. The improved strategy incorporates variable track overlap ratios to achieve a constant growth in the shell and core area. The low-cycle-fatigue behavior is described based on cyclic deformation curves and strain-based fatigue life curves. The lifetimes are fitted based on the Manson-Coffin-Basquin relationship. A characterization of the microstructure and the Lack-of-Fusion (LoF)-defect-structure in the as-built state is performed using optical light microscopy and high-resolution computed tomography (CT) respectively. The failure mechanism under loading is described in terms of LoF-defects-evolution and crack growth mechanism based on an interrupted LCF test with selected test parameters. After failure, scanning electron microscopy, digital and optical light microscopy and CT are used to describe the failure mechanisms both in the longitudinal direction and in the cross section of the specimens. The fatigue lives obtained are comparable with results from previous related studies and are shorter than those of traditionally manufactured (wrought) Ti-6Al-4V. In this study new experimental data and understanding of the mechanical behavior under application-relevant loading conditions (high temperature, cyclic plasticity) is gained. Furthermore, a better understanding of the role of LoFdefects and AM-typical microstructural features on the failure mechanism of LMD Ti-6Al-4V is achieved.
Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts
(2019)
This work aims for an yield function description of additively manufactured (AM) parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures.
EBSD/CT-Scans from in-house additively manufactured specimen extract the unique microstructural topology which is converted to a representative volume element (RVE) with grain structure and crystal orientations.
Crystal plasticity model parameters on this RVE are calibrated and validated by means of mechanical testing under different texture angles. From virtual experiments on this RVE, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation.
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.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to Low Cycle Fatigue (LCF) tests at operating temperature (300°C), the microstructure (phases, crystallographic texture, and grain morphology), the mesostructure (defect shape and distribution), and subsurface RS on the LCF samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
Grain boundary energy effect on grain boundary segregation in an equiatomic high-entropy alloy
(2020)
Grain boundary (GB) Segregation has a substantial effect on the microstructure evolution and properties of polycrystalline alloys. The mechanism of nanoscale segregation at the various GBs in multicomponent alloys is of great challenge to reveal and remains elusive so far. To address this issue, we studied the GB segregation in a representative equiatomic FeMnNiCoCr high-entropy alloy (HEA) aged at 450 °C. By combining transmission Kikuchi diffraction, atom probe tomography analysis and a density-based thermodynamics modeling, we uncover the nanoscale segregation behavior at a series of well-characterized GBs of different characters. No segregation occurs at coherent twin boundaries; only slight nanoscale segregation of Ni takes place at the low-angle GBs and vicinal \Sigma 29b coincidence site lattice GBs. Ni and Mn show cosegregation of high levels at the general high-angle GBs with a strong depletion in Fe, Cr, and Co. Our density-based thermodynamic model reveals that the highly negative energy of mixing Ni and Mn is the main driving force for nanoscale cosegregation to the GBs. This is further assisted by the opposite segregation of Ni and Cr atoms with a positive enthalpy of mixing. It is also found that GBs of higher interfacial energy, possessing lower atomic densities (higher disorder and free volume), show higher segregation levels. By clarifying the origins of GB segregations in the FeMnNiCoCr HEA, the current work provides fundamental ideas on nanoscale segregation at crystal defects in multicomponent alloys.
Additively manufactured metallic materials have already started to find application in safety-relevant components. However, this has only happened for certain materials and specific applications and loading conditions, since there is still an extensive lack of knowledge as well as of historical data regarding their mechanical behaviour. This contribution aims to address this lack of understanding and historical data concerning the creep behaviour of the austenitic stainless steel 316L manufactured by Laser-Powder-Bed-Fusion (L-PBF) and the low-cycle-fatigue behaviour of the titanium alloy Ti-6Al-4V manufactured by Laser-Metal-Deposition (LMD). Furthermore, it aims to assess their mechanical behaviour against their conventional counterparts. With that in mind, specimens from conventional and additive materials are tested and their mechanical behaviour analysed based on characteristic curves. To understand the damage behaviours the materials are characterized by destructive and non-destructive techniques before and after failure.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
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.
Eine kritische Aufgabe im Rahmen der Etablierung von Prozess-Struktur-Eigenschafts-Performance-Beziehungen bei der additiven Fertigung (AM) von Metallen ist die Ermittlung von zuverlässigen und gut dokumentierten Kennwerten zum Materialverhalten sowie das Schaffen von Wissen über die Struktur-Eigenschafts-Korrelation. Schließlich ist dies die Grundlage für die Entwicklung gezielterer Prozessoptimierungen und zuverlässigerer Lebensdauer-Vorhersagen. In diesem Zusammenhang zielt dieser Beitrag darauf ab, Daten und Erkenntnisse über das Kriechverhalten des austenitischen Edelstahls 316L zu liefern, der mittels Laser-Powder-Bed-Fusion (L-PBF) hergestellt wird. Um dieses Ziel zu erreichen, wurden Proben aus konventionellem warmgewalztem sowie AM-Material gemäß den bestehenden Normen für konventionelles Material geprüft und vor und nach dem Versagen mikrostrukturell charakterisiert. Die Probekörper wurden aus einzelnen Blöcken des AM-Materials gefertigt. Die Blöcke wurden mit einer Standard-Scan- und Aufbaustrategie hergestellt und anschließend wärmebehandelt. Das Kriechverhalten wird anhand der Kriechlebensdauer und ausgewählter Kriechkurven und Kennwerte beschrieben und vergleichend bewertet. Der Einfluss von Defekten und Mikrostruktur auf das Materialverhalten wird anhand von zerstörenden und zerstörungsfreien Auswertungen an ausgewählten Proben analysiert. Der AM-Werkstoff zeigt kürzere Kriechlebensdauern, erreicht das sekundäre Kriechstadium deutlich schneller und bei geringerer Dehnung und weist eine geringere Kriechduktilität im Vergleich zu seinem konventionellen Gegenstück auf. Das Kriechschädigungsverhalten des AM-Werkstoffs ist eher mikrostruktur- als defektgesteuert und ist durch die Bildung intergranularer Kriechrisse gekennzeichnet. Als kritische Merkmale werden die Versetzungsdichte sowie die Versprödung der Korngrenzen identifiziert. Die Mikro-Computertomographie (µCT) erweist sich als Alternative zur Metallographie, um die Kriechschädigung zu analysieren.
Die Erzeugung von Erneuerbaren Energien unterliegt starken Schwankungen, die von konventionellen Kraftwerken ausgeglichen werden müssen, um das Stromnetz stabil zu halten. Für die konventionellen Kraftwerke bedeutet dies eine zunehmend zyklische Fahrweise, die zu häufigeren Last- und Temperaturwechseln führt. Von den eingesetzten Werkstoffen fehlen Daten zum Verhalten unter zyklischer Fahrweise. Ziel dieser Arbeit ist es daher, für P92, einen als Rohrleitungswerkstoff eingesetzten hochwarmfesten Stahl, zu untersuchen, welche Auswirkungen zyklische Fahrweisen auf die Schädigungsprozesse und Lebensdauern haben.
Da durch den zyklischen Betrieb eine verstärkte Schädigung durch Ermüdungsprozesse zu erwarten ist, wurden dehnungskontrollierte isotherme (LCF) und nicht-isotherme (TMF) Ermüdungsversuche mit und ohne Haltezeit bei verschiedenen Temperaturen bzw. Temperaturintervallen durchgeführt. Mit den Haltezeitversuchen soll dabei das Kriech-Ermüdungs-Verhalten untersucht werden. Bei den TMF-Versuchen wurde zusätzlich die Temperaturrate variiert, um näher an den realen Lastwechselgeschwindigkeiten zu prüfen. Schließlich wurden auf Basis der durchgeführten LCF- und TMF-Versuche betriebsnahe Versuchsprozeduren entwickelt, um unterschiedliche Betriebsmodi in einem Versuch abzubilden.
Die durchgeführten mechanischen Versuche stellen eine umfangreiche Basis zu Ermüdungsdaten an P92 dar. Neben der Abhängigkeit der Lebensdauer von Temperatur, Temperaturintervall und –rate, sowie Dehnung und Haltezeit, konnte auch das Entfestigungsverhalten genauer charakterisiert werden. Sowohl Haltezeiten als auch das Reduzieren der Temperaturrate können die Lebensdauer erheblich verringern. Dabei kommt es gerade bei vermeintlich kleinen Dehnungen, bei denen die Streckgrenze nur leicht überschritten wird, zu einer Lebensdauerreduzierung. Haltezeiten verstärken zudem die zyklische Entfestigung. Die fraktographische Analyse der Proben hat ergeben, dass es keinen direkten Zusammenhang zwischen der Entfestigung und der Bildung von Nebenrissen gibt. Stattdessen zeigen EBSD- und TEM-Untersuchungen, dass es zur Bildung einer Subkornstruktur kommt und die Entfestigung auf dem Verschwinden von Kleinwinkelkorngrenzen beruht. Während bei den LCF-Proben eine reine Ermüdungsschädigung vorliegt, konnte bei einigen TMF-Proben eine kriechdominierende Schädigung nachgewiesen werden. Die betriebsnahen Zyklen zeigen, dass sich mit den durchgeführten Versuchen das reale Betriebsverhalten gut abschätzen lässt. Da es jedoch auch Parameterkombinationen gibt, bei denen keine Änderung des Entfestigungs- und Lebensdauerverhaltens auftritt, sollte genau bekannt sein, welche Belastungen in einem Bauteil auftreten.
Die Eigenschaften verschiedener Werkstoffe werden behandelt und typische Werkstoffkennwerte angegeben. Es werden Arten der Beanspruchung von Bauteilen und Werkstoffen vorgestellt, die diese in technischen Anwendungen unterworfen sind. Im Betrieb von Bauteilen kann Materialschädigung und unter Umständen auch Versagen eintreten. Mögliche Mechanismen und Ursachen werden erläutert und Einblicke in die Methodik der Schadensanalyse gegeben.
Systematic microstructure design requires reliable thermodynamic descriptions of each and all microstructure elements. While such descriptions are well established for most bulk phases, thermodynamic assessment of microstructure defects is challenging because of their individualistic nature. In this paper, a model is devised for assessing grain boundary thermodynamics based on available bulk thermodynamic data. We propose a continuous relative atomic density field and its spatial gradients to describe the grain boundary region with reference to the homogeneous bulk and derive the grain boundary Gibbs free energy functional. The grain boundary segregation isotherm and phase diagram are computed for a regular binary solid solution, and qualitatively benchmarked for the Pt–Au system. The relationships between the grain boundary's atomic density, excess free volume, and misorientation angle are discussed. Combining the current density-based model with available bulk thermodynamic databases enables constructing databases, phase diagrams, and segregation isotherms for grain boundaries, opening possibilities for studying and designing heterogeneous microstructures.
Die Werkstoffklassen
(2020)
Es werden die vier Werkstoffklassen Metalle, Keramiken, Polymere und Verbundwerkstoffe sowie ihre Untergruppen vorgestellt. Die metallischen Werkstoffe umfassen die Eisen- wie die Nichteisenwerkstoffe und ihre Legierungen. Neben den Ingenieurkeramiken werden auch Glas und Glaskeramik, Naturstoffe und Erdstoffe sowie Baustoffe behandelt.
Mit der Initiative MaterialDigital fördert das BMBF seit dem letzten Jahr ein wichtiges Instrument zur Digitalisierung der Materialwissenschaft und Werkstofftechnik in Deutschland. In der ersten Phase dieser Initiative wird seit Juli 2019 die Plattform MaterialDigital von einem Konsortium aufgestellt. Ziel dieser Plattform ist der Aufbau eines virtuellen Materialdatenraums, um zusammen mit allen Interessenten die Systematisierung des Umgangs mit Werkstoffdaten voranzutreiben. In einer zweiten Phase werden akademische F&E-Projekte voraussichtlich Anfang 2021 gefördert. In jedem dieser Projekte wird an einer konkreten Fragestellung das Themenfeld „Digitalisierung der Materialwissenschaft und Werkstofftechnik“ adressiert und multidisziplinär bearbeitet. In einer dritten Phase werden im Rahmen industriegeführter vorwettbewerblicher Verbundprojekte mit der gleichen Zielsetzung gefördert.
Segregation to grain boundaries affects their cohesion, corrosion, and embrittlement and plays a critical role in heterogeneous nucleation. In order to quantitatively study segregation and low-dimensional phase separation at grain boundaries, here, we apply a density-based phase-field model. The current model describes the grain-boundary thermodynamic properties based on available bulk thermodynamic data, while the grain-boundary-density profile is obtained using atomistic simulations. To benchmark the performance of the model, Mn grain-boundary segregation in the Fe–Mn system is studied. 3D simulation results are compared against atom probe tomography measurements conducted for three alloy compositions. We show that a continuous increase in the alloy composition results in a discontinuous jump in the segregation isotherm. The jump corresponds to a spinodal Phase separation at grain boundary. For alloy compositions above the jump, we reveal an interfacial transient spinodal phase separation.
The transient spinodal phenomenon opens opportunities for knowledge-based microstructure design through the chemical manipulation of grain boundaries. The proposed density-based model provides a powerful tool to study thermodynamics and kinetics of segregation and phase changes at grain boundaries.
A γ-analogue of the superalloy CMSX-4 that does not contain the strengthening γ′ -phase and only consists of the γ-solid solution of nickel has been designed, solidified as single-crystals of different orientations, and tested under creep conditions in the temperature range between 1150 and 1288 °C. The tests have revealed a very high creep anisotropy of this alloy, as was previously found for CMSX-4 at supersolvus temperature of 1288 °C. This creep anisotropy could be explained by the dominance of 〈011〉{111} octahedral slip. Furthermore, the analysis of the creep data has yielded a high value of the creep activation energy, Qc≈442 kJ/mol, which correlates with the high activation energy of Re diffusion in Ni. This supports the hypothesis that dislocation motion in the γ-matrix of Re-containing superalloys is controlled by the diffusion of the Re atoms segregating at the dislocation core. The Norton stress exponent n is close to 5, which is a typical value for pure metals and their alloys. The absence of γ′ -reprecipitation after high-temperature creep tests facilitates microstructural investigations. It has been shown by EBSD that creep deformation results in an increasing misorientation of the existing low angle boundaries. In addition, according to TEM, new low angle boundaries appear due to reactions of the a/2 〈011〉 mobile dislocations and knitting of new networks.
Due to the diversity of materials and the processes associated with their production and use, the complexity of the lifecycles of materials and the multitude of academic and industrial researchers participating in generation of data for material design impose a huge challenge. The topical goal of digitalizing materials and processes can only be adequately addressed by consolidating the efforts of all stakeholders in this field. There are many scattered activities, but there is a demand for an elimination of redundancies as well as an advance in acceptance and a common basis in the digitalization of materials. Furthermore, data analysis methods play an important role in both, the experimental and simulation-based digital description of materials, but they have been poorly structured so far.
Therefore, the two joint projects Platform Material Digital (PMD, materialdigital.de) and Materials open Laboratory (Mat-o-Lab, matolab.de) aim to contribute to a standardized description of data processing methods in materials research. Besides stimulating the formation of a collaborative community in this respect, their main technical goals are the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications. In this regard, data management in accordance with the FAIR (findability, accessibility, interoperability, reuseability) principles is addressed. There is a common agreement in the scientific community following current discussions that data is supposed to be conform to these principles. This includes storage, processing and querying of data in a preferably standardized form.
To meet the challenge to contextualize material data in a way that is consistent with all stakeholders, all necessary information on the condition of the material including production and application-related changes have to be made available via a uniform, machine-readable description. For this purpose, ontologies are to be used since they allow for machine-understandable knowledge representations and conceptualizations that are needed for data management and the digitalization in the field of materials science.
As first efforts in PMD and Mat-o-Lab, application ontologies are created to explicitly describe processes and test methods. Thereby, the well-known tensile test of metals at room temperature was described ontologically in accordance with the respective ISO standard 6892-1:2019-11.
The efforts in creating this tensile test application ontology are shown in this presentation. Especially, the path of ontology development based on standards to be pursued is focused, which is in accordance with the generic recommendations for ontology development and which is supposed to be exemplary for the creation of other application ontologies.
Thermal cycling of a Ni-excess NiTi alloy was conducted between 50 °C and liquid nitrogen temperature to induce martensitic transformations and to reverse them after. The starting point was an annealed and slowly cooled state, the end point a sample thermally cycled 1500 times. Positron annihilation lifetime spectra and Coincidence Doppler Broadening profiles were obtained in various states and at various tem- peratures. It was found that the initial state was low in defects with positron lifetimes close to that of bulk NiTi. Cycling lead to a continuous build-up of a defect structure up to 20 0 −50 0 cycles after which saturation was reached. Two types of defects created during cycling were identified, namely pure dislo- cations and vacancies attached to dislocations.
The phase-like behavior of grain boundaries (GBs), recently evidenced in several materials, is opening up new possibilities in the design of alloy microstructures. In this context, GB phase diagrams are contributing to a predictive description of GB segregation and (interfacial) phase changes. The influence of chemo-mechanical solute-GB interactions on the GB phase diagram remains elusive so far. This is particularly important for multi-component alloys where the elastic interactions among solute atoms, of various sizes and bonding energies, can prevail, governing a complex co-segregation phenomenon. Recently, we developed a density-based model for GB thermodynamics that intrinsically accounts for GB elasticity in pure elements. In this work, we incorporate the homogeneous and heterogeneous elastic energies associated with the solutes into the density-based framework. We derive the multi-component homogeneous elastic energy by generalizing the continuum misfitting sphere model and extend it for GBs. The density-based free energy functional directly uses bulk CALPHAD thermodynamic data. The model is applied to binary and ternary Al alloys. We reveal that the elastic energy can profoundly affect the GB solubility and segregation behavior, leading to Cu segregation in otherwise Cu-depleted Al GBs. Consequently, GB segregation transition, i.e., a jump in the GB segregation as a function of alloy composition, is revealed in Al-Cu and Al-Cu-Mg alloy systems with implications for subsequent GB precipitation in these alloys. CALPHAD-informed elasticity-incorporated GB phase diagrams enable addressing a broader range of GB phenomena in engineering multi-component alloys.
Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated.
Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance.
The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures. To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF). Tensile specimens were machined from these AM bulk materials for three different inclinations: 0◦, 45◦, and 90◦ relative to the build plate. Dynamic Young’s modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography (μCT), and texture analysis with electron backscatter diffraction (EBSD). These investigations revealed that the specimens exhibited near full density and the detected defects were spherical. Furthermore, the residual stresses in the loading direction were between −74 ± 24 MPa and 137 ± 20 MPa, and the EBSD measurements showed a preferential ⟨110⟩ orientation parallel to the build direction. A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture.
Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) should contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications.
Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused.
Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) is supposed to contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications.
Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts within the joint project PMD in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused. Furthermore, the presentation includes a live demonstration of queries possibly performed to query data that was uploaded in the PMD triple store.
The discovery of the high entropy concept at the beginning of the 3rd millennium lead to a worldwide increase in metallurgical research, as the possible element combinations seemed nearly endless and the range of applications wide. In the early years of research, one of the main goals was the discovery of a single-phase high entropy alloy. As research evolved, it was found that properties could be enhanced by opening the HE-concept towards multiphase alloys, and from the wide area of possibilities our group chose a tuning of the properties towards high temperature application.
Compositionally complex Al10Co25Cr8Fe15Ni36Ti6 alloy, which is single-phase at high temperature, around 1200°C, shows a three phase morphology at intermediate temperatures, around 800°C. A high temperature homogenization procedure has to be applied in order to decrease the segregation induced by the dendritic growth. Subsequent annealing promotes the formation of the strengthening γ' precipitates. The alloy shows a positive lattice misfit between the γ and the γ' phase, which can be an indicator for good creep properties.
The microstructure can be optimized by adding trace elements such as Mo and Hf, known as γ and γ' strengtheners in Ni-based superalloys, respectively. Atom probe measurements show that Mo segregates into the γ matrix, and Hf prefers the γ' precipitates, where it increases the lattice parameter and thus also the lattice misfit, by about 50%. The alloy family shows interesting mechanical properties, especially the Al9.5Co25Cr8Fe15Ni36Ti6Hf0,5 alloy – its tensile properties are better than those of commercial Alloy 800H and IN617 at temperatures up to 700°C.
For more than half a century, spinodal decomposition has been a key phenomenon in considering the formation of secondary phases in alloys. The most prominent aspect of the spinodal phenomenon is the lack of an energy barrier on its transformation pathway, offering an alternative to the nucleation and growth mechanism. The classical description of spinodal decomposition often neglects the influence of defects, such as grain boundaries, on the transformation because the innate ability for like-atoms to cluster is assumed to lead the process. Nevertheless, in nanocrystalline alloys, with a high population of grain boundaries with diverse characters, the structurally heterogeneous landscape can greatly influence the chemical decomposition behavior. Combining atom-probe tomography, precession electron diffraction and density-based phase-field simulations, we address how grain boundaries contribute to the temporal evolution of chemical decomposition within the miscibility gap of a Pt-Au nanocrystalline system. We found that grain boundaries can actually have their own miscibility gaps profoundly altering the spinodal decomposition in nanocrystalline alloys. A complex realm of multiple interfacial states, ranging from competitive grain boundary segregation to barrier-free low-dimensional interfacial decomposition, occurs with a dependency upon the grain boundary character.
The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures.
To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF).
Tensile specimens were machined from these AM bulk materials for three different inclinations relative to the build plate. Dynamic Young's modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography, and texture analysis with electron backscatter diffraction (EBSD). A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture.
This presentation shows some experimental results of the characterization of the creep behavior of LPBF 316L, which has been poorly studied and understood to date. The presentation includes results regarding the mechanical properties, the initial microstructural state and its evolution under loading, and the damage mechanism. This work was done within the BAM focus area materials project AGIL. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant was also tested.
Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results are used for selecting the optimal technological parameters such as applied pressure and processing time
Manufacturing defects, high residual stress (RS), and microstructures affect the structural integrity of laser powder bed fusion (LPBF) Ti-6Al-4V. In this study, the individual effect of these factors on fatigue performance at elevated temperature (300 °C) was evaluated. Material in as-built condition and subjected to post-processing, including two heat treatments and hot isostatic pressing, was investigated. It was found that in the absence of tensile RS, the fatigue life at elevated temperature is primary controlled by the defects; and densification has a much stronger effect than the considered heat treatments on the improvement of the mechanical performance.
Results of an extended TMF test program on grade P92 steel in the temperature range of 620 °C - 300 °C, comprising in-phase (IP) and out-of-phase (OP) tests, partly performed with symmetric dwells at Tmax/Tmin, are presented. In contrast to previous studies, the low-strain regime is also illuminated, which approaches flexible operation in a power plant with start/stop cycles. At all strain amplitudes, the material performance is characterized by continuous cyclic softening, which is retarded in tests at lower strains but reaches similar magnitudes in the course of testing. In the investigated temperature range, the phase angle does not affect fatigue life in continuous experiments, whereas the IP condition is more detrimental in tests with dwells. Fractographic analyses indicate creep-dominated and fatigue-dominated damage for IP and OP, respectively. Analyses of the (micro)hardness distribution in the tested specimens suggest an enhanced microstructural softening in tests with dwell times for the low- but not for the high-strain regime. To rationalize the obtained fatigue data, the fracture-mechanics-based D_TMF concept, which was developed for TMF life assessment of ductile alloys, was applied. It is found that the D_TMF parameter correlates well with the measured fatigue lives, suggesting that subcritical growth of cracks (with sizes from a few microns to a few millimeters) governs failure in the investigated range of strain amplitudes.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model.
It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and ΔCTOD value.
Systematic microstructure design requires reliable thermodynamic descriptions and phase diagrams of each and all microstructure elements. While such descriptions are well established for most bulk phases, thermodynamic assessment of crystal defects is greatly challenged by their individualistic aspects. In this talk, we present a density-based thermodynamic concept to describe defects based on available bulk thermodynamic data. Here dealing with grain boundaries (GBs), we apply this concept to compute GB (phase) diagram. Applications to segregation engineering of GBs in bulk and nanocrystalline alloys will be presented. We further develop this model to include the effect of elastic interactions due to atom size mismatch and obtain the corresponding GB (phase) diagram for the ternary Al-Cu-Li system.
Interfacial Spinodals
(2021)
Despite their finite spatial extent, interfaces can have profound impacts on microstructure properties. This is because of their distinct phase-like properties distinguishing them from the adjacent homogeneous bulk structure. When noticed by solute atoms, interfaces can experience their own chemical phase changes. In this talk, we investigate the constrained states of chemically decomposed phases at interfaces. A density-based theory of interfaces is proposed to describe the confined chemical decomposition at general grain boundaries. Here the grain boundary is viewed as a lesser dense, defected structure with reference to the corresponding bulk structure. Using this picture, the thermodynamic origins of interfacial spinodal phenomena are revealed. We also show that transient interfacial spinodals can be activated over a large alloy composition range, enabling kinetic engineering of interfacial chemistry.
From molecular dynamics simulations and the capillary fluctuation method, the solid-liquid interfacial free energy has been computed for the B2-liquid interface in the Cu-Zr system. Consistent with previous results for the FCC-liquid interface in Cu-Zr and Al-Sm but atypical of most alloys, was found to increase as the temperature is lowered. In addition, the temperature dependence was obtained for model Lennard-Jones B2-liquid alloys. In all cases the unusual temperature dependence of is correlated with an atomic structure of the interfacial region characterized by a misalignment of the number density peaks between solvents and solutes. In cases where the number density peaks are aligned, the typical temperature dependence is observed. The results are discussed in terms of the Gibbs theory of the thermodynamics of interfaces. It is proposed that the unique interfacial structure and the atypical temperature dependence of are hallmarks of an easy glass forming alloy.
Iron aluminides depict a sustainable and light-weight material class which could be employed in many applications requiring high strength at intermediate to high temperatures. According to first results, the alloy Fe-26Al-4Mo-0.5Ti-1B surpasses conventional materials in wet corrosion resistance and creep resistance up to 650 °C. For these reasons, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated to transfer these findings into a standardised materials dataset and to derive best practices for processing. In the first place, a set of different microstructures adjusted by varying casting methods, wall thicknesses and heat treatments was investigated and correlated with hardness on macro and micro scale. Correlations were drawn between solidification rates and resulting grain sizes and hardness. The effect of vacancy hardening was only verified for wall thickness as low as 2.5 mm. Moreover, a common decrease of macrohardness after a heat treatment at 1000 °C for 100 h was observed irrespective of casting process or wall thickness. This effect was linked with an unexpected decrease of the complex boride phase fraction which acts as a hardening phase.
Die Digitalisierung von Materialien und Prozessen stellt eine große Herausforderung dar, die nur durch eine Bündelung der Bemühungen aller Beteiligten in diesem Bereich erreicht werden kann. Bei einer derartigen digitalen Beschreibung spielen Datenanalysemethoden, eine Qualitätssicherung von Prozessen inklusive Input- und Output-Daten sowie die Interoperabilität zwischen Anwendungen nach den FAIR-Prinzipien eine wichtige Rolle. Dies umfasst das Speichern, Verarbeiten und Abfragen von Daten in einer vorzugsweise standardisierten Form (Beteiligung von Normungsgremien).
Zur Bewältigung dieser Herausforderung ist eine mit allen Stakeholdern konsistente Kontextualisierung der Materialdaten anzustreben, d.h. alle erforderlichen Informationen über den Zustand des Materials einschließlich produktions- und anwendungsbezogener Änderungen müssen über eine einheitliche, maschinenlesbare Beschreibung verfügbar gemacht werden. Dazu werden Wissensrepräsentationen und Konzeptualisierungen ermöglichende Ontologien verwendet. Eine zentrale Betrachtungsweise in diesem Zusammenhang ist die Realisierung von (automatisierten) Datenpipelines, die eine Beschreibung und Verfolgung von Daten ausgehend von ihrer Erzeugung, bspw. in einem Messgerät, bis zu ihrer globalen Verwendung in möglicherweise verschiedenen Kontexten beinhalten.
Erste Bemühungen und Ansätze zu diesen Problemstellungen führten im Projekt Innovations-Plattform Material Digital (PMD, materialdigital.de) zur Erstellung von Anwendungsontologien, die Prozesse und Testmethoden explizit beschreiben. Dabei wurde u.a. der Zugversuch an Metallen bei Raumtemperatur nach ISO 6892-1 ontologisch beschrieben. Diese als Beispiel dienende Ontologieentwicklung wird in dieser Präsentation vorgestellt. Weiterhin wurde, ausgehend von der domänenspezifischen Entwicklung von Anwendungsontologien, eine Kernontologie erstellt, die eine übergeordnete Verbindung von ontologischen Konzepten aufgrund der Verwendung gleichen Vokabulars und semantischer Verknüpfungen erlaubt. Diese sowie die das PMD-Projekt selbst werden ebenfalls in dieser Präsentation vorgestellt.
The Gibbs free energy of a grain boundary is a complex thermodynamic function of temperature, pressure, and composition. These complexities add to the intrinsic crystallographic and chemical constraints imposed by the adjacent bulk phase. Recently we have proposed a density-based model for assessing grain boundary thermodynamics that enables a CALPHAD-informed description of the grain boundary. As such, the Gibbs free energy of the grain boundary is directly linked with available CALPHAD thermodynamic data. In this talk, new aspects of interfacial segregation and phase transformation are revealed by benchmarking the current model for various experimental cases, including several steels, high-entropy alloys and aluminum alloys. The effects of elastic interactions on the grain boundary segregation and the application of the model to a nanocrystalline Pt-Au alloy, with numerous grain boundaries of various characters, will be discussed.
Zur Bewältigung der Herausforderung bei der Digitalisierung von Materialien und Prozessen ist eine mit allen Stakeholdern konsistente Kontextualisierung von Materialdaten anzustreben, d.h. alle erforderlichen Informationen über den Zustand des Materials einschließlich produktions- und anwendungsbezogener Änderungen müssen über eine einheitliche, maschinenlesbare Beschreibung verfügbar gemacht werden. Dazu werden Wissensrepräsentationen und Konzeptualisierungen ermöglichende Ontologien verwendet. Erste Bemühungen in den beiden Projekten Plattform Material Digital und Materials-open-Laboratory führten zur Erstellung von Anwendungsontologien, die Prozesse und Testmethoden explizit beschreiben. Dabei wurde u.a. der Zugversuch an Metallen bei Raumtemperatur nach DIN EN ISO 6892-1 ontologisch beschrieben. Diese als Beispiel dienende Ontologieentwicklung wird in dieser Präsentation vorgestellt.
Porosity in single-crystal nickel-base superalloys is removed by hot isostatic pressing (HIP) at temperatures above gamma’-solvus where the material is very soft and ductile. For example, single-crystal nickel-base superalloy CMSX-4 is HIPed at temperature 1288 °C, which is slightly higher than the gamma’-solvus temperature of this alloy equal to about 1280 °C. It is assumed that pore shrinking during HIP is mostly due to dislocation creep. Such a modelling of HIP of CMSX-4 was started in our group on the base of results of creep tests of [001] single-crystals at 1288 °C [1]. However, it was found later [2] that the alloy CMSX-4 shows very strong creep anisotropy at 1288 °C. Therefore, for calibration of the creep law, creep tests of different orientations under different stress levels are required at the HIP temperature. This was the main task of present work. Single-crystals of CMSX-4 of axial orientations [001], [011], [123] and [111] were cast by VIAM Moscow and tested by BAM Berlin under creep conditions at 1288 °C and stress levels between 4 MPa and 16 MPa. At all stress levels, the creep rate increases by an order of magnitude when changing the orientation from [001] to [111] with [011] and [123] orientations in between. Such a character of creep anisotropy corresponds to the orientation dependence of the Schmid factor for octahedral glide.
The crystal viscoplasticity model developed in [1] was improved to better represent the time induced softening observed during creep. The creep tests for different stresses and orientations as well as pore closure were simulated. The results of pore closure simulation are compared with measurements of porosity decrease during Hiping.