RESUMEN

The importance of cryopreservation in tissue engineering is unceasingly increasing. Preparation, cryopreservation, and storage of tissue-engineered constructs (TECs) at an on-site location offer a convenient way for their clinical application and commercialization. Partial freezing initiated at high sub-zero temperatures using ice-nucleating agents (INAs) has recently been applied in organ cryopreservation. It is anticipated that this freezing technique may be efficient for the preservation of both scaffold mechanical properties and cell viability of TECs. Infrared thermography is an instrumental method to monitor INAs-mediated freezing of various biological entities. In this paper, porous collagen-hydroxyapatite (collagen-HAP) scaffolds were fabricated and characterized as model TECs, whereas infrared thermography was proposed as a method for monitoring the crystallization-related events on their partial freezing down to -25 °C. Intra- and interscaffold latent heat transmission were descriptively evaluated. Nucleation, freezing points as well as the degree of supercooling and duration of crystallization were calculated based on inspection of respective thermographic curves. Special consideration was given to the cryoprotective agent (CPA) composition (Snomax®, crude leaf homogenate (CLH) from Hippophae rhamnoides, dimethyl sulfoxide (Me2SO) and recombinant type-III antifreeze protein (AFP)) and freezing conditions ('in air' or 'in bulk CPA'). For CPAs without ice nucleation activity, thermographic measurements demonstrated that the supercooling was significantly milder in the case of scaffolds present in a CPA solution compared to that without them. This parameter (ΔT, °C) altered with the following tendency: 10 Me2SO (2.90 ± 0.54 ('scaffold in a bulk CPA') vs. 7.71 ± 0.43 ('bulk CPA', P < 0.0001)) and recombinant type-III AFP, 0.5 mg/ml (2.65 ± 0.59 ('scaffold in a bulk CPA') vs. 7.68 ± 0.34 ('bulk CPA', P < 0.0001)). At the same time, in CPA solutions with ice nucleation activity the least degree of supercooling and the longest crystallization duration (Δt, min) for scaffolds frozen 'in air' were documented for CLH from Hippophae rhamnoides (1.57 ± 0.37 °C and 21.86 ± 2.93 min) compared to Snomax, 5 µg/ml (2.14 ± 0.33 °C and 19.91 ± 4.72 min), respectively). Moreover, when frozen 'in air' in CLH from Hippophae rhamnoides, collagen-HAP scaffolds were shown to have the longest ice-liquid equilibrium phase during crystallization and the lowest degree of supercooling followed by alginate core-shell capsules and nanofibrous electrospun fiber mats made of poly ɛ-caprolactone (PCL) and polylactic acid (PLA) (PCL/PLA) blend. The paper offers evidence that infrared thermography provides insightful information for monitoring partial freezing events in TECs when using different freezing containers, CPAs and conditions. This may further TEC-specific cryopreservation with enhanced batch homogeneity and optimization of CPA compositions of natural origin active at warm sub-zero temperatures.

Asunto(s)

Criopreservación , Hielo , Congelación , Criopreservación/métodos , Termografía , Durapatita , alfa-Fetoproteínas , Crioprotectores/química , Colágeno

RESUMEN

The nitriding of forging tools is an industrially established standard used to increase the hardness of the tool surface layer and reduce wear. However, this modification of the tool surface layer, as well as the microstructural changes that occur during this operation due to the thermo-mechanical load, cannot be considered during wear calculations with the widely used Archard wear model in the context of FE simulations. Based on previous work, this study further develops two tempering tests for the investigation of the hardness evolution of two nitride profiles based on H11 tool steel. Here, significant tempering effects could be observed depending on temperature, mechanical stress superposition and time. The results are used for setting up a new material model that is implemented in an existing numerical wear model. The validation is carried out in two laboratory forging test series. The evaluation shows that the hardness development in terms of tempering effects of a nitrided forging tool can be numerically predicted, especially for high forging cycles. However, due to the unexpected occurrence of adhesion effects, only limited applicability of the wear prediction then carried out is achieved.

RESUMEN

As a result of global economic and environmental change, the demand for innovative, environmentally-friendly technologies is increasing. Employing solid lubricants in rolling contacts can reduce the use of environmentally harmful greases and oils. The aim of the current research was the development of a solid lubricant system with regenerative properties. The layer system consisted of a molybdenum (Mo) reservoir and a top layer of molybdenum trioxide (MoO3). After surface wear, Mo is supposed to react with atmospheric oxygen and form a new oxide. The determination of the wear volume of thin layers cannot be measured microscopically, which is why the wear behavior is initially determined on the nano level. In this work, single Mo and MoO3 coatings prepared by physical vapor deposition (PVD) are characterized by nano testing. The main objective was to determine the wear volume of the single coatings using a newly developed method considering the initial topology. For this purpose, nano-wear tests with different wear paths and normal forces were carried out and measured by in situ scanning probe microscopy (SPM). Based on the characteristic values determined, the coefficient of wear was determined for wear modeling according to Sarkar. The validation of the wear model developed was carried out by further wear tests on the respective mono layers.

RESUMEN

The present work deals with adjusting a fine-grained microstructure in iron-rich iron-aluminium alloys using the ECAP-process (Equal Channel Angular Pressing). Due to the limited formability of Fe-Al alloys with increased aluminium content, high forming temperatures and low forming speeds are required. Therefore, tool temperatures above 1100 °C are permanently needed to prevent cooling of the work pieces, which makes the design of the ECAP-process challenging. For the investigation, the Fe-Al work pieces were heated to the respective hot forming temperature in a chamber furnace and then formed in the ECAP tool at a constant punch speed of 5 mm/s. Besides the chemical composition (Fe9Al, Fe28Al and Fe38Al (at.%-Al)), the influences of a subsequent heat treatment and the holding time on the microstructure development were investigated. For this purpose, the average grain size of the microstructure was measured using the AGI (Average Grain Intercept) method and correlated with the aforementioned parameters. The results show that no significant grain refinement could be achieved with the parameters used, which is largely due to the high forming temperature significantly promoting grain growth. The holding times in the examined area do not have any influence on the grain refinement.

RESUMEN

Thermomechanical treatment (TMT) describes the effect of thermal and mechanical conditions on the microstructure of materials during processing and offers possible integration in the forging process. TMT materials exhibit a fine-grained microstructure, leading to excellent mechanical properties. In this study, a two-step TMT upsetting process with intermediate cooling is used to demonstrate possibilities for a process-integrated treatment and corresponding properties. A water-air-based cooling system was designed to adjust different phase configurations by varying the target temperature and cooling rate. Four different thermal processing routes and four combinations of applied plastic strains are investigated in standardized mechanical tests and metallographic analyses. The applied TMT results in a finely structured bainitic microstructure of the investigated tempering steel AISI 4140 (42CrMo4) with different characteristics depending on the forming conditions. It can be shown that the demands of the standard (DIN EN ISO 683) in a quenched and tempered state can be fulfilled by means of appropriate forming conditions. The yield strength can be enhanced up to 1174 MPa while elongation at break is about 12.6% and absorbed impact energy reaches 58.5 J without additional heat treatment when the material is formed after rapid cooling.

RESUMEN

As one of the oldest shaping manufacturing processes, forging and especially hot forging is characterized by extreme loads on the tool. The thermal load in particular is able to cause constant changes in the hardness of the surface layer, which in turn has a decisive influence on the numerical estimation of wear. Thus, also during numerical wear, modeling hardness changes need to be taken into account. Within the scope of this paper, a new implementation of a numerical wear model is presented, which, in addition to dynamic hardness models for the base material, can also take into account the properties of a nitride wear protection layer as a function of the wear depth. After a functional representation, the new model is applied to the wear calculation of a multi-stage industrial hot forging process. The applicability of the new implementation is validated by the evaluation of the occurring hardness, wear depths and the locally associated removal of the wear protection layer. Consecutively, a tool life calculation module based on the calculated wear depth is implemented and demonstrated. In general, a good agreement of the results is achieved, making the model suitable for detailed 2D as well as large 3D Finite Element calculations.