Wolfgang Tillmann

In vitro and in vivo evaluation of biodegradable, open-porous scaffolds made of sintered magnesium W4 short fibres

A cytocompatible and biocompatible, degradable, open-porous, mechanically adaptable metal scaffold made of magnesium alloy W4 melt-extracted short fibres was fabricated by liquid phase sintering. Cylindrical samples (3×5 mm) of sintered W4 short fibres were evaluated under in vitro (L929, HOB, eudiometer, weight loss) and in vivo conditions (rabbits: 6 and 12 weeks). The in vitro corrosion environment (e.g., temperature, flow, composition of corrosion solution, exposure time) significantly influenced the corrosion rates of W4 scaffolds compared with corrosion in vivo. Corrosion rates under cell culture conditions for 72 h varied from 1.05 to 3.43 mm y(-1) depending on the media composition. Corrosion rates measured in eudiometric systems for 24 h were ~24-27 times higher (3.88-4.43 mm y(-1)) than corrosion in vivo after 6 weeks (0.16 mm y(-1)). Moreover, it was found that the cell culture media composition significantly influences the ionic composition of the extract by selectively dissolving ions from W4 samples or their corrosion products. A pilot in vivo study for 6 and 12 weeks demonstrated active bone remodelling, no foreign body reaction and no clinical observation of gas formation during W4 scaffold implantation. Long-term in vivo studies need to be conducted to prove complete degradation of the W4 scaffold and total replacement by the host tissue.

Effect of the addition of low rare earth elements (lanthanum, neodymium, cerium) on the biodegradation and biocompatibility of magnesium

Rare earth elements are promising alloying element candidates for magnesium alloys used as biodegradable devices in biomedical applications. Rare earth elements have significant effects on the high temperature strength as well as the creep resistance of alloys and they improve magnesium corrosion resistance. We focused on lanthanum, neodymium and cerium to produce magnesium alloys with commonly used rare earth element concentrations. We showed that low concentrations of rare earth elements do not promote bone growth inside a 750 μm broad area around the implant. However, increased bone growth was observed at a greater distance from the degrading alloys. Clinically and histologically, the alloys and their corrosion products caused no systematic or local cytotoxicological effects. Using microtomography and in vitro experiments, we could show that the magnesium-rare earth element alloys showed low corrosion rates, both in in vitro and in vivo. The lanthanum- and cerium-containing alloys degraded at comparable rates, whereas the neodymium-containing alloy showed the lowest corrosion rates.

Biocompatibility of rapidly solidified magnesium alloy RS66 as a temporary biodegradable metal

Biodegradable magnesium-based alloys are very promising materials for temporary implants. However, the clinical use of magnesium-based alloys is often limited by rapid corrosion and by insufficient mechanical stability. Here we investigated RS66, a magnesium-based alloy with extraordinary physicochemical properties of high tensile strength combined with a high ductility and a homogeneous grain size of ~1 μm which was obtained by rapid solidification processing and reciprocal extrusion. Using a series of in vitro and in vivo experiments, we analyzed the biodegradation behavior and the biocompatibility of this alloy. In vitro, RS66 had no cytotoxic effects in physiological concentrations on the viability and the proliferation of primary human osteoblasts. In vivo, RS66 cylinders were implanted into femur condyles, under the skin and in the muscle of adult rabbits and were monitored for 1, 2, 3, 4 and 8 weeks. After explantation, the RS66 cylinders were first analyzed by microtomography to determine the remaining RS66 alloy and calculate the corrosion rates. Then, the implantation sites were examined histologically for healing processes and foreign body reactions. We found that RS66 was corroded fastest subcutaneously followed by intramuscular and bony implantation of the samples. No clinical harm with transient gas cavities during the first 6 weeks in subcutaneous and intramuscular implantation sites was observed. No gas cavities were formed around the implantation site in bone. The corrosion rates in the different anatomical locations correlated well with the local blood flow prior to implantation. A normal foreign body reaction occurred in all tissues. Interestingly, no enhanced bone formation could be observed around the corroding samples in the condyles. These data show that RS66 is biocompatible, and due to its interesting physicochemical properties, this magnesium alloy is a promising material for biodegradable implants.

Sliding and Rolling Wear Behavior of HVOF-Sprayed Coatings Derived from Conventional, Fine and Nanostructured WC-12Co Powders

Fine structured and nanostructured materials represent a promising class of feedstock for future applications, which has also attracted increasing interest in the thermal spray technology. Within the field of wear protection, the application of fine structured or nanostructured WC-Co powders in the High Velocity Oxy-Fuel flame spraying technique (HVOF) provides novel possibilities for the manufacturing of cermet coatings with improved mechanical and tribological characteristics. In this study the tribological behavior of HVOF sprayed coatings derived from conventional, fine and nanostructured WC-12Co powders under sliding and rolling wear are investigated and the results are compared to C45 steel (Mat.-No. 1.0503). In addition, sliding and rolling wear effects on a microscopic level are scrutinized. It has been shown that under optimized spray conditions the corresponding fine and nanostructured WC-12Co coatings are able to obtain higher wear resistances and lower friction coefficients than the conventional coatings. This can be attributed to several scaling effects of the microstructure and to the phase evolution of the coating, which are discussed.

Effect of Residual Stress on the Wear Resistance of Thermal Spray Coatings

The wear resistance of thermal spray coatings mainly depends on coating properties such as the microstructure, hardness, and porosity, as well as on the residual stress in the coating. The residual stress is induced by a variety of influences e.g., temperature gradients, difference of the thermal expansion coefficient of the coating/substrate materials, and the geometry of the components. To investigate the residual stress, the impulse excitation technique was employed to measure the Young’s and shear moduli. The residual stress was determined by the hole-drilling method and x-ray diffraction. Pin-on-Disk and Pin-on-Tube tests were used to investigate the wear behavior. After the wear tests, the wear volume was measured by means of a 3D-profilometer. The results show that the value of the residual stress can be modified by varying the coating thickness and the substrate geometry. The compressive stress in the HVOF-sprayed WC-Co coatings has a significant positive influence on the wear resistance whereas the tensile stress has a negative effect.

Measurement of the Young’s Modulus of Thermal Spray Coatings by Means of Several Methods

Thermally sprayed coatings are usually defined by their hardness, porosity, roughness, and wear resistance. Even though the Young’s modulus is an essential property, which describes the mechanical behavior of the coated components during their use, only few efforts have been made in the past to determine this property. The most common measurement methods of the Young’s modulus of thermally sprayed coatings are tensile tests, bending tests, and nanoindentations. During the tensile and bending tests a sliding of the splats can occur due to the laminar structure of the thermally sprayed coatings, influencing the measurement value. When using the nanoindentation test, only the elastic behavior of some splats can be determined because of a minimal measuring volume. However, the Young’s modulus of thermally sprayed coatings can also be determined by means of a resonant method, called impulse excitation technique. In this paper, the values of the Young’s moduli of thermally sprayed coatings, measured by several methods, are compared with each other and correlated to the microstructure of the coatings, investigated by means of scanning electron microscopy.

Improved Tool Surfaces for Incremental Bulk Forming Processes of Sheet Metals

Sheet-bulk metal forming is a process used to manufacture load-adapted parts with high precision. However, bulk forming of sheet metals requires high forces, and thus tools applied for the operational demand have to withstand very high contact pressures, which lead to high wear and abrasion. The usage of conventional techniques like hardening and coating in order to reinforce the surface resistance are not sufficient enough in this case. In this paper, the tool resistance is improved by applying filigree bionic structures, especially structures adapted from the Scarabaeus beetle to the tool’s surface. The structures are realized by micromilling. Despite the high hardness of the tool material, very precise patterns are machined successfully using commercially available ball-end milling cutters. The nature-adapted surface patterns are combined with techniques like plasma nitriding and PVD coating, leading to a multilayer coating system. The effect of process parameters on the resistance of the tools is analyzed experimentally and compared to a conventional, unstructured, uncoated, only plasma nitrided forming tool. Therefore, the tools are used for an incremental bulk forming process on 2 mm thick metal sheets made of aluminum. The results show that the developed methodology is feasible to reduce the process forces and to improve the durability of the tools.

Innovative Tools to Improve Incremental Bulk Forming Processes

Sheet-bulk metal forming is an innovative process with a high potential to generate load-adapted parts with high precision. Bulk forming processes of sheet metals especially require high process forces, resulting in an intense contact pressure and, thus, in a very high abrasive and adhesive wear. As a method to reduce or avoid these common wear phenomena, even hardened or coated tool surfaces are not sufficient. The objective of this paper is to show an improvement of the tool resistance during an incremental forming process by an adapted tool design and the application of structured tool surfaces combined with coatings. For the tool surface the structure of the scarabaeus beetle serves as the basis for a bionic structure. This structure was manufactured by micromilling. Despite the high hardness of the tool material and the complex geometry of the forming tools, very precise patterns were machined successfully using ball-end milling cutters. The combination of bionic structures with coating techniques like physical vapor deposition (PVD) on plasma nitrided tool surfaces is very promising. In this work, the influence of process parameters (workpiece material, lubrication, tool design, stepwise infeed) on the tool resistance during the forming operation was analyzed experimentally. The results of the optimized forming tools were compared to conventional, unstructured, uncoated, and only plasma nitrided forming tools. The different tools were applied to 2 mm thick metal sheets made of aluminum (AlMg3) and steel (non-alloy quality steel DC04). As a result, the process forces could be reduced by a modified shape and surface of the tools. Thus, the lifetime of the tools can be enhanced.

Influence of Surface Modifications on Friction, Using High-Feed Milling and Wear Resistant PVD-Coating for Sheet-Metal Forming Tools

Increasing technological requirements, as well as the demand for an efficient production demands high performance materials and enhanced manufacturing processes. The development of a new manufacturing process, sheet-bulk metal forming (SBMF), is one approach to produce lightweight forming parts with an increased number of functional properties while, at the same time, combining the advantages of sheet and bulk metal forming. For SBMF processes, the specific adjustment of the friction between tool and workpiece for a specifically designed material flow, which is called tailored friction, is of great importance. The reduction of friction is essential in order to ensure a homogeneous forming zone. However, a higher friction can be used to control the material flow to increase the local thickness of the work piece for additional functional integration. This paper shows the development of surface structures for SBMF tools by means of high-feed milling. Process parameters like the tilt angle or the feed are varied to influence the surface parameters of the structures, which results in different tribological properties of the forming tool. The structured surfaces are subsequently coated with a wear resistant CrAlN coating, processed by a magnetron-sputtering process (PVD) to enhance the lifetime and performance of the forming tool. Finally, a ring compressing test is used to investigate the tribological behavior of the coated structures.

Wear Analysis of Thermal Spray Coatings on 3D Surfaces

Even though the application of thermal spray coatings on complex geometries gained a greater interest in the last decade, the effect of different geometrical features on the wear behavior is still ill-defined. In this study, the wear resistance of FTC-FeCSiMn coated 3D surfaces was investigated. The wear test was carried out by means of two innovative testing procedures. The first test is a Pin-on-Tubes test where the rotating motion is realized by a lathe chuck. The specimens in the second test were fixed on the table and a robot arm operated the pin. This wear test was applied on specimens with concave or convex surfaces. The residual stresses, which were determined by means of an incremental hole-drilling method, show a dependency on the substrate geometry. The obtained stresses were put in relation to the different radii. After the wear test, a 3D-profilometer determined the wear volume and the sections of the coatings were characterized by a scanning electron microscope. The results indicate that the wear resistance is strongly influenced by the geometry of the substrate.