2.1.1. Heat Treatment
In this study, the martensitic stainless chromium steel X46Cr13 was used. The chemical composition and the permitted limits are shown in
Table 1.
Thermodynamic calculations were performed for the minimum (solid line) and maximum (dashed line) permissible alloy content using JMatPro
® V7.0 (Sene Software Ltd., Guildford, UK), compare
Table 1. This includes the calculation of the phase diagram, see
Figure 1 (left), and the chemical element distribution (carbon (black line) and chromium (blue line)) in austenite in equilibrium state as a function of temperature, see
Figure 1 (right). It can be observed in
Figure 1 (left) that from approximately 800 °C (max) and 817 °C (min), the transformation of ferrite into austenite starts. Besides austenite, there are carbides. With increasing temperature, the mass fraction of the carbides decreases, and the austenite fraction increases. In
Figure 1 (right), it can be seen that with increasing temperature, the contents of carbon and chromium in austenite increase. This is due to the increasing solubility of the carbides. A maximum of the carbon and chromium content is reached at approximately 1062 °C (min) and 1160 °C (max). Continuous time-temperature diagrams (CCT) indicate the resulting phases and hardness as a function of the austenitizing temperature and the cooling rate, compare
Figure 2. The phase diagram, the chemical composition of austenite and the CCT enable the possibility to design the heat treatment and to classify the heat treatment results in terms of metal physics.
Figure 2 shows the phase composition and the resulting hardness as a function of the cooling rate. It can be clearly seen that the hardness decreases as the cooling rate decreases. The hardness varies from a maximum of 652 to 139 HV. It has to be noted that the austenitizing temperature is 980 °C. If the austenitizing temperature is different, the CCT changes. In general, with increasing austenitizing temperature, the transformation lines shift to longer times, i.e., the steel transforms more slowly. This can be explained by the increase in the mass proportion of alloying elements in austenite with increasing austenitizing temperature, comparing the mass content of chromium,
Figure 1 (right). With increasing carbon content, martensite start temperature and martensite finish temperature decrease, and stabilized retained austenite can be present at room temperature. At high temperatures, grain growth takes place due to the minimization of the surface energy. This means that with increasing holding time at high temperature, the grains grow. Coarser grains generally also lead to a reduction in the conversion and precipitation effort, as there are fewer germination or impurity sites, such as grain boundaries, in the lattice. The heat treatment carried out within the framework of the study is intended to exploit these effects in a targeted manner. The initial condition (soft annealed) and three heat treatment variations were realized, see
Table 2 and
Figure 3.
It should be noted that the heat treatments carried out within the scope of the study are partly different from the typical heat treatment carried out in industry, such as hardening and tempering at high temperatures (quenching and tempering), in order to specifically show the individual heat treatment influences of cooling rate and holding time. In
Figure 3, the recording of the temperature profile of the hardening process ends before quenching in oil. A rough estimate shows that the cooling rate between 800 and 500 °C, based on Reference [
27], is among 100 K/s (high-speed oil) and 20 K/s (normal speed oil).
The differently heat-treated material microstructures are compared in
Figure 4. The soft annealed condition (SA) shows distributed globular carbides. Occasional carbides can also be seen at grain boundaries. In the conditions SC and also LH, carbide accumulations (possibly pearlite) are visible at the grain boundaries. Although the holding time of 20 h is considerably longer than with SC (0.5 h), the grain sizes look similar. A grain size comparison according to ISO 643, 2020 [
28], using standardized image series tables from ASTM E 112:2013 [
29], showed an average grain diameter of approximately 18.5 µm for condition SC and an average grain diameter of approximately 26.5 µm for LH. The ratio of the area shares of the grain boundary carbides (dark) was quantified in a phase analysis (threshold analysis). The thermally stable carbides (according to JMatPro
®: M
23C
6, M
7C
3) seem to stabilize the grain boundaries and have apparently minimized grain growth. At the condition SC, the area shares of the grain boundary carbides are approximately 20.6%, slightly higher than at LH, with approximately 15.2%. This indicates a higher precipitation kinetics during cooling at condition SC due to the finer grains. For the other heat treatment conditions, it is not possible to determine the grain size, as grain boundaries cannot be traced. The image H shows the hardened condition. It should be mentioned that when comparing different images of conditions H, a difference in the number of carbides was noticed, which indicates a dissimilar distribution of the carbides in the initial condition (segregation).
Figure 5 shows the hardness and notched bar impact energy of the specimens that have been heat-treated differently. It is noticeable that the soft-annealed condition has the lowest hardness of approximately 200 HV10 and at the same time, compared to the other heat treatment conditions (LH and H), high notched bar impact energy. The condition annealed at 1030 °C for half an hour with slow cooling (SC) can bear a higher notched bar impact energy than the soft-annealed condition (SA), at a hardness of approximately 540 HV10. Condition LH has a slightly higher hardness of about 590 HV10. This can be attributed, among other things, to the fact that during the long holding time of 20 h, the diffusion processes are close to the equilibrium state and thus more carbon is dissolved in the austenitic matrix compared to the heat treatment condition SC. According to Reference [
30], the lower toughness can be attributed to pre-eutectoid carbide precipitations along the former austenitic grain boundaries and relatively coarse grains. The highest hardness of 660 HV10 and at the same time the lowest notched bar impact energy of approximately
ENBI = 4.5 J are shown in the hardened condition (H). It should be noted that the notched bar impact energy is generally at a low level.
Figure 6 shows the macroscopic surfaces of the impact test specimens. Condition SA has a shiny area, and this indicates a crystalline structure and therefore a brittle fracture. The surfaces of the conditions SC, LH and H are more matte and show hardly any differences between them. In all four conditions, there is a largely flat fracture surface, and no shear lips or similarly strongly deformed areas are visible. It can be seen that despite the different heat treatment conditions (SC, LH and H) and hardness values, the fracture surfaces look very similar and are almost fractured purely brittle.
Figure 7 displays the fracture surfaces recorded by scanning electron microscopy (SEM), determined with an acceleration voltage of 25 kV and a working distance of about 9–10 mm. The lower magnifications show back-scattered electron (BSD) images and the higher magnifications show secondary electrons (SE) images for the respective heat treatment condition of the different notched bar impact test specimens. In all conditions, transcrystalline and inter-crystalline cleavage fractures as well as inter-crystalline and transcrystalline slip fractures appear to occur in varying proportions. The differentiation between intergranular and transcrystalline fracture surfaces is mostly not clearly possible due to the heterogeneity of the fracture surfaces caused by the carbides.
In condition SA, a transcrystalline fracture is visible. The dimple structure of the different conditions indicates that the carbides trigger the more ductile areas and thus prevent further deformation. The dimple structure can therefore be interpreted as ductile deformation of a transcrystalline fracture. The visible differences are apparently determined by the carbide distribution and size. With smaller and more finely distributed carbides, the structure looks more differentiated. This can be seen, for example, when comparing the condition LH and the condition H. Condition H shows smaller and finely distributed carbides. In condition SC, isolated grain boundaries are visible. In condition LH, the grain boundaries are more clearly visible in comparison to the conditions SA, SC and H. Hence, the fracture surface appears more faceted. If the grain boundaries are embrittled by precipitation and therefore the bonds along the grain boundaries are sufficiently weak, intergranular brittle fracture occurs. The crack can spread more easily along the weakened grain boundaries. Mayer et al. showed that the increasing presence of carbide precipitates at the former austenite grain boundaries has a negative effect on toughness [
31]. This was found when they investigated various hardening processes for the steel X37CrMoV5-1 regarding the resulting mechanical properties. The fracture behavior is therefore also influenced by the cooling behavior. However, despite the microstructural differences of the fracture surfaces, the overall appearance is very similar.
2.1.2. Conception and Characterization of the Vibration System
For the experimental investigations, a vibration system was developed to generate the ultrasonic vibrations. It was conceived and manufactured as a longitudinal oscillator in “λ-half design”, as described, for example, in Reference [
32]. This common structure was designed with the help of a FEA to estimate the resonant frequency. The oscillator consists of upper and lower mass elements and a screw for preload, all made of Ti-6Al-4V,
Figure 8. In addition, the seven copper electrodes transfer the voltage to the six piezoelectric disks. These transform the applied electric field into a linear motion due to the inverse piezoelectric effect. It becomes possible to tune the system to the desired resonant frequency using the masses. The mounting of the oscillator was realized by means of contact clamping at the node-point, as this is where the smallest strains take place, with the housing, and this was connected by a thread with the baseplate. A plastic bushing for the cable and corresponding O-rings at the connection points seal the inner against the use of lubricants. A preload of approximately 50 N m was used to tighten the screw in order to prevent the components of the oscillator from chattering and to a significant change in the resonant frequency of the system. This would result in the controller stopping due to high energy losses. To minimize the influence on the resonant frequency of the system through an additional mass, the specimens had only a small height (4 mm). The upper mass element has an internal thread (M14 × 1) and connects the specimen by a screw. The hexagonal profile with a width across flats (WAF) of 30 mm allowed for a material specific torque of up to 100 N m for the specimens with condition SA, SC and LH, 40 N m for the hardened specimens and 50 N m for the specimens made of brass. Those torques were proven to ensure a strong connection for an almost lossless oscillation.
For the generation of predefined surface microstructures, determining of the amplitude of the relative motion between the tool and the various heat-treated specimens was necessary. Therefore, a single-point laser vibrometer was used to achieve the relation between the output power of the generator and the amplitude at the specimen surface before each single experiment. The corresponding measurement setup is shown in
Section 2.2.
Figure 9 shows a frequency sweep to achieve the lowest needed voltage while maintaining the target amplitude for a specimen in the SA condition. The determined resonant frequency,
fUS, was about 19 kHz with this testing method. This value was used for all UVSM experiments as fixed frequency.
In addition, non-contact scanning measurements using a three-dimensional (3D) laser vibrometer were carried out to investigate the vibration system in more detail. The 3D laser vibrometer measurement allows simultaneous detection of the displacement in the spatial directions by evaluating the interference patterns of three laser beams reflected from the measurement object. It was excited directly by a signal from the measuring device using a so-called “periodic chirp”, i.e., from 0 to 25 kHz. Thus, both the natural frequencies and the vibration modes in all three spatial directions were determined. The results of this investigation are shown in the diagram in
Figure 10, where the amplitude is given in dB.
The analysis of the plots from
Figure 10 exhibits a resonance frequency in the relevant range, at approximately 20.3 kHz. There is a difference of more than 10 dB between the z-axis and the other two axes, which indicates a clear dominance of the vibration in the intended direction. The minor differences in the radial x- and y-directions can be explained by the slightly asymmetric geometry of the actuator and workpiece. The excitation frequency of 19 kHz used with the other generator is close to the measured resonance frequency, whereby the z-oscillation also dominates here.
When interpreting the deflection shape, it can be determined that a quasi-homogeneous oscillation in the z-direction is present, see
Figure 11a, with negligible vibration in the perpendicular directions x and y, but only in the sub-micrometer range. In addition, a slight deflection of the surface of the specimen centered towards the edges can be detected, which is evident from the sharp increase in the color scale in the range from 1.0 to 1.4 µm, see
Figure 11b. However, since the field to be processed by UVSM covers an area of 1 × 1 cm, arranged centrally, these effects are negligible for surface analysis as well as the wear progress of the tools.
2.1.3. Surface Design and Simulation
To characterize the surface microstructures generated by UVSM, at first, their geometry was simulated assuming a geometrically exact tool corner with a radius of
rε = 30 µm. For this purpose, a self-developed Matlab-based simulation tool was used, which has already been described in detail in References [
4,
5].
Corresponding to the two extreme cases—with (peak follows on valley) and without (peak follows on peak) structural displacement—these were simulated for the cutting speeds of
vc = 20 m/min (in the following denoted as vc20),
vc = 50 m/min (vc50) and
vc = 80 m/min (vc80), whereby the value of the feed was kept constant. The resulting surfaces are shown in
Table 3. In addition, the respective surface parameters for the surface magnification (
Sdr) and the surface texture isotropy (
Str) were derived from the ISO 25178-2 [
33]. Consequently, the
Str values strongly depend on the structural displacement: surfaces with a structural displacement have a much more isotropic character than those without. The value of the developed interfacial area ratio increases with the number of elements per scale-limited surface, whereby the difference between the surfaces for
vc = 50 m/min and
vc = 80 m/min is almost negligible. However, the structural displacement also has an influence on the
Sdr value, which shows the following example: despite the fact that they image fewer elements, the surface generated with
vc = 80 m/min results in combination with a structural displacement in a higher value of the developed interfacial ratio than those created with
vc = 50 m/min and without exhibiting any structural displacement. Subsequently, a comparison with laser-microscopically measured surfaces is possible. In addition, the influence of the steel’s material behavior, regarding plastic deformation, can be detected, since the kinematic simulation is solely based on the mathematical operation of the Boolean intersection and neglects plastic effects of material separation. Thus, quantitative values, such as the achieved structural height, and qualitative conclusions, such as for burr formation, can be derived.
In order to characterize the simulated and the machined surface microstructures, profile extractions in the direction of primary motion (a) and feed motion (b) have been made, see
Figure 12. Due to the small distance shown (right), the path curvature at (a), resulting from the tool circumference, is negligible. It shows the clearly sinusoidal curve in the direction of the cutting speed, which results from the superposition of the ultrasonic vibration. The structure height in this direction corresponds to the selected oscillation amplitude, defined here in this paper as peak-peak-value. The profile in the feed direction also shows the existing kinematic roughness. In both cases, it is irrelevant for the shape of the profile at which position (x- or y-value) the respective extraction is placed, only a height shift would occur. The symmetrical shape in the direction of feed motion becomes clear, as the corner radius is still completely engaged. In the real UVSM process, this should also be ensured by the fact that the angles of the major and minor cutting edge are identical.