4.3. Material Hardness Results
The hardness results for the measurements carried out on the
x-y plane are presented in
Table 4 by means of statistical parameters, i.e., the mean, standard deviation, median, and relative standard deviation.
To verify the potential of using hardness as an indirect indicator for assessing the tensile strength of the Ti6Al4V alloy, Vickers hardness (HV) measurements were carried out for six groups of samples: AS, HT, and DB (samples subjected to tensile testing), as well as ASW, HTW, and DBW (samples not subjected to tensile testing). Each hardness value represents the average of 10 independent measurements, through which it was possible to determine not only the mean value but also the standard deviation, median, and relative standard deviation (%RSD).
The highest average hardness was recorded for the ASW sample (412.7 HV), which was produced using the DMLS method in its as-built state, without annealing and without prior mechanical loading. The hardness of the HTW sample (printed and annealed but not subjected to tensile testing) was 356.9 HV, while the DBW sample (drawn bar, also untested) measured 336.7 HV. These values are slightly higher than those of their corresponding tensile-tested counterparts: AS—347.1 HV, HT—392.9 HV, and DB—294.7 HV. This suggests that performing the tensile test may, in some cases, lead to localized modifications in the material’s structure—such as surface work hardening or microscopic deformation—resulting in slight changes (in most cases, reductions) in hardness.
It is worth noting, however, the unusual result observed for the HT sample, which, despite being annealed, shows greater hardness (392.9 HV) than its corresponding untested counterpart, HTW (356.9 HV). This may indicate structural inhomogeneity, local phase transformations, or the influence of micro-deformations that are introduced during the tensile testing process. Possible variations in the specific locations where the hardness measurements were taken on the sample should also be considered.
From the standpoint of result uniformity, the most stable values were obtained for the DBW (1.3% RSD) and DB (2.2% RSD) samples, confirming the high quality and consistency of the microstructure in the material derived from the drawn bar. In contrast, the samples produced using the DMLS method, particularly the HTW and ASW, showed significantly greater result dispersion (%RSD of 5.8% and 5.5%, respectively), which may stem from the inherent anisotropy of additive materials and local differences in density and phase distribution.
A comparison of the hardness results with the tensile strength values enables an analysis of the potential correlations between these properties. The AS sample, characterized by a tensile strength of approximately 1450 MPa, had an average hardness of 347.1 HV, while the DB sample, with the lowest tensile strength (~950 MPa), reached a hardness of 294.7 HV. As expected, higher hardness translated into higher strength, which confirms the validity of using empirical relationships such as the Cahoon model or other classic HV–UTS correlations.
However, the HT sample disrupts this simple correlation. Despite having greater hardness than the AS sample (392.9 HV vs. 347.1 HV), it achieved significantly lower tensile strength (~1050 MPa). This indicates that surface hardness does not fully reflect the strength properties of the heat-treated material. This may result from the fact that heat treatment modifies not only the local hardness but also the internal microstructure, the distribution of α and β phases, dislocation density, and the residual stress distribution—all of which are critical parameters for the material’s behavior under tensile loading.
The analyses of both the mean values and standard deviations lead to the conclusion that hardness can be a useful but insufficient indicator for indirectly estimating the strength of Ti6Al4V materials, particularly in their heat-treated state. For the as-built samples (AS and DB), the HV–UTS relationship shows strong consistency, justifying the use of predictive models in the context of additive manufacturing without annealing or when using conventional materials. However, for heat-treated materials, it is necessary to consider additional structural parameters, which may require extending the correlation model or employing more advanced predictive techniques (e.g., machine learning).
Additionally, the fact that the samples not subjected to tensile testing (ASW, HTW, and DBW) exhibited higher hardness compared to their tensile-tested counterparts suggests the potential influence of mechanical deformation on subsequent hardness measurements—even though the HV test itself is considered minimally invasive. This further reinforces the need to perform hardness measurements in a controlled manner, taking into account the material’s loading history.
Importantly, the samples not subjected to tensile testing (ASW, HTW, and DBW) exhibited higher hardness values compared to their tensile-tested counterparts. At first glance, this appears contrary to the classical phenomenon of strain hardening; however, additional mechanical and structural effects must be considered. During the tensile test, local relaxation of residual stresses and redistribution of the dislocation structure may occur, leading to reduced post-test hardness. The literature suggests that in materials with a martensitic microstructure (such as the α′ phase that is present in the AS samples), these effects can result in strain softening or may even initiate micro-recrystallization within the necking region [
15,
21] (Brodsky and Thompson, 1984; Qiu et al., 2015). Additionally, local temperature increases during testing (adiabatic heating) may induce micro-annealing [
11], and, in additively manufactured structures, partial stress relaxation due to plastic deformation is also possible [
14]. As a result, hardness measurements taken after tensile testing may yield lower values, despite the simultaneous occurrence of classical strain hardening. Similar observations for Ti6Al4V were also reported by Bermingham et al. (2011) and Yadollahi and Shamsaei (2017) [
9,
13].
In summary, the hardness analysis confirms this test’s potential as a supplementary indicator for assessing the mechanical properties of Ti6Al4V. However, its effectiveness depends on technological consistency, microstructural homogeneity, and knowledge of the processing conditions. Only under such conditions is it possible to build reliable and stable predictive models of tensile strength based on hardness measurements.
4.4. Determination of Material Strength Based on Hardness Measurement Results
The presented results of the hardness measurements of Ti6Al4V alloy samples made from a drawn bar and the additive method show differences. The DB samples are characterized by the lowest hardness value, which is also reflected in the strength results obtained via the static tensile test. The difference between the specimen under tension (DB specimen) and the as-built sample (DBW specimen) is 42 HV. This difference may indicate changes in the structure of the material resulting from clamping the testing machine’s jaws on the sample during the test, as well as the static tensile test itself. Similar differences are observed in the AS and ASW samples, where the difference is 65.6 HV, and in the HT and HTW samples, where the difference is 36 HV.
The analysis of the results of the hardness tests on the x–y plane showed that the ASW and HT samples have the hardest structure, and the difference between them is 19.8 HV. The heat-treated printed samples (HTW) and printed samples without heat treatment (AS) show a similar hardness—the difference is 9.8 HV. The largest value for the dispersion of hardness in the results was observed for the ASW sample, at 22.8 HV.
When analyzing only the hardness results for those specimens taken from the samples not subjected to the static tensile test, where there are no changes in the material caused by tensile forces, it is noted that the ASW sample has the highest hardness, and the DBW has the lowest. The results of the tensile strength tests are similar, with the highest value for the AS sample and the lowest for DB. This highlights the relationship between the hardness and strength of the material.
The performed hardness measurements made it possible to determine the material strength indirectly. To determine the tensile strength in an analytical manner using the results of the hardness measurements, the formula described in Ref. [
5] was used, which is presented below:
where:
H—Vickers hardness value or HV,
C—material factor, and
n—strengthening factor.
The next stage used Equation (1) to carry out analytical calculations and to determine the local tensile strengths for the obtained values of hardness measurements on the x-y plane of the sample cross-section. To determine the tensile strength on the basis of the hardness tests, specimens taken from those samples not subjected to the strength test were used and compared with the material strength when determined through a static tensile test.
Figure 9,
Figure 10 and
Figure 11 show the material strength results (UTS), calculated on the basis of hardness tests for the ASW, HTW, and DBW samples, respectively. The presented graphs show the strength values in terms of points compliant with the hardness measurements (UTS), their average value, and the average strength value obtained based on the static tensile test, together with the confidence intervals. To calculate the UTS, the cyclic hardening factor for the Ti6Al4V alloy with a value of
n = 0.9 was used, as reported in Ref. [
22]. Two extreme values of the C coefficient have been proposed, which, after converting the UTS, are within the assumed confidence interval.
Figure 9 presents the charts for the ASW sample for two values of the material coefficient, C = 1.9 and C = 2.1.
Figure 10 shows the graphs for the HTW sample for two values of the material factor, C = 2.3 and C = 2.5.
Figure 11 presents the graphs for the DBW sample for two values of the material factor, C = 2.3 and C = 2.6.
Table 5,
Table 6 and
Table 7 show the calculation results of the UTS mean value, standard deviation, median, and relative standard deviation for the ASW, HTW, and DBW samples, respectively.
A comparison of the results of the experimental tests with the results obtained analytically shows that it is possible to use the hardness tests to determine the strength of the material. The presented test results show that the average UTS values determined through the hardness tests were within the accepted confidence intervals, as determined on the basis of the results of the static tensile test. The different values of the C coefficient are due to the effect of the relevant treatment that was applied and the resulting variable material structure. In each of the presented cases, two extreme values of C were given, between which the strength values are close to the experimental average value.
4.5. Analysis of the Material Microstructure Test
Figure 12 shows photos of the individual microstructures of samples made of the Ti6Al4V alloy.
Figure 12a,b show the microstructure of a printed sample in the as-built condition, subjected to strength tests (AS specimen).
Figure 12c,d show the microstructure of a printed sample, subjected to heat treatment and after the tensile test (HT specimen).
Figure 12e,f show the microstructure of a sample made of a pulled bar after testing its mechanical properties (DB specimen).
Figure 12g shows the structure of the printed sample in the as-built condition, without undergoing the tensile test (ASW specimen).
Figure 12h shows the microstructure before the strength tests of a heat-treated printed sample (HTW specimen).
Figure 12a,c,e,g,h show the microstructure in the gripping part (P1). Finally,
Figure 12b,d,f show the microstructure in the measuring part (P2).
The AS specimen is characterized by a clearly visible martensitic α′ phase structure with a strongly acicular (needle-like) morphology. The grains are elongated in the z-axis direction (the layer-building direction), indicating directional solidification during processing. The α′ martensite forms as a result of the very rapid cooling that is inherent to the additive manufacturing process and the absence of any subsequent heat treatment. This microstructure is typical for as-built 3D-printed materials and is responsible not only for their very high hardness and tensile strength but also for their brittleness and limited ductility. The observed fractures in the tensile-tested sample are consistent with this interpretation—the material exhibits no significant plastic deformation before failure.
In the case of the HT specimen, a more balanced mixture of α (matrix) and β (darker regions) phases is visible, with grains that are less elongated and more equiaxed. The reduced presence of acicular martensitic α′ indicates its decomposition as a result of thermal exposure. Although the microstructure transformed toward a more ductile form, the mechanical properties did not improve. This may be due to an excessive heat treatment temperature (above the β-transus) or an insufficient holding time, which led to incomplete stabilization of the α + β phases and degradation of the microstructure.
The DB specimen exhibits a homogeneous, fine-grained α + β structure that is typical of plastically worked Ti6Al4V products. The α phase appears in plate-like or lamellar form, uniformly distributed within the β matrix. The absence of a grain orientation suggests isotropic mechanical behavior. This microstructure provides well-balanced mechanical properties, combining good strength and ductility. Its uniformity forms a reliable basis for predictive modeling and serves as a reference point for additively manufactured materials.
In the ASW specimen, which is microstructurally identical to the AS specimen but has not been subjected to mechanical deformation, an intense presence of martensitic α′ is also observed, with the grain structure aligned along the layer-building direction (z-axis). The absence of deformation marks or residual stress indicators suggests an ‘undisturbed’ material condition post-printing. This sample enables the evaluation of the isolated effect of tensile testing. When compared to the AS specimen, the microstructural differences are minimal, indicating that neither the HV test nor the tensile test significantly alters the deep internal structure. However, both may influence the residual stress state and local deformation characteristics (e.g., dislocation density).
The HTW specimen, which was printed and heat-treated similarly to the HT specimen but was not subjected to tensile loading, exhibits a visibly α + β phase structure composed of larger, less well-defined grains compared to the HT specimen. The absence of mechanical deformation (tensile test) likely resulted in a lack of dynamic grain refinement. The presence of a coarser microstructure may explain both the lower repeatability of hardness measurements and a potential decrease in mechanical performance. This specimen suggests that heat treatment alone may not be sufficient to optimize the material properties—controlled cooling or additional mechanical processing steps might be necessary.
Table 8 presents a comparative summary of the specimens based on their resulting microstructures. The as-built additively manufactured specimens (AS and ASW) exhibit a characteristic martensitic α′ structure, which is responsible for high hardness and strength, but also contributes to significant brittleness. Heat treatment (HT and HTW) leads to decomposition of the martensite and the emergence of a more classical α + β phase mixture; however, the effectiveness of this transformation depends strongly on the heat treatment parameters. In the present study, the applied thermal processing did not significantly improve the mechanical properties. The specimens made from drawn bar material (DB and DBW) demonstrate the most predictable and balanced microstructure, serving as a reference state for comparison.
The lack of a noticeable influence of tensile testing on the macroscopic microstructure of the samples indicates that the dominant factors modifying the internal structure are the manufacturing method (additive vs. conventional) and the applied heat treatment, rather than mechanical deformation during testing.
Both the AS specimen (after tensile testing) and the ASW specimen (untested) represent the characteristic microstructure that is formed by the DMLS (direct metal laser sintering) process. A common feature of these samples is the presence of the martensitic α′ phase, forming a dense, acicular (needle-like) structure with a columnar arrangement aligned along the z-axis—the direction of layer-wise additive manufacturing.
The α′ martensite forms as a result of extremely rapid cooling during the metal printing process. It is a metastable phase that is hard and brittle. The directional grain alignment leads to anisotropy in its mechanical properties. The lack of observable microstructural differences between the AS and ASW specimens suggests that tensile loading does not significantly alter the overall grain morphology, although it may locally affect the stress distribution and dislocation density.
The application of heat treatment in the HT and HTW specimens caused significant changes in the material’s structure. The transformation of the α′ martensite into a classical biphasic α + β microstructure is evident. The α grains exhibit a more rounded (spheroidal) morphology, while the β phase appears between them in the intergranular regions.
Although this structure is typical of annealed titanium alloys, the analyzed samples do not display full microstructural homogeneity, and the grains remain relatively coarse. The HT sample, which underwent tensile testing, shows slightly more refined grains compared to the HTW, suggesting that tensile deformation may have promoted partial microstructural reorganization or activated dynamic recrystallization processes.
Despite the phase transformation, the mechanical properties of the HT and HTW specimens deteriorated compared to the as-built condition, which could be attributed to non-optimal annealing parameters, for example, an excessively high temperature leading to overgrowth of the β phase.
The DB specimen (after tensile testing) represents a conventional microstructure that is typical of plastically worked materials. It features a fine lamellar α + β structure, uniformly distributed across the sample cross-section. The absence of preferential grain orientation indicates that the material is isotropic, which results in consistent and predictable mechanical behavior.
Comparison of the microstructures in the P1 (grip section) and P2 (gauge section, fracture zone) regions for selected Ti6Al4V specimens enables an assessment of the influence of tensile loading on local structural changes in the material.
In the AS specimen (additively manufactured, without heat treatment), both P1 and P2 reveal a distinct columnar martensitic α′ microstructure that is characteristic of DMLS-fabricated materials in the as-built state. However, in region P2—the fracture zone—this microstructure shows local disturbances: the acicular α′ phase is partially deformed and disrupted, likely due to tensile stresses and local thermal effects during fracture. Subtle changes in needle orientation and density suggest an increase in dislocation density and the initiation of microcracks. These features indicate that although the overall phase composition remains unchanged, the tensile test introduces localized structural reorganization in the fracture zone.
In the HT specimen (additively manufactured and heat-treated), region P1 displays a balanced α + β microstructure with relatively uniform, spheroidal grains that are typical of annealed titanium alloys. In contrast, region P2 exhibits greater irregularity, with disrupted phase boundaries and a more scattered grain morphology. These changes may indicate grain boundary motion or intragranular deformation induced by tensile loading. In both the AS and HT specimens, it is evident that while tensile testing does not cause phase transformation, it does affect the arrangement and integrity of the microstructure—particularly in DMLS materials, where anisotropy and residual stresses are already present, due to the layer-wise manufacturing process.
For the DB specimen (drawn bar, no heat treatment, and subjected to tensile testing), the differences between P1 and P2 are significantly less pronounced than in the printed samples. Region P1 shows a classic fine lamellar α + β structure that is uniformly distributed and with no preferential grain orientation, confirming the isotropy and homogeneity of conventionally processed Ti6Al4V. In region P2 (the fracture zone), the same general structure is preserved, although the local elongation of α lamellae and slight blurring of phase boundaries can be observed—likely a result of tensile-induced strain and localized stress concentration.
Compared to the printed specimens, the microstructural changes in region P2 of the DB sample are more subtle, confirming the greater structural resistance of the conventional material to tensile deformation. The drawn bar material exhibits high microstructural stability and resistance to localized damage, which translates into more favorable mechanical properties and reduced scatter in terms of both the hardness and tensile strength results.
Microstructural analysis of the Ti6Al4V alloy specimens revealed significant differences resulting from the manufacturing method, the heat treatment, and the presence of mechanical deformation. Samples produced via additive manufacturing (DMLS) in the as-built condition were characterized by a needle-like, columnar martensitic α′ structure, which promotes high hardness and strength but limits ductility and microstructural uniformity. The application of heat treatment led to a transformation into a biphasic α + β structure; however, no significant improvement in mechanical properties was observed, indicating the need for optimization of the annealing parameters.
In contrast, the microstructures of specimens prepared from the drawn bar material exhibited the highest degree of homogeneity and stability, with a fine-grained α + β structure that is typical of conventionally processed titanium alloys, offering a favorable balance between strength and ductility. The effect of tensile deformation on the microstructure was marginal, primarily involving localized strain-induced modifications.
These findings confirm the critical role of microstructures in shaping the mechanical performance of Ti6Al4V and highlight the importance of carefully selecting the manufacturing method and heat treatment parameters in the context of additive technologies for titanium alloys.