Influence of wavelength on laser absorption
Absorption of laser energy by a material is highly dependent on the laser’s operating wavelength, the size of feedstock particles and its material properties. Given the importance of laser wavelength for PBF processing, there have been very few studies on the effect of wavelength on metal powder feedstock. Previous studies relied on the absorptivity of bulk material [20] [27]. Therefore, for this study, it was important to measure the physical absorptivity of the powder used instead of using absorption for bulk materials available in literature. Figure 7 presents the optical (laser) absorption coefficients for common SLM materials within the range of 400 to 1100 nm, measured using an Ocean HDX Vis NIR as specified in section 2.3. Powder absorption is seen to vary significantly with laser wavelength. For instance, the absorptivity of Ti6Al4V increases by 14% when using a 450-nm laser source compared with a 1064-nm fibre laser. However, for highly reflective and conductive materials such as copper, absorption is increased by 78% when using a 450-nm laser source. Since this study focuses on Ti6Al4V, the absorptivity at 808 nm and 450 nm will be used to calculate the normalised energy density as discussed in section (2.4.2).
Influence of wavelength on surface temperature
As the first stage of this study, the surface temperature of Ti6Al4V powder was measured to determine the maximum achievable temperature and to monitor the thermal cycle. The surface temperature increases as the laser beam enters the measurement spot, rapidly reaching peak temperature before slowly receding to room temperature after the laser spot has passed. Three temperature transients were recorded and averaged for a range of scan speeds (10 mm/min to 500 mm/min). The maximum temperature attained is plotted in Fig. 8 for laser irradiation at both 808 nm and 450 nm. For both wavelengths, higher temperatures were recorded at slower scanning speeds, due to the higher energy input generated. The maximum temperature reached at each scanning speed is noticeably different for the two wavelengths, with the maximum surface temperature reached at 450 nm higher by approximately 12% compared to that at 808 nm. At 10 mm/min, the maximum temperature for 450 nm was 1920 0C and for 808 nm was 1760 0C. This 12% higher average temperature correlates well with the measured 11% higher absorption for the shorter wavelength light.
Temperature transients are plotted in Fig. 9 for 808-nm and 450-nm laser irradiation at a speed of 50 mm/min, showing the temperature within the measurement spot as the laser beam passes through. The 450-nm laser achieved a maximum temperature within 260 ms whereas the 808-nm laser achieved this after 530 ms. This phenomenon can be related to the absorption spectrum of Ti6Al4V powder, where more energy is absorbed and converted to heat at a shorter wavelength, allowing the shorter wavelength laser source to achieve a maximum temperature faster. However, at speeds of 50 mm/min or below, a large fluctuation in temperature of approximately ± 100 0C was observed, as can be seen in Fig. 9. This is possibly due to keyhole formation caused by the increase in interaction time, similar to the effect reported by Matthews et al. [28].
Influence of the wavelength on the morphology of single laser tracks
Single tracks were processed using 450-nm and 808-nm wavelength lasers in order to determine the influence of wavelength, and therefore absorptivity, on single-track geometric features. Surface morphology and cross-sectional geometric characteristics of single tracks were investigated. Table 5 documents the melt-pool depth and width for 14 sets of laser parameters that produced reportable results, i.e. some amount of melting was observed. The table represents the melt pool depth, width and the feature produced for different parameters.
Table 5 A summary of single-track processing parameters and resultant melt pool characteristics Melt pool top surface morphology
Figure 10 shows the top surface morphology of single tracks produced by the two different wavelength lasers for a range of scan speeds at fixed power (3.5 W). This determines whether the surface will exhibit a continuous smooth morphology, a coarse irregular morphology or contain a number of keyholes. Increasing the scanning speed results in narrower track width for both 450 nm and 808 nm. Further reduction of the scanning speed results in keyhole formation due to excessive energy input.
Morphology varied significantly with scan speed for both laser wavelengths. At high speeds above 300 mm/s, both lasers had insufficient energy to form a melt pool, and solid structures were not possible. This was a result of the lower peak temperature reached due to the rapidly moving laser source. Powder was sintered to some extent, but the resultant samples had little or no mechanical strength and easily crumbled when physically handled. Similar behaviour was observed at very low scan speeds of 10 mm/min or slower, in this case producing non-periodic keyholes. The keyholes can be attributed to the higher incident energies, where a high melt pool temperature is attained at slow scanning speeds.
For the 450-nm laser, the process window is much wider compared to that at 808 nm. This is due to higher absorptivity at the shorter wavelength. At 450 nm, a continuous and smooth top surface was formed at scanning speeds ranging from 50 to 200 mm/min (Fig. 10). However, at scanning speeds above 200 mm/min, the balling phenomena starts to appear until the energy input is insufficient to melt powder at speeds above 400 mm/min. This phenomenon is commonly observed for metals processed with lower energy densities, as reported by Yadroitsev et al. [29], where energy density was insufficient to melt powder at high scanning speeds resulting in severe balling. On the contrary, a stable process window for 808 nm is observed from 50 to 100 mm/min, with keyholes forming at 50 mm/min or below. Between 100 and 300 mm/min, we observe discontinuous melt pools with balling. Above 300 mm/min, the energy was found to be insufficient to form melt pools.
The width of the track generally increased with energy density; for the 450-nm laser, the track was generally wider than at 808 nm, due to higher absorption. This is illustrated by Fig. 11, which plots the average width of the melt pool track measured at the top surface as a function of scanning speed. For example, at 100 mm/ min, the width of the track was 208.2 μm when the 450-nm laser was used, compared to 182.8 μm for the 808-nm laser. The width of tracks processed using the 450-nm laser remained above 200 μm for speeds below 200 mm/min, whereas for 808 nm, the track width narrowed below 200 μm at speeds above 50 mm/min.
Four hundred fifty-nanometre lasers produced better track surface quality at a scan speed of 100 mm/min at 3.5 W compared to 808-nm laser as observed in Fig. 10. This power is substantially lower than that currently used in commercial SLM systems (typically 100–900 W) and anything reported in the literature. The 808-nm laser produced satisfactory results in terms of morphology, but at a slower speed of 50 mm/min due to its lower absorption compared to 450 nm. All of this has been achieved whilst exhibiting a high wall plug efficiency of 70% compared to the typical 20% of fibre lasers.
Morphology of cross-sectioned tracks
Scanning speed affects energy density and is therefore a dominant parameter in influencing the shape and morphology of a single track. When the scanning speed was below 50 mm/min, the energy input was high enough for lasers at both wavelengths to penetrate deeply and create keyholes. Figure 12 shows the cross-section of tracks processed with the 450-nm and 808-nm lasers at different scanning speeds, allowing comparison of the depth and width characteristics of the tracks. The depth and width of tracks reduce with increasing scan speed for both wavelengths. Furthermore, it can be noted that the penetration depth is 20–40% deeper for the 450-nm laser compared to 808 nm. Figure 13 shows the relation between the geometric features of single tracks and scanning speed, plotting the reduction in melt pool depth (a) and width (b) as scanning speed increases from 10 to 400 mm/min. For the same scanning speed, tracks produced using 450 nm light are generally wider than those using 808 nm (Fig. 13b). The track narrows from 416 to 165 μm with increasing scanning speed up to 400mm/min for 450 nm, whereas for 808 nm, the track width narrows from 395 to 281 μm for a maximum speed of 300 mm/min.
Wavelength also has a significant influence on the melt pool depth. This can be described using Fig. 13a, which plots the melt pool depth as a function of scan speed. At the same scan speed, keyhole formation occurred with a deeper penetration depth when processed with 450 nm compared with 808 nm. In addition, keyhole formation for 450 nm was more prominent at speeds below 50 mm/min, whereas for 808 nm, keyholes were observed for speeds below 10 mm/min. Four hundred fifty nanometre also exhibited deeper penetration than 808 nm. Generally, there is a wider processing window for 450 nm compared to 808 nm. This provides flexibility in terms of process adaptability and capacity to improve the SLM process. It also allows the use of lower powers and makes it possible to scan at faster speeds.
Multilayer fabrication
Processing regions for 450–808 nm powder bed fusion of Ti6Al4V
Several variables need to be considered in order to achieve high part density in SLM, such as scan speed, layer thickness, power and hatch distance. The combination of these variables needs to be carefully explored for any given laser power to avoid the introduction of defects related to insufficient wettability or poor overlapping. Results from the single-track experiments can provide an estimate of the melt pool morphology under different processing parameters, allowing a selection of suitable process parameters for fabrication of multilayer samples. In this section, the effect of wavelength on microstructure, part density and processing parameters is investigated.
According to our analysis of the dimensionless processing data (normalisation) discussed in Section 2.2.2, the key SLM parameters and their interaction with each other were considered to determine the minimum energy required to melt Ti6Al4V. Laser power P ( 3.5 W), scanning speed v (25–400 mm/min) hatch spacing Hd (100–200 μm) and layer thickness l (50–100 μm) were selected and normalised as summarised in Table 6. Multilayer samples were processed to a size of 7 mm × 7 mm × 2 mm. Figure 14 shows the normalised processing diagram, which represents the required energy input,\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \), to be absorbed by a material for specific volume 2rBl∗ as isopleth dashed lines. The y-axis \( \frac{\mathbf{1}}{{\boldsymbol{h}}^{\ast}} \) , where E0 on x-axis as log10 scale.
Table 6 Experimental parameters investigated for Ti6Al4V Accordingly, it was evident that a high value of (\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) > 8) would lead to excessive energy input which results in the formation of voids and keyholes. In contrast, low energy input (\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \)<2) will be insufficient to fuse the material or generate sufficient wettability, leading to imperfect parts. The highest density samples of density greater than 90% were produced in a region between 2 < \( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \)< 8 for selected laser power and wavelengths.
The effect of v∗ was more pronounced than h∗on the density of the parts. For instance, increasing the v∗ will provide\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) values below the threshold of the material. Adjustment of hatch distance to maintain the optimal\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) within the range of (2<\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) < 8) was not sufficient to improve the density of parts. As the scanning speed increased above v∗ = 0.072 (equivalent to 300 mm/min), an inconsistent melt pool was formed, as shown in Fig. 15. The optimal results were achieved at scanning speeds below v∗ < 0.048 (equivalent to 200 mm/min), whilst spattering was observed at v∗ < 0.012 (equivalent to 50 mm/min) as a result of excessive energy input. The maximum processing range was generally higher for 450 nm compared to 808 nm.
The effect of the normalised h∗was noticeable when the v∗ was within the effective range from 0.012 to 0.048 (equivalent to 50–200 mm/min). In general, the hatch distance affects the thermal history of the process, and therefore influences the microstructure, density and process efficiency [20]. As can be seen in Fig. 16, decreasing the overlap of laser paths by selecting a normalised overlap 1/h∗> 0.5 leads to excessive energy being delivered into the powder. This high energy causes vaporisation spatter and the formation of keyholes, which reduces part density, as shown in Fig. 16c. Reducing the 1/h∗ to <0.3 leads to poor weldability between the tracks resulting in sintered powder between tracks that deteriorates density and mechanical properties (Fig. 16a).
The normalised overlapping 1/h∗ within the range of 0.3–0.5 was found to be optimal for increased part density which also showed smoother surface finish as can be seen in Fig. 16b.
The layer thickness significantly affected the required energy to melt the material \( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \). The excessive\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) points on the normalised diagram were shifted from the “optimal” region to “insufficient” region when a layer thickness of 100 μm was applied. Correspondingly, the experimental results at a layer thickness of 100 μm showed insufficient bonding between layers. In contrast, the use of 50-μm layer thickness showed solid bonding and higher density parts. Therefore, a wider range of feasible processing parameters is permitted for layer thicknesses of 50 μm and below.
Microstructure and mechanical properties
Part density
By selecting the appropriate processing parameters associated with the SLM process, high density parts (> 90%) can be achieved. Figure 17a represents the density values of parts fabricated utilising 808-nm laser within the normalised range of 2 <\( {\boldsymbol{E}}_{\mathbf{0}}^{\ast } \) < 8. The density varies from 79.15 to 93.42% of the theoretical value implying the presence of deficiencies. The highest density of 93.42% was achieved at a scanning speed of 75 mm/s, hatch distance of 157 μm and 50-μm layer thickness, as shown in Fig. 18a. For a thick layer of 100 μm, higher energy input is needed to achieve sufficient bonding between layers. Such input cannot be achieved using this level of laser power even when scanning speeds are reduced. The density of specimens reduced as a consequence of applying excessive energy when a scanning speed of 50 mm/min was used or 100 μm hatch distance was applied.
The density of specimens fabricated using the 450-nm laser was similar to that of specimens fabricated with the 808-nm laser. Over the range of scanning speeds from 50 to 200 mm/min, the density of samples processed using 450nm varied between 83.31 and 94.16% of that of bulk material, as shown in Fig. 17b. For 450 nm, at a scanning speed of 25 mm/min, large holes and over-melting were evident in the specimen, resulting from excessive energy input. The maximum density of 94.16% was achieved at a scanning speed of 75 mm/min, as shown in the top surface microscope image in Fig. 18b. A maximum density of 93% is observed in specimens fabricated using 808 nm. This density can be achieved at 450 nm at a scanning speed of 100 mm/min. The slower scanning speeds can be expected to allow the melt pool to settle for longer in its molten state, resulting in a wider melt pool, with lower cooling rates potentially reducing stresses and resulting in an overall improved surface. By using 3.5 W laser of 450-nm wavelength, this study was able to manufacture parts of density above 94%, with further improvement, approaching comparable densities of > 99% manufactured by conventional 200–1000 W lasers. Therefore, as an alternative to ever-increasing laser powers in order to improve processing speed and part density (particularly for reflective materials), laser wavelength offers a further variable enabling low power diode lasers to process materials effectively. In general, defects in the sample which lower the density of fabricated parts in this study can be related to several “real world” uncertainties, such as instability in the laser focal length as the laser traverses the powder bed and the inaccuracy of the deposition system.
Microstructure (XRD)
The microstructure of Ti6Al4V is characterised by a combination of α phases and β phases at room temperature. These phases are related to the thermal gradient and the solidification of the melt pool in the SLM process [30]. Generally, parts produced by SLM predominantly show the ά martensite microstructures only, as a result of the fast cooling rate associated with the process [31]. In comparison to SLM, for Ti6Al4V by EBM, the temperature of the powder bed is normally held at 600 °C, which is above the temperature of martensitic transformation (575 °C). This leads to lamellar (α+ β) microstructure in the as-manufactured microstructure. The cooling rate is the influential factor that controls the transformation of ά martensite to (α+ β) during the process. As reported by Ahmed et al. [32], the ά phase forms at rapid cooling rates higher than 410 °C/s, which is exceeded in the SLM process. However, a cooling rate between 20 and 410 °C/s would give time for the β phase to form, which can either be achieved by maintaining the powder bed temperature above 575 °C or slow processing speed in order to reduce the cooling rate.
In this study, the relatively slow scanning speed of the diode laser maintains the temperature above β transus for a longer period of time compared to SLM, thereby reducing the cooling rate and promoting the development of the β phase. As a result, the XRD pattern in Fig. 19 shows a presence of two types of microstructures: ά phase and β phase with both laser wavelengths (450 and 808 nm).
The cooling rate in this study was calculated using Eq. (11). The pyrometer was used to measure the temperature transient. The cooling rate was calculated from the time taken for the temperature to drop from the β transus temperature (Tβ transus = 994 °C) to the end of the martensitic transformation temperature (Tms= 575 °C), as described for Ti6Al4V by Ahmed and Rack [32]. In this study, the range of parameters used developed a cooling rate in the range of 750 to 1400 oC/S. Even though the cooling rate of the DAM process exceeded the critical cooling rate of 410 oC/s, it is still comparatively slower than SLM and EBM. Table 7 summarises the different processes and both the cooling rate and microstructure associated with the different process parameters. The high absorptivity of 450-nm and 808-nm lasers allows the use of low powers at slow scanning speeds ranging from 75 to 100 mm/min. This maintains the temperature above the β transus for a longer period of time, thus reducing the cooling rate and developing the β phase in as-built samples, similar to results achieved by Simonelli et al. [33]. The author successfully obtained α + β microstructure in the SLM process by reducing laser power and scanning speed, which as a result increased the diffusion time and reduced the cooling rate.
$$ \mathrm{Cooling}\ \mathrm{rate}\ \left({}^{\circ}\mathrm{C}{s}^{-1}\right)=\frac{\Delta \mathrm{T}}{\Delta \mathrm{t}}=\left|\frac{{\mathrm{T}}_{\upbeta\ \mathrm{transus}}\ \left({}^{\circ}\mathrm{C}\right)-{\mathrm{T}}_{\mathrm{ms}}\ \left({}^{\circ}\mathrm{C}\right)}{{\mathrm{t}}_{\upbeta\ \mathrm{transus}}\left(\mathrm{s}\right)-{\mathrm{t}}_{\mathrm{ms}}\left(\mathrm{s}\right)}\right| $$
(11)
Table 7 A comparsion of cooling rate and corresponding microstructures of Ti6Al4V processed using SLM ,EBM and DAM
The polarised light micrograph was used to identify the top surface microstructure of specimens as shown in Fig. 20. The microstructure was dominated by a mixture of Widmanstätten and Martensite. Figure 20b shows that ά has decomposed into equilibrium (α+β) basketweave microstructure with different sizes and orientations, using the 450-nm laser. Similar results obtained with a slightly higher amount of martensite ά microstructure compared with 450 nm, as shown in Fig. 20a. This can be related to the high absorption of 450 nm which is prolonging the time above the transus temperature and decreasing the cooling rate.
Nanoindentations (hardness and elastic modulus)
In this section, the top surface of the highest density parts is further investigated for their hardness and elastic properties using the nanoindentation technique suggested by Fischer-Cripps [35]. In general, the formation of the microstructure (Widmanstätten and Martensite) in final parts has a significant influence on mechanical properties. According to He et al., the presence of Martensite (ά) microstructure leads to increase hardness of parts and decrease elasticity [36]. The measured microhardness by Thijs et al. of SLM parts has a Vickers hardness within the range of 381–479 (3.70–4.69 GPa) [31]. He et al. also reported the microhardness to be 395 Hv (3.7GPa) and the elastic modulus was 107 GPa [36]. On the other hand, the microhardness of EBM parts was around 3.2–3.5 GPa and the elastic modulus was 118 GPa as reported by Facchini et al. [37]. In this study, the nanoindentation hardness of parts processed using the 450-nm laser and 808 nm was found to be 4.59 GPa and 4.7 GPa, respectively. The elastic modulus for 450 nm and 808 nm was measured to be 114 GPa and 111 GPa, respectively. Figure 21 plots the average hardness and elastic modulus for samples produced at laser power of 3.5 W, scanning speed 75 mm/min and hatch distance 157 μm.