Microstructure and Corrosion Properties of CP-Ti Processed by Laser Powder Bed Fusion under Similar Energy Densities

doi:10.1007/s40195-022-01376-9

Abstract

Abstract:

In this work, two types of CP Ti cubes with similar volumetric energy densities (VED) but different process parameters were produced using laser powder bed fusion (LPBF) method. The corrosion behavior of the fabricated specimens was investigated by conducting electrochemical impedance spectroscopy (EIS) and polarization experiments in simulated body fluid (SBF) solution at 37 °C. The results indicated that the microstructure and porosities, which are of great importance for biomedical applications, can be controlled by changing the process parameters even under constant energy densities. The sample produced with a lower laser power (E1) was featured with a higher level of porosity and thinner alpha laths, as compared with the sample fabricated with a higher laser power (E2). Moreover, results obtained from the bioactivity tests revealed that the sample produced with a higher laser power conferred a slight improvement in the bioactivity due to the higher amount of porosity. Lower laser power and hence higher porosity level promoted the formation of bone-like apatite on the surface of the printed specimens. The potentiodynamic polarization tests revealed inferior corrosion resistance for the fabricated sample with higher porosity. Moreover, the EIS results after different immersion times indicated that a stable oxide film was formed on the surface of samples for all immersion times. After 1 and 3 days of immersion, superior passivation behavior was observed for the sample fabricated with lower laser power. However, very similar impedance and phase values were observed for all the samples after 14 days of immersion.

Key words: Additive manufacturing, Laser powder bed fusion, Energy density, Corrosion, Microstructure, CP Titanium

Mohammad Hossein Mosallanejad, Saber Sanaei, Masoud Atapour, Behzad Niroumand, Luca Iuliano, Abdollah Saboori. Microstructure and Corrosion Properties of CP-Ti Processed by Laser Powder Bed Fusion under Similar Energy Densities[J]. Acta Metallurgica Sinica (English Letters), 2022, 35(9): 1453-1464.

Figures/Tables 15

Fig. 1 a Spherical powders of commercially pure Ti used in this work, b schematic of the produced samples along with the analyzed plane

Table 1 LPBF process parameters used for the manufacturing of the samples

Sample	P (W)	V (mm/s)	h (mm)	d (mm)	VED (J/mm³)
E1	75	700	0.098	0.025	43.73
E2	95	900	0.098	0.025	43.08

Table 2 Properties of Ti used in the Rosenthal equation

Melting point (K)	Thermal conductivity (W/m K)	Thermal diffusivity (m²/s)	Substrate temperature (K)	Laser absorption coefficient during LPBF
1940	31 [38]	0.9 × 10^-5 [39]	298	0.56 [40]

Table 3 Chemical composition of the used SBF solution

Reagent	Composition (g/l)
NaCl	8.035
KCl	0.225
CaCl₂	0.292
NaHCO₃	0.355
Na₂SO₄	0.072
MgCl₂·6H₂O	0.311
K₂HPO₄·3H₂O	0.231
1.0_M-HCl	39 ml

Fig. 2 Low magnification SEM micrographs of a sample E1, b sample E2, and high magnification SEM micrographs of c sample E1, d sample E1

Fig. 3 Melt pool geometry simulated by Rosenthal equation: a XZ view, b XY view

Fig. 4 Impedance spectra of E2 (a, b, c), E1 (d, e, f) samples recorded after different immersion time in SBF solution: a, c Bode-Phase (log|Z| vs. log f) and b, d Bode-Z (phase angle vs. log f)

Fig. 5 Equivalent circuits used for fitting the EIS data of E1 and E2 samples after immersed in SBF solution for first days 1, 3, 7 (a), last days 14 days (b)

Table 4 Fitted results of the EIS data of the E2 samples after different immersion time in SBF solution

Materials/conditions	R_s (Ω cm²)	CPE_dl (F ${\mathrm{cm}}^{-2} {\mathrm{s}}^{ -n}$)	n₁	R_ct (Ω cm²)	CPE_dl (F ${\mathrm{cm}}^{-2} {\mathrm{s}}^{ -n}$)	n₂	R_coat (Ω cm²)	R_p
Day1	50.10	1.72 × ${10}^{-5}$	0.88	8.00 × ${10}^{5}$	-	-	-	8.10 × ${10}^{5}$
Day3	40.41	5.60 × ${10}^{-5}$	0.75	3.15 × ${10}^{5}$	-	-	-	3.15 × ${10}^{5}$
Day7	55.21	8.42 × ${10}^{-5}$	0.72	2.81 × ${10}^{5}$	-	-	-	2.81 × ${10}^{5}$
Day14	30.43	3.91 × ${10}^{-5}$	0.79	4.43 × ${10}^{5}$	9.01 × ${10}^{-5}$	0.60	150	4.43 × ${10}^{5}$

Table 5 Fitted data of the results of EIS tests of E1 samples after different immersion time in SBF solution

Materials/ conditions	R_s (Ω cm²)	CPE_dl (F ${\mathrm{cm}}^{-2} {\mathrm{s}}^{ -n}$)	n₁	R_ct (Ω cm²)	CPE_dl (F ${\mathrm{cm}}^{-2} {\mathrm{s}}^{ -n}$)	n₂	R_coat (Ω cm²)	R_p
Day1	40.28	1.18 × ${10}^{-5}$	0.83	4.38 × ${10}^{5}$	-	-	-	4.38 × ${10}^{5}$
Day3	37.07	3.58 × ${10}^{-5}$	0.80	2.10 × ${10}^{5}$	-	-	-	2.10 × ${10}^{5}$
Day7	24.21	1.84 × ${10}^{-5}$	0.78	2.18 × ${10}^{5}$	1.67 × ${10}^{-4}$	0.62	321	2.18 × ${10}^{5}$
Day14	30.43	6.58 × ${10}^{-5}$	0.81	4.75 × ${10}^{5}$	6.34 × ${10}^{-5}$	0.66	8160	4.83 × ${10}^{5}$

Fig. 6 Potentiodynamic polarization results and SEM images recorded for E1 (a, c), E2 (b, d) after polarization tests after 14 days in SBF solution

Table 6 Results obtained from potentiodynamic polarization curves for E1 and E2 samples after 1 and 14 days immersion in SBF solution

	Day	i_corr (A/cm²)	E_corr (V)
E1	1	4.4 × 10^-8 (± 0.08)	- 0.407 (± 0.01)
E1	14	6.3 × 10^-8 (± 0.09)	- 0.303 (± 0.02)
E2	1	2.3 × 10^-8 (± 0.01)	- 0.515 (± 0.03)
E2	14	5.7 × 10^-8 (± 0.02)	- 0.108 (± 0.01)

Fig. 7 SEM images and elemental analysis of E1 (a-c), E2 (d-f) samples immersed in SBF solution for 21 days

Fig. 8 SEM analyses of the surface of E1 (a) and E2 (b) samples after 21 days immersion in SBF

Fig. 9 a pH value of SBF solutions during soaking of samples and b changes in the concentration of calcium and phosphorus ions in SBF solution during 1 and 21 days

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