Pub Date : 2024-11-10DOI: 10.1016/j.mtla.2024.102290
Y. Sakamoto , S. Ishihara , K. Masuda , W. Yamazaki , M. Shimura
In Sn/Cu plating, whiskers are formed because of the formation of intermetallic compounds (IMCs) at the Sn/Cu interface and along the Sn grain boundaries. Many previous studies have focused on the mechanism of whisker formation and the change in whisker density over time. However, only a few studies have focused on the formation and growth behavior of IMCs and the correlation between IMCs and whiskers. Furthermore, no studies have quantitatively investigated the time-dependent changes in the formation and growth behavior of IMCs and whiskers using mathematical formulas. In this study, Sn/Cu plating was applied to a 7–3 brass substrate, and the formation and growth of IMCs at the Sn/Cu interface and the behavior of whisker formation were studied. An approximate equation was derived based on the reaction kinetics to quantitatively express the time-dependent changes in both parameters. Three differences were observed between the formation behaviors of IMCs and whiskers. First, no incubation time tth was observed for IMC formation, but it was for whiskers. Second, the whisker density increased until t = 10 d and then saturated. However, the IMC density increased until t = 70 d and then became saturated. Third, the IMC density in the cross section is 7–10 times higher than the whisker density, and the rate constant of the IMCs is smaller than that of the whiskers.
在锡/铜电镀过程中，由于金属间化合物（IMC）在锡/铜界面和锡晶界的形成，会形成晶须。以前的许多研究都侧重于晶须形成的机理以及晶须密度随时间的变化。然而，只有少数研究关注 IMC 的形成和生长行为，以及 IMC 和晶须之间的相关性。此外，还没有研究使用数学公式对 IMC 和晶须的形成和生长行为随时间的变化进行定量研究。本研究将锡/铜电镀应用于 7-3 黄铜基底，研究了锡/铜界面上 IMC 的形成和生长以及晶须的形成行为。根据反应动力学推导出了一个近似方程，以定量表示这两个参数随时间的变化。在 IMC 和晶须的形成行为之间观察到三个不同点。首先，IMC 的形成没有孵育时间 tth，而晶须的形成有孵育时间 tth。其次，晶须密度在 t = 10 d 前一直在增加，然后达到饱和。然而，IMC 密度在 t = 70 d 前一直在增加，然后趋于饱和。第三，横截面上的 IMC 密度是晶须密度的 7-10 倍，IMC 的速率常数小于晶须的速率常数。
{"title":"Study on changes in intermetallic compounds and whisker formation over time in Sn/Cu plating","authors":"Y. Sakamoto , S. Ishihara , K. Masuda , W. Yamazaki , M. Shimura","doi":"10.1016/j.mtla.2024.102290","DOIUrl":"10.1016/j.mtla.2024.102290","url":null,"abstract":"<div><div>In Sn/Cu plating, whiskers are formed because of the formation of intermetallic compounds (IMCs) at the Sn/Cu interface and along the Sn grain boundaries. Many previous studies have focused on the mechanism of whisker formation and the change in whisker density over time. However, only a few studies have focused on the formation and growth behavior of IMCs and the correlation between IMCs and whiskers. Furthermore, no studies have quantitatively investigated the time-dependent changes in the formation and growth behavior of IMCs and whiskers using mathematical formulas. In this study, Sn/Cu plating was applied to a 7–3 brass substrate, and the formation and growth of IMCs at the Sn/Cu interface and the behavior of whisker formation were studied. An approximate equation was derived based on the reaction kinetics to quantitatively express the time-dependent changes in both parameters. Three differences were observed between the formation behaviors of IMCs and whiskers. First, no incubation time t<sub>th</sub> was observed for IMC formation, but it was for whiskers. Second, the whisker density increased until t = 10 d and then saturated. However, the IMC density increased until t = 70 d and then became saturated. Third, the IMC density in the cross section is 7–10 times higher than the whisker density, and the rate constant of the IMCs is smaller than that of the whiskers.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102290"},"PeriodicalIF":3.0,"publicationDate":"2024-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656466","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-09DOI: 10.1016/j.mtla.2024.102289
Pengyuan Li , Hongyong Xia , Wei Shang , Shuang Zhang , Xiang Li , Yongqing Fu , Junjie Xu , Longlong Dong
CoCrFeNi high-entropy alloy (HEA) has distinctive properties such as high hardness and good corrosion resistance, however, its low strength or poor yield strength at room temperature limits its wide-range applications in industry. Herein, Cr23C6 particles reinforced CoCrFeNi composites with graphene nanoplates as a precursor were fabricated using in-situ reaction spark plasma sintering and cold rolling annealing processes. Results showed that the microstructure of the CoCrFeNi HEA and their composites were face-centered cubic structures before and after annealing, and Cr23C6 particles were precipitated inside the matrix during SPS. The precipitated Cr23C6 particles exerted strong pinning forces to migrate dislocations and grain boundaries, effectively refining the grains during the annealing process. After cold rolling, Cr23C6/CoCrFeNi composites showed a typically banded deformation structure. After annealing, fine equiaxed grains were distributed around the deformed grains, and the proportion of equiaxed grains was increased with the annealing time. The yield strength (YS) of Cr23C6/CoCrFeNi composites was significantly higher than that of CoCrFeNi alloy after cold rolling and annealing. When annealed for 20 min, the YS and elongation of Cr23C6/CoCrFeNi composites with 0.3 wt% graphene addition were 1100 MPa and 6 %, respectively. The YS was 68.2 % higher than that of the CoCrFeNi alloy. We have identified that the improvement of mechanical properties of Cr23C6/CoCrFeNi composites is mainly attributed to grain refinement, dislocation strengthening, precipitation strengthening, and load transfer strengthening, among which dislocation strengthening plays a major role.
{"title":"Interfacial engineering reaction strategy of in-situ Cr23C6/CoCrFeNi composites with network structure for high yield strength","authors":"Pengyuan Li , Hongyong Xia , Wei Shang , Shuang Zhang , Xiang Li , Yongqing Fu , Junjie Xu , Longlong Dong","doi":"10.1016/j.mtla.2024.102289","DOIUrl":"10.1016/j.mtla.2024.102289","url":null,"abstract":"<div><div>CoCrFeNi high-entropy alloy (HEA) has distinctive properties such as high hardness and good corrosion resistance, however, its low strength or poor yield strength at room temperature limits its wide-range applications in industry. Herein, Cr<sub>23</sub>C<sub>6</sub> particles reinforced CoCrFeNi composites with graphene nanoplates as a precursor were fabricated using <em>in-situ</em> reaction spark plasma sintering and cold rolling annealing processes. Results showed that the microstructure of the CoCrFeNi HEA and their composites were face-centered cubic structures before and after annealing, and Cr<sub>23</sub>C<sub>6</sub> particles were precipitated inside the matrix during SPS. The precipitated Cr<sub>23</sub>C<sub>6</sub> particles exerted strong pinning forces to migrate dislocations and grain boundaries, effectively refining the grains during the annealing process. After cold rolling, Cr<sub>23</sub>C<sub>6</sub>/CoCrFeNi composites showed a typically banded deformation structure. After annealing, fine equiaxed grains were distributed around the deformed grains, and the proportion of equiaxed grains was increased with the annealing time. The yield strength (YS) of Cr<sub>23</sub>C<sub>6</sub>/CoCrFeNi composites was significantly higher than that of CoCrFeNi alloy after cold rolling and annealing. When annealed for 20 min, the YS and elongation of Cr<sub>23</sub>C<sub>6</sub>/CoCrFeNi composites with 0.3 wt% graphene addition were 1100 MPa and 6 %, respectively. The YS was 68.2 % higher than that of the CoCrFeNi alloy. We have identified that the improvement of mechanical properties of Cr<sub>23</sub>C<sub>6</sub>/CoCrFeNi composites is mainly attributed to grain refinement, dislocation strengthening, precipitation strengthening, and load transfer strengthening, among which dislocation strengthening plays a major role.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102289"},"PeriodicalIF":3.0,"publicationDate":"2024-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-07DOI: 10.1016/j.mtla.2024.102283
Zhening Yang , Alexander Richter , Hui Sun , Zi-Kui Liu , Allison M. Beese
In joining Fe-alloys and Cu-containing alloys to access the high strength of steels and corrosion resistance of Cu-alloy, cracking is widely observed due to the significant Cu microsegregation during the solidification process, resulting in an interdendritic Cu-rich liquid film at the end of solidification. By fabricating functionally graded materials (FGMs) that incorporate additional elements like Ni in the transition region between these terminal alloy classes, the hot cracking can be reduced. In the present work, the joining of stainless steel 316L (SS316L) and Monel400 by modifying the Ni concentration in the gradient region was studied. A new hot cracking criterion based on hybrid Scheil-equilibrium approach was developed and validated with monolithic multi-layer samples within the SS316L-Ni-Monel400 three-alloy system and a SS316L to 55/45 wt% SS316L/Ni to Monel400 FGM sample fabricated by direct energy deposition (DED). The new hot cracking criterion, based on the hybrid Scheil-equilibrium approach, is expected to help design FGM paths between other Fe-alloys and Cu-containing alloys as well.
{"title":"Circumventing cracking in grading 316L stainless steel to Monel400 through compositional modifications in directed energy deposition","authors":"Zhening Yang , Alexander Richter , Hui Sun , Zi-Kui Liu , Allison M. Beese","doi":"10.1016/j.mtla.2024.102283","DOIUrl":"10.1016/j.mtla.2024.102283","url":null,"abstract":"<div><div>In joining Fe-alloys and Cu-containing alloys to access the high strength of steels and corrosion resistance of Cu-alloy, cracking is widely observed due to the significant Cu microsegregation during the solidification process, resulting in an interdendritic Cu-rich liquid film at the end of solidification. By fabricating functionally graded materials (FGMs) that incorporate additional elements like Ni in the transition region between these terminal alloy classes, the hot cracking can be reduced. In the present work, the joining of stainless steel 316L (SS316L) and Monel400 by modifying the Ni concentration in the gradient region was studied. A new hot cracking criterion based on hybrid Scheil-equilibrium approach was developed and validated with monolithic multi-layer samples within the SS316L-Ni-Monel400 three-alloy system and a SS316L to 55/45 wt% SS316L/Ni to Monel400 FGM sample fabricated by direct energy deposition (DED). The new hot cracking criterion, based on the hybrid Scheil-equilibrium approach, is expected to help design FGM paths between other Fe-alloys and Cu-containing alloys as well.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102283"},"PeriodicalIF":3.0,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-07DOI: 10.1016/j.mtla.2024.102282
Emanuela Cerri, Emanuele Ghio
Al-Si-Mg alloys are widely used for manufacturing components via laser powder bed fusion in various industrial applications where ductility and the capacity to accommodate the strain hardening are key criteria. The ductility of the laser powder bed-fused Al alloys has become a crucial property due to their fine cellular microstructure. Post-processing heat treatments improve ductility, but resultant microstructural changes affect the work-hardening behaviour, deformability, and uniform elongation values. This study aims to investigate the work-hardening capability, uniform elongation and deformability of AlSi7Mg and AlSi10Mg samples after different post-processing heat treatments by using tensile tests, optical and scanning electron microscopies. At aging temperatures below 200 °C, the fully cellular structure of eutectic Si governs both the work-hardening behaviour and the strengthening mechanisms, despite the precipitation phenomenon. When direct-aging temperatures exceed 200 °C, the coarsening of the Si-eutectic network modifies work-hardening behavior (Stages 1–3), accentuating the effects induced by the precipitates. Artificial aging highlights the role of precipitates in controlling both work-hardening properties and deformability.
{"title":"On the work-hardening behaviour of the additively manufactured Al-Si-Mg alloys: Composite-like versus networked microstructure","authors":"Emanuela Cerri, Emanuele Ghio","doi":"10.1016/j.mtla.2024.102282","DOIUrl":"10.1016/j.mtla.2024.102282","url":null,"abstract":"<div><div>Al-Si-Mg alloys are widely used for manufacturing components via laser powder bed fusion in various industrial applications where ductility and the capacity to accommodate the strain hardening are key criteria. The ductility of the laser powder bed-fused Al alloys has become a crucial property due to their fine cellular microstructure. Post-processing heat treatments improve ductility, but resultant microstructural changes affect the work-hardening behaviour, deformability, and uniform elongation values. This study aims to investigate the work-hardening capability, uniform elongation and deformability of AlSi7Mg and AlSi10Mg samples after different post-processing heat treatments by using tensile tests, optical and scanning electron microscopies. At aging temperatures below 200 °C, the fully cellular structure of eutectic Si governs both the work-hardening behaviour and the strengthening mechanisms, despite the precipitation phenomenon. When direct-aging temperatures exceed 200 °C, the coarsening of the Si-eutectic network modifies work-hardening behavior (Stages 1–3), accentuating the effects induced by the precipitates. Artificial aging highlights the role of precipitates in controlling both work-hardening properties and deformability.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102282"},"PeriodicalIF":3.0,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656462","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-06DOI: 10.1016/j.mtla.2024.102286
Christopher M. Sample, Anthony G. Spangenberger, Diana A. Lados
Cold spray is an additive manufacturing process that accelerates powder particles to supersonic speeds to create repairs and bulk depositions with fine-grained microstructures, high density, and good mechanical properties. Fatigue property measurement for these novel materials is critical for their use in safety-critical components, which can be accelerated with the use of ultrasonic fatigue testing. In this work, ultrasonic (20 kHz) and conventional (20 Hz) fatigue studies were conducted on as-sprayed bulk Al-6061 and conventional wrought Al-6061-T6. Complementary fatigue studies of surface preparation (surface finish and residual stress) and fatigue specimen geometry (round versus flat), as well as hole-drilling residual stress measurements, were undertaken to minimize the influence of these confounding variables. Cold spray Al-6061 exhibits fatigue frequency sensitivity, whereas the wrought material does not. Tensile testing at varied strain rates indicates that a portion of the fatigue frequency effect can be attributed to strain rate sensitivity. Fractographic studies show that crack initiation occurs from unbonded powder particles at the surface at high stress amplitude, and transitions sub-surface at lower stress amplitude. The results of these studies were used to create frequency-corrective models of S-N data and Kitagawa-Takahashi diagrams that can be used to design for fatigue crack initiation and growth resistance.
{"title":"Ultrasonic and conventional fatigue behavior, strain rate sensitivity, and structural design methods for wrought and cold spray Al-6061","authors":"Christopher M. Sample, Anthony G. Spangenberger, Diana A. Lados","doi":"10.1016/j.mtla.2024.102286","DOIUrl":"10.1016/j.mtla.2024.102286","url":null,"abstract":"<div><div>Cold spray is an additive manufacturing process that accelerates powder particles to supersonic speeds to create repairs and bulk depositions with fine-grained microstructures, high density, and good mechanical properties. Fatigue property measurement for these novel materials is critical for their use in safety-critical components, which can be accelerated with the use of ultrasonic fatigue testing. In this work, ultrasonic (20 kHz) and conventional (20 Hz) fatigue studies were conducted on as-sprayed bulk Al-6061 and conventional wrought Al-6061-T6. Complementary fatigue studies of surface preparation (surface finish and residual stress) and fatigue specimen geometry (round versus flat), as well as hole-drilling residual stress measurements, were undertaken to minimize the influence of these confounding variables. Cold spray Al-6061 exhibits fatigue frequency sensitivity, whereas the wrought material does not. Tensile testing at varied strain rates indicates that a portion of the fatigue frequency effect can be attributed to strain rate sensitivity. Fractographic studies show that crack initiation occurs from unbonded powder particles at the surface at high stress amplitude, and transitions sub-surface at lower stress amplitude. The results of these studies were used to create frequency-corrective models of S-N data and Kitagawa-Takahashi diagrams that can be used to design for fatigue crack initiation and growth resistance.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102286"},"PeriodicalIF":3.0,"publicationDate":"2024-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142700377","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-05DOI: 10.1016/j.mtla.2024.102284
Sunando Banerjee, Akhand Pratap Singh, G. Mohan Kumar, Chandan Srivastava
Microstructural evolution, electrochemical corrosion and hydrogen permeation in pulse electrodeposited Ni-Mo coatings (2, 4, 8, and 11wt% Mo) were investigated. Electrochemical impedance spectroscopy and potentiodynamic polarization measurements revealed improved corrosion resistance at an optimum Mo content. The corrosion current density icorr and polarization resistance Rp values obtained were 13.8 μA/cm2 and 1745 Ωcm2 respectively for pure Ni coating while the icorr and Rp values obtained were 1.7 μA/cm2 and 5406 Ωcm2 respectively for Ni-4wt% Mo coating. Further, increase in the Mo content beyond 4 wt% increased the corrosion rate. Nevertheless, corrosion resistance of Ni-Mo coatings was found to be higher than the pure Ni coating. Ni-Mo coatings contained relatively Mo-enriched clusters in a solid solution matrix. The highest corrosion resistance of Ni-4wt% Mo coating was due to lower energy (001) and (111) textures, lower energy grain boundary constitution, and low coating strain. In Ni-4wt% Mo coating, Mo-enriched Ni-Mo nanoclusters inhibited hydrogen passage by providing a torturous path. In contrast, a high fraction of high-angle grain boundaries (compared to pure Ni coating) facilitated hydrogen permeation leading to a similar extent of hydrogen permeation through pure Ni and Ni-4wt% Mo coatings.
研究了脉冲电沉积镍钼涂层（2、4、8 和 11wt% Mo）的微观结构演变、电化学腐蚀和氢渗透。电化学阻抗谱和电位极化测量结果表明，在最佳钼含量下，耐腐蚀性能有所提高。纯 Ni 涂层的腐蚀电流密度 icorr 和极化电阻 Rp 值分别为 13.8 μA/cm2 和 1745 Ωcm2，而 Ni-4wt% Mo 涂层的 icorr 和 Rp 值分别为 1.7 μA/cm2 和 5406 Ωcm2。此外，当 Mo 含量超过 4 wt% 时，腐蚀速率也会增加。尽管如此，Ni-Mo 涂层的耐腐蚀性仍高于纯 Ni 涂层。镍钼涂层在固溶体基体中含有相对富集的钼簇。镍-4wt%钼涂层的耐腐蚀性能最高是由于较低能量的（001）和（111）纹理、较低能量的晶界构成以及较低的涂层应变。在镍-4wt%钼涂层中，钼富集的镍-钼纳米团簇提供了一条曲折的路径，从而抑制了氢的通过。相反，高角度晶界的高比例（与纯镍涂层相比）促进了氢的渗透，导致氢在纯镍和 Ni-4wt% Mo 涂层中的渗透程度相似。
{"title":"Effect of texture, grain boundary constitution, and molybdenum partitioning on corrosion and hydrogen permeation behavior of pulse electrodeposited Ni-Mo coatings","authors":"Sunando Banerjee, Akhand Pratap Singh, G. Mohan Kumar, Chandan Srivastava","doi":"10.1016/j.mtla.2024.102284","DOIUrl":"10.1016/j.mtla.2024.102284","url":null,"abstract":"<div><div>Microstructural evolution, electrochemical corrosion and hydrogen permeation in pulse electrodeposited Ni-Mo coatings (2, 4, 8, and 11wt% Mo) were investigated. Electrochemical impedance spectroscopy and potentiodynamic polarization measurements revealed improved corrosion resistance at an optimum Mo content. The corrosion current density <em>i<sub>corr</sub></em> and polarization resistance <em>R<sub>p</sub></em> values obtained were 13.8 μA/cm<sup>2</sup> and 1745 Ωcm<sup>2</sup> respectively for pure Ni coating while the <em>i<sub>corr</sub></em> and <em>R<sub>p</sub></em> values obtained were 1.7 μA/cm<sup>2</sup> and 5406 Ωcm<sup>2</sup> respectively for Ni-4wt% Mo coating. Further, increase in the Mo content beyond 4 wt% increased the corrosion rate. Nevertheless, corrosion resistance of Ni-Mo coatings was found to be higher than the pure Ni coating. Ni-Mo coatings contained relatively Mo-enriched clusters in a solid solution matrix. The highest corrosion resistance of Ni-4wt% Mo coating was due to lower energy (001) and (111) textures, lower energy grain boundary constitution, and low coating strain. In Ni-4wt% Mo coating, Mo-enriched Ni-Mo nanoclusters inhibited hydrogen passage by providing a torturous path. In contrast, a high fraction of high-angle grain boundaries (compared to pure Ni coating) facilitated hydrogen permeation leading to a similar extent of hydrogen permeation through pure Ni and Ni-4wt% Mo coatings.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102284"},"PeriodicalIF":3.0,"publicationDate":"2024-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656570","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-05DOI: 10.1016/j.mtla.2024.102285
Masoud Shekargoftar , Samira Ravanbakhsh , Vinicius Sales de Oliveira , Joseph Buhagiar , Nicolas Brodusch , Stéphanie Bessette , Carlo Paternoster , Frank Witte , Andranik Sarkissian , Raynald Gauvin , Diego Mantovani
Magnesium (Mg) alloys have emerged as promising materials for biodegradable implants in orthopedic, oral, and cardiovascular applications. Despite their potential, high corrosion rate, and release of diatomic hydrogen in the surrounding environment remain the unmet challenges. In this research, oxygen plasma ion immersion implantation (O-PIII) was investigated in an attempt to modify the degradation rate of Mg-2Y-2Zn-1Mn alloy. In particular, the effects of pulse duration (tpd) and pressure (p) on the degradation rate were investigated. For all the investigated conditions, plasma treatment enriched the surface chemical composition with O, forming a Mg- and Y- rich oxide layer. Mg and Y elements were mainly concentrated at grain boundaries. The concurrent phenomena of sputtering and energetic implantation led to crystalline Y2O3 formation. Electrochemical investigations confirm that the degradation rate of samples decreased significantly, from ∼0.23 mm/y for untreated to ∼0.07 mm/y for O-PIII conditions. These findings demonstrate the effectiveness of O-PIII in changing surface properties and controlling corrosion rate of Mg alloys.
{"title":"Effects of plasma surface modification of Mg-2Y-2Zn-1Mn for biomedical applications","authors":"Masoud Shekargoftar , Samira Ravanbakhsh , Vinicius Sales de Oliveira , Joseph Buhagiar , Nicolas Brodusch , Stéphanie Bessette , Carlo Paternoster , Frank Witte , Andranik Sarkissian , Raynald Gauvin , Diego Mantovani","doi":"10.1016/j.mtla.2024.102285","DOIUrl":"10.1016/j.mtla.2024.102285","url":null,"abstract":"<div><div>Magnesium (Mg) alloys have emerged as promising materials for biodegradable implants in orthopedic, oral, and cardiovascular applications. Despite their potential, high corrosion rate, and release of diatomic hydrogen in the surrounding environment remain the unmet challenges. In this research, oxygen plasma ion immersion implantation (O-PIII) was investigated in an attempt to modify the degradation rate of Mg-2Y-2Zn-1Mn alloy. In particular, the effects of pulse duration (<em>t<sub>pd</sub></em>) and pressure (<em>p</em>) on the degradation rate were investigated. For all the investigated conditions, plasma treatment enriched the surface chemical composition with O, forming a Mg- and Y- rich oxide layer. Mg and Y elements were mainly concentrated at grain boundaries. The concurrent phenomena of sputtering and energetic implantation led to crystalline Y<sub>2</sub>O<sub>3</sub> formation. Electrochemical investigations confirm that the degradation rate of samples decreased significantly, from ∼0.23 mm/y for untreated to ∼0.07 mm/y for O-PIII conditions. These findings demonstrate the effectiveness of O-PIII in changing surface properties and controlling corrosion rate of Mg alloys.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102285"},"PeriodicalIF":3.0,"publicationDate":"2024-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656510","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ultrastructure and organisation of collagen fibres is essential to tissue function, due to the loadbearing properties of collagen. Current techniques used to create aligned collagen tissue equivalents use the contractile ability of cells to remodel and align collagen fibres or utilise highly specialised pieces of equipment. The aim of this study is to develop a novel and rapid method to produce acellular aligned collagen sheets by combining horizontal shear flow (HSFlow) and the established RAFT method to remove excess fluid from a hydrogel.
Force applied to the gel during the HSFlow process was measured to allow replication of the method. Quantification of fibres and cellular alignment revealed a significant difference between HSFlow and control samples, where both cells and collagen fibres showed alignment in the direction of shear flow, compared to the randomly aligned RAFT controls. Mechanical properties were also measured and revealed that HSFlow does not appear to improve the strength of the constructs despite the improved alignment, therefore further optimisation is needed to strengthen the constructs.
In conclusion, we developed a novel and rapid technique to generate flat sheets of aligned collagen without relying on the contractile ability of cells to rearrange collagen fibres. This rapid method has potential to be used in the fabrication of a scaffold to mimic anisotropic tissues for regenerative medicine.
{"title":"Rapid biofabrication of cell-free, anisotropic collagen tissues using a novel horizontal shear flow technique","authors":"Alessandra Grillo , Maria Caluianu , Augustin Barna , Avantika Mair , Arnau Garriga Casanovas , Vivek Mudera , Alvena Kureshi","doi":"10.1016/j.mtla.2024.102281","DOIUrl":"10.1016/j.mtla.2024.102281","url":null,"abstract":"<div><div>Ultrastructure and organisation of collagen fibres is essential to tissue function, due to the loadbearing properties of collagen. Current techniques used to create aligned collagen tissue equivalents use the contractile ability of cells to remodel and align collagen fibres or utilise highly specialised pieces of equipment. The aim of this study is to develop a novel and rapid method to produce acellular aligned collagen sheets by combining horizontal shear flow (HSFlow) and the established RAFT method to remove excess fluid from a hydrogel.</div><div>Force applied to the gel during the HSFlow process was measured to allow replication of the method. Quantification of fibres and cellular alignment revealed a significant difference between HSFlow and control samples, where both cells and collagen fibres showed alignment in the direction of shear flow, compared to the randomly aligned RAFT controls. Mechanical properties were also measured and revealed that HSFlow does not appear to improve the strength of the constructs despite the improved alignment, therefore further optimisation is needed to strengthen the constructs.</div><div>In conclusion, we developed a novel and rapid technique to generate flat sheets of aligned collagen without relying on the contractile ability of cells to rearrange collagen fibres. This rapid method has potential to be used in the fabrication of a scaffold to mimic anisotropic tissues for regenerative medicine.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102281"},"PeriodicalIF":3.0,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142573444","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-30DOI: 10.1016/j.mtla.2024.102279
Bonnie C. Whitney , Theron M. Rodgers , Anthony G. Spangenberger , Aashique A. Rezwan , David Montes de Oca Zapiain , Diana A. Lados
Laser powder bed fusion (LPBF) additive manufacturing makes near-net-shaped parts with reduced material cost and time, rising as a promising technology to fabricate Ti-6Al-4 V, a widely used titanium alloy in aerospace and medical industries. However, LPBF Ti-6Al-4 V parts produced with 67° rotation between layers, a scan strategy commonly used to reduce microstructure and property inhomogeneity, have varying grain morphologies and weak crystallographic textures that change depending on processing parameters. This study predicts LPBF Ti-6Al-4 V solidification at three energy levels using a finite difference-Monte Carlo method and validates the simulations with large-area electron backscatter diffraction (EBSD) scans. The developed model accurately shows that a 〈001〉 texture forms at low energy and a 〈111〉 texture occurs at higher energies parallel to the build direction but with a lower strength than the textures observed from EBSD. A validated and well-established method of combining spatial correlation and general spherical harmonics representation of texture is developed to calculate a difference score between simulations and experiments. The quantitative comparison enables effective fine-tuning of nucleation density input, which shows a nonlinear relationship with increasing energy level. Future improvements in texture prediction code and a more comprehensive study of with different energy levels will further advance the optimization of LPBF Ti-6Al-4 V components. These developments contribute a novel understanding of crystallographic texture formation in LPBF Ti-6Al-4 V, the development of robust model validation and calibration pipeline methodologies, and provide a platform for mechanical property prediction and process parameter optimization.
激光粉末床熔融（LPBF）快速成型制造技术可制造近网状零件，同时降低材料成本并缩短时间，是制造航空航天和医疗行业广泛使用的钛合金--Ti-6Al-4 V 的一项前景广阔的技术。然而，层间旋转 67° 生产的 LPBF Ti-6Al-4 V 零件（一种常用于减少微观结构和性能不均匀性的扫描策略）具有不同的晶粒形态和随加工参数变化的弱晶体纹理。本研究采用有限差分蒙特卡罗方法预测了 LPBF Ti-6Al-4 V 在三个能级上的凝固情况，并通过大面积电子反向散射衍射 (EBSD) 扫描验证了模拟结果。所建立的模型精确地表明，在低能量下会形成〈001〉纹理，而在与製造方向平行的较高能量下会出现〈111〉纹理，但其强度低于 EBSD 观察到的纹理。结合纹理的空间相关性和一般球形谐波表示法，我们开发了一种经过验证的成熟方法，用于计算模拟和实验之间的差异分值。通过定量比较，可以对成核密度 (N0) 输入进行有效微调，成核密度与能级的增加呈非线性关系。未来纹理预测代码的改进和对不同能级 N0 的更全面研究将进一步推动 LPBF Ti-6Al-4 V 组件的优化。这些进展有助于对 LPBF Ti-6Al-4 V 晶体纹理形成的新理解，有助于开发稳健的模型验证和校准管道方法，并为机械性能预测和工艺参数优化提供了一个平台。
{"title":"Solidification and crystallographic texture modeling of laser powder bed fusion Ti-6Al-4V using finite difference-monte carlo method","authors":"Bonnie C. Whitney , Theron M. Rodgers , Anthony G. Spangenberger , Aashique A. Rezwan , David Montes de Oca Zapiain , Diana A. Lados","doi":"10.1016/j.mtla.2024.102279","DOIUrl":"10.1016/j.mtla.2024.102279","url":null,"abstract":"<div><div>Laser powder bed fusion (LPBF) additive manufacturing makes near-net-shaped parts with reduced material cost and time, rising as a promising technology to fabricate Ti-6Al-4 V, a widely used titanium alloy in aerospace and medical industries. However, LPBF Ti-6Al-4 V parts produced with 67° rotation between layers, a scan strategy commonly used to reduce microstructure and property inhomogeneity, have varying grain morphologies and weak crystallographic textures that change depending on processing parameters. This study predicts LPBF Ti-6Al-4 V solidification at three energy levels using a finite difference-Monte Carlo method and validates the simulations with large-area electron backscatter diffraction (EBSD) scans. The developed model accurately shows that a 〈001〉 texture forms at low energy and a 〈111〉 texture occurs at higher energies parallel to the build direction but with a lower strength than the textures observed from EBSD. A validated and well-established method of combining spatial correlation and general spherical harmonics representation of texture is developed to calculate a difference score between simulations and experiments. The quantitative comparison enables effective fine-tuning of nucleation density <span><math><mrow><mo>(</mo><msub><mi>N</mi><mn>0</mn></msub><mo>)</mo></mrow></math></span> input, which shows a nonlinear relationship with increasing energy level. Future improvements in texture prediction code and a more comprehensive study of <span><math><msub><mi>N</mi><mn>0</mn></msub></math></span> with different energy levels will further advance the optimization of LPBF Ti-6Al-4 V components. These developments contribute a novel understanding of crystallographic texture formation in LPBF Ti-6Al-4 V, the development of robust model validation and calibration pipeline methodologies, and provide a platform for mechanical property prediction and process parameter optimization.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102279"},"PeriodicalIF":3.0,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142656569","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Synthetic bone-like apatites (i.e. biomimetic apatites) increasingly attract attention in the field of bone substitutes due to their similarity to natural bone mineral and their intrinsic surface reactivity, as opposed to conventional hydroxyapatite. Associations with a range of bioactive species can be a way to further tailor their properties after implantation. In the present work, we have focused on the preparation of hybrid materials combining biomimetic apatites, doped or not with antibacterial Ag+ ions for added antimicrobial pertinence, and two biophenolic compounds, namely chlorogenic acid (CA) and sinapic acid (SA). Using complementary characterization techniques, especially FTIR and Raman spectroscopies, as well as Monte Carlo computational simulations, we elucidate the possible interaction between such biophenolic molecules and apatite. The follow-up of isotherms of adsorption also pointed out the quantitative sorption of CA and SA onto biomimetic apatites, potentially up to larger extents than reported so far in the literature for apatitic substrates. Finally, antioxidant properties of prepared hybrids were measured via free radical scavenging tests using DPPH as reactant, showing that the studied phytotherapeutic agents retained antioxidant properties after the adsorption process. This work thus evidences that bone-like apatites can be quantitatively associated to biophenolic bioactive agents to further modulate their properties as smart bone substitutes, providing them additional antioxidant features, among others.
与传统的羟基磷灰石相比，人工合成的类骨磷灰石（即仿生磷灰石）因其与天然骨矿的相似性及其固有的表面反应性而日益受到骨替代品领域的关注。与一系列生物活性物质的结合可以进一步调整其植入后的特性。在本研究中，我们重点制备了仿生磷灰石与两种生物酚类化合物（绿原酸（CA）和山奈酸（SA））的混合材料，前者掺杂或不掺杂抗菌Ag+离子以增加抗菌相关性，后者掺杂或不掺杂抗菌Ag+离子以增加抗菌相关性。利用互补表征技术，特别是傅立叶变换红外光谱和拉曼光谱，以及蒙特卡罗计算模拟，我们阐明了这些生物酚类分子与磷灰石之间可能存在的相互作用。对吸附等温线的跟踪研究也指出了 CA 和 SA 在仿生磷灰石上的定量吸附，其吸附量可能比目前文献中报道的磷灰石基质的吸附量更大。最后，使用 DPPH 作为反应物，通过自由基清除试验测量了制备的混合体的抗氧化特性，结果表明所研究的植物治疗剂在吸附过程后仍具有抗氧化特性。因此，这项研究证明，类骨磷灰石可与生物酚类生物活性剂定量结合，进一步调节其作为智能骨替代品的特性，使其具有额外的抗氧化功能等。
{"title":"Biomimetic apatites functionalized with antioxidant phytotherapeutics: The case of chlorogenic and sinapic phenolic compounds","authors":"Omar Baklouti , Olivier Marsan , Fabrice Salles , Jalloul Bouajila , Hafed El-Feki , Christophe Drouet","doi":"10.1016/j.mtla.2024.102271","DOIUrl":"10.1016/j.mtla.2024.102271","url":null,"abstract":"<div><div>Synthetic bone-like apatites (i.e. biomimetic apatites) increasingly attract attention in the field of bone substitutes due to their similarity to natural bone mineral and their intrinsic surface reactivity, as opposed to conventional hydroxyapatite. Associations with a range of bioactive species can be a way to further tailor their properties after implantation. In the present work, we have focused on the preparation of hybrid materials combining biomimetic apatites, doped or not with antibacterial Ag<sup>+</sup> ions for added antimicrobial pertinence, and two biophenolic compounds, namely chlorogenic acid (CA) and sinapic acid (SA). Using complementary characterization techniques, especially FTIR and Raman spectroscopies, as well as Monte Carlo computational simulations, we elucidate the possible interaction between such biophenolic molecules and apatite. The follow-up of isotherms of adsorption also pointed out the quantitative sorption of CA and SA onto biomimetic apatites, potentially up to larger extents than reported so far in the literature for apatitic substrates. Finally, antioxidant properties of prepared hybrids were measured via free radical scavenging tests using DPPH as reactant, showing that the studied phytotherapeutic agents retained antioxidant properties after the adsorption process. This work thus evidences that bone-like apatites can be quantitatively associated to biophenolic bioactive agents to further modulate their properties as smart bone substitutes, providing them additional antioxidant features, among others.</div></div>","PeriodicalId":47623,"journal":{"name":"Materialia","volume":"38 ","pages":"Article 102271"},"PeriodicalIF":3.0,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142573447","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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