This work explores ceramic additive manufacturing in combination with liquid metal infiltration for the production of degradable interpenetrating phase magnesium/hydroxyapatite(Mg/HA) composites. Material extrusion ad...This work explores ceramic additive manufacturing in combination with liquid metal infiltration for the production of degradable interpenetrating phase magnesium/hydroxyapatite(Mg/HA) composites. Material extrusion additive manufacturing was used to produce stoichiometric,and calcium deficient HA preforms with a well-controlled open pore network, allowing the customization of the topological relationship of the composite. Pure Mg and two different Mg alloys were used to infiltrate the preforms by means of an advanced liquid infiltration method inspired by spark plasma sintering, using a novel die design to avoid the structural collapse of the preform. Complete infiltration was achieved in 8 min, including the time for the Mg melting. The short processing time enabled to restrict the decomposition of HA due to the reducing capacity of liquid Mg. The pure Mg-base composites showed compressive yield strength above pure Mg in cast state. Mg alloy-based composites did not show higher strength than the bare alloys due to grain coarsening, but showed similar mechanical properties than other Mg/HA composites that have significantly higher fraction of metallic phase. The composites showed faster degradation rate under simulated body conditions than the bare metallic component due to the formation of galvanic pairs at microstructural level. Mg dissolved preferentially over HA leaving behind a scaffold after a prolonged degradation period. In turn, the fast production of soluble degradation products caused cell metabolic changes after 24 h of culture with not-diluted material extracts. The topological optimization and reduction of the degradation rate are the topics for future research.展开更多
Magnesium and calcium phosphates composites are promising biomaterials to create biodegradable load-bearing implants for bone regeneration. The present investigation is focused on the design of an interpenetrated magn...Magnesium and calcium phosphates composites are promising biomaterials to create biodegradable load-bearing implants for bone regeneration. The present investigation is focused on the design of an interpenetrated magnesium- tricalcium phosphate (Mg-TCP) composite and its evaluation under immersion test. In the study, TCP porous preforms were fabricated by robocasting to have a prefect control of porosity and pore size and later infiltrated with pure commercial Mg through current-assisted metal infiltration (CAMI) technique. The microstructure, composition, distribution of phases and degradation of the composite under physiological simulated conditions were analysed by scanning electron microscopy, elemental chemical analysis and X-ray diffraction. The results revealed that robocast TCP preforms were full infiltrated by magnesium through CAMI, even small pores below 2 μm have been filled with Mg, giving to the composite a good interpenetration. The degradation rate of the Mg-TCP composite displays lower value compared to the one of pure Mg during the first 24 h of immersion test.展开更多
Biodegradable magnesium implants offer a solution for bone repair without the need for implant removal.However,concerns persist regarding peri-implant gas accumulation,which has limited their widespread clinical accep...Biodegradable magnesium implants offer a solution for bone repair without the need for implant removal.However,concerns persist regarding peri-implant gas accumulation,which has limited their widespread clinical acceptance.Consequently,there is a need to minimise the mass of magnesium to reduce the total volume of gas generated around the implants.Incorporating porosity is a direct approach to reducing the mass of the implants,but it also decreases the strength and degradation resistance.This study demonstrates that the infiltration of a calcium phosphate cement into an additively manufactured WE43 Mg alloy scaffold with 75% porosity,followed by hydrothermal treatment,yields biodegradable magnesium/hydroxyapatite interpenetrating phase composites that generate an order of magnitude less hydrogen gas during degradation than WE43 scaffolds.The enhanced degradation resistance results from magnesium passivation,allowing osteoblast proliferation in indirect contact with composites.Additionally,the composites exhibit a compressive strength 1.8 times greater than that of the scaffolds,falling within the upper range of the compressive strength of cancellous bone.These results emphasise the potential of the new biodegradable interpenetrating phase composites for the fabrication of temporary osteosynthesis devices.Optimizing cement hardening and magnesium passivation during hydrothermal processing is crucial for achieving both high compressive strength and low degradation rate.展开更多
基金supported by the Czech Science Foundation (grant 19-22662S)Czech Nano Lab project LM2018110 funded by MEYS CR is gratefully acknowledged for the support of the measurements at CEITEC Nano Research Infrastructure+2 种基金MCL acknowledges to Brno Ph.D. Talent scholarship and to the Brno University of Technology Internal Project: CEITEC VUT-J-19-5915SDT acknowledges to CONACYTSNI and SIP-IPN (SAPPI 20220438)LV acknowledges to project no. NU20-08-00150 (MH, Czechia)。
文摘This work explores ceramic additive manufacturing in combination with liquid metal infiltration for the production of degradable interpenetrating phase magnesium/hydroxyapatite(Mg/HA) composites. Material extrusion additive manufacturing was used to produce stoichiometric,and calcium deficient HA preforms with a well-controlled open pore network, allowing the customization of the topological relationship of the composite. Pure Mg and two different Mg alloys were used to infiltrate the preforms by means of an advanced liquid infiltration method inspired by spark plasma sintering, using a novel die design to avoid the structural collapse of the preform. Complete infiltration was achieved in 8 min, including the time for the Mg melting. The short processing time enabled to restrict the decomposition of HA due to the reducing capacity of liquid Mg. The pure Mg-base composites showed compressive yield strength above pure Mg in cast state. Mg alloy-based composites did not show higher strength than the bare alloys due to grain coarsening, but showed similar mechanical properties than other Mg/HA composites that have significantly higher fraction of metallic phase. The composites showed faster degradation rate under simulated body conditions than the bare metallic component due to the formation of galvanic pairs at microstructural level. Mg dissolved preferentially over HA leaving behind a scaffold after a prolonged degradation period. In turn, the fast production of soluble degradation products caused cell metabolic changes after 24 h of culture with not-diluted material extracts. The topological optimization and reduction of the degradation rate are the topics for future research.
基金funding from the European Union's Horizon 2020 research and innovation programme under the Marie Sklodowska-Curieco-financed by the South Moravian Region under Grant No.665860+2 种基金the project CEITEC 2020(LQ1601) with financial support from the Ministry of Education,Youth and Sports of the Czech Republic under the National Sustainability Program Ⅱfounded by the Brno City Municipalitythe project CB.177700,and COFAA-IPN(SIP project 20144443)
文摘Magnesium and calcium phosphates composites are promising biomaterials to create biodegradable load-bearing implants for bone regeneration. The present investigation is focused on the design of an interpenetrated magnesium- tricalcium phosphate (Mg-TCP) composite and its evaluation under immersion test. In the study, TCP porous preforms were fabricated by robocasting to have a prefect control of porosity and pore size and later infiltrated with pure commercial Mg through current-assisted metal infiltration (CAMI) technique. The microstructure, composition, distribution of phases and degradation of the composite under physiological simulated conditions were analysed by scanning electron microscopy, elemental chemical analysis and X-ray diffraction. The results revealed that robocast TCP preforms were full infiltrated by magnesium through CAMI, even small pores below 2 μm have been filled with Mg, giving to the composite a good interpenetration. The degradation rate of the Mg-TCP composite displays lower value compared to the one of pure Mg during the first 24 h of immersion test.
基金supported by the Ministry of Health of the Czech Republic(NW24-10-00195)the Brno University of Technology projects CEITEC VUT/FCH-J-23-8367 and CEITEC VUT-JL 24-8642CzechNanoLab Research Infrastructure supported by Ministry of Education,Youth and Sports of the Czech Republic(LM2023051)providing access to some devices used for this study.
文摘Biodegradable magnesium implants offer a solution for bone repair without the need for implant removal.However,concerns persist regarding peri-implant gas accumulation,which has limited their widespread clinical acceptance.Consequently,there is a need to minimise the mass of magnesium to reduce the total volume of gas generated around the implants.Incorporating porosity is a direct approach to reducing the mass of the implants,but it also decreases the strength and degradation resistance.This study demonstrates that the infiltration of a calcium phosphate cement into an additively manufactured WE43 Mg alloy scaffold with 75% porosity,followed by hydrothermal treatment,yields biodegradable magnesium/hydroxyapatite interpenetrating phase composites that generate an order of magnitude less hydrogen gas during degradation than WE43 scaffolds.The enhanced degradation resistance results from magnesium passivation,allowing osteoblast proliferation in indirect contact with composites.Additionally,the composites exhibit a compressive strength 1.8 times greater than that of the scaffolds,falling within the upper range of the compressive strength of cancellous bone.These results emphasise the potential of the new biodegradable interpenetrating phase composites for the fabrication of temporary osteosynthesis devices.Optimizing cement hardening and magnesium passivation during hydrothermal processing is crucial for achieving both high compressive strength and low degradation rate.