@article{SeifertGruberGburecketal.2021, author = {Seifert, Annika and Gruber, Julia and Gbureck, Uwe and Groll, J{\"u}rgen}, title = {Morphological control of freeze-structured scaffolds by selective temperature and material control in the ice-templating process}, series = {Advanced Engineering Materials}, volume = {24}, journal = {Advanced Engineering Materials}, number = {3}, doi = {10.1002/adem.202100860}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-256330}, year = {2021}, abstract = {Herein, it is aimed to highlight the importance of the process parameter choice during directional solidification of polymer solutions, as they have a significant influence on the pore structure and orientation. Biopolymer solutions (alginate and chitosan) are directionally frozen, while systematically varying parameters such as the external temperature gradient, the temperature of the overall system, and the temperatures of the cooling surfaces. In addition, the effect of material properties such as molecular weight, solution concentration, or viscosity on the sample morphology is investigated. By selecting appropriate temperature gradients and cooling surface temperatures, aligned pores ranging in size between (50 ± 22) μm and (144 ± 56) μm are observed in the alginate samples, whereas the pore orientation is influenced by altering the external temperature gradient. As this gradient increases, the pores are increasingly oriented perpendicular to the sample surface. This is also observed in the chitosan samples. However, if the overall system is too cold, that is, using temperatures of the lower cooling surface down to -60 °C combined with low temperatures of the upper cooling surface, control over pore orientation is lost. This is also found when viscosity of chitosan solutions is above ≈5 Pas near the freezing point.}, language = {en} } @article{SeifertGrollWeichholdetal.2021, author = {Seifert, Annika and Groll, J{\"u}rgen and Weichhold, Jan and Boehm, Anne V. and M{\"u}ller, Frank A. and Gbureck, Uwe}, title = {Phase Conversion of Ice-Templated α-Tricalcium Phosphate Scaffolds into Low-Temperature Calcium Phosphates with Anisotropic Open Porosity}, series = {Advanced Engineering Materials}, volume = {23}, journal = {Advanced Engineering Materials}, number = {5}, doi = {10.1002/adem.202001417}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-256311}, year = {2021}, abstract = {The current study aims to extend the material platform for anisotropically structured calcium phosphates to low-temperature phases such as calcium-deficient hydroxyapatite (CDHA) or the secondary phosphates monetite and brushite. This is achieved by the phase conversion of highly porous α-tricalcium phosphate (α-TCP) scaffolds fabricated by ice-templating into the aforementioned phases by hydrothermal treatment or incubation in phosphoric acid. Prior to these steps, α-TCP scaffolds are either sintered for 8 h at 1400 °C or remain in their original state. Both nonsintered and sintered α-TCP specimens are converted into CDHA by hydrothermal treatment, while a transformation into monetite and brushite is achieved by incubation in phosphoric acid. Hydrothermal treatment for 72 h at 175 °C increases the porosity in nonsintered samples from 85\% to 88\% and from 75\% to 88\% in the sintered ones. An increase in the specific surface area from (1.102 ± 0.005) to (9.17 ± 0.01) m2 g-1 and from (0.190 ± 0.004) to (2.809 ± 0.002) m2 g-1 due to the phase conversion is visible for both the nonsintered and sintered samples. Compressive strength of the nonsintered samples increases significantly from (0.76 ± 0.11) to (5.29 ± 0.94) MPa due to incubation in phosphoric acid.}, language = {en} } @article{HolzmeisterWeichholdGrolletal.2021, author = {Holzmeister, Ib and Weichhold, Jan and Groll, J{\"u}rgen and Zreiqat,, Hala and Gbureck, Uwe}, title = {Hydraulic reactivity and cement formation of baghdadite}, series = {Journal of the American Ceramic Society}, volume = {104}, journal = {Journal of the American Ceramic Society}, number = {7}, doi = {10.1111/jace.17727}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-259457}, pages = {3554-3561}, year = {2021}, abstract = {In this study, the hydraulic reactivity and cement formation of baghdadite (Ca\(_{3}\)ZrSi\(_{2}\)O\(_{9}\)) was investigated. The material was synthesized by sintering a mixture of CaCO\(_{3}\), SiO\(_{2}\), and ZrO\(_{2}\) and then mechanically activated using a planetary mill. This leads to a decrease in particle and crystallite size and a partial amorphization of baghdadite as shown by X-ray powder diffraction (XRD) and laser diffraction measurements. Baghdadite cements were formed by the addition of water at a powder to liquid ratio of 2.0 g/ml. Maximum compressive strengths were found to be ~2 MPa after 3-day setting for a 24-h ground material. Inductively coupled plasma mass spectrometry (ICP-MS) measurements showed an incongruent dissolution profile of set cements with a preferred dissolution of calcium and only marginal release of zirconium ions. Cement formation occurs under alkaline conditions, whereas the unground raw powder leads to a pH of 11.9 during setting, while prolonged grinding increased pH values to approximately 12.3.}, language = {en} } @article{HeiligSandnerJordanetal.2021, author = {Heilig, Philipp and Sandner, Phoebe and Jordan, Martin Cornelius and Jakubietz, Rafael Gregor and Meffert, Rainer Heribert and Gbureck, Uwe and Hoelscher-Doht, Stefanie}, title = {Experimental drillable magnesium phosphate cement is a promising alternative to conventional bone cements}, series = {Materials}, volume = {14}, journal = {Materials}, number = {8}, issn = {1996-1944}, doi = {10.3390/ma14081925}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-236633}, year = {2021}, abstract = {Clinically used mineral bone cements lack high strength values, absorbability and drillability. Therefore, magnesium phosphate cements have recently received increasing attention as they unify a high mechanical performance with presumed degradation in vivo. To obtain a drillable cement formulation, farringtonite (Mg\(_3\)(PO\(_4\))\(_2\)) and magnesium oxide (MgO) were modified with the setting retardant phytic acid (C\(_6\)H\(_{18}\)O\(_{24}\)P\(_6\)). In a pre-testing series, 13 different compositions of magnesium phosphate cements were analyzed concentrating on the clinical demands for application. Of these 13 composites, two cement formulations with different phytic acid content (22.5 wt\% and 25 wt\%) were identified to meet clinical demands. Both formulations were evaluated in terms of setting time, injectability, compressive strength, screw pullout tests and biomechanical tests in a clinically relevant fracture model. The cements were used as bone filler of a metaphyseal bone defect alone, and in combination with screws drilled through the cement. Both formulations achieved a setting time of 5 min 30 s and an injectability of 100\%. Compressive strength was shown to be ~12-13 MPa and the overall displacement of the reduced fracture was <2 mm with and without screws. Maximum load until reduced fracture failure was ~2600 N for the cements only and ~3800 N for the combination with screws. Two new compositions of magnesium phosphate cements revealed high strength in clinically relevant biomechanical test set-ups and add clinically desired characteristics to its strength such as injectability and drillability.}, language = {en} } @article{GoetzHoleczekGrolletal.2021, author = {G{\"o}tz, Lisa-Marie and Holeczek, Katharina and Groll, J{\"u}rgen and J{\"u}ngst, Tomasz and Gbureck, Uwe}, title = {Extrusion-Based 3D Printing of Calcium Magnesium Phosphate Cement Pastes for Degradable Bone Implants}, series = {Materials}, volume = {14}, journal = {Materials}, number = {18}, issn = {1996-1944}, doi = {10.3390/ma14185197}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-246110}, year = {2021}, abstract = {This study aimed to develop printable calcium magnesium phosphate pastes that harden by immersion in ammonium phosphate solution post-printing. Besides the main mineral compound, biocompatible ceramic, magnesium oxide and hydroxypropylmethylcellulose (HPMC) were the crucial components. Two pastes with different powder to liquid ratios of 1.35 g/mL and 1.93 g/mL were characterized regarding their rheological properties. Here, ageing over the course of 24 h showed an increase in viscosity and extrusion force, which was attributed to structural changes in HPMC as well as the formation of magnesium hydroxide by hydration of MgO. The pastes enabled printing of porous scaffolds with good dimensional stability and enabled a setting reaction to struvite when immersed in ammonium phosphate solution. Mechanical performance under compression was approx. 8-20 MPa as a monolithic structure and 1.6-3.0 MPa for printed macroporous scaffolds, depending on parameters such as powder to liquid ratio, ageing time, strand thickness and distance.}, language = {en} }