{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,2,19]],"date-time":"2026-02-19T04:51:37Z","timestamp":1771476697160,"version":"3.50.1"},"reference-count":45,"publisher":"MDPI AG","issue":"6","license":[{"start":{"date-parts":[[2020,6,12]],"date-time":"2020-06-12T00:00:00Z","timestamp":1591920000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Ministry of Agriculture, Forestry and Tourism (MIPAAF)","award":["RECOVER project, call 3549, project no. CUPJ57G17000150008"],"award-info":[{"award-number":["RECOVER project, call 3549, project no. CUPJ57G17000150008"]}]},{"DOI":"10.13039\/501100007074","name":"Fondazione con il Sud","doi-asserted-by":"publisher","award":["HApECOrk project, 2015-0243"],"award-info":[{"award-number":["HApECOrk project, 2015-0243"]}],"id":[{"id":"10.13039\/501100007074","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Marine Drugs"],"abstract":"<jats:p>Fish industry by-products constitute an interesting platform for the extraction and recovery of valuable compounds in a circular economy approach. Among them, mussel shells could provide a calcium-rich source for the synthesis of hydroxyapatite (HA) bioceramics. In this work, HA nanoparticles have been successfully synthesized starting from mussel shells (Mytilus edulis) with a two steps process based on thermal treatment to convert CaCO3 in CaO and subsequent wet precipitation with a phosphorus source. Several parameters were studied, such as the temperature and gaseous atmosphere of the thermal treatment as well as the use of two different phosphorus-containing reagents in the wet precipitation. Data have revealed that the characteristics of the powders can be tailored, changing the conditions of the process. In particular, the use of (NH4)2HPO4 as the phosphorus source led to HA nanoparticles with a high crystallinity degree, while smaller nanoparticles with a higher surface area were obtained when H3PO4 was employed. Further, a selected HA sample was synthesized at the pilot scale; then, it was employed to fabricate porous 3D scaffolds using the direct foaming method. A highly porous scaffold with open and interconnected porosity associated with good mechanical properties (i.e., porosity in the range 87\u201389%, pore size in the range 50\u2013300 \u03bcm, and a compressive strength \u03c3 = 0.51 \u00b1 0.14 MPa) suitable for bone replacement was achieved. These results suggest that mussel shell by-products are effectively usable for the development of compounds of high added value in the biomedical field.<\/jats:p>","DOI":"10.3390\/md18060309","type":"journal-article","created":{"date-parts":[[2020,6,15]],"date-time":"2020-06-15T03:17:32Z","timestamp":1592191052000},"page":"309","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":47,"title":["Mussel Shell-Derived Macroporous 3D Scaffold: Characterization and Optimization Study of a Bioceramic from the Circular Economy"],"prefix":"10.3390","volume":"18","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7884-0443","authenticated-orcid":false,"given":"Stefania","family":"Scialla","sequence":"first","affiliation":[{"name":"Institute of Nanotechnology (NANOTEC), National Research Council (CNR), Campus Ecoteckne, Via Monteroni, 73100 Lecce, Italy"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8865-2032","authenticated-orcid":false,"given":"Francesca","family":"Carella","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"given":"Massimiliano","family":"Dapporto","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1526-7915","authenticated-orcid":false,"given":"Simone","family":"Sprio","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"given":"Andreana","family":"Piancastelli","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"given":"Barbara","family":"Palazzo","sequence":"additional","affiliation":[{"name":"Ghimas SpA, C\/O Ditech S.c.a.r.l., Campus Ecotekne, 73100 Lecce, Italy"}]},{"given":"Alessio","family":"Adamiano","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6596-560X","authenticated-orcid":false,"given":"Lorenzo","family":"Degli Esposti","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7813-8347","authenticated-orcid":false,"given":"Michele","family":"Iafisco","sequence":"additional","affiliation":[{"name":"Institute of Science and Technology for Ceramics (ISTEC), National Research Council (CNR), Via Granarolo 64, 48018 Faenza, Italy"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6339-716X","authenticated-orcid":false,"given":"Clara","family":"Piccirillo","sequence":"additional","affiliation":[{"name":"Institute of Nanotechnology (NANOTEC), National Research Council (CNR), Campus Ecoteckne, Via Monteroni, 73100 Lecce, Italy"}]}],"member":"1968","published-online":{"date-parts":[[2020,6,12]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"1190","DOI":"10.1016\/j.jclepro.2018.06.262","article-title":"Synthesis of nanomaterials from various wastes and their new age applications","volume":"197","author":"Sammadar","year":"2018","journal-title":"J. Clean. Prod."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"352","DOI":"10.1016\/j.jenvman.2018.12.041","article-title":"An overview of the recent trends on the waste valorization techniques for food wastes","volume":"233","author":"Nayak","year":"2019","journal-title":"J. Environ. Manag."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"40","DOI":"10.1039\/C2BM00071G","article-title":"A tissue engineering approach based on the use of bioceramics for bone repair","volume":"1","author":"Salinas","year":"2012","journal-title":"Biomater. Sci."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"3413","DOI":"10.1016\/j.biomaterials.2006.01.039","article-title":"Biodegradable and bioactive porous polymer\/inorganic composite scaffolds for bone tissue engineering","volume":"27","author":"Rezwan","year":"2006","journal-title":"Biomaterials"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"202","DOI":"10.3389\/fbioe.2015.00202","article-title":"Bioceramics and Scaffolds: A Winning Combination for Tissue Engineering","volume":"3","author":"Baino","year":"2015","journal-title":"Front. Bioeng. Biotechnol."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"1705","DOI":"10.1111\/j.1151-2916.1998.tb02540.x","article-title":"Bioceramics","volume":"81","author":"Hench","year":"2005","journal-title":"J. Am. Ceram. Soc."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"5474","DOI":"10.1016\/j.biomaterials.2005.02.002","article-title":"Porosity of 3D biomaterial scaffolds and osteogenesis","volume":"26","author":"Karageorgiou","year":"2005","journal-title":"Biomaterials"},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"1903055","DOI":"10.1002\/adfm.201903055","article-title":"Additive Manufacturing Approaches for Hydroxyapatite-Reinforced Composites","volume":"29","author":"Milazzo","year":"2019","journal-title":"Adv. Funct. Mater."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"363","DOI":"10.1016\/j.msec.2018.03.022","article-title":"Biphasic calcium phosphate scaffolds with controlled pore size distribution prepared by in-situ foaming","volume":"9","author":"Novotna","year":"2019","journal-title":"Mater. Sci. Eng. C"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"1557","DOI":"10.1021\/acsbiomaterials.7b00232","article-title":"Fabrication and properties of Ca-P bioceramic spherical granules with interconnected porous structure","volume":"3","author":"Li","year":"2017","journal-title":"ACS Biomater. Sci. Eng."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"4839","DOI":"10.1016\/j.ceramint.2012.11.076","article-title":"Influence of the calcination temperature on morphological and mechanical properties of highly porous hydroxyapatite scaffolds","volume":"39","author":"Scalera","year":"2013","journal-title":"Ceram. Int."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"5425","DOI":"10.1007\/s10853-010-4708-9","article-title":"Fabrication of ceramic components with hierarchical porosity","volume":"45","author":"Colombro","year":"2010","journal-title":"J. Mater. Sci."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"37","DOI":"10.1016\/j.actbio.2018.08.026","article-title":"3D-printed bioceramic scaffolds: From bone tissue engineering to tumour therapy","volume":"79","author":"Ma","year":"2018","journal-title":"Acta Biomater."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"494","DOI":"10.1111\/ijac.13133","article-title":"Effect of magnesium silicate on 3D gel-printing of hydroxyapatite ceramic composite scaffold","volume":"16","author":"He","year":"2019","journal-title":"Int. J. Appl. Ceram. Technol."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1021\/acsbiomaterials.7b00615","article-title":"Fabrication aspects of porous biomaterials in orthopedic applications: A review","volume":"4","author":"Babaie","year":"2018","journal-title":"ACS Biomater. Sci. Eng."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"1771","DOI":"10.1111\/j.1551-2916.2006.01044.x","article-title":"Processing routes to macroporous ceramics: A review","volume":"89","author":"Studart","year":"2006","journal-title":"J. Am. Ceram. Soc."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.pcrysgrow.2012.11.001","article-title":"Progress on the preparation of nanocrystalline apatites and surface characterization: Overview of fundamental and applied aspects","volume":"59","author":"Iafisco","year":"2013","journal-title":"Prog. Cryst. Growth Charact. Mater."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"160","DOI":"10.1007\/s10971-016-4038-8","article-title":"Synthesis of HA\/\u03b2-TCP bioceramic foams from natural products","volume":"79","author":"Vila","year":"2016","journal-title":"J. Sol Gel Sci. Technol."},{"key":"ref_19","unstructured":"Kim, S.K. (2013). Hydroxyapatite and calcium phosphates from marine sources: Extraction and characterization. Marine Biomaterials: Characterization, Isolation and Applications, CRC Press."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"e01588","DOI":"10.1016\/j.heliyon.2019.e01588","article-title":"Syntheses of hydroxyapatite from natural sources","volume":"5","author":"Koshy","year":"2019","journal-title":"Heliyon"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"3457","DOI":"10.1016\/j.ceramint.2016.11.163","article-title":"One step method to synthesize flower-like hydroxyapatite architecture using mussel shell bio-waste as a calcium source","volume":"43","author":"Kumar","year":"2017","journal-title":"Ceram. Int."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"614","DOI":"10.1016\/j.vacuum.2017.06.008","article-title":"Facile synthesis and characterization of hydroxyapatite particles for high value nanocomposites and biomaterials","volume":"146","author":"Miculescu","year":"2017","journal-title":"Vacuum"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"015010","DOI":"10.1088\/2057-1976\/aa54f5","article-title":"Mechanochemical synthesis of nanocrystalline hydroxyapatite from Mercenaria clam shells and phosphoric acid","volume":"3","author":"Pal","year":"2017","journal-title":"Biomed. Phys. Eng. Express"},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"607","DOI":"10.1016\/j.matchemphys.2014.11.016","article-title":"Synthesis of nano-hydroxyapatite (nHA) from waste mussel shells using a rapid microwave method","volume":"149","author":"Shavandi","year":"2015","journal-title":"Mater. Chem. Phys."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"2383","DOI":"10.1016\/j.jeurceramsoc.2015.10.020","article-title":"A novel route for the synthesis of macroporous bioceramics for bone regeneration","volume":"36","author":"Dapporto","year":"2016","journal-title":"J. Eur. Ceram. Soc."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"1047","DOI":"10.1080\/10643389.2016.1202669","article-title":"Marine shells: Potential opportunities for extraction of functional and health-promoting materials","volume":"46","author":"Hou","year":"2016","journal-title":"Crit. Rev. Environ. Sci. Technol."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"75","DOI":"10.1016\/j.resconrec.2003.08.005","article-title":"Recycling waste oyster shells for eutrophication control","volume":"41","author":"Kwon","year":"2004","journal-title":"Res. Conserv. Recycl."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"4884","DOI":"10.1016\/j.jece.2017.09.010","article-title":"Biphasic apatite-carbon materials derived from pyrolysed fish bones for effective adsorption of persistent pollutants and heavy metals","volume":"5","author":"Piccirillo","year":"2017","journal-title":"J. Environ. Chem. Eng."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"53","DOI":"10.1016\/j.proche.2014.05.007","article-title":"The characteristics of green calcium oxide derived from aquatic materials","volume":"9","author":"Soisuwan","year":"2014","journal-title":"Procedia Chem."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"115275","DOI":"10.1016\/j.watres.2019.115275","article-title":"Hydrid life cycle assessment of agro-industrial wastewater valorisation","volume":"170","author":"Chen","year":"2020","journal-title":"Water Res."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"326","DOI":"10.1016\/j.jhazmat.2019.01.040","article-title":"A facile synthesis of hydroxyapatite for effective removal strontium ion","volume":"368","author":"Xia","year":"2019","journal-title":"J. Hazard. Mater."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"237","DOI":"10.1016\/j.jinorgbio.2012.06.004","article-title":"Silica xerogels and hydroxyapatite nanocrystals for the local delivery of platinum\u2013bisphosphonate complexes in the treatment of bone tumors: A mini-review","volume":"117","author":"Iafisco","year":"2012","journal-title":"J. Inorg. Biochem."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"1155","DOI":"10.1111\/ijac.13422","article-title":"Role of strontium in spray drying of hydroxyapatite: A comparative study on physical properties","volume":"17","author":"Bastan","year":"2020","journal-title":"Appl. Ceram. Technol."},{"key":"ref_34","unstructured":"Belpassi, A., Dolcini, L., and Martinetti, R. (2002). A Process for the Production of Porous Calcium Phosphate Articles for Bone Regeneration and as a Support for Cells and the Porous Articles Themselves. (EP1411035), European Patent Office."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"223","DOI":"10.1111\/ijac.12249","article-title":"The effects of calcium-to-phosphorus ratio on the densification and mechanical properties of hydroxyapatite ceramic","volume":"12","author":"Tan","year":"2015","journal-title":"Int. J. Appl. Ceram. Technol."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"S4487","DOI":"10.1179\/1432891714Z.000000000725","article-title":"Thermal stability and mechanical properties of zirconia-hydroxyapatite composites","volume":"18","author":"Li","year":"2014","journal-title":"Mater. Res. Innov."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"142","DOI":"10.1016\/j.matlet.2013.09.059","article-title":"A scalable synthesis of non-agglomerated and low-aspect ratio hydroxyapatite nanocrystals using gelatinized starch matrix","volume":"113","author":"Yang","year":"2013","journal-title":"Mater. Lett."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"78","DOI":"10.1016\/j.msec.2015.10.002","article-title":"Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite","volume":"59","author":"Fahami","year":"2016","journal-title":"Mater. Sci. Eng. C"},{"key":"ref_39","doi-asserted-by":"crossref","unstructured":"Predoi, D., Iconaru, S.L., Predoi, M.V., Motelica-Heino, M., Guegan, R., and Buton, N. (2019). Evaluation of antibacterial activity of zinc-doped hydroxyapatite colloids and dispersion stability using ultrasound. Nanomaterials, 9.","DOI":"10.3390\/nano9040515"},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"2171","DOI":"10.1021\/acsabm.9b00151","article-title":"Faster biomineralization and tailored mechanical properties of marine resources-derived hydroxyapatite scaffolds with tunable interconnected porous architecture","volume":"2","author":"Hadagalli","year":"2019","journal-title":"ACS Appl. Bio Mater."},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"577","DOI":"10.1016\/j.actbio.2007.11.002","article-title":"Mechanical behaviour of porous hydroxyapatite","volume":"4","author":"He","year":"2008","journal-title":"Acta Biomater."},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"173","DOI":"10.1016\/j.cej.2007.10.016","article-title":"Low-pressure synthesis and characterisation of hydroxyapatite derived from mineralised red algae","volume":"137","author":"Walsh","year":"2008","journal-title":"Chem. Eng. J."},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"121","DOI":"10.1016\/j.matlet.2013.01.081","article-title":"Thermal stability of nanohydroxyapatite synthesized from sea shells through wet chemical synthesis","volume":"97","author":"Santhosh","year":"2013","journal-title":"Mater. Lett."},{"key":"ref_44","unstructured":"Coelho, A. (2007). Topas Academic v4.1, Coelho Software."},{"key":"ref_45","unstructured":"Klung, H.P., and Alexander, L.E. (1974). X-ray Diffraction Procedures for Polycrystalline and Amorphous Materials, Wiles."}],"container-title":["Marine Drugs"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1660-3397\/18\/6\/309\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T09:38:17Z","timestamp":1760175497000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1660-3397\/18\/6\/309"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2020,6,12]]},"references-count":45,"journal-issue":{"issue":"6","published-online":{"date-parts":[[2020,6]]}},"alternative-id":["md18060309"],"URL":"https:\/\/doi.org\/10.3390\/md18060309","relation":{},"ISSN":["1660-3397"],"issn-type":[{"value":"1660-3397","type":"electronic"}],"subject":[],"published":{"date-parts":[[2020,6,12]]}}}