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Physical Properties of Acidic Calcium Phosphate Cements

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Physical Properties of Acidic Calcium Phosphate Cements Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology 1195 Physical Properties of Acidic Calcium Phosphate Cements JOHANNA UNOSSON ACTA UNIVERSITATIS UPSALIENSIS ISSN 1651-6214 ISBN 978-91-554-9081-2 UPPSALA urn:nbn:se:uu:diva-233637 2014 Dissertation presented at Uppsala University to be publicly examined in Polhemsalen, Ångströmlaboratoriet, Uppsala, Friday, 5 December 2014 at 09:15 for the degree of Doctor of Philosophy. The examination will be conducted in English. Faculty examiner: Professor Uwe Gbureck (University of Wuerzburg, Germany). Abstract Unosson, J. 2014. Physical Properties of Acidic Calcium Phosphate Cements. Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology 1195. 73 pp. Uppsala: Acta Universitatis Upsaliensis. ISBN 978-91-554-9081-2. The gold standard for bone replacement today, autologous bone, suffers from several disadvantages, such as the increased risk of infection due to the need for two surgeries. Degradable synthetic materials with properties similar to bone, such as calcium phosphate cements, are a promising alternative. Calcium phosphate cements are suited for a limited amount of applications and improving their physical properties could extend their use into areas previously not considered possible. For example, cement with increased strength could be used as load bearing support in selected applications. The focus of this thesis is, therefore, on how the physical properties of acidic calcium phosphate cements (brushite cements) are affected by compositional variations, with the ultimate aim of making it possible to formulate brushite cements with desired properties. In this thesis a method to measure the porosity of a cement was developed. This method is advantageous over existing methods as it is easy to use, requiring no advanced equipment. A model estimating the porosity of the hardened cement from the initial chemical composition was further formulated and the accuracy affirmed. Utilization of this model allows the porosity to be optimized by calculations rather than extensive laboratory work. The effect on strength and porosity of several compositional variations were also assessed and it was found that the optimal composition to achieve a high strength was: monocalcium phosphate particles in sizes <75µm, 10 mol% excess of beta-tricalcium phosphate, 1 wt% disodium dihydrogen pyrophosphate, and 0.5 M citric acid in a liquid-to-powder ratio of 0.22 ml/g. This composition gave the highest compressive strength historically measured for this type of cement, i.e., 74.4 (±10.7) MPa. Although such a high strength may not be necessary for all applications, it allows for the use of brushite cements in new applications. Furthermore, a high strength of the bulk allows for alterations to the cement that cause a decrease in strength. One application is fast degrading materials, allowing rapid bone ingrowth. A fast degradation is obtained with a high macroporosity, which would reduce strength. The high strength composition was therefore utilized to achieve brushite cement with a high macroporosity. Johanna Unosson, Department of Engineering Sciences, Applied Materials Sciences, Box 534, Uppsala University, SE-75121 Uppsala, Sweden. © Johanna Unosson 2014 ISSN 1651-6214 ISBN 978-91-554-9081-2 urn:nbn:se:uu:diva-233637 (http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-233637) Till min familj List of Papers This thesis is based on the following papers, which are referred to in the text by their Roman numerals. I Öhman, C., Unosson, J., Carlsson, E., Ginebra, MP., Persson, C., Engqvist, H., Porosity prediction of calcium phosphate cements based on chemical composition. Submitted II Engstrand Unosson, J., Persson, C., Engqvist, H., (2014) An evaluation of methods to determine the porosity of calcium phosphate cements. Journal of Biomedical Materials Research Part B: Applied Biomaterials, accepted III Engstrand, J., Persson, C., Engqvist, H., (2014) The effect of composition on mechanical properties of brushite cements. Journal of the Mechanical Behavior of Biomedical Materials, 29:81-90 IV Unosson, J., Engqvist, H., (2014) Development of a resorbable calcium phosphate cement with load bearing capacity. Bioceramics Development and Applications, 1(4):074 V Unosson, J., Montufar, E., Engqvist, H., Ginebra, MP., Persson, C., (2014) Brushite foams - the effect of Tween® 80 and Pluronic® F-127 on foam porosity and mechanical properties. Submitted VI Engstrand, J., Åberg, J., Engqvist, H., (2013) Influence of water content on hardening and handling of a premixed calcium phosphate cement. Materials Science and Engineering: C, 33(1):527-531 VII Åberg, J., Engstrand, J., Engqvist, H., (2013) Influence of particle size on hardening and handling of a premixed calcium phosphate cement. Journal of Materials Science: Materials in Medicine, 24(4):829-835 VIII Åberg, J., Engstrand Unosson, J., Engqvist, H., (2013) Setting mechanisms of an acidic premixed calcium phosphate cement. Bioceramics Development and Applications, 1(3):070 Reprints were made with permission from the respective publishers. Author’s Contributions Paper I Part of planning and writing. Large part of ex- perimental work. Papers II, III and IV All planning and experimental work. Major part of writing. Paper V Major part of planning, experimental work and writing. Paper VI Major part of planning and experimental work. Part of writing. Paper VII Major part of experimental work. Part of plan- ning and writing. Paper VIII Part of planning and experimental work. Major part of writing. Contents Introduction ................................................................................................... 11 Aims and objectives ...................................................................................... 13 Bone void fillers ............................................................................................ 14 Calcium phosphate biomaterials ................................................................... 16 Calcium phosphate cements .......................................................................... 18 Brushite cements ........................................................................................... 22 Premixed brushite cements ....................................................................... 23 Precursor material ......................................................................................... 25 Beta-tricalcium phosphate ........................................................................ 25 Monocalcium phosphate monohydrate .................................................... 26 Setting retardants ...................................................................................... 26 Cement preparation ....................................................................................... 28 Handling ........................................................................................................ 30 Injectability............................................................................................... 30 Setting time .............................................................................................. 32 Storage conditions .................................................................................... 33 Preparation ............................................................................................... 34 Reaction products.......................................................................................... 35 Phases ....................................................................................................... 35 Morphology after setting .......................................................................... 38 Effect of the MCPM particle size ........................................................ 38 Effect of the liquid ............................................................................... 38 Porosity ......................................................................................................... 41 Measuring the porosity of a brushite cement ........................................... 41 Volume changes during the reaction ........................................................ 43 The effect of particle size on porosity ...................................................... 45 The effect of preparation method on porosity .......................................... 46 Mechanical properties ................................................................................... 48 The effect of porosity on strength ............................................................ 48 The effect of filler content on strength ..................................................... 50 The effect of particle size on strength ...................................................... 52 The effect of liquid type on strength ........................................................ 52 Concluding remarks ...................................................................................... 54 Future perspectives ....................................................................................... 55 Svensk sammanfattning – De sura kalciumfosfatcementens fysikaliska egenskaper .................................................................................................... 57 Acknowledgements ....................................................................................... 60 Analytical techniques ...................................................................................
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