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Tailoring of cooling procedure during freeze-casting for bone replacement applications.
Šantavý, Tomáš ; Novotná, Lenka (oponent) ; Salamon, David (vedoucí práce)
Bachelor thesis focuses on preparation of hydroxyapatite ceramics by freeze-casting. Hydroxyapatite is an important ceramic material, due to its biocompatibility, biodegradability and bioactivity it has a wide range of use in medicinal applications especially in replacement of bone material. The chosen method, freeze-casting, is flexible, eco-friendly and we are able to achieve a high level of porosity. The method includes freezing, freeze drying and sintering which creates a porous structure of the prepared material. Objective of this bachelor thesis was to find out the impact on the created porosity and mechanical properties of the final material. Freezing rates were applied 3, 4, 5, 6, 7 and 26 m/s. During the experimental part it was established that the freezing rate has a significant influence on the newly formed inner microstructure, it directly influences the interlamellar distances and mechanical property which is compressive strength. With liquid nitrogen with a speed of 26 m/s the achieved compressive strength was of 15 MPa as well as the shortest interlamellar distances of 14-22 µm. With slower freezing rate the average interlamellar distances were 40-150 µm and compressive strength of 2-4 MPa with comparable porosity.
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Antibacterial properties of bioceramic materials
Achberger, Šimon ; Částková, Klára (oponent) ; Salamon, David (vedoucí práce)
Implant surgery carries a risk of infection caused by bacterial contamination of the implant surface. An effective way to inhibit proliferation of bacteria is via antibacterial surfaces, however, their usage is medically and technologically difficult. Previous research shows that cicada wing topography exhibits unique bactericidal properties. In this thesis, various topographies were fabricated using heat treatment under hydrothermal conditions. The goal was to produce a surface covered by high aspect ratio structures with 60–215 nm width and 200–300 nm length. A relative density of 85%, 12 hrs long heat treatment and solution pH 4 and 5,6 had a positive effect on formation of thin surface structures. Quantity of morphological changes was proportional to -tricalcium phosphate content.
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3d shaping of UV curable ceramic feedstock
Mišák, Jiří ; Salamon, David (oponent) ; Graule, Thomas (vedoucí práce)
The aim of this study was the development of printable, UV curable colloidal pastes for 3D robotic deposition of complex ceramic fibre networks. Additionally, shaping techniques of printed structures have been demonstrated. Printable and functional ceramic pastes based on hydroxyapatite have been successfully developed from UV curable compositions. Complex printed ceramic fibre networks and multilayers as well as enhancement of the fibre surface quality have been realised. It has been found that the control of particle-monomer/oligomer-surfactant interactions is essential to achieve printable pastes with adequate rheological properties. Using linear and cross-linking UV curable oligomers as dispersion media, very flexible structures result after UV curing. All printed, cured and additionally shaped structures have been transformed to macroscopic ceramics via thermal debinding and sintering without cracks or delamination between the layers. This has been achieved by using argon atmosphere during curing to prevent oxygen inhibition. The 3D robotic deposition in combination with UV curing is a novel and promising technique to produce complex functional ceramic structures. In this work, the benefits from the combination of 3D robotic deposition and UV solidification have been demonstrated in a new way by using cured and flexible 2 layer structures for folding processes, which lead to 3D structures that are very difficult or impossible to achieve with the employment of just direct 3D robotic deposition. On the basis of this research, versatile theory about preparing ceramic pastes for 3D robotic deposition of complex structures for various applications can be deduced.
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Kompozitní keramické materiály na bázi hydroxyapatitu
Vojtíšek, Jan ; Ptáček, Petr (oponent) ; Bartoníčková, Eva (vedoucí práce)
Tato práce se zabývala studiem biokeramických materiálů na bázi hydroxyapatitu. Tyto materiály jsou obecně velmi důležité pro lékařské účely, zejména při rekonstrukcích a náhradě kostního materiálu. Pro medicínské aplikace je možno využít inertní, bioaktivní nebo bioresorbovatelných materiálů. Jedním z častých „bioaktivních“ materiálů je hydroxyapatit, který tvoří velkou část lidské kosti. Hydroxyapatit je možno připravit velkou řadou postupů, přičemž jednou z nejběžnějších metod je precipitační reakce, která byla použita v této práci. Pro zlepšení biokompatibility kostní náhrady se využívá porézních struktur s odpovídající mechanickou stabilitou. Pro prvotní studium simulace chování biomateriálů v lidském těle se používají tzv. in vitro testy v roztocích na bázi syntetických tělních tekutin či buněčných medií. Experimentální část práce se zabývala syntézou kompozitních sloučenin na bázi hydroxyapatitových prášků a CA fází. Reakce mezi jednotlivými komponenty byla studována pomocí termické analýzy a žárové mikroskopie. Vzniklé produkty byly analyzovány z hlediska fázového složení pomocí rentgenové difrakce. Připravené prášky byly dále zpracovány na pěnové struktury pomocí in situ napěňování a slinutí při vhodné teplotě. In vitro testy, sledující chování připravených porézních produktů v syntetické tělní tekutině, byly provedeny po dobu 7, 14 a 28 dní. Sledované kompozity byly poté studovány z hlediska biokompatibility pomocí skenovací elektronové mikroskopie. Současně byla sledována změna koncentrace Ca2+ a PO43- iontů v testovaných tělních tekutinách.
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Příprava a charakterizace nástřiků hydroxyapatitu deponovaných technologii hybridního vodou-stabilizovaného plazmového hořáku z vodných roztoků
Antoš, Zdeněk ; Tkachenko, Serhii (oponent) ; Čížek, Jan (vedoucí práce)
Povlaky hydroxyapatitu jsou již dlouhou dobu v lékařství používány jako bariéra mezi kovovým jádrem náhrady a okolní živou tkání. Plazmový nástřik je běžně používanou technologií pro tvorbu takových povlaků. Tato práce se zabývá vlastnostmi povlaků hydroxyapatitu vytvořených technologií plazmového nástřiku s hybridním systémem stabilizace oblouku (WSP-H). Zároveň využívá inovativní metodu dávkování výchozího materiálu v podobě vodného roztoku (SPPS). Cílem práce bylo vyrobit vodné roztoky hydroxyapatitu a z nich poté deponovat nástřiky s využitím WSP-H. Tyto nástřiky byly charakterizovány z pohledu morfologie, chemického a fázového složení. Dále byly podrobeny biologickému testování biokompatibility kultivací a následnou analýzou buněk RAW 264.7 a MG-63. Nástřiky vytvořené SPPS vykazují výraznou členitost povrchu, která je vhodná pro biologickou aplikaci. Z testování biokompatibility bylo zjištěno, že tyto povlaky budou v lidském těle dobře tolerovány. Po dostatečné optimalizaci nástřikových parametrů a dosažení fázové čistoty nástřiku bude tento postup výroby povlaku hydroxyapatitu vhodnou náhradou starších metod.
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Structure and Properties of Collagen/HAP Nanocomposite Networks
Kopuletá, Ema ; Lehocký,, Marián (oponent) ; Amler,, Evžen (oponent) ; Jančář, Josef (vedoucí práce)
Polymer-based materials are some of the most promising materials for tissue engineering and controlled drug delivery. Collagen, as one of the most abundant proteins to be found in mammals, is especially interesting due to its tunable properties and excellent host reactions. This thesis is focused on the self-assembly and the mechanical properties of collagen in solution, its kinetics and general principles controlling the process. The effect of hydroxyapatite nanoparticles on the collagen self-assembly and mechanical properties is also investigated. Possible mechanisms of collagen/hydroxyapatite interactions are elucidated along with the description of structure evolution and properties at various structural levels. The shear rate dependences and viscoelastic behavior of collagen I and its nanocomposites with hydroxyapatite (HAP) were measured and interpreted molecularly. The structure of collagen I scaffolds was studied and the effect of HAP and cross-linking was determined. Finally, the results were discussed in terms of the applicability of collagen/hydroxyapatite nanocomposites in scaffolds for bone tissue regeneration.
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Tvarování hydroxyapatitu na mikro úrovni pro přípravu kostních náhrad
Pejchalová, Lucie ; Novotná, Lenka (oponent) ; Salamon, David (vedoucí práce)
Vhledem k celosvětovému stárnutí populace, dochází k častější potřebě opravy pohybového aparátu. V některých případech je proto nutno přejít v konečné fázi k implantaci kostní náhrady. Nejčastěji je pro svoji biokompatibilitu a bioaktivitu využíván hydroxyapatit, který je v kostech přirozeně zastoupen. Využití hydroxyapatitu jako materiálu pro kostní náhrady je omezeno mechanickou stabilitou v porézních systémech. Metoda, při které bylo dosaženo nejlepšího poměru mechanické stability a porozity, se nazývá freeze – casting. Tato metoda využívá tvorbu ledu (v případě vodných suspenzí) ke tvorbě lamelární struktury během kontrolovaného mražení. Dalším krokem je odstranění ledových krystalů lyofilizací. Následně je výsledná porézní lamelární struktura zpevněna slinutím. Změnou složení suspenze nebo podmínek mražení lze dosáhnout různé mezilamelární vzdálenosti, spojení lamel a porozity. V této práci byly připraveny keramické suspenze v objemovém zastoupení hydroxyapatitu 7,5 %, 10 %, 15 % a 20 %, které byly použity při přípravě porézních kostních náhrad metodou freeze – casting. Během mražení byla do struktur implementována 3D mřížka, která posloužila jako šablona pro síť kanálků (v průměru cca 800 mikrometrů). Po lyofilizaci byly následným ohřevem odstraněny z materiálu organické látky, včetně 3D mřížky. Výsledná biokeramická struktura dosáhla porozity víc než 90 % a velmi dobrého poměru mechanické stability a porozity. Implementace 3D mřížky se ukázala být vhodnou metodou pro kontrolovanou tvorbu kanálků s dostatečným rozměrem, sloužící k zvýšení bioaktivity materiálu.
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Synthesis of foamed bioceramics for potential medical applications
Doboš, Petr ; Šoukal, František (oponent) ; Palou, Martin (vedoucí práce)
The main aims of the diploma work were focused on the preparation of porous hydroxyapatite ceramics for potential biomedical applications. Hydroxyapatite slurries were synthesized by sol-gel and precipitation method. Then, the slurries were dried and calcinated at 1000 °C for phase control. These samples of HAP were analyzed by SEM, FTIR, and XRD. To prepare apatite porous ceramics, the slurries were foamed by polymeric sponge method and direct foaming method including (polymeric expancel and glass bubbles). The sintering temperature was established after 1000 °C by sponge method and 1200 °C by direct foaming. The microstructure measurement by SEM and structure analysis by MIP of both porous hydroxyaptite indicates the regular porosity including macro, meso and micropores with different pore size distribution. The average size of pores prepared by sponge method is found between 1-5 µm with mono-dispersed porosity. The total porosity is 63.5 % with the total surface area 3.048 1 m/g. Porous hydroxyapatite prepared from expancel showed a poly-dispersed porosity with three main areas: 50–100 µm, 5–10 µm and the third one in range 0.5–1 µm, respectively. The total porosity is 67.6 % with total surface area 19.090 3 m/g. The bioactivity of both was tested in SBF for 7 days. It was found that in precipitation method was observed non-compact bioactive layer. The results were measered by SEM analysis.
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Effect of bioceramic additives on morphology, physical and biological properties of collagen scaffolds for bone tissue engineering
Klieštiková, Nikola ; Poláček, Petr (oponent) ; Brtníková, Jana (vedoucí práce)
The diploma thesis deals with preparation of three-dimensional porous collagen composite scaffolds for bone tissue engineering and study of the effect of addition of bioceramic particles on morphological, biomechanical and biological properties. Theoretical part describes biomaterials and bioceramic particles used for scaffolds in bone tissue engineering and their fabrications method. As for experimental part, samples were prepared by the freeze-drying method. As tested material, type I collagen from porcine and bovine sources was combined with hydroxyapatite and mixture of -tricalcium phosphate and -tricalcium phosphate in ratios 1 : 1, 1 : 2 and 2 : 1. The effect of bioceramics solubility and particle sizes on scaffolds morphology, biomechanics and biocompatibility was evaluated. Addition of bioceramic particles changed the morphology of the samples. The pore size decreased, whereas the porosity was nearly the same in all tested samples. Bioceramic particles also made the collagen matrix of the scaffolds less hydrophilic, moreover they stabilized the scaffolds against the effect of enzymatic degradation. The biomechanical properties of the samples were tested in both dry and hydrated state. In dry state, the pure bovine collagen scaffolds reached the highest compressive strength, contrary in hydrated state, the samples containing bioceramic particles reached the highest value. None of the samples was cytotoxic and the most preferable environment for cell adhesion and proliferation was in the pure bovine collagen scaffolds and also in the composite scaffolds with ratio HAp : -TCP : 1 : 1.
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Rheological properties of biodegradable thermosensitive copolymers
Chamradová, Ivana ; Poláček, Petr (oponent) ; Vojtová, Lucy (vedoucí práce)
The general goal of the proposed diploma work was preparation, characterization and rheological study of well-defined “smart” injectable hydrogels from biodegradable, biocompatible, controlled life-time copolymers based on hydrophilic poly(ethylene glycol) (PEG) and hydrophobic poly(lactic acid)—co—poly(glycolic acid) (PLA/PGA) copolymer. Resulted thermosensitive PLGA—PEG—PLGA copolymer, which gels at body temperature, was additionally functionalized by itaconic anhydride (ITA) from renewable resources, bringing both reactive carbon double bonds and functional —COOH groups to polymer ends. Additionally, the PLGA—PEG—PLGA copolymer was modified by inorganic bioactive hydroxyapatite (HAp) for usage as injectable bone bioadhesive. Both functionalized ITA/PLGA—PEG—PLGA/ITA copolymer and PLGA—PEG—PLGA/HAp polymer composite affected rheological properties of original PLGA—PEG—PLGA copolymer deciding whether or not would be the new polymeric material suitable as injectable drug carrier or bone adhesive in medical applications. Experimental part of this thesis describes mainly characterization of viscoelastic properties of both unmodified and ITA or HAp modified PLGA—PEG—PLGA copolymer by test tube inverting method (TTIM) and dynamic rheological analysis. Advantage of TTIM is sol-gel visualization with determination of the critical gelation temperature and the critical gelation concentration. The rheological measurements provide information about viscosity and elasticity of the gel by the changes storage (G´) and loss (G´´) modulus. The prepared copolymers were additionally characterized by 1H NMR and GPC. Surface and HAp particles size was determined by both SEM and Laser Particles Size Analyzer. Both unmodified and ITA or HAp modified PLGA—PEG—PLGA copolymers exhibited sol-gel transitions induced by increasing temperature. Rheological properties of copolymers’ 6 to 24 wt% water solutions investigated either by TTIM or by rheometer were in good agreement. Evaluating by rheometer, the copolymers showed two cross-points, where G´= G´´. The first one very well corresponded with the first sol-gel transition found via TTIM. The maximum values of G´ representing the highest gel stiffness lie in the white gel observed by TTIM. The second cross-point constituted to the gel-suspension transition where white polymer is precipitated from the water. The gel stiffness grows with increasing polymer concentration in water. In comparison, ITA modification or addition of HAp (0, 10, 20, 30, 40, 50 wt%) caused increasing the gel stiffness of unmodified PLGA—PEG—PLGA copolymer and approximating the temperature of G´max closer to body temperature (37 °C). Investigated both ITA/PLGA—PEG—PLGA/ITA copolymer and PLGA—PEG—PLGA/HAp composite were proved to be suitable candidates as injectable systems for drug delivery or regenerative medicine in orthopedics or dental applications, respectively.
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