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1.
  • Atif, Abdul Raouf, 1996-, et al. (author)
  • A Universal Microfluidic Platform for In Vitro Biomaterial Evaluation
  • 2022
  • Conference paper (other academic/artistic)abstract
    • INTRODUCTION: Conventionally, the biological properties of biomaterials are evaluated using well plates. Although being a standardized method, it is static in terms of fluid flow and is far from the physiological conditions found in vivo. This work presents a versatile microfluidic system that allows for integration of different biomaterials (ceramic, metals and polymers) under dynamic conditions.METHODS: The Universal Biomaterial-on-Chip (UBOC) consisted of two separate 3D printed (Polylactic acid, Ultimaker 2+) structures: the upper layer which contains the channel through which medium can flow (Fig1A) and the bottom layer that holds and secures the biomaterial in place (Fig 1B). A glass coverslip was taped to the upper layer to tightly seal the channel. Subsequently, an oval Polydimethylsiloxane (PDMS) gasket (l=10mm,w=7mm, h=0.8mm) was inserted into the periphery of the channel in the upper layer. Furthermore, magnets (Ø=12mm, h=3mm) were glued on both sides of the bottom layer. To close the channel, two magnets were placed on the upper layer, causing attraction to the magnets in the bottom layer. The gasket would then directly interface with the biomaterial inside the bottom layer, creating a leak-free channel on its surface. MC3T3-E1 pre-osteoblasts were seeded in the UBOC platform (50,000 cells/cm2) on calcium-deficient hydroxyapatite (HA) (Ø=15mm) and clinical grade titanium (Ti) (Ø=12mm). The cells were cultured for a period of 5 days at a flow rate of 2 μl/min using supplemented MEM-α medium (Hyclone, 10% FBS, 1% Pen-Strep). On day 5, the cells were stained on-chip with Live/Dead stain (Calcein, Propidium Iodide and Hoechst) and subsequently imaged.RESULTS: HA and Ti samples were successfully integrated into the UBOC. Cells cultured on-chip displayed a high degree of viability and confluence on day 5 of culture on both HA and Ti substrates (Fig 2).DISCUSSION & CONCLUSIONS: UBOC presents the possibility for flexible in vitro biomaterial analysis as it allows for easy incorporation of flow to conventional cell culture regimes in a low-cost manner. Via this method,cells can be cultured on the biomaterial with exposure to fluid flow and controlled shear-stress. The platform is compatible with standard characterization methods, such as imaging and biochemical cell analysis. In addition, since the system is designed to be opened and closed, the biomaterial could be easily accessed, harvested and transferred to a regular tissue culture vessel,enabling standard off-chip biochemical assays and protocols to be performed for further analysis.
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2.
  • Atif, Abdul-Raouf, 1996-, et al. (author)
  • Experimental Characterization and Mathematical Modeling of the Adsorption of Proteins and Cells on Biomimetic Hydroxyapatite
  • 2022
  • In: ACS Omega. - : American Chemical Society (ACS). - 2470-1343. ; 7:1, s. 908-920
  • Journal article (peer-reviewed)abstract
    • Biomaterial development is a long process consisting of multiple stages of design and evaluation within the context of both in vitro and in vivo testing. To streamline this process, mathematical and computational modeling displays potential as a tool for rapid biomaterial characterization, enabling the prediction of optimal physicochemical parameters. In this work, a Langmuir isotherm-based model was used to describe protein and cell adhesion on a biomimetic hydroxyapatite surface, both independently and in a one-way coupled system. The results indicated that increased protein surface coverage leads to improved cell adhesion and spread, with maximal protein coverage occurring within 48 h. In addition, the Langmuir model displayed a good fit with the experimental data. Overall, computational modeling is an exciting avenue that may lead to savings in terms of time and cost during the biomaterial development process.
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4.
  • Bang, Le T., et al. (author)
  • Synthesis and assessment of metallic ion migration through a novel calcium carbonate coating for biomedical implants
  • 2020
  • In: Journal of Biomedical Materials Research. Part B - Applied biomaterials. - : Wiley. - 1552-4973 .- 1552-4981. ; 108:2, s. 429-438
  • Journal article (peer-reviewed)abstract
    • Titanium (Ti) implants are commonly regarded as well accepted by the body. However, metal ion release is still a cause for concern. A small decrease in pH, which can be caused by inflammation, may produce a large increase in the corrosion rate of Ti implants. Coating the alloy with a buffer layer could have a significant protective effect. In this study, a calcium carbonate coating was developed on commercially pure Ti and a Ti-6Al-4V alloy through a hydrothermal treatment of previously NaOH-treated surfaces in calcium-citric acid chelate complexes. The results showed that a superstructured calcite coating layer formed on the Ti substrate after treatment at 170 degrees C for 3 hr. The coating was approx. 1 mu m thick and covered the substrate surface uniformly. When prolonging the hydrothermal treatment from 5 hr to 24 hr, the rhombohedral structure of calcite was observed in addition to the superstructure of calcite. Dissolution test results showed no significant differences in solution pH between the coated- and un-coated samples. However, the CaCO3 coating reduced by approx. 2-5 times the Ti and V ion release from the substrate as compared to the uncoated material, at pH 4. CaCO3 and hydroxyapatite (HA) coatings gave nonsignificant effects at neutral pH although the HA coating showed a trend for better results at the longer time points. The reduction in metal ion release from the substrate and the buffering ability of the CaCO3 coating encourage further studies on this coating for clinical applications.
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5.
  • Berg, Camilla, et al. (author)
  • ACP-Mg particles for treatment of dental hypersensitivity : a mode of action study
  • 2019
  • Conference paper (other academic/artistic)abstract
    • Introduction/purpose:Dental hypersensitivity is a common clinical condition usually associated with exposed dentinal tubules. Occlusion of those, hindering fluid movement as a response to external stimuli, is one approach to reduce pain.[1] The occluding agent should induce mineralization and have a good filling effect. In this study, particles (200-400 nm) of Amorphous Calcium Phosphate with Mg (ACP-Mg) were used aiming to evaluate the mode of action with in-vitro studies on dentine as well as degradation properties in buffered systems.Methods:Degradation properties and ion-release was monitored by dispersing the particles in Tris-HCl (10 mg/mL) storing the dispersions at 37 °C.  In-vitro testing was performed on 1 mm thick dentine discs cut from extracted human molars. Specimens were etched in 35 % phosphoric acid, rinsed with DI-water followed by treatment by applying a gel formulation containing the particles using a soft bristled toothbrush, brushing 1 min on each side and leaving the specimen to rest for 3 min. Treatment was repeated four times during one day and samples were incubated at 37 °C in artificial saliva.Results:In vitro tests and degradation studies showed that ACP-Mg particles induced formation of Hydroxyapatite (HA). ICP-OES, XRD and SEM showed that there was a rapid release of all ions up to 6 hours followed by a re-precipitation of HA at 24 hours with a lower Mg-content. The crystallinity increased with time as the concentration of all ions decreased in the solutions. Morphological evaluation for the in-vitro tests showed that HA-like structures formed already after 24 hours on the dentine surface.  Cross-sections revealed that the particles reached as far as 80 µm from the surface and tubules, fully occluded by HA-like structures, was visible at comparable depths after 7 days.Conclusions:ACP-Mg particles can be used to reduce dentine hypersensitivity by effective occlusion of dentine tubules via rapid formation of surface and intra-tubular HA.References:1. Splieth CH, Tachou A. 2013. Epidemiology of dentin hypersensitivity. Clin Oral Investig. 17:3–8. 
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6.
  • Berg, Camilla, et al. (author)
  • Amorphous Calcium Magnesium Phosphate Particles for Treatment of Dentin Hypersensitivity : A Mode of Action Study
  • 2020
  • In: ACS Biomaterials Science & Engineering. - : AMER CHEMICAL SOC. - 2373-9878. ; 6:6, s. 3599-3607
  • Journal article (peer-reviewed)abstract
    • Occlusion of exposed dentin tubules may eliminate or reduce dentin hypersensitivity by hindering fluid movements within the tubules. In this study, the mode of action of spherical particles of amorphous calcium magnesium phosphate (180-440 nm in diameter) was studied. A degradation study of the particles in Tris-HCl buffer showed that the particles continuously released Ca2+, Mg2+, and phosphate, and XRD analysis revealed the formation of hydroxyapatite (HA) after 1 week. The occluding effect and efficacy of the spherical particles as an occluding agent were evaluated in an in vitro study. The ACMP particles were incorporated in a gel intended for at-home use and tested on extracted human molars. Application of the particles followed by incubation in artificial saliva resulted in occlusion of exposed tubules, and examination with SEM showed that the particles could penetrate the tubules down to 100 mu m from the dentin surface. Transformation of the particles into nanocrystalline HA-structures (nanoHA) was initiated at the dentin surface within 12 h of application, and tubule penetration of the particles, accompanied by further ion release and diffusion of ions, resulted in deep intratubular occlusion in the majority of the tubules within 3 days from application. NanoHA was tightly adhered to the tubule walls, filling the entire tubule volume after 7 days. The results of this study demonstrate the mode of action of the amorphous calcium magnesium phosphate particles in occluding exposed dentin tubules. Interaction with saliva and transformation of the particles within the tubules inducing further mineralization indicate that the particles may be used as an effective treatment to reduce dentin hypersensitivity.
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8.
  • Berg, Camilla, et al. (author)
  • Bulk nanobubbles as soft templates in the fabrication of inorganic core-shell particles
  • 2023
  • In: Ceramics International. - : Elsevier. - 0272-8842 .- 1873-3956. ; 49:11, s. 16501-16513
  • Research review (peer-reviewed)abstract
    • Hollow microstructured-and nanostructured-materials (also known as core-shell particles) have got great attention as advanced materials due to their fascinating physicochemical properties and favourable application prospects in many fields. In recent years, a variety of synthesis strategies have been explored to fabricate core-shell particles with different morphologies, compositions, microstructures, and thereby versatile functionalities. Among the synthesis strategies, soft-templating with the usage of nanobubbles is a feasible and effective one. Many inorganic core-shell particles have been prepared by using nanobubbles as a template. Nevertheless, studies in this field have not been reviewed comprehensively yet. Herein, the paper firstly reviewed several critical aspects of nanobubbles, such as the formation methods, stability and stabilization strategies of nano-bubbles; Secondly, characteristics of core-shell particles prepared by using nanobubbles soft template were summarized, including formation mechanisms, morphologies, etc.; Lastly, concerns regarding nanobubbles as soft templates were also briefly discussed.
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9.
  • Berg, Camilla (author)
  • Ceramic Core–Shell Particles : Synthesis and Use within Dentistry
  • 2021
  • Doctoral thesis (other academic/artistic)abstract
    • Dentin hypersensitivity is one of the most prevalent conditions related to oral health, affecting a large share of the adult population. Shortcomings with the available treatment options are related to non-ideal particle sizes and degradation properties. An improved clinical outcome could possibly be obtained using a bioactive occluding agent that can offer a high, continuous release of ions, as well as having a particle size that allows for penetration into the dentin tubules. The work in this thesis focused on the development and investigation of a synthesis approach for calcium phosphate core–shell particles and the use of those in the treatment of dentin hypersensitivity. The overall aim was to increase the knowledge about the synthesis and to evaluate the in vitro performance of amorphous calcium magnesium phosphate (ACMP) particles when used as an occluding agent. The synthesis of the core-shell particles was based on precipitation reactions in aqueous solutions and the synthesized materials were studied in terms of morphological, structural, and compositional aspects. Resulting particles had diameters ranging from 400 nm–1. 5 µm (depending on reaction conditions), with morphologies and structures that were shown to correlate with the ionic radius and the concentration of the substituting ion. This insight resulted in the possibility to control the outcome of the reaction and to extend the synthesis to other alkaline earth phosphates. The mechanism of formation was suggested to be the simultaneous precipitation of primary nanoparticles (NPs) and the formation of gas bubbles that could function as soft templates.A study of the degradation properties together with a series of in vitro studies, using a dentin-disc model, indicated that the ACMP particles may be a promising candidate for clinical use. The material was shown to offer a rapid and continuous release of Ca2+, Mg2+, and phosphate, aiding surface, as well as intratubular occlusion and mineralization. Additional use of a fluoride toothpaste resulted in incorporation of F– in the mineralized material. This could enhance the in vivo performance due to the known benefits of including F– in dental tissues, e.g. decreased solubility. The ACMP particles were, furthermore, shown to be more efficient in terms of degree of occlusion when compared to other similar products available on the market. The intratubular mineralization was additionally mitigating the effect of an acid attack, which is of importance for a long-lasting effect in clinical use.
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10.
  • Berg, Camilla, et al. (author)
  • Comparative study of technologies for tubule occlusion and treatment of dentin hypersensitivity
  • 2021
  • In: Journal of Functional Biomaterials. - : MDPI. - 2079-4983. ; 12:2
  • Journal article (peer-reviewed)abstract
    • This study aimed to evaluate the occluding/remineralization performance and resistance to acid attacks of the mineralization layer formed by a tooth-desensitizing gel containing amorphous calcium magnesium phosphate (ACMP) particles and compare it to six other desensitizing products available on the market. Similar comprehensive studies are few and there is especially a lack of studies that are up to date. A dentin-disc model was used for in vitro evaluation of the desensitizing toothpastes/gels. Application of the products was performed twice daily for seven days. One set of specimens were evaluated using scanning electron microscopy (SEM) directly after the final treatment and another set was evaluated after an acid challenge, exposing specimens to 2 wt% citric acid. The ACMP desensitizing gel was the only product resulting in complete occlusion by the formation of mineralized material on the dentin surface and inside the tubules. Particle deposition was dominant after treatment with the other desensitizing products, with little or no mineralization, resulting in partial occlusion only. Sensodyne Repair & Protect and Oral-B Pro-Expert showed the highest resistance toward acid attacks. Material inside the tubules remained relatively unaffected by acid attacks in all specimens. The results in this study indicated a great variability among the occluding agents in terms of occlusion and acid resistance of the mineralization layer. The high degree of occlusion and intra-tubular mineralization that could mitigate the effect of acid solubilization indicate that the ACMP desensitizing gel may be a superior option for the treatment of dentin hypersensitivity.
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11.
  • Berg, Camilla, et al. (author)
  • Electron microscopy evaluation of mineralization on peritubular dentin with amorphous calcium magnesium phosphate microspheres
  • 2020
  • In: Ceramics International. - : Elsevier BV. - 0272-8842 .- 1873-3956. ; 46:11, s. 19469-19475
  • Journal article (peer-reviewed)abstract
    • Dentin hypersensitivity can be reduced by the use of a remineralization agent to hinder movement of fluids within the dentin tubules. Penetration of particles into the tubules and a continuous release of Ca2+ and phosphate ions can induce the mineralization of a material mimicking the mineral component of dentin, sealing the tubules. In this work, we have used complementary electron microscopy techniques to investigate the ultrastructure of dentin and crystallization and occlusion effects when using amorphous calcium magnesium phosphate (ACMP) microspheres on extracted human molars. Application of the particles in a gel intended for athome use resulted in intra-tubular mineralization of a carbonate substituted hydroxyapatite (HA). Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) showed that crystallization was initiated on the peritubular dentin (PTD) with undirected crystal growth leading to the formation of a porous material. We additionally investigated the effects from using a fluoride toothpaste to potentially improve the remineralization and anti-cariogenic properties of the ACMP microspheres. Energy dispersive x-ray spectroscopy (EDX) using TEM in scanning mode (STEM) showed that fluoride incorporation resulted in an increase in aspect ratio of the crystals, crystal growth directed towards the center of the tubule lumen and densification of the mineralized material. Thus, ACMP microspheres are promising alternatives as occluding agents and the efficacy of the particles could be further improved with the complementary use of a fluoride toothpaste.
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12.
  • Berg, Camilla, et al. (author)
  • Ion substitution induced formation of spherical ceramic particles
  • 2019
  • In: Ceramics International. - : ELSEVIER SCI LTD. - 0272-8842 .- 1873-3956. ; 45:8, s. 10385-10393
  • Journal article (peer-reviewed)abstract
    • How to precipitate ceramic nano- and microspheres in water based solutions only using inorganic ions is a challenge. In this study, spherical particles of alkaline earth phosphates and fluorides were synthesized using a precipitation reaction. Substituting ions, through inhibition of crystal growth, was used to induce sphere formation and to alter the morphology, size and composition of the spheres. The difference in ionic radius between the substituting ion (Mg, Ca and Sr) and the main cation (Sr and Ba) influenced the critical concentration to allow for sphere formation as well as the crystallinity. The larger difference, the lower was the concentration needed to form spheres. Low concentrations of Mg was enough to generate amorphous spheres of Sr- and Ba- phosphates whereas higher concentrations were needed if the radius difference were smaller. An increasing degree of substitution leads to a decrease in crystallinity of precipitated particles. The degree of substitution was determined to 16-55% where a low degree of ion substitution in the phosphates resulted in the formation of spheres (500-800 nm) with rough surfaces composed of apatite like phases. A higher degree of substitution resulted in amorphous spheres (500 nm- (1) mu m) with smooth surfaces.
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13.
  • Berg, Camilla, et al. (author)
  • Synthesis of Ion Substituted Ceramic Core-Shell Particles for Dental Applications
  • 2018
  • Conference paper (peer-reviewed)abstract
    • Calcium phosphate spheres are interesting alternatives for dental applications due to their chemical similarity to teeth and biocompatibility. A spherical shape with a hollow cores allows for loading of therapeutic agents for drug delivery which potentially could be combined with other applications such as tooth remineralization and treatment of hypersensitivity.Precipitation reactions are one of the techniques used for synthesizing spherical particles, but little is known about the mechanism behind the sphere formation, which makes tuning of the material properties challenging. Previously, it has been shown that substituting ions can influence the crystallization process, which can enable greater control during the synthesis.In this study, several different substituting ions has been used in the synthesis of alkaline earth phosphates, to further investigate their role in sphere formation and to develop a robust synthesis technique.Particles of alkaline earth phosphates (Ca, Sr and Ba) were synthesized with a precipitation reaction. Solutions with constituent anions and cations were mixed at room temperature, and substituting ions (Mg, Ca or Sr) were added before heating at 60-100 °C. Reaction times varied between 10 minutes to 24 hours. Characterization of precipitates was performed with SEM, DLS and FIB to analyze morphology, size and cross-sections of the spheres. Crystal structure and atomic composition was analyzed with XRD and ICP-OES.Without substituting ions, precipitates had no specific shape and crystallized in an apatitic structure or as a hydrogenated phosphate. Substituting ions stabilized the initial amorphous phase during the reaction, hindering rapid crystal growth which allowed for self-assembly into hollow, spherical particles with a diameter between 300-700 nm. The phase composition and degree of ion substitution in the precipitates depended on the size and concentration of the substituting ions. The amount of substitution was determined in the range between 5-30 %, where precipitates with a low degree of substitution crystallized in a structure similar to β-tricalcium phosphate, whereas materials with a higher degree of substitution had an amorphous structure.In this study it was shown that it was possible to obtain hollow, spherical particles of calcium-, strontium- and barium phosphate, by using substituting ions during a precipitation reaction. This indicates that the approach can be used to tailor the properties of spherical particles intended for dental applications.
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14.
  • Bojan, Alicja J., 1980, et al. (author)
  • A new bone adhesive candidate- does it work in human bone? An ex-vivo preclinical evaluation in fresh human osteoporotic femoral head bone
  • 2022
  • In: Injury-International Journal of the Care of the Injured. - : Elsevier BV. - 0020-1383 .- 1879-0267. ; 53:6, s. 1858-1866
  • Journal article (peer-reviewed)abstract
    • Introduction: The fixation of small intraarticular bone fragments is clinically challenging and an obvious first orthopaedic indication for an effective bone adhesive. In the present study the feasibility of bonding freshly harvested human trabecular bone with OsStic(R), a novel phosphoserine modified cement, was evaluated using a bone cylinder model pull-out test and compared with a commercial fibrin tissue adhesive. Methods: Femoral heads (n=13) were collected from hip fracture patients undergoing arthroplasty and stored refrigerated overnight in saline medium prior to testing. Cylindrical bone cores with a pre-inserted bone screw, were prepared using a coring tool. Each core was removed and glued back in place with either the bone adhesive (alpha-tricalcium phosphate, phosphoserine and 20% trisodium citrate solution) or the fibrin glue. All glued bones were stored in bone medium at 37 degrees C. Tensile loading, using a universal testing machine (5 kN load cell), was applied to each core/head. For the bone adhesive, bone cores were tested at 2 (n=13) and 24 (n=11) hours. For the fibrin tissue adhesive control group (n=9), bone cores were tested exclusively at 2 hours. The femoral bone quality was evaluated with micro-CT. Results: The ultimate pull-out load for the bone adhesive at 2 hours ranged from 36 to 171 N (mean 94 N, SD 42 N). At 24 hours the pull-out strength was similar, 47 to 198 N (mean 123 N, SD 43 N). The adhesive failure usually occurred through the adhesive layer, however in two samples, at 167 N and 198 N the screw pulled out of the bone core. The fibrin tissue adhesive group reached a peak force of 8 N maximally at 2 hours (range 2.8-8 N, mean 5.4 N, SD 1.6 N). The mean BV/TV for femoral heads was 0.15 and indicates poor bone quality. Conclusion: The bone adhesive successfully glued wet and fatty tissue of osteoporotic human bone cores. The mean ultimate pull-out force of 123 N at 24 hours corresponds to similar to 300 kPa shear stress acting on the bone core. These first ex-vivo results in human bone are a promising step toward potential clinical application in osteochondral fragment fixation. (C) 2022 The Authors. Published by Elsevier Ltd.
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15.
  • Carter, Sarah-Sophia, 1994-, et al. (author)
  • PDMS leaching and its implications for on-chip studies focusing on bone regeneration applications
  • 2020
  • In: Organs-on-a-Chip. - : Elsevier. - 2666-1020. ; 2
  • Journal article (peer-reviewed)abstract
    • Polydimethylsiloxane (PDMS) is among the most widely used materials for organ-on-chip systems. Despite itsmultiple beneficial characteristics from an engineering point of view, there is a concern about the effect of PDMSon the cells cultured in such devices. The aim of this study was to enhance the understanding of the effect of PDMSon cellular behavior in a context relevant for on-chip studies. The focus was put on an indirect effect of PDMS,namely leaching of uncrosslinked oligomers, particularly for bone regeneration applications. PDMS-based chipswere prepared and analyzed for the potential release of PDMS oligomers within the microfluidic channel whenkept at different flow rates. Leaching of uncrosslinked oligomers from PDMS was quantified as silicon concen-tration by inductively coupled plasma - optical emission spectrometry and further confirmed by mass spec-trometry. Subsequently, PDMS-leached media, with a silicon concentration matching the on-chip experiment,were prepared to study cell proliferation and osteogenic differentiation of MC3T3-E1 pre-osteoblasts and humanmesenchymal stem cells. The silicon concentration initially detected in the media was inversely proportional tothe tested flow rates and decreased to control levels within 52 h. In addition, by curing the material overnightinstead of 2 h, regardless of the curing temperature (65 and 80 C), a large reduction in silicon concentration wasfound, indicating the importance of the PDMS curing parameters. Furthermore, it was shown that PDMS oligo-mers enhanced the differentiation of MC3T3-E1 pre-osteoblasts, this being a cell type dependent effect as nochanges in cell differentiation were observed for human mesenchymal stem cells. Overall, this study illustrates theimportance of optimization steps when using PDMS devices for biological studies, in particular PDMS curingconditions and extensive washing steps prior to an experiment.
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16.
  • Chen, Song, et al. (author)
  • Novel Fast-Setting Mineral Trioxide Aggregate : Its Formulation, Chemical-Physical Properties, and Cytocompatibility
  • 2018
  • In: ACS Applied Materials and Interfaces. - : AMER CHEMICAL SOC. - 1944-8244 .- 1944-8252. ; 10:24, s. 20334-20341
  • Journal article (peer-reviewed)abstract
    • One of the main drawbacks that limits the application of mineral trioxide aggregate (MTA) in dental field is its long setting time. Mineral trioxide aggregate with accelerated setting properties and excellent chemical-physical and biological properties is still required. In this study, an innovative mineral trioxide aggregate, which consists of calcium silicates, calcium aluminates, and zirconium oxide, was designed to obtain fast-setting property. The optimized formulation can achieve initial setting in 10 min and final setting in 15 min, which are much faster than commercial mineral trioxide aggregate. In addition, the optimized fast-setting MTA showed adequate radiopacity and good biocompatibility. The ion concentrations after storage in water for 1 day were 52.3 mg/L Ca, 67.7 mg/L Al, 48.8 mg/L Si, and 11.7 mg/L Mg. The hydration products of hardened cements were investigated by X-ray diffraction, scanning electron microscopy, and Fourier transform infrared, showing the accelerated setting time was due to the formation of honeycomb-like calcium silicate hydrate gel. The novel MTA could be a promising material for dental applications.
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17.
  • Dong, Zhiyun, et al. (author)
  • Silk fibroin hydrogels induced and reinforced by acidic calcium phosphate : A simple way of producing bioactive and drug-loadable composites for biomedical applications
  • 2021
  • In: International Journal of Biological Macromolecules. - : Elsevier. - 0141-8130 .- 1879-0003. ; 193, s. 433-440
  • Journal article (peer-reviewed)abstract
    • Silk fibroin (SF) hydrogels have attracted extensive interest in biomedical applications due to their biocompatibility and wide availability. However, their generally poor mechanical properties limit their utility. Here, injectable, ready-to-use SF-based composites, simultaneously induced and reinforced by acidic calcium phosphates, were prepared via a dual-paste system requiring no complex chemical/physical treatment. The composite was formed by mixing a monocalcium phosphate monohydrate paste with a β-tricalcium phosphate/SF paste. The conformational transition of SF in an acidic environment forms continuous networks, and the acidic calcium phosphate, brushite and monetite, formed simultaneously in the networks during mixing. The composites displayed a partly elastomeric compression behavior, with mechanical properties increasing with an increasing calcium phosphate and β-sheet content at the lower calcium phosphate contents evaluated (22.2–36.4 wt%). While the stiffness was still relatively low, the materials presented a high elasticity and ductility, and no failure at stresses in the range of failure stresses of trabecular bone. Furthermore, the calcium phosphate confers bioactivity to the material, and the composites with a promising in vitro cell response also showed potential as drug vehicles, using vancomycin as a model drug. These dual-paste systems exhibit potential utility in biomedical applications, such as bone void fillers and drug vehicles.
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19.
  • Filho, Luimar Correa, et al. (author)
  • The Effect of Coating Density on Functional Properties of SiNx Coated Implants
  • 2019
  • In: Materials. - : MDPI AG. - 1996-1944. ; 12:20
  • Journal article (peer-reviewed)abstract
    • Ceramic coatings may be applied onto metallic components of joint replacements for improved wear and corrosion resistance as well as enhanced biocompatibility, especially for metal-sensitive patients. Silicon nitride (SiNx) coatings have recently been developed for this purpose. To achieve a high coating density, necessary to secure a long-term performance, is however challenging, especially for sputter deposited SiNx coatings, since these coatings are insulating. This study investigates the time-dependent performance of sputter-deposited SiNx based coatings for joint applications. SiNx coatings with a thickness in the range of 4.3–6.0 µm were deposited by reactive high power impulse magnetron sputtering onto flat discs as well as hip heads made of CoCrMo. SiNx compositional analysis by X-ray photoelectron spectroscopy showed N/Si ratios between 0.8 and 1.0. Immersion of the flat disks in fetal bovine serum solution over time as well as short-term wear tests against ultra-high molecular weight polyethylene (UHMWPE) discs showed that a high coating density is required to inhibit tribocorrosion. Coatings that performed best in terms of chemical stability were deposited using a higher target power and process heating.
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21.
  • Filho, Luimar, et al. (author)
  • The effect of N, C, Cr, and Nb content on silicon nitride coatings for joint applications
  • 2020
  • In: Materials. - : MDPI AG. - 1996-1944. ; 13:8
  • Journal article (peer-reviewed)abstract
    • Ceramic coatings are an alternative to achieve or maintain a high wear resistance of metallic surfaces, and simultaneously allow for a reduction in metal ion release. Silicon nitride based (SiNx) coatings deposited by high power impulse magnetron sputtering (HiPIMS) have shown potential for use in joint implants seen from an improved chemical stability in combination with a good adhesion. The aim of this study was to investigate the effect of N, C, Cr and Nb content on the tribocorrosive performance of 3.7 to 8.8 µm thick SiNx coatings deposited by HiPIMS onto CoCrMo discs to improve  the mechanical properties and/or chemical stability of SiNx .Coating composition was evaluated by X-ray photoelectron spectroscopy (XPS) and the surface roughness by Vertical Scanning Interferometry (VSI). Hardness and Young’s modulus were investigated by nanoindentation and coating adhesion was measured by scratch tests. Multidirectional wear tests against UHMWPE pins were performed for 2 million cycles in bovine serum solution (25%) at 37°C, at an estimated contact pressure of 2.1 MPa.Coatings with a relatively low hardness tended to fail earlier in the wear test, due to chemical reactions and eventually dissolution, accelerated by the tribological contact. In fact, while no definite correlation could be observed between coating composition (N: 42.6-55.5 at%, C: 0-25.7 at%, Cr: 0 or 12.8 at%, and Nb: 0-24.5 at%) and wear performance, it was apparent that high-purity and/or -density coatings (i.e. low oxygen content and high nitrogen content) were desirable to prevent coating and/or counter surface wear. Coatings deposited with a higher energy fulfilled the target profile in terms of low surface roughness (Ra<20nm), adequate adhesion (Lc2>30N), chemical stability over time in the tribocorrosive environment, as well as low polymer wear, presenting potential for a future application in joint bearings.
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22.
  • Filho, Luimar, et al. (author)
  • Towards Functional Silicon Nitride Coatings for Joint Replacements
  • 2019
  • In: Coatings. - : MDPI AG. - 2079-6412. ; 9:2
  • Journal article (peer-reviewed)abstract
    • Silicon nitride (SiNx) coatings are currently under investigation as bearing surfaces for joint implants, due to their low wear rate and the good biocompatibility of both coatings and their potential wear debris. The aim of this study was to move further towards functional SiNx coatings by evaluating coatings deposited onto CoCrMo surfaces with a CrN interlayer, using different bias voltages and substrate rotations. Reactive direct current magnetron sputtering was used to coat CoCrMo discs with a CrN interlayer, followed by a SiNx top layer, which was deposited by reactive high-power impulse magnetron sputtering. The interlayer was deposited using negative bias voltages ranging between 100 and 900 V, and 1-fold or 3-fold substrate rotation. Scanning electron microscopy showed a dependence of coating morphology on substrate rotation. The N/Si ratio ranged from 1.10 to 1.25, as evaluated by X-ray photoelectron spectroscopy. Vertical scanning interferometry revealed that the coated, unpolished samples had a low average surface roughness between 16 and 33 nm. Rockwell indentations showed improved coating adhesion when a low bias voltage of 100 V was used to deposit the CrN interlayer. Wear tests performed in a reciprocating manner against Si3N4 balls showed specific wear rates lower than, or similar to that of CoCrMo. The study suggests that low negative bias voltages may contribute to a better performance of SiNx coatings in terms of adhesion. The low wear rates found in the current study support further development of silicon nitride-based coatings towards clinical application.
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24.
  • Filho, Luimar, et al. (author)
  • Wear performance of a new biocompatible silicon nitride for biomedical applications
  • Other publication (other academic/artistic)abstract
    • Ceramics are used in bearings of joint implants due to their high wear resistance and biocompatibility. Silicon nitride (Si3N4) is a biomaterial with bacteriostatic properties, high wear resistance, it shows slow dissolution in aqueous environments and contains mainly biocompatible ions. In this work sintering additives SrO, MgO and SiO2 were used in order to gain improvement in biocompatibility, over the commonly used Al2O3 and Y2O3. This substitution may however have a substantial effect on the wear properties of the material, and the aim of the study was to evaluate these properties in a relevant setting. Si3N4 was sintered by spark plasma sintering in the shape of discs for later grinding and polishing. The wear resistance was evaluated by multidirectional pin-on-disc wear tests against ultra-high molecular weight polyethylene pins. Tests were performed in bovine serum solution at 37 °C for 2 million cycles. The surface roughness of the materials was measured by an optical surface profiler, phase composition by X-ray diffraction, surface morphology by scanning electron microscopy, and the pH of the wear lubricant was measured at intervals of half a million cycles. The surface roughness of the ceramic discs and UHMWPE pins was in accordance with the biomedical standard, and the XRD measurements and SEM images showed the presence of α- and β-phase silicon nitride. The multidirectional wear tests showed a low wear factor and a comparable coefficient of friction to previous work, showing promise for application in joint implants. No difference between the material groups could be found in terms of UHMWPE pin wear. However, the dissolution of the materials over time may be a concern for biotribological applications.
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25.
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26.
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27.
  • Fowler, Lee, et al. (author)
  • Antibacterial investigation of titanium-copper alloys using luminescent Staphylococcus epidermidis in a direct contact test
  • 2019
  • In: Materials science & engineering. C, biomimetic materials, sensors and systems. - : ELSEVIER SCIENCE BV. - 0928-4931 .- 1873-0191. ; 97, s. 707-714
  • Journal article (peer-reviewed)abstract
    • Commercially pure titanium (CP-Ti), used as oral implants, is often populated by various bacterial colonies in the oral cavity. These bacteria can cause Peri-implantitis, leading to loss of bone tissue and failure of implants. With the increased awareness of antibiotic resistance, research has been directed towards alternative solutions and recent findings have indicated titanium-copper (Ti-Cu) alloys as a promising antibacterial material. The aim of this study was to produce homogeneous Ti-Cu alloys, with various concentrations of copper, and to characterise their antibacterial properties through direct contact tests, using luminescent bacteria, in addition to traditional materials characterisation techniques. Samples of CP-Ti and four different Ti-Cu alloys (1, 2.5, 3 and 10 wt%Cu) were produced in an arc-furnace, heated treated and rapidly quenched. X-ray diffraction revealed that Ti2Cu, was present only in the 10 wt%Cu alloy, however, scanning electron microscopy (SEM) indicated precipitates at the grain boundaries of the 3 wt%Cu alloy, which were confirmed to be of a copper rich phase by energy dispersive x-ray spectroscopy (EDS) analysis. EDS line scans confirmed that the alloys were homogenous. After 6 h, a trend between copper content and antibacterial rate could be observed, with the 10 wt%Cu alloy having the highest rate. SEM confirmed fewer bacteria on the 3 wt%Cu and especially the 10 wt%Cu samples. Although the 10 wt%Cu alloy gave the best antibacterial results, it is desired that the Cu concentration is below similar to 3 wt%Cu to maintain similar mechanical and corrosive performance as CP-Ti. Therefore, it is proposed that future work focuses on the 3 wt%Cu alloy.
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28.
  • Fowler, Lee, et al. (author)
  • Development of Antibacterial Ti-Cu-x Alloys for Dental Applications : Effects of Ageing for Alloys with Up to 10 wt% Cu
  • 2019
  • In: Materials. - Switzerland : MDPI. - 1996-1944. ; 12:23
  • Journal article (peer-reviewed)abstract
    • Peri-implantitis, a disease caused by bacteria, affects dental implants in patients. It is widely treated with antibiotics, however, with growing antibiotic resistance new strategies are required. Titanium-copper alloys are prospective antibacterial biomaterials, with the potential to be a remedy against peri-implantitis and antibiotic resistance. The aim of this study was to investigate Ti-Cux alloys, exploring how Cu content (up to 10 wt%) and ageing affect the material properties. Electron microscopy, X-ray diffraction, hardness testing, bacteriological culture, and electrochemical testing were employed to characterize the materials. It was found that alloys with above 3 wt% Cu had two phases and ageing increased the volume fraction of Ti2Cu. An un-aged alloy of 5 wt% Cu showed what could be Ti3Cu, in addition to the α-Ti phase. The hardness gradually increased with increased Cu additions, while ageing only affected the alloy with 10 wt% Cu (due to changes in microstructure). Ageing resulted in faster passivation of the alloys. After two hours the aged 10 wt% Cu alloy was the only material with an antibacterial effect, while after six hours, bacteria killing occurred in all alloys with above 5 wt% Cu. In conclusion, it was possible to tune the material and antibacterial properties of Ti-Cux alloys by changing the Cu concentration and ageing, which makes further optimization towards an antibacterial material promising.
  •  
29.
  • Fowler, Lee, et al. (author)
  • Effect of copper ion concentration on bacteria and cells
  • 2019
  • In: Materials. - Switzerland : MDPI. - 1996-1944. ; 12:22
  • Journal article (peer-reviewed)abstract
    • In the oral cavity, dental implants—most often made of commercially pure titanium—come in contact with bacteria, and antibacterial management has been researched extensively to improve patient care. With antibiotic resistance becoming increasingly prevalent, this has resulted in copper being investigated as an antibacterial element in alloys. In this study, the objective was to investigate the copper ion concentrations at which cyto-toxicity is avoided while bacterial inhibition is ensured, by comparing Cu ion effects on selected eukaryotes and prokaryotes. To determine relevant copper ion concentrations, ion release rates from copper and a 10 wt. % Cu Ti-alloy were investigated. Survival studies were performed on MC3T3 cells and Staphylococcus epidermidis bacteria, after exposure to Cu ions concentrations ranging from 9 × 10−3 to 9 × 10−12 g/mL. Cell survival increased from <10% to >90% after 24 h of exposure, by reducing Cu concentrations from 9 × 10−5 to 9 × 10−6 g/mL. Survival of bacteria also increased in the same range of Cu concentrations. The maximum bacteria growth was found at 9 × 10−7 g/mL, probably due to stress response. In conclusion, the minimum inhibitory concentrations of Cu ions for these prokaryotes and eukaryotes were found in the range from 9 × 10−5 to 9 × 10−6 g/mL. Interestingly, the Cu ion concentration correlating to the release rate of the 10 wt. % Cu alloy (9 × 10−8 g/mL) did not kill the bacteria, although this alloy has previously been found to be antibacterial. Further studies should investigate in depth the bacteria-killing mechanism of copper.
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30.
  • Fowler, Lee, et al. (author)
  • Investigation of copper alloying in a TNTZ-Cux alloy
  • 2019
  • In: Materials. - Switzerland : MDPI. - 1996-1944. ; 12:22
  • Journal article (peer-reviewed)abstract
    • Alloying copper into pure titanium has recently allowed the development of antibacterial alloys. The alloying of biocompatible elements (Nb, Ta and Zr) into pure titanium has also achieved higher strengths for a new alloy of Ti-1.6 wt.% Nb-10 wt.% Ta-1.7 wt.% Zr (TNTZ), where strength was closer to Ti-6Al-4V and higher than grade 4 titanium. In the present study, as a first step towards development of a novel antibacterial material with higher strength, the existing TNTZ was alloyed with copper to investigate the resultant microstructural changes and properties. The initial design and modelling of the alloy system was performed using the calculation of phase diagrams (CALPHAD) methods, to predict the phase transformations in the alloy. Following predictions, the alloys were produced using arc melting with appropriate heat treatments. The alloys were characterized using energy dispersive X-ray spectroscopy in scanning transmission electron microscopy (STEM-EDS) with transmission Kikuchi diffraction (TKD). The manufactured alloys had a three-phased crystal structure that was found in the alloys with 3 wt.% Cu and higher, in line with the modelled alloy predictions. The phases included the α-Ti (HCP-Ti) with some Ta present in the crystal, Ti2Cu, and a bright phase with Ti, Cu and Ta in the crystal. The Ti2Cu crystals tended to precipitate in the grain boundaries of the α-Ti phase and bright phase. The hardness of the alloys increased with increased Cu addition, as did the presence of the Ti2Cu phase. Further studies to optimize the alloy could result in a suitable material for dental implants.
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31.
  • Fu, Le, et al. (author)
  • Biodegradable Si3N4 bioceramic sintered with Sr, Mg and Si for spinal fusion : Surface characterization and biological evaluation
  • 2018
  • In: Applied Materials Today. - : Elsevier BV. - 2352-9407. ; 12, s. 260-275
  • Journal article (peer-reviewed)abstract
    • Silicon nitride (Si3N4) is an industrial ceramic used in spinal fusion and maxillofacial reconstructionbecause of its excellent mechanical properties and good biocompatibility. This study compares the sur-face properties, apatite formation ability, bacterial infection, cell-biomaterial interactions, and in vivotoxicity (zebrafish) of newly developed Si3N4 bioceramics (sintered with bioactive sintering additivesSrO, MgO and SiO2) with two standard biomaterials; titanium (Ti) and traditional Si3N4 bioceramics (sin-tered with standard sintering additives Al2O3 and Y2O3). In general, Si3N4 bioceramics (both the newlydeveloped and the traditional) displayed less in vitro bacterial affinity than Ti, which may arise fromdifferences in the surface properties between these two types of material. The newly developed Si3N4bioceramics developed lower biofilm coverage and thinner biofilm, compared to traditional Si3N4 bioce-ramics. The effects of ionic dissolution products (leach) on proliferation and differentiation of MC3T3-E1cell were also investigated. Ionic dissolution products containing moderate amount of Sr, Mg and Siions (approximately 4.72 mg/L, 3.26 mg/L and 3.67 mg/L, respectively) stimulated osteoblast prolifera-tion during the first 2 days in culture. Interestingly, ionic dissolution products from the traditional Si3N4bioceramics that contained small amount of Si and Y ions achieved the greatest stimulatory effect foralkaline phosphatase activity after 7 days culture. The toxicity of ionic dissolution products was investi-gated in a putative developmental biology model: zebrafish (Danio rerio). No toxicity, or developmentalabnormalities, was observed in zebrafish embryos exposed to ionic dissolution products, for up to 144 hpost fertilization. These newly developed Si3N4 bioceramics with bioactive sintering additives show greatpotential as orthopedic implants, for applications such as spinal fusion cages. Future work will focus onevaluation of the newly developed Si3N4 bioceramics using a large animal model.
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32.
  • Fu, Le, et al. (author)
  • Doping of tantalum, niobium, and hafnium in a translucent ZrO2-SiO2 nanocrystalline glass-ceramic
  • 2022
  • In: Journal of the European Ceramic Society. - : Elsevier. - 0955-2219 .- 1873-619X. ; 42:4, s. 1731-1742
  • Journal article (peer-reviewed)abstract
    • The addition of dopant(s) is an effective strategy to regulate the microstructure and properties of ZrO2-based ceramics. In this study, we investigated the effects of ternary element alloying, namely tantalum (Ta), niobium (Nb), and hafnium (Hf) elements, on the microstructure and transformability of ZrO2 nanocrystallites in a ZrO2SiO2 nanocrystalline glass-ceramic (NCGC) during sintering and thermal treatments. The ternary dopants enhanced the transformability of tetragonal ZrO2 (t-ZrO2) nanocrystallites during sintering, i.e., the dopants acted as t-ZrO2 destabilizer. The Ta, Nb and Hf elements dissolved in ZrO2 nanocrystallites, forming ZrO2 solid solution. Meanwhile, lamella nanotwins were formed within many ZrO2 nanocrystallites. No obvious segregation of dopants was detected at ZrO2 grain boundaries. t-ZrO2 and monoclinic (m) ZrO2 nanocrystallites were metastable in thermal treatments process, with "t" to "m" and the reverse "m" to "t" polymorphic transformation occurred simultaneously. Meanwhile, t-ZrO2 and m-ZrO2 nanocrystallites had a great tendency to grow larger during thermal treatments.
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33.
  • Fu, Le, et al. (author)
  • Enhanced Bacteriostatic Properties of Ti Alloys by Surface Nitriding
  • 2023
  • In: Biomedical Materials &amp; Devices. - : Springer Nature. - 2731-4812 .- 2731-4820. ; 1, s. 760-771
  • Journal article (peer-reviewed)abstract
    • Surface nitriding has been widely used to improve the surface physicochemical properties of Ti alloys. However, the currently utilized surface nitriding methods, such as laser nitriding, typically require expensive and complicated instruments, which makes surface nitriding a less cost-effective process. Meanwhile, the antibacterial properties of surface-nitrided Ti alloy implants have not been evaluated. Thereafter, in this study, we were aiming to develop an effective, simple, and cost-effective surface nitriding strategy to enhance the antimicrobial properties of Ti alloy implants. The surface nitriding strategy was realized by wet-chemical etching and thermal treatment at controlled conditions. Results showed that the above surface modification treatments exerted significant effects on the phase composition and morphology of the newly formed phases on the surface of Ti samples. Crystalline TiN and TiO2 formed after treatments. Meanwhile, amorphous nitrides and oxynitride were also presented on the sample surfaces. The surface-modified Ti samples showed a bacterial inhibition effect compared with the non-treated Ti ones, and the bacterial inhibition effect was attributed to the released ammonia species from the surface of Ti samples. The surface modification strategy shows promise to improve the bacteriostatic property of Ti implants in dental and orthopedic fields.
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34.
  • Fu, Le, et al. (author)
  • Fabrication of mechanically robust nanoporous ZrSiO4 ceramics at low temperature with a low doping level of Mn dopant
  • 2024
  • In: International Journal of Applied Ceramic Technology. - : John Wiley & Sons. - 1546-542X .- 1744-7402. ; 21:3, s. 1954-1964
  • Journal article (peer-reviewed)abstract
    • Zircon (ZrSiO4) ceramics have been widely used in many fields due to their excellent physical and chemical properties. However, ZrSiO4 ceramics typically possess moderately low mechanical properties, which hinders their wider application. Meanwhile, elevated temperatures (similar to 1500 degrees C) are required to obtain high-purity synthetic ZrSiO4 ceramics, which is time- and energy-consuming. In the present study, we prepared mechanically robust ZrSiO4 ceramics at low temperature (similar to 1170 degrees C) with a low doping level of Mn dopant (<2 mol%). The ZrSiO4 ceramic processed by hot isostatic pressing with .5 mol% Mn dopant achieved the highest flexural strength (512 MPa), elastic modulus (341 GPa), and nanohardness (20.8 GPa). These values are significantly higher than conventional ZrSiO4 ceramics. The strengthening mechanisms of the prepared ZrSiO4 ceramics were attributed to the formation of homogeneously-distributed nanopores due to incomplete densification and submicron ZrSiO4 grains (similar to 300 nm). The nanopores avoided stress concentration and deflected microcracks during loading, and the submicron ZrSiO4 grains endowed the ZrSiO4 ceramics with grain refinement strengthening. The results reported in this study would offer guidance to fabricate mechanically robust ZrSiO4 ceramics at low temperatures with a low doping level of dopant.
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35.
  • Fu, Le, et al. (author)
  • Far from equilibrium ultrafast high-temperature sintering of ZrO2-SiO2 nanocrystalline glass-ceramics
  • 2023
  • In: Journal of The American Ceramic Society. - : John Wiley & Sons. - 0002-7820 .- 1551-2916. ; 106:7, s. 4005-4012
  • Journal article (peer-reviewed)abstract
    • Ultrafast high-temperature sintering (UHS) is a novel sintering technique with ultrashort firing cycles (e.g., a few tens of seconds). The feasibility of UHS has been validated on several ceramics and metals; however, its potential in consolidating glass-ceramics has not yet been demonstrated. In this work, an optimized carbon-free UHS was utilized to prepare ZrO2-SiO2 nanocrystalline glass-ceramics (NCGCs). The phase composition, grain size, densification behavior, and microstructures of NCGCs prepared by UHS were investigated and compared with those of samples sintered by pressureless sintering. Results showed that NCGCs with a high relative density (similar to 95%) can be obtained within similar to 50 s discharge time by UHS. The UHS processing not only hindered the formation of ZrSiO4 and cristobalite but also enhanced the stabilization of t-ZrO2. Meanwhile, owing to the ultrashort firing cycles, the UHS technology allowed the NCGCs to be consolidated in a far from equilibrium state. The NCGCs showed a microstructure of spherical monocrystalline ZrO2 nanocrystallites embedded in an amorphous SiO2 matrix.
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36.
  • Fu, Le, et al. (author)
  • Glass-Ceramics in Dentistry : A Review
  • 2020
  • In: Materials. - : MDPI AG. - 1996-1944. ; 13:5
  • Research review (peer-reviewed)abstract
    • In this review, we first briefly introduce the general knowledge of glass-ceramics, including the discovery and development, the application, the microstructure, and the manufacturing of glass-ceramics. Second, the review presents a detailed description of glass-ceramics in dentistry. In this part, the history, property requirements, and manufacturing techniques of dental glass-ceramics are reviewed. The review provided a brief description of the most prevalent clinically used examples of dental glass-ceramics, namely, mica, leucite, and lithium disilicate glass-ceramics. In addition, we also introduce the newly developed ZrO2-SiO2 nanocrystalline glass-ceramics that show great potential as a new generation of dental glass-ceramics. Traditional strengthening mechanisms of glass-ceramics, including interlocking, ZrO2-reinforced, and thermal residual stress effects, are discussed. Finally, a perspective and outlook for future directions in developing new dental glass-ceramics is provided to offer inspiration to the dental materials community.
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37.
  • Fu, Le, et al. (author)
  • Highly translucent and strong ZrO2-SiO2 nanocrystalline glass ceramic prepared by sol-gel method and spark plasma sintering with fine 3D microstructure for dental restoration
  • 2017
  • In: Journal of the European Ceramic Society. - : Elsevier BV. - 0955-2219 .- 1873-619X. ; 37, s. 4067-4081
  • Journal article (peer-reviewed)abstract
    • Balance of better mechanical strength and good translucency for dental restorative materials is alwaysa challenge. A translucent glass ceramic/ceramic with improved mechanical properties or a strongglass ceramic/ceramic with good translucency would therefore be interesting for dental application.Nanocrystalline glass ceramics (NCGC) attract a lot attention because of their superior optical andmechanical properties. This study aims to obtain ZrO2-SiO2 nanocrystalline glass-ceramic that possesseshigh mechanical strength as well as excellent translucency by controlling the content, size, and connectionof nanocrystalline ZrO2 in a ZrO2-SiO2 glass-ceramic material. Toward this end, well-homogenized nano-powders with three different compositions, 45%ZrO2-55%SiO2 (molar ratio, 45Zr), 55%ZrO2-45%SiO2(55Zr), and 65%ZrO2-35%SiO2 (65Zr), were synthesized, followed by a fast sintering process. Highly-translucent nanocrystalline glass ceramics composed of tetragonal ZrO2 were obtained. Samples withhigh zirconia content showed that the structure of the skeleton was predominately built by nano-sizedellipsoidal ZrO2 particles bonded by grain boundaries, with amorphous SiO2 filling the voids betweenthe ZrO2 particles. The achieved flexural strength measured by piston-on-three-ball test was as high as1014 MPa. To our knowledge, this is one of the highest flexural strength values of glass ceramics everreported, which is higher than transparent zirconia and alumina ceramics. The 3D structure of nanocrys-talline zirconia in silica matrix did enhance the flexural strength of the NCGC. The results of this studysuggest that the new ZrO2-SiO2 NCGC has great potential of using as dental restoration.
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38.
  • Fu, Le, et al. (author)
  • Liquid-phase sintering of ZrO2-based nanocrystalline glass-ceramics achieved by multielement co-doping
  • 2023
  • In: Journal of The American Ceramic Society. - : John Wiley & Sons. - 0002-7820 .- 1551-2916. ; 106:4, s. 2702-2715
  • Journal article (peer-reviewed)abstract
    • Liquid-phase sintering (LPS) is an effective pathway to assist the densification of ceramics. However, it has seldom been used to densify glass-ceramics. In the present study, a multielement co-doping strategy has been utilized to achieve LPS of a ZrO2-SiO2 nanocrystalline glass-ceramic. Compared with undoped samples densified by solid-state sintering, doping of equimolar Al, Y, and Ca promoted the densification of the glass-ceramic at lower temperatures with a faster densification rate. Ternary doping enhanced coarsening of ZrO2 nanocrystallites during sintering and annealing. The distribution of dopants was carefully observed with X-ray energy-dispersive spectrometry technique in scanning electron transmission microscopy mode. Results showed that the three dopants showed different distribution behaviors. After sintering, Y dopants were predominately distributed in ZrO2 nanocrystallites, whereas parts of Al and Ca dopants were distributed in ZrO2 nanocrystallites and part of them co-segregated at the ZrO2/SiO2 heterointerfaces. Meanwhile, the segregation of Ca dopant at some intergranular films among ZrO2 nanocrystallites was observed. Redistribution of dopants did not occur during annealing.
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39.
  • Fu, Le, et al. (author)
  • Microstructure of rapidly-quenched ZrO2-SiO2 glass-ceramics fabricated by container-less aerodynamic levitation technology
  • 2023
  • In: Journal of The American Ceramic Society. - : John Wiley & Sons. - 0002-7820 .- 1551-2916. ; 106:4, s. 2635-2651
  • Journal article (peer-reviewed)abstract
    • In this work, an aerodynamic levitation technology (ALT) was utilized to prepare ZrO2-SiO2 glass-ceramics with two different ZrO2 contents, that is, 35 mol% and 50 mol%. The glass-ceramics were partially melted at similar to 2000 degrees C or fully melted at similar to 3000 degrees C by ALT, followed by rapid quenching to obtain spherical glass-ceramic beads. The phase compositions and microstructures of the glass-ceramics were characterized. Crystallization of ZrO2 occurred during the solidification process and ZrO2 content, processing temperature, and the addition of yttrium (3 mol%) affected the crystalline phase of ZrO2. No ZrSiO4 or crystalline SiO2 were formed during the solidification process and the glass-ceramics were away from thermodynamic equilibrium due to rapid quenching. The glass-ceramics showed a microstructure of irregular-shaped ZrO2 micro-aggregates embedded in an amorphous SiO2 matrix, with lamellar twins and lattice defects formed within ZrO2 crystals. For samples prepared at similar to 3000 degrees C, a liquid-liquid phase separation occurred in the melt, which eventually resulted in the formation of large and irregular-shaped ZrO2 aggregates. In comparison, for samples prepared at similar to 2000 degrees C, pre-existed ZrO2 crystals formed during heating acted as nucleation sites during the cooling process, followed by grain growth to form large ZrO2 aggregates. Solidification and microstructure formation mechanisms were proposed to elucidate the solidification process during rapid cooling and the microstructure of the glass-ceramics obtained.
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40.
  • Fu, Le, et al. (author)
  • Observation of yttrium oxide segregation in a ZrO2-SiO2 glass-ceramic at nanometer dimensions
  • 2020
  • In: Journal of The American Ceramic Society. - : WILEY. - 0002-7820 .- 1551-2916. ; 103:12, s. 7147-7158
  • Journal article (peer-reviewed)abstract
    • Dopant segregation at grain boundaries (GBs) in ceramics has been widely reported, while whether similar segregation behavior occurs in glass-ceramics remains unknown. The distribution of dopant in glass-ceramics may be totally different due to the existence of glass phase. This study examines the distribution of Y3+ ions in a ZrO2-SiO2 glass-ceramic. Two samples were prepared by hot pressing, yttrium oxide-doped, and undoped 65 mol% ZrO2-35 mol% SiO2 nanocrystalline glass-ceramics (NCGCs). The NCGCs had the same microstructure, that is, ZrO2 nanoparticles (NPs) embedded in an amorphous SiO2 matrix. XRD results showed that the undoped NCGC was composed of 20.9 wt% (weight percentage) monoclinic ZrO2 (m-ZrO2) and 79.1 wt% tetragonal ZrO2 (t-ZrO2), while the yttrium oxide-doped NCGC was composed of 9.6 wt% m-ZrO2 and 90.4 wt% t-ZrO2. X-ray energy-dispersive spectrometry (EDS) results in scanning electron transmission microscopy (STEM) mode demonstrated that Y3+ ions segregated both on the surface of ZrO2 NPs and within the thin intergranular glass film (with a thickness of approximately 7 angstrom) between ZrO2 NPs in the yttrium oxide-doped NCGC. Interestingly, no obvious Y signals were detected in the amorphous SiO2 matrix. Density functional theory calculation results showed that Y3+ ions had a strong segregation tendency in the GB area and the segregation of Y3+ ions increased the work of separation of GB layer. These findings provide new understanding of the segregation behavior of dopant in glass-ceramics, which may offer useful guidance for other researchers to tailor the properties of glass-ceramics through GB engineering.
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41.
  • Fu, Le, et al. (author)
  • Size-driven phase transformation and microstructure evolution of ZrO2 nanocrystallites associated with thermal treatments
  • 2021
  • In: Journal of the European Ceramic Society. - : Elsevier. - 0955-2219 .- 1873-619X. ; 41:11, s. 5624-5633
  • Journal article (peer-reviewed)abstract
    • Thermal stability of nanocrystallites plays an important role in the manufacturing and application of nanocrystalline ceramics/glass-ceramics. This study explores the effects of thermal treatments on the microstructures of two ZrO2-SiO2 nanocrystalline glass-ceramics (NCGCs), an undoped one and a yttria-doped one. The two assintered NCGCs were composed of tetragonal (t) and monoclinic (m) ZrO2 nanocrystallites, and SiO2 component was amorphous. t-ZrO2 and m-ZrO2 nanocrystallites were metastable during thermal treatment. The content of m-ZrO2 in the undoped ZrO2-SiO2 NCGC first increased after thermal treating at 850 degrees C for 5 h, then decreased after thermal treating at and above 950 degrees C. After thermal treating at 1250 degrees C for 5 h, t-ZrO2 nanocrystallites experienced a rapid phase transformation during cooling, resulting the formation of 88.6 vol% m-ZrO2. Sizedriven phase transformation was utilized to explain the metastability of t-ZrO2 and m-ZrO2 nanocrystallites. In contrast, the content of m-ZrO2 in the yttria-doped ZrO2-SiO2 NCGC continuously decreased with the increase of thermal treatment temperature. The addition of yttria improved the phase stability of t-ZrO2 up to at least 1250 degrees C. Crystallite size of both t-ZrO2 and m-ZrO2 nanocrystallites increased with the increase of thermal treatment temperature in the two NCGCs. The presence of residual thermal stress in the as-sintered NCGCs changed the lattice spacing of t-ZrO2 and m-ZrO2 nanocrystallites, and the stress can be released after thermal treatment. Thermal treatment exerts significant influences on the microstructure of ZrO2-SiO2 NCGCs.
  •  
42.
  • Fu, Le, et al. (author)
  • Spark plasma sintering of biodegradable Si3N4 bioceramic with Sr, Mg and Si as sintering additives for spinal fusion
  • 2018
  • In: Journal of the European Ceramic Society. - : Elsevier BV. - 0955-2219 .- 1873-619X. ; 38:4, s. 2110-2119
  • Journal article (peer-reviewed)abstract
    • Silicon nitride (Si3N4) bioceramics with standard sintering additives (Al2O3 and Y2O3) are used in spinal fusion. Alternative Si3N4 bioceramics with biologically beneficial sintering additives could lead to improved osseoin- tegrative properties. The aim of this study is to obtain dense and strong Si3N4 bioceramics by using SrO, MgO and SiO2 as sintering additives, and evaluate the effect of these sintering additives on microstructures and properties of Si3N4 bioceramics. Raw powders with 10 wt% and 18 wt% sintering additives were sintered by spark plasma sintering. Samples sintered at 1750 °C, with an applied pressure of 60 MPa and a holding time of 3 min, showed the highest content of β-Si3N4 (94.9%). The mechanical properties of the developed Si3N4 bio- ceramics are comparable to the mechanical properties of currently used structural Si3N4 ceramics sintered with standard sintering additives (Al2O3 and Y2O3). The highest flexural strength of the developed Si3N4 bioceramics reached 1079 MPa. Ion release results showed that Sr2+,Mg2+ and Si4+ ions kept leaching out within 10 days’ immersion. The degradable Si3N4 bioceramics with adequate strength and biologically beneficial sintering ad- ditives show the promise for load bearing biomedical applications, such as spinal fusion.
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43.
  • Fu, L., et al. (author)
  • Three-Dimensional Insights into Interfacial Segregation at the Atomic Scale in a Nanocrystalline Glass-Ceramic
  • 2021
  • In: Nano Letters. - : American Chemical Society (ACS). - 1530-6984 .- 1530-6992. ; 21:16, s. 6898-6906
  • Journal article (peer-reviewed)abstract
    • The distribution of dopant atoms plays a key role in the effectiveness of doping, thereby requiring delicate characterizations. In this study, we found that energy-dispersive X-ray spectroscopy (EDX) and electron energy loss spectroscopy (EELS) techniques in scanning transmission electron microscopy (STEM) were not adequate to reveal the distribution of yttrium and the chemical composition of the ZrO2/SiO2 heterophase interface in an yttrium-doped ZrO2-SiO2 nanocrystalline glass-ceramic. Atom probe tomography (APT) is rarely utilized to characterize ceramics due to some inherent difficulties. However, we successfully revealed the three-dimensional distribution of ZrO2 nanocrystallites and SiO2 matrix at the atomic scale with APT under optimized and well-controlled conditions. We also found that the ZrO2 nanocrystallites had a special core-shell structure, with a thin Zr/Si interfacial layer as a shell and a ZrO2 solid solution as a core. Yttrium dopants showed interfacial segregation at both ZrO2 grain boundaries and the ZrO2/SiO2 heterophase interfaces.
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44.
  • Fu, Le, et al. (author)
  • Ultrastrong translucent glass ceramic with nanocrystalline, biomimetic structure
  • 2018
  • In: Nano letters (Print). - : American Chemical Society (ACS). - 1530-6984 .- 1530-6992. ; 18:11, s. 7146-7154
  • Journal article (peer-reviewed)abstract
    • Transparent/translucent glass ceramics (GCs) have broad applications in biomedicine, armor, energy, and constructions. However, GCs with improved optical properties typically suffer from impaired mechanical properties, compared to traditional sintered full-ceramics. We present a method of obtaining high-strength, translucent GCs by preparing ZrO2-SiO2 nanocrystalline glass ceramics (NCGCs), with a microstructure of monocrystalline ZrO2 nanoparticles (NPs), embedded in an amorphous SiO2 matrix. The ZrO2-SiO2 NCGC with a composition of 65%ZrO2-35%SiO2 (molar ratio, 65Zr) achieved an average flexural strength of 1 GPa. This is one of the highest flexural strength values ever reported for GCs. ZrO2 NPs have a core-shell structure, and the shell is a thin (2–3 nm) amorphous Zr/Si interfacial layer that provides strong bonding between the ZrO2 NPs and SiO2 matrix. The diffusion of Si atoms into the ZrO2 NPs forms a Zr-O-Si superlattice. Electron tomography results show that some of the ZrO2 NPs are connected in one direction, forming in situ ZrO2 nanofibers (with length of ~500 nm), and that the ZrO2 nanofibers are stacked in an ordered way in all three dimensions. The nano-architecture of the ZrO2 nanofibers mimics the architecture of mineralized collagen fibril in cortical bone. Strong interface bonding enables efficient load transfer from the SiO2 matrix to the 3D nano-architecture built by ZrO2 nanofibers and NPs, and the 3D nano-architecture carries the majority of the external load. These two factors synergistically contribute to the high strength of the 65Zr NCGC. This study deepens our fundamental understanding of the microstructure-mechanical strength relationship, which could guide the design and manufacture of other high-strength, translucent GCs.
  •  
45.
  • Fu, Le, et al. (author)
  • Understanding microstructure-mechanical properties relationship in ZrO2-SiO2 nanocrystalline glass-ceramics : The effect of ZrO2 content
  • 2022
  • In: Materials Science & Engineering. - : Elsevier. - 0921-5093 .- 1873-4936. ; 840
  • Journal article (peer-reviewed)abstract
    • The content of crystalline phase plays a significant role in manipulating the microstructure and mechanical properties of glass-ceramics. This study aims at exploring the optimum content of crystalline phase in ZrO2-SiO2 nanocrystalline glass-ceramics (NCGCs) in terms of obtaining the highest mechanical properties. To this end, the mechanical properties of ZrO2-SiO2 NCGCs with 70 mol%, 75 mol%, 80 mol% ZrO2 were tested and compared with those of the previously prepared NCGCs with ZrO2 content ranging from 35 mol% to 65 mol%. Results showed that 65 mol% was the optimum content of ZrO2 in terms of obtaining the highest flexural strength. The flexural strength of NCGCs with ZrO2 content over 65 mol% was lower than that of the NCGCs with 65 mol% ZrO2. This was because the NCGC with 65 mol% ZrO2 had a homogenous microstructure, with ZrO2 nano crystallites homogeneously distributed in an amorphous SiO2 matrix. Whereas, when ZrO2 content was increased to 75 mol%, ZrO2 nanocrystallites were not homogeneously distributed in the SiO2 matrix anymore. The formation of SiO2 "holes/canyon " due to ZrO2 grain coalescence resulted in the decrease of flexural strength. The fracture mechanism and wear properties of the NCGCs were also investigated.
  •  
46.
  • Gallinetti, Sara, 1985-, et al. (author)
  • Titanium reinforced calcium phosphate improves bone formation and osteointegration in ovine calvaria defects : a comparative 52 weeks study
  • 2021
  • In: Biomedical Materials. - : Institute of Physics Publishing (IOPP). - 1748-6041 .- 1748-605X. ; 16:3
  • Journal article (peer-reviewed)abstract
    • In a 52 week ovine calvaria implantation model, the restoration of cranial defects with a bare titanium mesh (Ti-mesh) and a titanium mesh embedded in a calcium phosphate (CaP-Ti) were evaluated in seven animals. During the study, no major clinical abnormalities were observed, and all sheep presented a normal neurologic assessment. Blood and cerebrospinal fluid analysis, made at termination, did not show any abnormalities. No indentation of the soft tissue was observed for either test article; however, the Ti-mesh burr-hole covers were associated with filling of the calvarial defect by fibrous tissue mainly. Some bone formation was observed at the bottom of the created defect, but no significant bone was formed in the proximity of the implant. The defect sites implanted with CaP-Ti were characterized by a moderate degradation of the calcium phosphate (CaP) that was replaced by mature bone tissue. Calcium-phosphate-filled macrophages were observed in all animals, indicating that they might play a vital role in osteogenesis. The newly formed bone was present, especially at the bony edges of the defect and on the dura side. Integration of the Ti-mesh in a CaP improved bone formation and osteointegration in comparison to a bare Ti-mesh.
  •  
47.
  • Garbani, M., et al. (author)
  • Allergen-loaded strontium-doped hydroxyapatite spheres improve allergen-specific immunotherapy in mice
  • 2017
  • In: Allergy. European Journal of Allergy and Clinical Immunology. - : Wiley. - 0105-4538 .- 1398-9995. ; 72:4, s. 570-578
  • Journal article (peer-reviewed)abstract
    • BackgroundImmunomodulatory interventions play a key role in the treatment of infections and cancer as well as allergic diseases. Adjuvants such as micro- and nanoparticles are often added to immunomodulatory therapies to enhance the triggered immune response. Here, we report the immunological assessment of novel and economically manufactured microparticle adjuvants, namely strontium-doped hydroxyapatite porous spheres (SHAS), which we suggest for the use as adjuvant and carrier in allergen-specific immunotherapy (ASIT).Methods and ResultsScanning electron microscopy revealed that the synthesis procedure developed for the production of SHAS results in a highly homogeneous population of spheres. SHAS bound and released proteins such as ovalbumin (OVA) or the major cat allergen Fel d 1. SHAS-OVA were taken up by human monocyte-derived dendritic cells (mdDCs) and murine DCs and did not have any necrotic or apoptotic effects even at high densities. In a murine model of ASIT for allergic asthmatic inflammation we found that OVA released from subcutaneously injected SHAS-OVA led to a sustained stimulation of both CD4+ and CD8+ T-cells. ASIT with SHAS-OVA as compared to soluble OVA resulted in similar humoral responses but in a higher efficacy as assessed by symptom scoring.ConclusionWe conclude that SHAS may constitute a suitable carrier and adjuvant for ASIT with great potential due to its unique protein-binding properties.
  •  
48.
  • Ghajeri, Farnaz, et al. (author)
  • The Influence of Residuals Combining Temperature and Reaction Time on Calcium Phosphate Transformation in a Precipitation Process
  • 2022
  • In: Journal of Functional Biomaterials. - : MDPI. - 2079-4983. ; 13:1
  • Journal article (peer-reviewed)abstract
    • Precipitation is one of the most common processes to synthesize hydroxyapatite, which is the human body’s mineral forming bone and teeth, and the golden bioceramic material for bone repair. Generally, the washing step is important in the precipitation method to remove the residuals in solution and to stabilize the phase transformation. However, the influence of residuals in combination with the reaction temperature and time, on calcium phosphate formation, is not well studied. This could help us with a better understanding of the typical synthesis process. We used a fixed starting ion concentration and pH in our study and did not adjust it during the reaction. XRD, FTIR, ICP-OES, and SEM have been used to analyze the samples. The results showed that combining residuals with both reaction temperature and time can significantly influence calcium phosphate formation and transformation. Dicalcium phosphate dihydrate formation and transformation are sensitive to temperature. Increasing temperature (60◦C) can inhibit the formation of acidic calcium phosphate or transform it to other phases, and further the particle size. It was also observed that high reaction temperature (60◦C) results in higher precipitation efficiency than room temperature. A low ion concentration combining reaction temperature and time could still significantly influence the calcium phosphate transformation during the drying. © 2022 by the authors. 
  •  
49.
  • Guillet, Claire, et al. (author)
  • Bone formation beyond the skeletal envelope using calcium phosphate granules packed into a collagen pouch-a pilot study
  • 2023
  • In: Biomedical Materials. - : Institute of Physics Publishing (IOPP). - 1748-6041 .- 1748-605X. ; 18:3
  • Journal article (peer-reviewed)abstract
    • In this proof-of-concept, bone neoformation beyond the skeletal envelope is explored by using a collagen pouch (n = 6) packed with calcium phosphate (CaP) granules placed over the frontal bone in sheep (n = 3). At 13 weeks, macroscopic examination showed specimens covered by an adherent fibrinous envelope with slight vascularization. Histology revealed colonization of the implant by newly formed woven bone and fibrous connective tissue. Surface osteoblasts as well as material-filled macrophages, lymphocytes, polymorphonuclear cells and giant cells were also found in large quantities surrounding the newly formed bone tissue inside the collagen pouch. On the side facing the recipient bone, the collagen membrane had to a large extent been resorbed and bridging bone formation was clearly visible between the test article and recipient bone. On the other side facing soft tissue, the collagen pouch remained intact with a visible fibrous capsule. This study demonstrated that the use of a collagen sleeve as a container for CaP granules allows for good neoformation beyond the skeletal envelope with bridging bone formation clearly visible between the test article and recipient bone. Additionally, in this model, macrophages rather than osteoclasts appear to modulate CaP granule resorption and remodeling into new bone. This construct opens new perspectives for treatment methods that could be used for bone augmentation and restoration of cranio-maxillofacial defects and malformations.
  •  
50.
  • Guo, Hua, et al. (author)
  • Quantitative phase analyses of biomedical pyrophosphate-bearing monetite and brushite cements by solid-state NMR and powder XRD
  • 2020
  • In: Ceramics International. - : Elsevier BV. - 0272-8842 .- 1873-3956. ; 46:8, s. 11000-11012
  • Journal article (peer-reviewed)abstract
    • We present a comprehensive composition analysis of calcium phosphate cements (CPCs) incorporating increasing amounts of bioactive pyrophosphate species (up to 17 wt% P2O7). These cements comprise primarily poorly ordered monetite (CaHPO4) or brushite (CaHPO4 center dot 2H(2)O) and are investigated for enhanced osteoinductive bone/tooth implants. The specimens were characterized by magic-angle spinning (MAS) P-31 and H-1 nuclear magnetic resonance (NMR) spectroscopy along with powder X-ray diffraction (PXRD). P-31 MAS NMR was employed to quantify the major monetite/brushite constituents, the crystalline and amorphous pyrophosphates, as well as various minor orthophosphate by-products. The NMR-derived contents of the crystalline phases accorded well with those from Rietveld analyses of the corresponding PXRD data. The amounts of crystalline and amorphous pyrophosphate depended on the precise cement precursor mixture and preparation conditions, which together with their distinct structural roles may enable the design of cements with a tunable P2O74 - release into aqueous solutions.
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