Parameters microstructure of ZrO2(Y2O3)-Bioglass, sintered at 1300°C.
\\n\\n
Dr. Pletser’s experience includes 30 years of working with the European Space Agency as a Senior Physicist/Engineer and coordinating their parabolic flight campaigns, and he is the Guinness World Record holder for the most number of aircraft flown (12) in parabolas, personally logging more than 7,300 parabolas.
\\n\\nSeeing the 5,000th book published makes us at the same time proud, happy, humble, and grateful. This is a great opportunity to stop and celebrate what we have done so far, but is also an opportunity to engage even more, grow, and succeed. It wouldn't be possible to get here without the synergy of team members’ hard work and authors and editors who devote time and their expertise into Open Access book publishing with us.
\\n\\nOver these years, we have gone from pioneering the scientific Open Access book publishing field to being the world’s largest Open Access book publisher. Nonetheless, our vision has remained the same: to meet the challenges of making relevant knowledge available to the worldwide community under the Open Access model.
\\n\\nWe are excited about the present, and we look forward to sharing many more successes in the future.
\\n\\nThank you all for being part of the journey. 5,000 times thank you!
\\n\\nNow with 5,000 titles available Open Access, which one will you read next?
\\n\\nRead, share and download for free: https://www.intechopen.com/books
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Preparation of Space Experiments edited by international leading expert Dr. Vladimir Pletser, Director of Space Training Operations at Blue Abyss is the 5,000th Open Access book published by IntechOpen and our milestone publication!
\n\n"This book presents some of the current trends in space microgravity research. The eleven chapters introduce various facets of space research in physical sciences, human physiology and technology developed using the microgravity environment not only to improve our fundamental understanding in these domains but also to adapt this new knowledge for application on earth." says the editor. Listen what else Dr. Pletser has to say...
\n\n\n\nDr. Pletser’s experience includes 30 years of working with the European Space Agency as a Senior Physicist/Engineer and coordinating their parabolic flight campaigns, and he is the Guinness World Record holder for the most number of aircraft flown (12) in parabolas, personally logging more than 7,300 parabolas.
\n\nSeeing the 5,000th book published makes us at the same time proud, happy, humble, and grateful. This is a great opportunity to stop and celebrate what we have done so far, but is also an opportunity to engage even more, grow, and succeed. It wouldn't be possible to get here without the synergy of team members’ hard work and authors and editors who devote time and their expertise into Open Access book publishing with us.
\n\nOver these years, we have gone from pioneering the scientific Open Access book publishing field to being the world’s largest Open Access book publisher. Nonetheless, our vision has remained the same: to meet the challenges of making relevant knowledge available to the worldwide community under the Open Access model.
\n\nWe are excited about the present, and we look forward to sharing many more successes in the future.
\n\nThank you all for being part of the journey. 5,000 times thank you!
\n\nNow with 5,000 titles available Open Access, which one will you read next?
\n\nRead, share and download for free: https://www.intechopen.com/books
\n\n\n\n
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Pityana",slug:"sisa-pityana",email:"spityana@csir.co.za",position:null,institution:null},{id:"177716",title:"Dr.",name:"Olawale",middleName:null,surname:"Popoola",fullName:"Olawale Popoola",slug:"olawale-popoola",email:"PopoolaO@tut.ac.za",position:null,institution:null},{id:"283922",title:"Mr.",name:"Sadiq",middleName:null,surname:"Raji",fullName:"Sadiq Raji",slug:"sadiq-raji",email:"rajchandy2355@gmail.com",position:null,institution:null},{id:"292715",title:"Dr.",name:"Fatai",middleName:null,surname:"Aramide",fullName:"Fatai Aramide",slug:"fatai-aramide",email:"AramideFO@tut.ac.za",position:null,institution:null}]},book:{id:"8558",title:"Aerodynamics",subtitle:null,fullTitle:"Aerodynamics",slug:"aerodynamics",publishedDate:"February 10th 2021",bookSignature:"Mofid Gorji-Bandpy and Aly-Mousaad Aly",coverURL:"https://cdn.intechopen.com/books/images_new/8558.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"35542",title:"Prof.",name:"Mofid",middleName:null,surname:"Gorji-Bandpy",slug:"mofid-gorji-bandpy",fullName:"Mofid Gorji-Bandpy"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}}},ofsBook:{item:{type:"book",id:"6170",leadTitle:null,title:"Arid Environments and Sustainability",subtitle:null,reviewType:"peer-reviewed",abstract:"Arid environments are basically associated with water scarcity. Therefore, soils will have an extremely low moisture level to support plant and animal life as well as human social life. Sustainability is the long durability of systems and processes within various adapted environmental conditions. Recently, systematic scientific studies on arid environments and sustainability have become more attractive, critical, and sound than the previous years. Sharing such experiences related to different environmental circumstances will absolutely help scientists and decision-makers to have better interpretation of their own environment. By learning lessons, appropriate, fast, and effective approaches require to implement for overwhelming such problems. Such actions will certainly lead to more secure and sustainable environments for plant, animal, and human life.",isbn:"978-1-78923-155-7",printIsbn:"978-1-78923-154-0",pdfIsbn:"978-1-83881-316-1",doi:"10.5772/intechopen.68381",price:119,priceEur:129,priceUsd:155,slug:"arid-environments-and-sustainability",numberOfPages:118,isOpenForSubmission:!1,hash:"e0649511530c554a4cd5baf9432a4d3c",bookSignature:"Hasan Arman and Ibrahim Yuksel",publishedDate:"May 23rd 2018",coverURL:"https://cdn.intechopen.com/books/images_new/6170.jpg",keywords:null,numberOfDownloads:3067,numberOfWosCitations:6,numberOfCrossrefCitations:5,numberOfDimensionsCitations:11,numberOfTotalCitations:22,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"May 30th 2017",dateEndSecondStepPublish:"June 20th 2017",dateEndThirdStepPublish:"November 25th 2017",dateEndFourthStepPublish:"December 25th 2017",dateEndFifthStepPublish:"February 25th 2018",remainingDaysToSecondStep:"4 years",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:"Edited by",kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"143532",title:"Prof.",name:"Hasan",middleName:null,surname:"Arman",slug:"hasan-arman",fullName:"Hasan Arman",profilePictureURL:"https://mts.intechopen.com/storage/users/143532/images/system/143532.png",biography:"Dr. Hasan Arman has been a professor in the Geology Department at United Arab Emirates University, College of Science, since 2008. He has been head of the department since August 2018. He received his BSc and MSc from Hacettepe and Istanbul Universities, Turkey, in 1984 and 1986, respectively. He obtained a Ph.D. from the University of Arizona, USA, in 1992. He worked as a postdoc at the University of Nevada, Reno, USA, from 1992 to 1993. He worked as a researcher at Tokai University, Japan, from 1995 to 1997 on a Japanese Monbusho Scholarship. He was also a faculty member at the Civil Engineering Department, Sakarya University, Turkey, between 1993 and 2008. Dr. Arman has taught several different courses at undergraduate and graduate levels. His research interests include rock mechanics, engineering geology, environmental degradation, sustainability, water resources, global warming, climate change, and renewable and sustainable energy sources. Dr. Arman has a number of publications in different peer-reviewed national and international scientific journals.",institutionString:"United Arab Emirates University",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"2",institution:{name:"United Arab Emirates University",institutionURL:null,country:{name:"United Arab Emirates"}}}],coeditorOne:{id:"143271",title:"Prof.",name:"Ibrahim",middleName:null,surname:"Yuksel",slug:"ibrahim-yuksel",fullName:"Ibrahim Yuksel",profilePictureURL:"https://mts.intechopen.com/storage/users/143271/images/4856_n.png",biography:"Prof. Dr. Ibrahim Yuksel received his undergraduate degree from Gazi University, Turkey in 1988. His MSc. experience from UK. He has studied in his area in MidKent College, in Chatham, UK. His Ph.D. degree from Karadeniz Technical University, Turkey in 2000. Dr. Yuksel is a civil engineer and has about 30 years of experience in hydraulic engineering. His study area is renewable and sustainable energy, especially hydro energy. \n\nHe studied in Karadeniz Technical University, Department of Civil Engineering (1991-2005) and Sakarya University, Technology Faculty, Civil Engineering, Department (2005-2014) in Turkey.\n\nSince 2014, he has been working for Yildiz Technical University, Faculty of Civil Engineering, Department of Civil Engineering, Hydraulics Division, in Istanbul, Turkey\n\nHe has a lot of experiences such as director, manager, member of universities board, Erasmus Coordinator etc. \n\nDuring to his study experience he delivered some lessons about his subject in 10 European Countries (Italy, Germany, Portugal, Hungary, Poland, Slovenia, Republic of Czech, etc.)",institutionString:null,position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"0",institution:null},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"136",title:"Environmental Sustainability",slug:"environmental-sciences-environmental-sustainability"}],chapters:[{id:"58289",title:"Strategies to Enhance Sustainability of Land Resources in Arid Regions",slug:"strategies-to-enhance-sustainability-of-land-resources-in-arid-regions",totalDownloads:817,totalCrossrefCites:1,authors:[{id:"212830",title:"Dr.",name:"Selen",surname:"Deviren Saygın",slug:"selen-deviren-saygin",fullName:"Selen Deviren Saygın"}]},{id:"59125",title:"Simulating the Productivity of Desert Woody Shrubs in Southwestern Texas",slug:"simulating-the-productivity-of-desert-woody-shrubs-in-southwestern-texas",totalDownloads:637,totalCrossrefCites:0,authors:[{id:"31229",title:"Dr.",name:"James R.",surname:"Kiniry",slug:"james-r.-kiniry",fullName:"James R. 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This requires extensive analysis of developing trends in scientific research in order to offer our readers relevant content. Creating the book catalogue is also based on keeping track of the most read, downloaded and highly cited chapters and books and relaunching similar topics. I am also responsible for consulting with our Scientific Advisors on which book topics to add to our catalogue and sending possible book proposal topics to them for evaluation. Once the catalogue is complete, I contact leading researchers in their respective fields and ask them to become possible Academic Editors for each book project. Once an editor is appointed, I prepare all necessary information required for them to begin their work, as well as guide them through the editorship process. I also assist editors in inviting suitable authors to contribute to a specific book project and each year, I identify and invite exceptional editors to join IntechOpen as Scientific Advisors. 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"18285",title:"ZrO2-Bioglass Dental Ceramics: Processing, Structural and Mechanics Characterization",doi:"10.5772/22334",slug:"zro2-bioglass-dental-ceramics-processing-structural-and-mechanics-characterization",body:'\n\t\t
The continuous evolution in the development and use of ceramics in various applications, which have hitherto not been considered, have been studied in order to reduce costs and increase the mechanical properties, promoting a longer life applications, with quality assurance.
\n\t\t\tWhen considering the use of ceramics in structural materials as materials for implants and implant components, it can be noted as acceptable to meet the demands from the work of mastication, bending fracture strength of about 250MPa and toughness fracture, fracture toughness, about 3MPa.m1/2. It is understood that results of these characterizations above indicators guarantees of reliability (ANUSAVICE, 2005).
\n\t\t\tThe polycrystalline tetragonal zirconia is widely used as an agent for other toughened ceramics, because this material has a phase transformation induced by stress, a change of metastable tetragonal phase to monoclinic phase is accompanied by a volume expansion (3-6%), as specialized bibliographies. The transformation absorbs part of the energy required for crack propagation, with an increase in fracture toughness.
\n\t\t\tBioglasses are bioactive materials, which are based on the following hypothesis: "The biocompatibility of an implant material is great if the material provides the formation of normal tissue on its surface and, additionally, if it establishes a seamless interface capable of withstanding the loads that normally occur at the site of implantation"(KOHN; DUCHEYNE; AWERBUCH, 1992).
\n\t\t\tThe use of Bioglasses as sintering additives was studied by Amaral (AMARAL, 2002) in Si3N4 and Huang (HUANG, 2003) in ZrO2. This practice reduced the final sintering temperature, without significantly affecting the properties of these materials for dental applications.
\n\t\t\tIn the present work was used as sintering additive, a Bioglass system CaO-P2O5-SiO2-MgO, for application as biomaterial. The use of this additive reduced the final sintering temperature, reducing the manufacturing cost of the product while maintaining the biocompatibility of the product. The bioactive, by having the thermal expansion coefficient close to the materials used in coatings in cosmetic dental implants, improve the adhesion between implant components based on ZrO2 and the crown (prosthetic) teeth. It is expected that the Bioglass intergranular additive occupies the interstices and gaps of zirconia and thereby minimize the internal porosity, increasing the mechanical strength and fracture toughness in sintered materials at low temperatures, since the interstices and voids represent the possibility of appearance of micro cracks.
\n\t\t\tThe main objective of this study is to evaluate the microstructural aspects and the physical and mechanical properties of Y-TZP ceramics, ZrO2(Y2O3), sintered, and Bioglass system 3CaO-P2O5-SiO2-MgO as an additive to liquid phase sintering.
\n\t\tThe materials used in this work were commercially available:
\n\t\t\tTetragonal yttria stabilized Zirconia (ZrO2) ceramic Y-TZP containing 3mol% Y2O3, with particle average size of 0.97 µm;Ca (H2PO4) 2.H2O, high purity (99.99%); CaCO3, high purity (99.99%); SiO2, high purity (99.99%) and MgO, high purity (99.99%).
\n\t\tThe necessary procedures of processing steps and characterization of materials used in this work are shown in Figure 1.
\n\t\t\tFlowchart of activities
Was evaluated the content of Bioglass on the results of densification, flexural strength and fatigue, shrinkage during sintering, and the effects on the microstructural configuration. To determine density variations were measured and weighed the compressed green and after sintering.
\n\t\t\tIt was prepared a composition of Bioglass, based on 52.75wt% CaOP2O5, 30wt%SiO2, 17.25wt% MgO. This composition was studied by Oliveira (OLIVEIRA et al., 1997) and presented biocompatibility with high bioactivity.
\n\t\t\t\tThe powders were mixed in a rotary mill for 2 hours using pot stirring rod and polypropylene, in the midst of isopropyl alcohol with zirconia balls for sintered necessary homogenization.
\n\t\t\t\tOnce mixed, the powders were dried in an oven (110°C) for 24 hours, sieved (sieve 63m) and melted at a temperature of 1550°C, the air in a platinum crucible for 2 hours with a heating rate of 10°C/min. The cast (Bioglass) was then rapidly quenched in water at room temperature to obtain better fragmentation and amorphization.
\n\t\t\t\tThe Bioglass was taken to the oven for drying, and subsequently fragmented with the use of an agate mortar, ground and passed through a sieve of 32m. The powder, after screening, was subjected to characterization using the techniques of X-Ray Diffraction, Scanning Electron Microscopy (SEM) and Dilatometry.
\n\t\t\tCompositions were prepared from powder mixtures, adding distinct Bioglass content ranging from 3 to 5 and 10wt% by weight in the mixture with ZrO2 (Y2O3). Higher values were inviable, since their low mechanical properties due to the small degree of densification, as the evaluations carried out previously by Habibe (HABIBE, 2007).
\n\t\t\t\tThe raw materials were mixed in attrition mill amid isopropyl alcohol and stirred at 1000 rpm for 2 hours. For every 100g of powder mixtures during milling were used 180g of zirconia balls of sintered with an average diameter of 2mm. The stirring rod and grinding chamber, used herein, are made of polypropylene, to prevent contamination of powder mixtures for possible chafing with the surfaces in contact.
\n\t\t\t\tAfter milling, drying was performed for each mixture, using the vacuum absorption of excess fluid. The drying process was completed in an oven at a temperature of 100°C for 24 hours. The powders were then subjected to screens: 425, 125, 63 and 32m. Again it was used agate mortar for each overflow of sieves.
\n\t\t\t\n\t\t\t\t\t\t
The coefficients of thermal expansion and glass transition temperature of the compositions were determined by dilatometry using dilatometer - BAHR Thermoanalyse GmbH DIL801L 2000 Model, furnace 7040 (1600°C). Samples of 3mm x 3mm, 10mm in length were prepared with standard measure based on Al2O3, and heated air, heating rate 25°C/min and cooling at 5°C/min.
\n\t\t\t\t\t\n\t\t\t\t\t\t
The phases present, both the powders of departure and the powder mixture were identified by X-Ray Diffraction, using diffractometer model XRD-6000 Shimadzu, which is a radiation ‘Cu-K’, with scanning between 20° and 80°, applying step angle of 0.05° and 3 seconds to scan for point counting. The peaks were identified by comparison with JCPDS standard file (JCPDS, 1988).
\n\t\t\t\t\t\n\t\t\t\t\t\t
The powders were observed, the morphology of the particles by analysis by scanning electron microscopy - SEM, LEO 1450VP microscope using EDS and WDS engaged. In the analysis, the powders were coated with thin film of gold and observed using backscattered electron beam, allowing verification by the difference in tone, the phases and morphology of the particles. Were checked by X-Ray Diffraction, the results of possible chemical or crystallographic changes during the stages of milling and compacting the powder mixture.
\n\t\t\t\t\tThe study focuses on the compatibility analysis (green density) and concentration of monoclinic phase in the samples to be subjected to sintering.
\n\t\t\t\tPrior to tests of flexion characterizations were performed for density, hardness, fracture toughness, microstructure and surface phases.
\n\t\t\t\t\t\n\t\t\t\t\t\t
Density of the green bodies was determined by geometric method. The samples were measured in caliper with an accuracy of 0.01mm, and subsequently weighed on analytical balance (10-5g). To a greater degree of accuracy, there were 15 measurements of each sample to obtain an average value reliably.
\n\t\t\t\t\t\n\t\t\t\t\t\t
The phases present in sintered samples were identified by X-Ray Diffraction using radiation "Cu-K ", scan from 10° to 80°, the step angle of 0.05° and speed of 3 sec/point count. The peaks were identified by comparison with JCPDS file.
\n\t\t\t\t\tQuantification of volume fraction of monoclinic phase (FM) was calculated from the integrated intensities of monoclinic peaks (\n\t\t\t\t\t\t\t
For which:
\n\t\t\t\t\twhere: (\n\t\t\t\t\t\t\t
The calculation of the penetration depth of X-rays on the surface was analyzed based on the absorption of these rays by the material. The penetration depth of X-rays was given by equation (3) (KLUG, ALEXANDER, 1974):
\n\t\t\t\t\twith
\n\t\t\t\t\twhere:
\n\t\t\t\t\th = penetration depth [μm];
\n\t\t\t\t\t\n\t\t\t\t\t\t
I = intensity of X-ray beam diffracted
\n\t\t\t\t\tI0 = intensity of X-ray beam focused,
\n\t\t\t\t\tμ = absorption coefficient;
\n\t\t\t\t\tw = weight fraction of component or element;
\n\t\t\t\t\tρ = density [g/cm3] (Zr = 6.511; O = 1.354; Y = 4.472; ZrO2.3%Y2O3 = 6.051).
\n\t\t\t\t\t\n\t\t\t\t\t\t
We performed observations of the sintered samples by scanning electron microscopy LEO 1450VP coupled with WDS. To observe the microstructure, the samples were ground and polished according to the procedure mentioned below. After mounting the samples in bakelite, thinning was performed in automatic grinding with diamond paste of particle size, in mesh, from 180 to 600, for the total removal of the inlay material and obtain a flat surface for analysis.
\n\t\t\t\t\tThen the samples were polished with diamond pastes, the sequence of 15, 9, 6, 3 and 1m. To reveal the grain boundaries, surfaces polished attack suffered heat to air at 1,400°C for 15 min using a heating rate of 30°C/min to minimize the effects of temperature on grain size. The distribution of grain sizes were measured in order to study the influence of Bioglass on the content of final grain size of ZrO2 with the purpose of these results are also correlated with the results of mechanical properties. The distribution of grain sizes were measured using image analyzer microscope, LEICA, aimed at studying the influence of Bioglass on the content of final grain size of ZrO2. These results were also correlated with the results of mechanical properties.
\n\t\t\t\tThe methodology used to determine the hardness of the samples followed the ASTM C 1327-99, which provides the standard test method to obtain the Vickers hardness of advanced ceramics.
\n\t\t\tThe methodology for determining the values of fracture toughness by Vickers indentation of the samples followed the recommendations of ASTM C 1421-99. This is the pattern for obtaining the fracture toughness of advanced ceramics at room temperature.
\n\t\t\tFor the analysis of flexural-bodies were used for proof-polished, dimensions (in mm) 45 x 4 x 3, as previously described. The flexural strength at room temperature, (σf) was evaluated by the collapse load of the body of evidence points determined by the method \'4 points\', following the specifications dictated by the standard DIN EN 843-1 (ASTM C 1161-90) with download speed of 0.5mm/min and with a spacing of 40mm and 20mm between the rollers of support and loading, (I1 and I2, respectively) as shown in Figure 2, using a universal machine mechanical testing kN MTS-250.
\n\t\t\t\tSchematic representation of resistance to bending in four points. The polished face is turned down (
The flexural strength of the specimens was calculated using Equation 5.
\n\t\t\t\twhere:
\n\t\t\t\t\n\t\t\t\t\tf = resistance to bending (MPa);
\n\t\t\t\tFA = breaking load (N);
\n\t\t\t\tb = measure the width of the samples (mm);
\n\t\t\t\th = height measurement of samples (mm);
\n\t\t\t\tI1 = wider spacing between the rollers loading (mm);
\n\t\t\t\tI2 = smaller spacing between the rollers loading (mm).
\n\t\t\tThe identification and characterization procedures aimed to verify whether the characteristics of materials and products are expected in the present work, meet the conditions of sufficient quality when applying the final ceramic as dental materials.
\n\t\t\tThe main objective focuses on the characterization of raw material, identifying the origin of each material used, assessing the crystallographic characteristics and morphological profile of the post in question. This goal aims to confirm whether such characteristics of powders, and mixtures of the powders were suitable for the final density of sintered.
\n\t\t\t\tPowders of Zirconia — ZrO2(Y2O3) — and Bioglass were characterized by SEM and the results are shown in Figures 3 and 4. The zirconia powder used in this study was produced through a spray-drying, with additions of ligands, which promote the agglomeration of spherical shapes, as shown in Figure 3. These ligands are used to facilitate compaction of the samples.
\n\t\t\t\t\tParticle morphology of ZrO2(Y2O3) as received.
In Figure 4 are performed by SEM micrographs of samples of Bioglass powder, sifted after. One observes the presence of acicular particles presenting larger dimensions than the sieve, the intrinsic characteristics of glassy materials.
\n\t\t\t\t\tMorphology of the Bioglass after fragmentation and sieving.
The Bioglasses, after collection, were screened on meshes of up to 32m in order to minimize the effect of their distribution in the zirconia matrix, increasing the compaction of the mixtures of powders, where the density on the green of the samples ranged from 48% to 42% due to the addition of Bioglass matrix ZrO2(Y2O3). Reducing the particle size of Bioglass facilitating the spreading of the fluid (liquid phase) during the sintering step.
\n\t\t\t\tThe green relative density of the compacts are shown in Figure 5.
\n\t\t\t\t\tEffect of the addition of Bioglass on the green density of compacts.
Note that there is a slight reduction in relative density due to the addition of Bioglass in its composition. This behavior occurs through the morphology of Bioglass, highly irregular (Figure 5), compared to the powder of ZrO2(Y3O2), used in these experiments. Be considered negligible differences in green density, sintering behavior observed in the samples with different amounts of Bioglass.
\n\t\t\t\t\t\n\t\t\t\t\t\tFigure 6 shows representative micrographs of samples sintered at each composition studied. For comparative analysis of dense material, some samples of ZrO2(Y2O3) were without Bioglass sintered at 1500°C/2 hours.
\n\t\t\t\t\tIt is observed the presence of equiaxed grains of ZrO2 in the whole area analyzed. Were obtained in all cases, with 3, 5 or 10wt% of Bioglass, microstructures were quite similar. There is also the presence of voids between grains resulting from the elimination of residual porosity and intergranular phase during thermal attack.
\n\t\t\t\t\tFrom the micrographs presented in Figure 6 and Table 4.4 lists the microstructural parameters, to verify whether the presence of liquid phase formed from the fusion of glass particles interfered with grain growth of ZrO2.
\n\t\t\t\t\tAnalyzing the results of Table 1 can be stated that the content of Bioglass little or almost nothing, interferes with the average grain size of ZrO2 and density of grains per unit area, as shown in Figure 6.
\n\t\t\t\t\tThese microstructural characteristics are a direct function of initial grain size and sintering temperature used. Dense ZrO2 sintered solid phase is usually obtained at temperatures around 1500°C. In this temperature range, depending on the sintering time applied, the average grain size can vary from 0.5m to 1m, whose sizes are the result of higher levels with very long sintering, such as 1500°C/8h.
\n\t\t\t\t\tThe use of relatively low sintering temperatures, as from 1200 to 1350°C, hinders the growth of the grains of the matrix, thus increasing the population of grain per unit area. In this study, the use of liquid phase has as one of several objectives to facilitate the densification at low temperatures, minimizing the grain growth, which could hamper the
\n\t\t\t\t\tMicrographs of ceramics ZrO2(Y2O3)-Bioglass.
(ZrO2: Bioglass) wt% | \n\t\t\t\t\t\t\t\tMedium Size Grain (μm) | \n\t\t\t\t\t\t\t\tDensity of grains (No. grains /μm2) | \n\t\t\t\t\t\t\t
100:00 (1500°C) | \n\t\t\t\t\t\t\t\t0.803 ± 0.121 | \n\t\t\t\t\t\t\t\t3.405 | \n\t\t\t\t\t\t\t
97:03 | \n\t\t\t\t\t\t\t\t0.325 ± 0.065 | \n\t\t\t\t\t\t\t\t9.982 | \n\t\t\t\t\t\t\t
95:05 | \n\t\t\t\t\t\t\t\t0.329 ± 0.076 | \n\t\t\t\t\t\t\t\t9.964 | \n\t\t\t\t\t\t\t
90:10 | \n\t\t\t\t\t\t\t\t0.333 ± 0.070 | \n\t\t\t\t\t\t\t\t9.939 | \n\t\t\t\t\t\t\t
Parameters microstructure of ZrO2(Y2O3)-Bioglass, sintered at 1300°C.
growth and propagation of cracks during the fracture of the material, knowing that the cracks propagate in this material so intergranular (following the grain boundaries), and has also the beneficial effect of martensitic transformation (tetragonal to monoclinic, as indicated by T→M), which occurs when the crack is tetragonal grain, and exerts compressive stress on them.
\n\t\t\t\tThese tests are carried out to verify the effect of the addition of Bioglass in the temperature of maximum shrinkage of the sintered body by the derivative of the shrinkage versus time. Thus have been able to verify the relationship between the percentage of Bioglass with the rates of dimensional variation of the material versus time and temperature.
\n\t\t\t\t\tThe results of dilatometric analysis performed on samples previously consolidated raw material monolithic, had coefficients of thermal expansion (200-1200°C) to 10.6x10-6/°C tetragonal zirconia polycrystal (Y-TZP) and 10.2x10-6/°C for Bioglass.
\n\t\t\t\t\tFrom the results, there is compatibility between the thermal expansion coefficients of the two phases (ZrO2-Bioglass) for the formation of the composite ceramic-ceramic primary requirement for development of dual-phase ceramic materials (MEYERS, CHAWLA, 1998), due to reduction of residual stresses are generated between the phases of the composite and rigid after cooling.
\n\t\t\t\t\t\n\t\t\t\t\t\tTable 2 presents the results of calculations concerning the average values of the coefficients of thermal expansion, carried out for all compositions in this work, based on the weighting between the coefficients of thermal expansion and modulus of elasticity of the components of mixtures. These values are important in determining the residual stress generated between the phases in sintered.
\n\t\t\t\t\tConcentration of Bioglass (wt%) | \n\t\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t||
Modulus of Elasticity E (GPa)\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\tThermal Expansion Coefficient α (x 10-6/°C) | \n\t\t\t\t\t\t\t\tModulus of Elasticity E (GPa) | \n\t\t\t\t\t\t\t\tThermal Expansion Coefficient α (x 10-6/°C) | \n\t\t\t\t\t\t\t\tThermal Expansion Coefficient α (x 10-6/°C) | \n\t\t\t\t\t\t\t|
3 | \n\t\t\t\t\t\t\t\t90 | \n\t\t\t\t\t\t\t\t10.2 | \n\t\t\t\t\t\t\t\t190 | \n\t\t\t\t\t\t\t\t10.6 | \n\t\t\t\t\t\t\t\t10.599 | \n\t\t\t\t\t\t\t
5 | \n\t\t\t\t\t\t\t\t10.594 | \n\t\t\t\t\t\t\t||||
10 | \n\t\t\t\t\t\t\t\t10.587 | \n\t\t\t\t\t\t\t
General Physical Characteristics of the composites.
The curves of shrinkage and shrinkage rate as a function of temperature and hold time showed the following highlights:
\n\t\t\t\t\t\n\t\t\t\t\t\t
Can be analyzed at temperatures up to 600°C. The most significant variations in this region occur at temperatures around 450°C. At this temperature there is a smooth change of the shrinkage, which can be attributed to the volatilization of organic substances present in the compact. These are derived from organic raw material, ZrO2(Y2O3), which has a binder, and stearin used in compaction of powders.
\n\t\t\t\t\t\n\t\t\t\t\t\t
The region represents the effect of temperature on the shrinkage of compacts, observed from 1,050°C. Observe that there is a characteristic temperature where the rate of shrinkage has a maximum.
\n\t\t\t\t\t\n\t\t\t\t\t\tFigure 7 shows the temperatures of shrinkage depending on the content of Bioglass. In this figure are also presented as the accumulated instantaneous values of shrinkage at these temperatures.
\n\t\t\t\t\tIt is observed that the samples are reduced maximum temperature decrease with increasing amount of Bioglass added. This behavior implies that a larger amount of glass reduces the temperature, the greater formation of liquid phase, which in turn allows a greater shrinkage of the compact. Samples without the presence of additives, have different behavior, because it is sintered by solid phase, and therefore governed by other mechanisms of sintering.
\n\t\t\t\t\tEffect of the addition of Bioglass in the temperatures of greatest rate of shrinkage.
It was observed that for samples with 3wt% of Bioglass, at temperatures below 1300°C, was not reached maximum retraction of the derivative and thus, levels of incorporation of the sintering cycle time initially proposed.
\n\t\t\t\t\tThe temperatures of maximum shrinkage determined for samples with 5 and 10wt% of Bioglass are respectively 1267°C and 1253°C.
\n\t\t\t\t\t\n\t\t\t\t\t\t
In this third area of analysis is taken into account the hold time at 1300°C. From the analysis of Figure7, we observed that the samples with higher concentrations of Bioglass, achieved larger decreases until the maximum temperature testing (1300 ° C).
\n\t\t\t\t\tFrom there, observing Figure 8, note that there is an evolution of the shrinkage in the first minutes of landing, in all situations where Bioglass is used as an additive. Comparatively, the blocks of ZrO2 sintered without the addition of Bioglass show continued growth as a function of hold time, because the weather influences the kinetics of densification of the sintered solid phase.
\n\t\t\t\t\tObserve that the first 20 minutes, in samples with Bioglass, retractions that occur faster when compared with the remaining time, always with a tendency to stabilize the rate of shrinkage (indicated by the rate of change of the curve). Both the rate of shrinkage and total shrinkage increases with increasing content of Bioglass. This is justified by the greater amount of liquid phase which facilitates the diffusion of the solid phase.
\n\t\t\t\t\tEffect of isotherm plateau in shrinkage of the ceramics sintered at 1,300°C.
The results seen above can be represented in percentage gains of shrinkage versus time of isotherm used. These results are shown in Figures 9 and 10.
\n\t\t\t\t\tAn important detail presented by the geometrical behavior of the curves with respect to the correlation between the percentage increase in Bioglass and gain decrease with residence time at 1300°C. The three curves show asymptotic behavior, with the rate of linear shrinkage with time tends to proportionality with the difference between the instantaneous rate and a maximum rate for each composition in Bioglass. Larger amounts of Bioglass cause lower coefficients of thermal expansion, in agreement with Table 2. Add to it that lower the green density implies an increase of spaces to be filled, so it will have a higher rate of shrinkage.
\n\t\t\t\t\tGains due to shrinkage of the content of Bioglass, for various treatment times.
It is evident that the ceramics with 3wt% of Bioglass have improved significantly with the use of level of sintering. At first, with 10 minutes of landing, there is a gain of 60%, indicating that this time was sufficient to reduce the viscosity of the glass, influencing their spread around the ZrO2 grains. Times lead to higher cumulative gains exceeding 85%, as in 120 minutes. Samples with 5 and 10wt% are less influenced by the time of landing, for sintering at 1300°C. Still, for the maximum times studied, 120 minutes, occur up to 20% gains, for ceramics with 5wt% Bioglass and 10% for ceramics with 10wt% of Bioglass. The level of decline observed in the samples will indicate that in all situations where Bioglass was used as an additive, and 1300°C, there is full densification of the ceramics studied. In the case of the ceramics of ZrO2(Y2O3), without addition of glass-forming liquid phase, the phenomenon does not occur.
\n\t\t\t\t\tGains decrease as a function of residence time, for each composition of Bioglass.
It is intended to report the results of analysis of the crystalline phases present in sintered samples, and studies the influence of Bioglass content on densification. With this it will have the assurance that the sintering conditions (temperature, time, rate of heating and cooling) were adequate for obtaining ceramics with adequate strength for use in dental applications.
\n\t\t\t\tThe research initiated by Habibe (HABIBE, 2007) showed that the addition of Bioglass in higher sintered ZrO2(Y2O3) to provide undesirable martensitic transformation (T→M), which promote a volumetric expansion of the ceramic matrix generating increasing porosity.
\n\t\t\t\tOne concern has been established to optimize the densification, taking into account the interrelationship between low sintering temperature, sintering time and microstructural features.
\n\t\t\t\tIn order to demonstrate the efficiency of the technique of X-Ray Diffraction in the characterization and measurement of the percentage of monoclinic and tetragonal phases of ZrO2(Y2O3) was proposed in this study, the use of determining the depth of penetration of radiation, based on parameters crystallographic theory.
\n\t\t\t\t\tUsing the parameters presented the results obtained when applying these equations (3 and 4), was approximately 7.3m. Grain sizes are below 0.5m, so there is a layer thick enough to be detected by diffraction, thus allowing the identification of transformation of monoclinic phase in sub-surface levels with considerable degree of accuracy.
\n\t\t\t\t\tIn pre-existing glasses of similar chemical composition to this study, obtained under the same conditions of melting and cooling, gave values of Vickers hardness near 6.2GPa, when subjected to thermal treatment time exceeding 30 minutes. The values of fracture toughness and resistance to bending found were 0.93MPa.m1/2 and 54MPa, respectively, for materials with rapid cooling (diamonds), and the values of 1.4MPa.m1/2 and 115MPa, respectively, for materials with slow cooling (vitro-ceramic) (OLIVEIRA, 1997).
\n\t\t\t\t\tThe percentage of transformed monoclinic phase after sintering, carried out according to Equations 1 and 2 are presented in Table 3 and illustrated in Figure 11.
\n\t\t\t\t\t\n\t\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t
0 | \n\t\t\t\t\t\t\t\t5.69 + 0.02 | \n\t\t\t\t\t\t\t
3 | \n\t\t\t\t\t\t\t\t6.71 + 0.06 | \n\t\t\t\t\t\t\t
5 | \n\t\t\t\t\t\t\t\t8.75 + 0.03 | \n\t\t\t\t\t\t\t
10 | \n\t\t\t\t\t\t\t\t14.37 + 0.05 | \n\t\t\t\t\t\t\t
Percentage of monoclinic phase in the sintered samples.
This behavior may be related to the gradient of contraction between the two phases (zirconia and Bioglass) after sintering, during cooling, since there is a difference between the thermal expansion coefficients between these materials (10.6x10-6/°C for zirconia and the Bioglass 10.2x10-6/°C). This difference promotes the generation of stress fields around the grains of ZrO2(Y2O3), which may exceed the maximum compressive stress needed to transform the tetragonal-monoclinic. Thus, the grains of ZrO2(Y2O3) tetragonal become monoclinic, with volume expansion of about 3 to 6% by volume (STEVENS, 1986), resulting in an overall structure microcracking, resulting in a reduction in density on the sample. In Figure 4.24 are the results related to this characterization.
\n\t\t\t\t\tMonoclinic phase concentration depending on the content of Bioglass in blocks sintered at 1300°C.
As previously noted, there is elevation of monoclinic fraction considering increasing the amount of additive. Associated with this transformation occurred during cooling, which is due to thermal residual stress motivated by the difference in thermal expansion coefficient between the phases, may be the reason for the reduction of relative density versus the contents of Bioglass as shown in Figure 12.
\n\t\t\t\t\tRelative density as a function of the content of Bioglass, sintered blocks to 1,300°C.
The analysis of X-ray diffraction patterns indicated the presence of considerable fraction of the tetragonal phase and residual fraction of monoclinic phase. Intergranular crystalline phases were not detected in any of sintered body, indicating that the intergranular phase of Bioglass originally made can be fully amorphous or so, the fractions present in the sintered samples are not detected in the diffractometer. This can be considered in the light of that, in previous work (OLIVEIRA et al., 1997).
\n\t\t\t\t\tBioglass cold considering controlled rates similar to those used in this study (10°C/min) showed the crystalline phases whitlockite and enstatite, and this last was not observed in this work. The possible crystallization of the Bioglass used in this work, and therefore the glass ceramics, may have contributed to the improvement of mechanical properties, with the increase in resistance (60 to 120MPa) and fracture toughness (1 to 1.5MPa.m1/2) in the glassy phase (OLIVEIRA et al., 1997).
\n\t\t\t\t\tIt is noteworthy that the material exhibits a tendency to decrease the densification with increasing amounts of Bioglass from 3wt%, and these results imply a direct function of increasing content of monoclinic phase transformed. Furthermore, the low density results on the composition submitted for “100-00”, suitable only for comparison purposes, since this is accomplished by sintering the solid phase, since there have Bioglass in its composition, which could trigger mechanisms unique liquid phase sintering.
\n\t\t\t\t\tThe results indicated that the dilatometry samples monolithic ZrO2(Y2O3) did not densify under these conditions because temperature and isothermal sintering times studied did not allow the efficient operation of the mechanisms for densification of the material. Moreover, samples with Bioglass showed maximum shrinkage temperature of about 1253, 1267 and 1328°C, for contents of Bioglass 10, 5 and 3wt% respectively. In all cases where it is applied Bioglass need for isothermal sintering at 1300°C for full densification is achieved. However, higher levels of Bioglass (ZrO2(Y2O3) containing 10wt% Bioglass) did not allow full densification, because during cooling, as proposed by previous study Habibe (HABIBE, 2007), there is generation of stress fields between the matrix and grain boundaries which promotes the phase transformation (T→M) that generates volume expansion and increased presence of pores and microcracks.
\n\t\t\t\tThe flexural strength, σf, the ceramic is directly proportional to the fracture toughness, KIC, as predicted by linear elastic fracture mechanics (KIM et al., 2000):
\n\t\t\t\t\tThe parameter "c" can be considered alternatively as the size of failure to initiate the fracture. Thus, the size of failure for start of fracture in samples of 3, 5 or 10wt% of Bioglass and sintered at 1300°C/2h, are valued between 80m and 230m.
\n\t\t\t\t\tThe maximum surface roughness, assessed during the preparation of specimens for bending tests/fatigue, was less than 0.30μ m. Whereas the roughness implies that a \'valley\' is half of a crack, it is concluded that the roughness used did not affect the test results.
\n\t\t\t\t\n\t\t\t\t\t\tTable 4 and Figure 13 present the results of Vickers hardness and fracture toughness, KIC, the samples sintered at different temperatures and fractional percentages of Bioglass.
\n\t\t\t\t\tHardness of sintered samples as a function of sintering temperature and amount of Bioglass.
Fracture toughness of sintered samples as a function of sintering temperature and amount of Bioglass.
The samples sintered at 1300°C, containing 3wt% of Bioglass showed higher hardness and toughness, respectively, 1170HV and 6.3MPa.m1/2. These results are related to indicators of relative density and low amount of martensitic transformation, shown in Figures 14 and 15.
\n\t\t\t\t\tIt is important to note that these samples show the best properties, possibly due to the high relative density, coming from the better spreading of the liquid formed during sintering and its penetration around the ZrO2 particles. These phenomenons facilitates the elimination of pores and reduce accumulation of glass triple joints, minimizing the generation of stress fields during cooling and therefore points in favor of crack propagation.
\n\t\t\t\tSamples of ZrO2(Y2O3), with addition of Bioglass, sintered at 1300°C and without addition of Bioglass (sintered at 1500°C) were tested for 4 point bending. The results are presented in Table 4 in Figure15.
\n\t\t\t\t\tBioglass (wt %) | \n\t\t\t\t\t\t\t\tVickers Hardness (HV) | \n\t\t\t\t\t\t\t\tKIC\n\t\t\t\t\t\t\t\t\t (MPa.m1/2) | \n\t\t\t\t\t\t\t\tFlexural Strength (MPa) | \n\t\t\t\t\t\t\t
0 (1500°C) | \n\t\t\t\t\t\t\t\t875 ± 95 | \n\t\t\t\t\t\t\t\t4.1 ± 0.5 | \n\t\t\t\t\t\t\t\t127.44 ± 57.15 | \n\t\t\t\t\t\t\t
3 | \n\t\t\t\t\t\t\t\t1,167 ± 80 | \n\t\t\t\t\t\t\t\t6.3 ± 0.2 | \n\t\t\t\t\t\t\t\t453.28 ± 74.64 | \n\t\t\t\t\t\t\t
5 | \n\t\t\t\t\t\t\t\t1,134 ± 76 | \n\t\t\t\t\t\t\t\t6.1 ± 0.4 | \n\t\t\t\t\t\t\t\t363.31 ±54.88 | \n\t\t\t\t\t\t\t
10 | \n\t\t\t\t\t\t\t\t926 ± 38 | \n\t\t\t\t\t\t\t\t5.0 ± 0.5 | \n\t\t\t\t\t\t\t\t303.00 ± 77.40 | \n\t\t\t\t\t\t\t
Vickers hardness, fracture toughness and Flexural strength of samples sintered.
Flexural strength of samples sintered at 1300°C, depending on the amount of Bioglass added to ZrO2 matrix.
It is observed that the variations in the composition in the flexural strength is shown similar to those observed in the behavior of relative density (Figure 12), hardness (Figure 13) and fracture toughness (Figure 14), ie, an elevation in the range from zero to 3wt% Bioglass and reduction in the range of 3 to 5wt% Bioglass. Such behavior suggests that the 3wt% level gives better distribution in the zirconia matrix, leading to the conclusion that the higher values are dispersed causing islands to concentrate on Bioglass, causing some weakening and partial degradation of those characteristics. Such behavior is indicative of the concentration 3wt% Bioglass in ZrO2(Y2O3) would be the best choice among the four discussed compositions. This without taking into account other factors that could influence the choice.
\n\t\t\t\tThe calculation of the average thermal residual stress generated during cooling of the sintered samples was based on the consideration that there is homogeneous distribution of second phase in ceramic matrix ZrO2, and is directly related to the difference in thermal expansion coefficients between the phases in the ZrO2 matrix and intergranular glassy phase, composed of Bioglass (TAYA et al., 1990; SHI et al., 1998).
\n\t\t\t\t\tWas not taken into account the hypothesis of partial crystallization of the glass or the temperature range where there is softening of the glass present. This average residual thermal stress in the two phases can be calculated as a function of the percentage of intergranular phase (or second) that integrates the system, according to Equations 7 and 8, proposed by Shi (SHI et al., 2000).
\n\t\t\t\t\tWhere σb and σm are the contours and residual stresses in the matrix, respectively. Em and Eb indicate the modulus of elasticity of matrix and grain boundaries (intergranular phase), respectively, and , m and b indicate the average thermal expansion coefficients, the matrix (index m) and the intergranular phase (index b), respectively. The average coefficient of thermal expansion of each composition varies, and is given by Equation 9:
\n\t\t\t\t\tWhere is the coefficient of thermal expansion of the composition; b, Cb, Eb are, respectively, coefficient of thermal expansion, Young\'s modulus and fraction of Bioglass (grain boundary), m, Cm, Em are respectively, the coefficient of thermal expansion, the fraction and the modulus of elasticity of ZrO2 matrix.
\n\t\t\t\t\tBy calculating the average coefficient of thermal expansion and residual stresses, it is found that when αm> αb or σb<0, the grain boundary is the transition between compression (intragranular) and tensile (matrix).
\n\t\t\t\t\tThe residual stress in a multiphase composite is developed due to the discrepancy between the modulus of elasticity and Thermal Expansion Coefficient (TEC) between the constituent phases. Due to the lower TEC of Bioglass, b, compared to the array of ZrO2, m, tensile residual stresses are developed in ZrO2 matrix during cooling from the sintering temperature. (BASU, VLEUGELS, 2001).
\n\t\t\t\t\tThe residual stress in zirconia matrix was calculated according to the model proposed by Taya (TAYA et al., 1990) and confirmed by Shi (SHI et al., 2000). In the calculations we used the modulus of elasticity (E) from 90GPa to 190GPa for the Bioglass and ZrO2. The calculation results of compressive residual stress at grain boundaries and tensile stress in the grains of ZrO2 matrix are shown in Figure 16, and provide a barrier to crack propagation, toughened materials.
\n\t\t\t\t\tThermal residual stress due to the content of Bioglass (intergranular phase)
The toughening of ceramics developed in this work may be related to several phenomena, such as tetragonal-monoclinic transformation, crack deflection, stress-induced martensitic transformation thermal residual porosity of the sintered samples, or other possible causes unrelated. It may be noted that increasing the intergranular phase (Bioglass) leads to increased % of monoclinic phase and increased porosity associated with this phenomenon.
\n\t\t\t\t\tHowever, increasing the amount of Bioglass leads to a greater accumulation of concentrations of glass in triple junctions, with consequent formation of stress concentration, which permits growth and propagation of cracks. The thermal residual stresses in ZrO2 matrix show a smaller and smaller effect as a function of the addition of Bioglass composition. However, there is a reduction in the contribution of residual stress on phase transformation (T→M), which can improve the toughness of ceramics.
\n\t\t\t\t\tMoreover, the presence of low amounts of Bioglass, facilitates the diffusional processes, reduce the possibility of transformation (T→M) to occur during cooling and increase the thermal residual stress between the phases, favoring the phase transformation during the emergence and growth of a crack, toughened material.
\n\t\t\t\t\tPrevious studies have shown that propagation of intergranular cracks of the type prevalent in ZrO2 based ceramic sintered by liquid phase (SHI et al., 1998, SUN et al., 2003, HUANG et al., 2003, SHI et al., 2000) due to the presence of glassy phase. The amount of intergranular phase in which the fracture toughness (KIC), the maximum can be achieved, Cb,m, when αb<m, is as follows:
\n\t\t\t\t\tWhere b Eb are the Thermal Expansion Coefficient (TEC) and Modulus of Elasticity of Bioglass, respectively, and m, and Em are, respectively, the Thermal Expansion Coefficient and Modulus of Elasticity of ZrO2 matrix.
\n\t\t\t\t\tThe calculated results show that a great theoretical value is achieved with 2.84wt% of Bioglass. This result is consistent with the composition of ZrO2-Bioglass composite composed of 97wt% ZrO2 and 3wt% Bioglass, which presents the best mechanical properties among the samples sintered at 1300°C/2h. Moreover, the results are consistent with previous work (SHI et al., 2000), which shows that only a small amount of intergranular glassy phase, an increase of fracture toughness can be obtained.
\n\t\t\t\tAfter the experiments, and based on these results, we can conclude that:
\n\t\t\tSamples of 3wt% Bioglass composition showed better densification compared to those of composition 0, 5 and 10wt% due to better spreading of the liquid phase between grains of ZrO2(Y2O3). These results are related to high density and low percentage of monoclinic ZrO2 phase, present in the sintered samples.
The addition of higher concentrations of additives in an increase in \'islands\' of Bioglass, the junctions between the grains of the matrix of ZrO2(Y2O3) causing residual stress fields, which led to greater amounts of martensitic transformations, after sintering, increasing the weakening of the material.
The results of mechanical characterization promote the use of Bioglass as sintering additive, instead of ZrO2(Y2O3) pure. Using the techniques of X-Ray Diffraction, high resolution, together with testing the hardness, fracture toughness, flexural strength at 4 points confirmed this statement.
The ceramic compositions suggested for studies, combined with the processing conditions (parameters of milling, pressing and sintering) were effective in obtaining the ceramic bodies of high relative density and with relatively fine grain. Regardless of the content of Bioglass added to zirconia, the average grain size of zirconia was in the order 0.30 to 0.35 m.
The additions of 3 and 5% of Bioglass produced an increase in hardness in relation to zirconia with 3wt%Y2O3, and also in relation to the addition of 10wt% of Bioglass, with values of 1240 and 1210HV for 3Y-TZP composites-Bioglass (97-3) and 3Y-TZP-Bioglass (95-5), respectively. These results are due to higher densification of samples submitted for 3wt% of Bioglass.
The authors acknowledge to the FAPESP for financial support, under Grants no. 04/04386-1 and 05/52971-3. They also thank the Fundação Euclides da Cunha - Universidade Federal Fluminense.
\n\t\tThere is sharply increasing demand for energy with the rapid growth of the global economy. The energy generation from sustainable sources, such as wind and solar, plays an important role in power supply. However, the intermittent nature and imbalanced regional distribution of the sustainable energy make them unable to stably supply the power [1]. The development of energy storage systems is an urgent requirement to meet the sufficient and stable power supply for industrial and residential usage. Although rechargeable lithium-ion batteries, dominant energy sources in each field, as high energy density providers have filled their position [2], lithium-ion batteries still have the limitations of poor cycle life and low power performance [3]. Supercapacitors (SCs), also known as ultracapacitor and electrochemical capacitors, are an emerging class of energy storage device, which possess high power density and tens of thousands of charge/discharge cycles [4, 5]. Figure 1 shows the Ragone plot of different energy conversion and storage devices. SCs have a unique position to bridge the gap between conventional capacitors and batteries. Compared with conventional capacitor, SCs possess higher specific energy density in several orders of magnitude. Moreover, SCs provide higher specific power density than batteries due to its unique charge storage mechanism.
\nRagone plot for various energy storage and conversion devices [
Based on different charge storage mechanisms, SCs are mainly divided into two categories, electrical double layer capacitors (EDLCs) and pseudocapacitors, as shown in Figure 2. EDLCs store the electrical charge by electrostatic force at the electrode-electrolyte interface, which is a physical process without involving electrochemical reactions on the electrode surface. In order to increase the capacitance and energy density of SCs, some electrochemically active materials, such as transition metal oxide and conducting polymers, have been explored as electrode materials for pseudocapacitors. The energy storage in pseudocapacitors originates from reversible surface faradaic redox reactions at the interface of electrolyte and electroactive materials.
\nSchematic diagram of (a) an electrical double layer capacitor and (b) a pseudocapacitor.
The capacitance of EDLCs is strongly dependent on effective surface area and the pore size distribution of the electrode [7, 8]. Typically, the carbon-based materials and their derivatives, including activated carbon, carbon nanotubes (CNTs) and graphene, with high conductivity, chemically-stability, and large surface area are widely utilized in EDLCs. Although the EDLCs possess high power density and excellent charge/discharge cycling stability, they suffer from low energy density owing to the relatively low capacitance of carbon-based materials. Pseudocapacitors can achieve significantly higher energy density, as compared to EDLCs, because they have a variety of oxidation states for redox charge transfer reactions. However, relatively low electrical conductivity and poor rate capability and cycle stability of pseudocapacitive materials limit their widespread commercial applications [9]. Therefore, carbon-based materials with high conductivity and distinct structures can be combined with pesudocapacitive materials to exhibit synergistic effects for supercapacitive performance, known as hybrid SCs.
\nCarbon material is EDLCs type for supercapacitor. In section 2.1, EDLCs has introduced their property, which store the electrical charge by electrostatic force at the electrode-electrolyte interface, as shown in Figure 2. It is not involving electrochemical reactions on the electrode surface. There are different types of carbon nanostructured materials, which can be used as single electrode materials due to their unique structural, mechanical, and electrical properties.
\nThey are round-shaped particles such as ultrafine activated carbon (AC), mesoporous carbon, carbon nanosphere, and carbon quantum dot, with a high specific area (AC: ⁓3000 m2 g−1) and an aspect ratio of nearly [10]. In addition, by tuning the pore size distribution and pore content, they can use as suitable supporting materials for composite electrodes.
\nThese are the high aspect ratio materials with fiber shaped and good electronic properties e.g. carbon nanotubes (CNT), carbon nanocoils, and carbon nanofibers (CNF), which facilitates the electrochemical reaction kinetics by 1-D charge transfer pathway.
\nThey are sheet like structures with high aspect ratio such as graphene, graphene oxide (GO) or reduced graphene oxide (rGO). In addition, they have high specific surface area, good mechanical strength, and excellent electrotonic conductivity, which helps them as promising electrode materials for SCs. For an example, single layered graphene has theoretical surface area of 2756 m2 g−1 and charge mobility of 200000 cm2 V−1 s−1 [11].
\nThese are the low dimensional building blocks such as carbon nanofoams or sponges with hierarchical porous channels, rich pore structures, higher electrical conductivity and better structural mechanical stability, which are extensively used in composite electrode materials for SCs. For an example, foam has high specific surface area with continuous electron transport path and large area of electrolyte-electrode interface.
\n\nTable 1 shows some examples of different carbon nanostructured materials such as carbon onions, carbon nanotubes, graphene, and templated carbon, which are used as electrode materials for EDLCs. Each carbon nanostructured materials have its advantages and disadvantages. For example, carbon onions have high power performance due to excellent conductivity with high accessible ion adsorption capacity but low capacitance of ⁓30 F g−1 [12]. On the other hand, CNTs have high energy density due to superior electrical properties and unique tubular structures for fast charge transportation but due to the high cost, their widespread applications are limited [13]. Recently, graphene has been attracted much attention as electrode materials for EDLC applications due to unique properties, like as ultrahigh specific surface area, unique conductivity, and exceptionally high mechanical strength [14]. However, the aggregation of sheets during electrode preparation limits the aspect of application. More recently, 3D porous carbon nanostructured materials are widely used for EDLCs because of rich pore structures and high surface areas but due to relative low conductivity and presence of micropores specific capacitance is insufficient at a high current density [15]. Therefore, it is necessary to construct composite materials by coupling the advantages of different types of carbon nanostructured materials and high energy electrode materials such as transition metal oxides, metal hydroxides and metal dichalcogenides (TMDs) to enhance the energy density without the compromise of power density and also meet the requirement for fabrication of high energy storage devices. In the composite electrode material, different types of carbon nanostructured materials not only contribute to high capacitance but also provide an easy conductive path for charge transportation due to conductive nature.
\nDifferent carbon nanostructures used as electrode materials for EDLCs with onion-like carbon, carbon nanotubes, graphene, activated carbon, carbide-derived carbon, and templated carbon [16].
Many metal oxide such as RuO2, MnO2, Fe3O4, V2O5, NiO, Co3O4, and TiO2, has been received significant attention and extensive studied as SC electrode materials due to Pseudo capacitance nature, which depends on the fast reversible redox reaction of electroactive species directly as well as in the vicinity of electrode surface [17, 18, 19, 20]. The redox behavior is due to the multivalent property of the above oxides which changes their oxidation states by interaction with protons or hydroxide ions reversibly. In spite of their excellent specific capacitance, they still suffer from low conductivity, low rate capability, poor stability and durability during the process of charge/discharge. In contrast carbon materials shows excellent performance in these regards but suffer from comparatively limited specific capacitance. Hence, the synergic integration of metal oxides with conducting carbon supports may form high potential carbon-metal oxide composite electrodes materials for SCs and hybrid devices because of their enhanced electrochemical performance through the combined effect of pseudocapacitive/faradaic charge storage and electrical double layer capacitance mechanisms [21, 22, 23].
\nAmong the metal oxides, ruthenium oxide (RuO2) has been considered as very common electrode materials for SCs in acidic medium due to their excellent pseudocapacity which is arising from high conductivity, good thermal stability, highly reversible redox reactions, three different oxidation states within 1.2 V, and high specific capacitance natures. The pseudocapacitance mechanism of RuO2 for SC electrodes can be described as equation [24]:
\nOr
\nHowever, its scarcity and high cost limits the fabrication of RuO2 based electrodes for potential applications. But, smartly use of composite materials by synergic integration of pseudocapacitive RuO2 materials with conductive carbonaceous substrates not only improves the capacitance but also reduces the cost of the electrode. Recent studies are more focus about the selecting the best carbonaceous substrate and the synthesis procedures to fabricate ruthenium oxide (RuO2)-coated on the porous carbonaceous substrates.
\nRuO2-CNT composite has been prepared by uniformly coating of RuO2 on the vertically aligned porous carbon nanotubes porous through atomic layer deposition (ALD) technique and further activation by voltammetry potential coulometry (Figure 3(a-c)) [25]. This ALD technique has many advantages such as deposition on large surface area, accurate thickness and exceptional uniformity for electrode designing in energy storage devises. The as-prepared RuO2-CNT composite shows excellent electrochemical performance as an electrode material for SC in respect of capacitance, power density and stability. Several publications have been reported the specific capacitance and power density of RuO2-CNT composite, which are around 650 F g−1 and 17 kW kg−1, respectively. Kaner
(a) Schematic presentation of RuOx deposited on the vertically aligned porous carbon nanotubes porous through ALD by sequential pulsing of Ru (EtCp)2 and oxygen. (b) and (c) SEM and TEM images of vertically aligned CNTs coated with ALD RuOx [
MnO2 has been considered as a promising pseudocapacitive electrode materials for energy storage applications due to low price, abundant reserve, high specific capacitance, and environmental environment benign nature and low toxicity in comparison to other transition-metal oxides. In general, the charge storage mechanism of MnO2 involves change in manganese oxidation state from +3 to +4 and the contribution of protons or alkali cations, which can be shown in the following equation [28].
\nWhere C+ represents protons or alkali cations (Li+, Na+, K+).
\nHowever, MnO2 based electrodes limits the capacity and power density due to their low surface area and poor electronic/ionic conductivity. Therefore, the composite of MnO2 with high-surface area and conducting carbonaceous materials may improve the electrochemical performance in terms of specific capacity, energy and power densities by providing the larger interfacial area between the MnO2 particles and the electrolyte solution [29].
\nGao
(a) Controlled growth of MnO2 nanostructured on CNT surface through facile redox method. (b) TEM images displaying coverage of MnO2 on the surface of CNT. (c) The cyclic curve of a MnO2-CNT nanowire composite at current density of 2 A g−1 [
Cobalt oxides has been received considerable attention as highly promising SC electrode materials due to their non-toxic, low cost, easy synthesis, environmentally friendly, and more importantly high theoretical capacitance (CoO: 4292 F g−1, Co3O4: 3560 F g−1) [35]. In addition, cobalt oxides exhibits outstanding electrochemical behaviour in alkaline as well as organic electrolyte, which is possible due to their ability to interact with the ions at the electrolyte surface as well as through the bulk of the material. The pseudocapacitance of cobalt oxides (CoO/Co3O4) are originates from the following redox reaction: [36]
\nCoO:
\nCo3O4:
\nHowever, the low electrical/ionic conductivity of cobalt oxides hinders their practical performance as SC electrodes. Most efficient way to improve their electrochemical performance is to form composites of cobalt oxides by incorporation into a carbon-based conducting supports. A Co3O4/AC composite SC electrode was reported by Iqbal
Recently, binary metal oxides such as NiCo2O4, NiFe2O4, CoFe2O4, ZnMnO4, and ZnCo2O4 have attracted much attention due to higher electrical conductivity than individual metal oxide and provide higher capacitance due to more affluent redox reaction than individual components [43]. Even though binary meal oxides possess better electrochemical performance than individual metal oxide extremely, they still suffer from inferior rate performance, low utilization rate and poor cycle stability. However, by incorporating carbon based materials improve their conductivity as well as power density due to high surface area, high conductivity and stable chemical properties of carbon based materials [44]. Kumar
Among the active materials, metal hydroxides have also been considered promising electrode materials for electrochemical SCs because of extremely high specific capacitance. Metal hydroxide in several forms such as Ni(OH)2, Co(OH)2, NiCo(OH)2, Cu(OH)2, FeOOH have been investigated as electrodes for SC [50, 51, 52]. These materials have large internal spaces for fast insertion and desertion of electrolyte ions. Moreover, these metal hydroxides can be synthesized using simple synthetic approaches. Metal hydroxide consists of stacked layers intercalated having interlayer space to occupy more ions hence larger capacitance.
\nNi(OH)2 is being considered as an attractive candidate as electrode in SCs because of its high theoretical capacitance (2358 F g−1). It can be prepared by a simple and low cost process. It has demonstrated good stability in alkaline electrolytes. Its low electrical conductivity is a barrier to achieve higher capacitance. Therefore, a thin region near the surface of nickel hydroxide contributes to the charge storage process due to diffusion-limited redox reactions. To obtain larger capacitance, it has to be utilized completely in the charge storage process. In this regard, researchers have generally adopted conductive additives to effectively improve utilization of active materials and result in larger capacitance. Kang
(a) A schematic of the growth process of 3D-Ni(OH)2/C/Cu, (b) Morphology of the as-synthesized 3D-Ni(OH)2/C/Cu electrode (inset: large-area uniform porous morphology of the 3D-Ni(OH)2/C/Cu), (c) Specific capacitance of 3DNi(OH)2/C and 3D-Ni(OH)2/C/Cu as a function of the current density based on the galvanostatic charge/discharge measurement [
Co(OH)2 has recently received increasing attention as electrode for SC application because of its low cost and high capacitance. Jagadale\n
Two possible reactions are suggested for the electrochemical reactions of Co(OH)2 in KOH electrolyte [57]:
\nCo(OH)2 nano-sheet-decorated graphene-CNT composite structure has been designed for SC application [58]. Suspensions method was used to prepare graphene-CNT composite by sonication and vacuum filtration. The graphene-CNT composite may offer high porosity with high conductivity, chemical stability and a three-dimensional structure. The vertically aligned Co(OH)2 nano-sheets were then deposited on 3D graphene-CNT composite by solution based process. The ASC of Co(OH)2 with graphene-CNT has shown a specific capacitance of 310 F g−1. The electrode exhibited an energy density of 172 W h kg−1 and maximum power density of 198 kW kg−1 in ionic liquid electrolyte 1-ethyl-3-methylimidazoliumbis(trifluoromethanesulfone)imide (EMI-TFSI). Zhang
FeOOH has been recognized is an attractive electrode material for SC due to low cost, high theoretical specific capacitance, and broad potential window. In addition, the unique tunnel structure of FeOOH with open permeable channels are beneficial for ion transportation and shorten the diffusion path for electrolyte ion diffusion [60]. However, the poor electrical conductivity and low specific surface area limited the use of FeOOH as a potential electrode for SC, which limited specific capacitance and rate capability [61]. Alternatively, composite system by assembling FeOOH on the carbon based supporting materials (AC, carbon black, graphene, etc.) can be enhance the capacitive performance. Shen
(a) Schematic illustrations of the fabrication procedure for the FeOOH//APDC f-SSC electrodes and flexibility and operating status as supercapacitor device, (b) The areal capacitance as a function of the discharge current density (Inset: SEM images of as-prepared γ-FeOOH nanosheets on a carbon cloth substrate), (c) CV curves of the FeOOH//APDC f-SSC at bent and flat statuses [
TMDs are layered inorganic materials with a chemical configuration of MX2, in which M is a transition metal element (M: Ti, Mo, V, W, Re, Ta), and X can be any chalcogenide element (X: S, Se, Te) (Figure 7(a)). Each MX2 unit cell is stacked together through Vander Waals force in such a way that transition metal layer is present in between the two chalcogen sheets [67]. On the basis of crystal structure, there are two types of phases of TMDs, which are metallic 1T phase with an octahedral structure and semiconducting 2H phase with a trigonal structure. Recently, TMDs have been attracted great attention as SC electrode materials due to their large surface area, low cost, variable oxidation states, high mechanical properties, high chemical stability and easy synthesis [68]. The variable oxidation states, large surface area, and active edges of TMDs allow electrical double layer and fast/reversible redox charge storage mechanisms and offer high energy storage capability in SCs. However, due to the inherently low conductivity, poor cycle life, large volume change during cycling and restacking limits their electrochemical performance as SC electrodes [69]. For example, Soon
(a) Different metal coordination and stacking sequence in TMD unit cells [
MoS2/MWCNT nanocomposite synthesized by a hydrothermal method exhibited a large surface area and fast ionic transport properties and showed a high specific capacitance of 452.7 F g−1 with good cycling stability (95.8% retention after 1000 cycles), which is almost three times larger than the bare MoS2 (149.6 to 452.7 F g−1) [71]. Ali
WS2 nanoplates supported on carbon fiber cloth (WS2/CFC) have been synthesized by a facile solvothermal process and used as electrode material for SC [77]. The 3D network of CFC not only prevent the agglomeration of WS2 nanoplates but also enhances the ion transport efficiency due to low charge transfer resistance (Rct) of 0.1 Ω. The as fabricated WS2/CFC electrode exhibited a high specific capacitance of 399 F g−1 at 1 A g−1 current density with cyclic retention of 99% over charge-discharge 500 cycles, which is higher than compared with bare WS2. In addition, developing such composite of WS2 with the carbon fibre helps for fabricating wearable SCs which are in demand for wearable electronics. Yang
(a) Schematic illustration of synthetic processes of WS2/N,S-rGO hybrid, (b) HRTEM, STEM and EDS elemental mapping images of WS2/N,S-rGO hybrid, and (c) The specific capacitances of the WS2, N,S-rGO and WS2/N,S-rGO hybrid at different current densities [
In the past few decades, SCs have been extensively studied as energy storage devices and more focusing area in the multidisciplinary science over the world. The selection of high performance SC electrode materials based on high specific capacitance, low internal resistance and good stability. In this article, we have reviewed the carbon-based composite materials (
This work was supported by the Ministry of Science and Technology (MOST) of Taiwan, under grant numbers 107-2113-M-845-001-MY3.
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