Classification of ferrites according to variation in molar ratio of Fe2O3 to modifier oxide.
\r\n\tThe fundamental research areas of Evolutionary Psychology can be divided into two broad categories: on the one hand, the basic cognitive processes, and the way they evolved within the species, and on the other, the adaptive social behaviors that derive from the theory of evolution itself: survival, mating, parenting, family and kinship, interactions with non-parents and cultural evolution. Indeed, Evolutionary Psychology explains at individual and group level the fundamental behaviors of social life, such as altruism, cooperation, competition, social exclusion, social support, etc. etc. Similar to the mechanisms of natural selection for physical characteristics, not only the mind follows biological laws, but also psychological abilities - such as the theory of mind, the ability to represent the intentions, thoughts, beliefs, and emotions of others - have had to adapt and must make themselves functional to the social life of individuals and groups. In addition, Sociology takes the same aspects into consideration, emphasizing the interaction, symbolic and otherwise, of individuals. The latter investigates the neural mechanisms underlying the same social behaviors that are of interest to evolutionary psychology. To study the neural correlates involved in such behaviors is necessary to understand the biological laws that underlie human behavior and brain functioning.
\r\n\r\n\tThis book aims to open a debate full of theoretical and experimental contributions among the different disciplines in social research, psychology, neuroscience, sociology, useful to give an innovative vision to the present research and future perspective on the topic.
",isbn:"978-1-83968-871-3",printIsbn:"978-1-83968-870-6",pdfIsbn:"978-1-83968-872-0",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!0,hash:"bd4df54e3fb185306ec3899db7044efb",bookSignature:"Dr. Rosalba Morese, Dr. Vincenzo Auriemma and Dr. Sara Palermo",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10450.jpg",keywords:"Evolutionary Psychology, Human Social Evolution, Human Social Behaviour, Social Cognition, Social Neuroscience, Functional Neuroimaging, Neuropsychology, Altruism, Cooperation, Social Exclusion, Social Support, Social Inclusion",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 18th 2020",dateEndSecondStepPublish:"December 21st 2020",dateEndThirdStepPublish:"February 24th 2021",dateEndFourthStepPublish:"May 15th 2021",dateEndFifthStepPublish:"July 14th 2021",remainingDaysToSecondStep:"a month",secondStepPassed:!0,currentStepOfPublishingProcess:3,editedByType:null,kuFlag:!1,biosketch:"Dr. Rosalba Morese is carrying out research in the framework of Neuroscience and Social Psychology. She currently works at the Institute of Public Health of Faculty of Biomedical Sciences and at the Faculty of Communication, Culture, and Society of Università Della Svizzera Italiana, Lugano, Switzerland.",coeditorOneBiosketch:"Dr. Vincenzo Auriemma's focus is on the study of empathy in human interactions. He studied at the University of Essex in England, the University of Pisa, Genoa, Rome in Italy, and the University of Italian Switzerland in Switzerland. He is the principal responsible for the 'PERSEO' research which analyzes the reasons for the 'drop-out' in psychology.",coeditorTwoBiosketch:"Researcher of the EUROPEAN INNOVATION PARTNERSHIP on Active and Healthy Ageing and Assistant Specialty Chief Editor for Frontiers in Psychology - Neuropsychology.",coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"214435",title:"Dr.",name:"Rosalba",middleName:null,surname:"Morese",slug:"rosalba-morese",fullName:"Rosalba Morese",profilePictureURL:"https://mts.intechopen.com/storage/users/214435/images/system/214435.jpg",biography:"Rosalba Morese obtained a degree in psychology at the University of Parma. She subsequently held various\nteaching positions at the Department of Psychology and the Faculty of Medicine and Surgery of the\nUniversity of Parma.\nHer training continued with the attainment of the title of PhD in Neuroscience at the University of Turin,\nduring which she acquired and developed interdisciplinary skills and point of view through the application\nof bioimaging and psychophysiological methods to investigate the neurophysiological mechanisms involved\nduring communication and social interactions.",institutionString:"Universita della Svizzera Italiana",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"6",totalChapterViews:"0",totalEditedBooks:"3",institution:{name:"Universita della Svizzera Italiana",institutionURL:null,country:{name:"Switzerland"}}}],coeditorOne:{id:"338363",title:"Dr.",name:"Vincenzo",middleName:null,surname:"Auriemma",slug:"vincenzo-auriemma",fullName:"Vincenzo Auriemma",profilePictureURL:"https://mts.intechopen.com/storage/users/no_image.jpg",biography:'He is pursuing a PhD in Sociology from the University of Salerno, Italy. He is a researcher of sociology and neurosociology at the University of Salerno, Italy. His focus is on the study of empathy in human interactions and he studied at the University of Essex in England, the University of Pisa, Genoa, Rome 3 in Italy and the University of Italian Switzerland in Switzerland. He has participated in national and international conferences with about 25 reports/communications. He is the principal responsible for the "PERSEO" research which analyzes the reasons for the "drop-out" in psychology, using the methodology of the Gounded Theory and analyzing empathy, fear and panic. He is Co-Editor for Frontiers. He is also a member of the Italian Society of Sociology (AIS).',institutionString:"University of Salerno",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"University of Salerno",institutionURL:null,country:{name:"Italy"}}},coeditorTwo:{id:"233998",title:"Dr.",name:"Sara",middleName:null,surname:"Palermo",slug:"sara-palermo",fullName:"Sara Palermo",profilePictureURL:"https://mts.intechopen.com/storage/users/233998/images/system/233998.jpeg",biography:"Sara Palermo is a MSc in Clinical Psychology and a PhD in Experimental Neuroscience. Moreover, she obtained the National Scientific Enabling Certificate for Associate Professorship in April 2017 (ASN-2017). She is an expert in experimental neuroscience, clinical neuropsychology and advance neuropsychological testing. Moreover, she performs multidimensional geriatric evaluation and basic neurological symptomatology detection in patients with neurodegenerative disorders. She is also engaged in Activation Likelihood Estimation meta-analysis of neuroimaging studies.\r\nShe worked as a postdoc research fellow at the Department of Neuroscience 'Rita Levi Montalcini” in Turin until July 2017. Since then she works as research fellow at the Department of Psychology in Turin. To date, she owns three research Group memberships at the University of Turin (Italy). She is a member of the 'Center for the Study of Movement Disorders” (research area: Neurology) and the 'Placebo Responses Mapping Group” (research area: Physiology) at the Department of Neuroscience, and a member of the 'Neuropsychology of cognitive impairment and central nervous system degenerative diseases Group” at the Department of Psychology (Research Area: Psychobiology and physiological psychology).\r\nThe main topics of her research are the study of awareness of illness, metacognitive-executive deficits in neuropsychiatric and neurological disorders, physical and cognitive frailty in the elderly, and placebo/nocebo phenomena. Interestingly, all of them may represent appealing perspectives from which to study how neuropsychological abnormalities can be explained in terms of brain activities and with the use of neuropsychiatric and neuropsychological batteries considering a neurocognitive approach. Given her research interests and scientific publications, she has been an ordinary member of the Italian Society of Neuropsychology (SINP), of the Italian Association of Psychogeriatrics (AIP), of the Italian Society of Neurology for Dementia (SiNdem), and – finally – of the international Society for Interdisciplinary Placebo Studies (SIPS). Importantly, she is a member of the European Innovation Partnership on Active and Healthy Aging (EIP on AHA), for which she is involved in the Action Group A3 Functional decline and frailty. \r\n\r\nSara Palermo is Panel Editor for 'EC Psychology and Psychiatry'. She was recently appointed as Specialty Chief Editor for 'Frontiers in Psychology - Neuropsychology'.",institutionString:"University of Turin",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"4",totalChapterViews:"0",totalEditedBooks:"3",institution:{name:"University of Turin",institutionURL:null,country:{name:"Italy"}}},coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"21",title:"Psychology",slug:"psychology"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"259492",firstName:"Sara",lastName:"Gojević-Zrnić",middleName:null,title:"Mrs.",imageUrl:"https://mts.intechopen.com/storage/users/259492/images/7469_n.png",email:"sara.p@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"5810",title:"Socialization",subtitle:"A Multidimensional Perspective",isOpenForSubmission:!1,hash:"bfac2e9c0ec2963193e9d15d617c6a01",slug:"socialization-a-multidimensional-perspective",bookSignature:"Rosalba Morese, Sara Palermo and Juri Nervo",coverURL:"https://cdn.intechopen.com/books/images_new/5810.jpg",editedByType:"Edited by",editors:[{id:"214435",title:"Dr.",name:"Rosalba",surname:"Morese",slug:"rosalba-morese",fullName:"Rosalba Morese"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"7818",title:"Social Isolation",subtitle:"An Interdisciplinary View",isOpenForSubmission:!1,hash:"db3b513d7d35476f333a0d4a3147935b",slug:"social-isolation-an-interdisciplinary-view",bookSignature:"Rosalba Morese, Sara Palermo and Raffaella Fiorella",coverURL:"https://cdn.intechopen.com/books/images_new/7818.jpg",editedByType:"Edited by",editors:[{id:"214435",title:"Dr.",name:"Rosalba",surname:"Morese",slug:"rosalba-morese",fullName:"Rosalba Morese"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"8262",title:"The New Forms of Social Exclusion",subtitle:null,isOpenForSubmission:!1,hash:"29bf235aa7659d3651183fe9ea49dc0d",slug:"the-new-forms-of-social-exclusion",bookSignature:"Rosalba Morese and Sara Palermo",coverURL:"https://cdn.intechopen.com/books/images_new/8262.jpg",editedByType:"Edited by",editors:[{id:"214435",title:"Dr.",name:"Rosalba",surname:"Morese",slug:"rosalba-morese",fullName:"Rosalba Morese"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"6494",title:"Behavior Analysis",subtitle:null,isOpenForSubmission:!1,hash:"72a81a7163705b2765f9eb0b21dec70e",slug:"behavior-analysis",bookSignature:"Huei-Tse Hou and Carolyn S. 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Since the introduction of controlled sintering process of ceramic, the methodology has gained rapid growth and well established as one of the most trustable synthesis method for the production of complex ceramic oxides with desired properties [1]. Sintering is categorized as bottom-up approach synthesis as it involves the construction of nanostructures in materials atom-by-atom, layer-by-layer, from small to large sizes [2]. Since twentieth century, energy efficiency and productivity are two important factors in choosing a particular methodology [3]; therefore, top-down approach synthesis method like mechanochemistry has emerged as one of the most promising candidates to replace known current methodologies like sintering, questioning the necessity for thermal treatment at high temperatures. However, there are advantages of sintering that are irreplaceable by other methodologies. Sintering offers matter transport through diffusion while maintaining the stoichiometry of the ceramic material. Commonly, a single phase ceramic oxide with low porosity can be achieved by sintering of the material to a range of 50–80% of its melting point [1]. With an appropriate sintering temperature, the material does not melt, while atomic diffusion can be activated to achieve a dense, compact, and high crystallinity material, which is essential for the fabrication process. Although the optimization of sintering parameters to achieve complete phases of complex ceramic oxides is crucial; however, the fundamental knowledge behind sintering: the correlation between microstructural properties induced by the thermal activation of sintering, with important behaviors like magnetic and optical properties, is important for the understanding of sintering mechanism.
\nMicrostructure of complex magnetic ceramic oxides consists of grains, grain boundaries, porosity, and defects structures. As complex as it is microstructural properties influence the behaviors of these complex ceramic oxides. For instance, microstructural properties like surface morphology, atomic arrangement, size and shape affect major macroscopic properties such as magnetic, optical, mechanical, electrical, and many other properties of complex ceramic oxides. These are known as the microstructural dependent behaviors of complex ceramic oxides. Nanomaterials exhibit unique behaviors compared to their bulk counterparts [4].
\nThere are some important behaviors related to magnetic ceramic oxides, which are size dependent. For instance, magnetic properties and particle, grain, or crystallite size are relevant to each other. When the particles are in nano-size, the percentage of amorphous grain boundary volumes in material is high compared to particles in micron size. The presence of large volume fraction of amorphous phase in the material hinders the exchange interaction between magnetic moments. Therefore, small particles are likely to exhibit weak ferromagnetic, superparamagnetic, and paramagnetic behaviors. Small size polycrystalline nickel zinc ferrite dissipates minimum energy [5]. The magnetocrystalline anisotropy energy, EA for ferrite can be defined by the following equation:
\nwhere K is the anisotropy constant, V is the volume of the crystal, and Ө is the angle between the easy axis and the direction of the field-induced magnetic field. When the grains are small in dimensions or below a critical size, they dissipate minimum energy, therefore, the energy required to create a new domain or shifting the domains is much higher than that required in maintaining the material as single domain. The effect of grain size changed some aspects of magnetic behavior of yttrium iron garnets [6]. Below a critical size, as the volume or size of the grains increases, grain size remains in the single-domain range, therefore, the EA value increases, the magnetocrystalline anisotropy energy becomes stronger and the coercivity (the energy required to change the direction of the magnetization) increases. After the grain size exceeds the critical size, intergranular domain walls are formed inside the grains, because the energy is not sufficient to maintain relatively big grains as single domains. Therefore, domain walls are created to reduce the overall energy of the system. Grain size has similar impact on the magnetic properties of hard ferrite, BaFe12O19, which has a critical size as well. Studies defined the critical size as the minimum grain volume that the anisotropy energy is able to overcome thermal agitation [7].
\nAnother important magnetic behavior is the measure or ability of a material to sustain a magnetic field within the material when external field applied. This is known as the magnetic permeability. Magnetic permeability is strongly influenced by the presence of grain boundaries or amorphous surfaces, as they will act as impediments to domain wall movement. Bulk materials have fewer grain boundaries, therefore, higher the permeability. This phenomenon especially noticeable in ferrites as their grain boundaries are thicker [4]. The effect of sintering soaking time on the microstructural properties of nickel zinc ferrite was investigated [8, 9]. Grain size increases with increasing soaking time. The increase of grain size is the main factor that causes the increase of initial permeability. Bulk materials have a low-volume fraction of grain boundary as shown in Figure 1. Volume fraction can be represented by:
\nSchematic representation of bulk and nanoparticles, and the definition of R, radius of a particle, and r, radius of the core of a particle.
where \n
Porosity is another microstructural feature that has the pinning effect on the movement of the domain walls. Porosity is abundant in complex magnetic ceramic oxide because it cannot be eliminated by heat treatment. Heat treatment offers grain growth, densification, and boundaries expansion. However, many pores are swept over by grain boundaries and remain within large grain [4]. Porosity and grain size effects sometimes seem inseparable because grain growth and densification happen simultaneously. In case of magnetic properties, saturation magnetization is associated with the following equation [10]:
\nwhere p is the porosity, Mo is the magnetization extrapolated to zero porosity. Therefore, we can conclude that saturation magnetization is porosity dependent while coercivity is size dependent. Previous study proved that the independence of coercivity from porosity, while saturation magnetization and remanence are independent from grain size effect [10]. In addition to porosity, other defects such as cracks, inclusions, foreign phases, strains, as well as dislocations would alter the magnetic behaviors of ferrites. Defects act as energy wells have a strong pinning effect on the domain wall motion and thus require higher activation energy to detach [4].
\nIt is believed that boundary region possesses higher energy compared to volume defects. Therefore, boundary region is a highly reactive region, which allows nucleation of new phases. As nanostructured materials have higher surface-to-volume ratio, they are reactive compared to their corresponding bulk materials. In ceramic materials, boundary region between phases and grains governs many properties and processes, for example, as fracture strength, plastic deformation, conductivity, dielectric loss, and phase transformation. All materials have interfacial energy and tension that can be calculated by same thermodynamic formulation [11]. Boundaries act as sinks and sources for the formation of lattice imperfections, diffusion, and phase transformations when deformation occurs. Some behaviors of ceramic oxides such as coercivity and permeability are strongly related to their boundaries [12]. The direction of magnetic moments within the material could be changed easily when the pinning effects of the boundary regions is diminished. Apparent permeability can be expressed as following [13]:
\nwhere p is the porosity, D is the average grain size, t is the effective thickness of boundary region, μb is the permeability of the boundary region, μo is the permeability free form the demagnetizing field. From the equation, notice that the thickness of boundary region has strong influence on the control of the magnetic properties of ferrites because the thickness of the boundary regions can be altered simply by small amount of additives, impurities, or phase transformations.
\nAttention has been paid to investigate synthesis techniques and their impacts on new materials, particularly nanostructured and nanocrystalline materials. Synthesis technique is strongly related to behaviors of the investigated nanomaterial because the chosen synthesis technique is responsible for tailoring the atomic and microstructure of the nanostructured material. Numerous published studies have improved our understanding of the effects of synthesis technique on the behaviors of complex magnetic ceramic oxide, especially technologically important hard and soft ferrites [5, 14, 15, 16]. Most of the significant findings show that the results are of limited significance unless the microstructures, chemical composition, defects, and atomic arrangement of the investigated ferrite are well-characterized. Generally speaking, the techniques of preparing ferrite are categorized into two: bottom-up and top-down approaches, as shown in Figure 2. Bottom-up approach synthesis is a ceramic powder processing approach that engages atoms, ions, molecules or particles as starting building blocks. By combining or assembling these building blocks, nanoscale clusters, or corresponding bulk materials are formed. Top-down approach synthesis is a ceramic powder processing approach that begins with micro-structured materials. The approach utilizes mechanical, chemical, or other form of energy to perform structural decomposition to obtain nanoscale materials. Both approaches have its advantages and drawback. For instance, bottom-up approach synthesis such as chemical processes and solid-state routes are capable of producing fine nanocrystalline materials with high purity and homogeneity. However, they have disadvantages like not environmental friendly, high cost of chemical precursors, solvent evaporation, and necessity for thermal treatment at high temperature. On the other hand, top-down approach synthesis like mechanochemical process is considered as green process because it minimizes damage to the environment, fast, economical, and can effectively take nanostructure forms [2]. However, contaminations, defects, and damages that were induced into the material system need to carefully take into account for good material production [15].
\nSchematic representations of (a) bottom-up and (b) top-down approaches.
Ferrites belong to a class of complex magnetic ceramic oxide. The crystal structure of ferrites can be observed as an interlocking network of cations and negatively charged divalent oxygen ions [4]. When a layer of oxygen ions is closely packed lines that connect the centers of these oxygen ions will form a network of equilateral triangles. The second layer of closely packed oxygen ions is arranged in such a way that the centers of these oxygen ions are superimposed with the centers of the equilateral triangles of the first layer. If a similar third layer repeats the same arrangement with the first layer, this arrangement is known as hexagonal close-packed structure in the type of “ababab” stacking sequence. On the other hand, if the third layer arranges in such a way that the centers of the oxygen lie directly over the centers of equilateral triangles adjacent to the ones used for hexagonal close-packed, this will produce a cubic close-packed with a stacking sequence of “abcabc.” Then, ferrites are further categorized according to their molar ratio of Fe2O3 to other oxide components (modifier oxide) present in the ceramic as presented in Table 1.
\nType | \nStructure | \nMolar ratio of Fe2O3 to modifier oxide | \nModifier oxide | \nExample | \n
---|---|---|---|---|
Magnetoplumbite | \nHexagonal | \n6:1 | \nGroup IIA divalent metal oxide. Example: BaO, SrO | \nBaFe12O19 | \n
Spinel | \nCubic | \n1:1 | \nTransition metal oxide. Example: NiO, ZnO | \nNi0.5Zn0.5Fe2O4 | \n
Garnet | \nCubic | \n3:5 | \nRare earth oxide | \nY3Fe3(FeO4)3 | \n
Classification of ferrites according to variation in molar ratio of Fe2O3 to modifier oxide.
Top-down and bottom-up approaches have their own advantages and drawback as mentioned in the previous section. Conventional solid-state process is a bottom-up approach ceramic processing method that involves neither wet chemical reactions nor vapor phase interactions. There are two important processing steps that will affect the quality of the end product: starting powder preparation and heat treatment. The solid-state process is considered as the simplest synthesis route for various ferrites. In the starting powder preparation stage, high-purity raw materials would mix together according to the stoichiometric balance of the final product. This mixing process is being carried out by either dry or wet milling media for a certain period to produce a homogenous distributed starting powder. Then, the starting powder will undergo a heat treatment, typically with the use of a furnace to obtain the final product.
\nThe conventional solid-state process is capable of producing advanced material with unique compositions such as refractory ceramics, glasses, and crystals. Previous research showed that conventional solid-state process was capable of producing particles between 100 nm and 1 micron [16]. However, conventional solid-state process may result in high synthesis temperature because diffusion reaction is limited under low temperature. Besides, this process may produce an incomplete reaction, which results in inhomogeneous products. Other issues of using this process are lack of control of the kinetics and the difficulties of producing desired end products [17]. In order to overcome the drawback of conventional solid-state process, the implementation of mechanical alloying in the starting powder preparation is recommended by many researchers. Apart from the practicality, mechanically activated starting powders exhibit nanostructures and high reactivity. Therefore, it provides an easy, fast, and economical option to produce the desired material. Previous studies showed that starting powder synthesized via mechanical alloying, had a relatively low sintering temperature for the formation of pure, single phase material [5, 7, 18, 19].
\nX-ray Diffraction (XRD) spectra of Ni0.5Zn0.5Fe2O4 after sintering from 600 to 1200°C are presented in Figure 3. In view of the results obtained, the occurrence of [121] peak in 600°C spectrum indicated incomplete reaction between raw materials to form a single phase powder. α-Fe2O3 existed as secondary phase at 600°C. The [121] peak shows the existence of secondary phase α-Fe2O3 in the Ni0.5Zn0.5Fe2O4 phase. The α-Fe2O3 phase disappeared when the sintering temperature was increased to 700°C. A complete Ni0.5Zn0.5Fe2O4 was formed as Zn2+ ions diffused into the tetrahedral sites while Ni2+ ions occupied the octahedral sites. As the starting powders were mechanically activated by high-energy ball milling by SPEX is the modal name of the dual mixer machine. Which was specially modified to achieve high speeds (approximately 1725 rpm) for the effective production of nanostructured particles; this enables the formation of single phase at a lower sintering temperature. It is worth mentioning that the synthesis temperature for single phase Ni-Zn ferrite for refluxing method is between 950 and 1150°C [20]; sol–gel technique requires more than 1000°C [21]; co-precipitation method requires 550–1000°C [22]. The intensity of the Bragg peaks increased, and the peak widths decreased with increasing sintering temperature indicating the increase of crystallinity and particle size.
\nX-ray diffraction patterns of Ni0.5Zn0.5Fe2O4 sintered from 600 to 1200°C.
Structural information was obtained from Rietveld refinement. The increase of lattice parameters and unit cell volume was observed. As shown in Figure 4, as the sintering temperature increased, the unit cell volume expanded, and Zn2+ ions diffused into the interstitial sites; this was crucial for the reaction as interstitial diffusion is the most important lattice diffusion mechanism [1]. Further increasing of sintering temperature (>900°C), a decrease in lattice parameters and unit cell volume was observed. This could be due to the small amount of Zn2+ ions evaporated from the lattice [8]. This is because zinc has a low-boiling point of 907°C. Mechanically activated starting material has high lattice strain as defects and inhomogeneity could be introduced into the system. This is known as the second order stress, which it modifies the materials by one grain to another or from one part of the grain to another on a microscopic scale. There was also first order stress induced by milling. This type of stress modifies the material uniformly across the entire material [23], causing a macroscopic variation on the material. By increasing the sintering temperature, relaxation can be attained for macro and micro stresses induced during milling.
\nUnit cell volume and lattice strain as a function of sintering temperature.
Figure 5 shows the evolution of particle size, crystallite size, and morphological properties of Ni0.5Zn0.5Fe2O4 with elevating sintering temperature. As a whole, bottom-up synthesis of soft ferrite, Ni0.5Zn0.5Fe2O4 acquires three stages of sintering. Initial stage of sintering can be observed for samples sintered at 600-, 700-, and 800°C. Phenomena such as rearrangement of particles and necking structure can be observed at this stage. At the intermediate stage (900-, 1000-, and 1100°C), further increase of sintering provides sufficient thermal energy for nanoparticles to move closer. Grain boundaries are formed. However, the most significant observation for intermediate stage is the formation of interconnected pores. Finally, the sample sintered at 1200°C exhibited the final stage of sintering. Isolated pores are observed, and rigid crystal structure is visible. The coarsening and densification of particles are observed with increasing sintering temperature.
\nAverage particle size and crystallite size as a function of sintering temperature; the evolution of morphology is shown in the inserted field emission scanning electron microscope (FESEM) micrographs.
The activation energy of particle growth of sintering is strongly related to the size evolution of the particles [24]. Size-dependent activation energy can be represented by the plot of log particle size (D) versus the reciprocal of absolute temperature (1/T) of Ni0.5Zn0.5Fe2O4 [25]. Three distinct stages of sintering can be observed in Figure 6. Activation energy is the lowest at initial stage, indicating the particles are nano-sized, which exhibit relatively largest surface area. Small thermal energy is enough to initiate the particle growth. Through intermediate and final stages, particle size increases, therefore, the activation energy for particle growth increases hence higher thermal energy is required for the densification and coarsening mechanisms in sintering [26]. As a summary during initial stage, particles rearranged themselves so that they are in tangential contact. This is to activate the material transport mechanism through diffusion. During this process, necking structures are formed between particles. At intermediate stage, densification occurs and the pores shrink to reduce their cross-section. As a result, interconnected pores are formed at the boundary regions. Densification and coarsening continue to occur; eventually, the pores become unstable and isolated at the final stage of sintering [1].
\nPlot of log D versus the reciprocal of absolute temperature (1/T) of Ni0.5Zn0.5Fe2O4 showing three stages of sintering.
High resolution transmission electron microscopy (HRTEM) is utilized to identify some unique features of each stage in terms of atomic arrangement, structural information, and defects like grain boundaries. In Figure 7a, a lattice spacing of 2.53 Å was measured for Ni0.5Zn0.5Fe2O4, corresponding to (113) lattice plane. A few particles rearrange themselves in such a way that they are in tangential contact. The contact points between particles are the material transport paths that allow diffusions to occur at early stage of sintering. In Figure 7b, it can be seen that the spheres begin to coalesce. The radius of the necking structure has reached a value of >0.50 of the particle radius. This indicated that at sintering temperature of 800°C, the particles are near the end of an initial stage of sintering [1].
\nHigh resolution transmission electron microscopy (TEM) images for Ni0.5Zn0.5Fe2O4 nanoparticles sintered at (a) 600°C, and (b) 800°C (initial stage of sintering).
In Figure 8a, it can be observed that two particles were brought together, and they are undergoing deformation in response to surface energy reduction. Massive lattice diffusion and material transport occur between these particles. In Figure 8b, grains adopt the shape of polyhedron with multiple faces, and the edge of the particle appears to have a clean crystalline surface, where amorphous phase diminishes at 1100°C. In the final stage of sintering (Figure 8c), a homogeneous atomic arrangement, with (113) lattice plane is formed.
\nHigh resolution TEM images for Ni0.5Zn0.5Fe2O4 nanoparticles sintered at (a) 900°C, (b) 1100°C (intermediate stage of sintering), and (c) 1200°C (final stage of sintering).
Figure 9a shows the M-H hysteresis loops of Ni0.5Zn0.5Fe2O4 sintered at various temperatures. The magnetic parameters are extracted from hysteresis loops. All the samples sintered from 600 to 1200°C exhibited less slanting, narrow sigmoid hysteresis loop. This indicates that the preparation of raw powder with modified high-speed mechanical alloying increases the reactivity of nanoparticles. Ferromagnetic phase exists in the sample even at low sintering temperatures such as 600 and 700°C. Figure 9b shows the plot of maximum magnetization at 10 kOe, M10kOe against sintering temperature. In view of the results obtained, the M10kOe values increase with increasing sintering temperature. At low sintering temperature, small particles exhibit surface distortion due to the interaction of transition metal ions in the lattice with oxygen atoms, causing a reduction in the resultant magnetic moment. This phenomenon is normally predominant in ultrafine particles because of their large surface to volume ratio. This effect becomes less influential at high sintering temperature as particle size increases. Volume fraction of amorphous phase decreases with increasing sintering temperature. Thus, the exchange interaction between particles increases with increasing volume fraction of crystalline phase. As a result, strong ferromagnetic behaviors are strengthened with erect, narrow, and well-defined sigmoid hysteresis loops are observed with increasing temperature. Coercivity has an indirect relationship with particle size. At low sintering temperature, there are amorphous phase and defects like grain boundaries in the sample. Therefore, the magnetocrystalline anisotropy is low because the crystalline volume fraction is low. Below a critical size (Dc ≈ 90 nm), coercivity increases with average particle size. As the sintering temperature increases, the crystalline volume fraction increases, the magnetocrystalline anisotropy is enhanced. To change the orientation of magnetic moment, higher energy is required to overcome this magnetocrystalline anisotropy energy. Therefore, below Dc, coercivity increases with increasing average particle size. Above this Dc, high magnetocrystalline anisotropy is not favorable in terms of energy level [27]. In order to reduce the overall energy of the system, domain walls are created causing the coercivity to decrease.
\nMagnetic parameters of bottom-up synthesis Ni0.5Zn0.5Fe2O4: (a) hysteresis loops at different sintering temperature, (b) plot of M10kOe versus sintering temperature, (c) plot of coercivity versus sintering temperature.
In Figure 10, a red shift of optical property is observed with increasing sintering temperature. It can be seen that the increase of crystallite is accompanied with the decrease of optical bandgap values (red-shift). This is thought to be due to size-dependent quantum confinement effect. Quantum confinement effect can be observed when the crystallite size is in the same order as the wavelength of the electron. The energy level at the microscopic level can be described by the expression [28]:
\nOptical properties of Ni0.5Zn0.5Fe2O4 nanoparticles sintered at different sintering temperature.
where h is the Planck constant, k is the wave factor (k = 2π/λ), m is the mass of electron. When the crystallite size is small, the wave vector k can be expressed as [28]:
\nwhere a is the crystallite size of the material and n is an integer. Based on Eqs. 5 and 6, the value of wave vector k has an inversely proportional relationship with the crystallite size. The crystallite size increased with increasing sintering temperature resulting in decrease of wave vector k value. When we substitute n = 1, 2, 3, and so on, for Eqs. 5 and 6, the difference between two consecutive energy becomes smaller. Therefore, energy bandgap values decrease with increasing crystallite size. This phenomenon happens when the motion of electrons is restricted in a nano-scale size.
\nSample with similar particle size, synthesized via mechanochemical process with optimized parameters [29] is chosen as a candidate for this comparative study with two parameters were chosen, which were milling at 8 hours (top-down approach) and sintering synthesis at 900°C (bottom-up approach). Figure 11 shows the XRD diffraction patterns milled at 8 hours and sintered at 900°C Ni0.5Zn0.5Fe2O4 nanoparticles. Nanoparticles that milled 8 hours exhibit a superimposition of broad diffraction reflections on the broad diffraction maximum or “hump,” indicating the presence of a highly disordered phase. Nanoparticles that sintered at 900°C exhibit a single phase pattern with sharp Braggs peaks.
\nX-ray diffraction patterns of Ni0.5Zn0.5Fe2O4 nanoparticles synthesized by different synthesis approaches.
Figure 12. shows the field emission scanning electron microscope (FESEM) micrographs and particle size distribution for nanoparticles synthesized by different synthesis approaches. As can be seen, nanoparticles that sintered at 900°C have a narrower size distribution compared to nanoparticles that milled at 8 hours. Commercial nanoparticles are uniform in size. Densification mechanism of sintering can be seen in Figure 12b. Small and large particles coexisted for both bottom-up and top-down approaches synthesized nanoparticles. However, particles with rigid and clear grain boundaries can be observed in sintered particles while top-down approach synthesized particles are agglomerated particles with randomly shaped boundaries.
\nFESEM micrographs and particle size distribution for (a) milled at 8 hours and (b) sintered at 900°C.
Figure 13 shows the M-H hysteresis loops of Ni0.5Zn0.5Fe2O4 nanoparticles synthesized via different synthesis approaches. Nanoparticles that milled at 8 hours exhibited complex disordering in structure. Therefore, it possesses canted spin arrangement that has significant implications on its magnetism. The maximum magnetization at 10 kOe is lower compared to nanoparticles that sintered at 900°C. On the other hand, nanoparticles that sintered at 900°C exhibited low coercivity with high saturation magnetization (the magnetization at 10 kOe had saturated). This indicated that the formation of single phase nickel zinc ferrite that exhibits soft ferrite magnetic properties. The optical bandgap values were 1.39–1.30 eV for sintered at 900°C and milled at 8 hours nanoparticles, respectively. Both bottom-up and top-down approaches synthesized nanoparticles exhibit same order optical bandgap value. It is evident that optical bandgap is a size-dependent behavior. However, defects that induced during mechanochemical process reduced the optical bandgap value of nanoparticles that milled at 8 hours. This is attributed to structural disorder bandgap narrowing effect.
\nM-H hysteresis loops of Ni0.5Zn0.5Fe2O4 nanoparticles synthesized by different synthesis approaches.
As most common approach for the fabrication of ceramic material, sintering shows some irreplaceable advantages. Sintering provides control on processing variables like sintering temperature, to achieve required microstructure for a particular set of properties. The synthesis temperature for single homogeneous phase can be lowered by mechanically activates the starting materials. Three stages of sintering mechanism can be observed in the experimental data of Ni-Zn ferrite. The observed evolutional relationship between microstructural, magnetic, and optical properties can be used to develop a useful framework for designing a sintering condition for final microstructure with desired properties. From the comparative study of top-down and bottom-up approaches carried out, we concluded that different synthesis methods produced ceramic materials with different behaviors. Top-down approach synthesis method has the ability to produce nanocrystalline particles, which then must be compacted without losing the refined microstructural properties, with high uniformity in terms of size, and morphological properties. This remains a challenge to this approach otherwise it is a versatile method. Bottom-up approach synthesis method is capable of producing particles with refined microstructures, which then high-purity single phase particles must be produced with particle size below 100 nm. This is relatively more difficult as single phase can only be achieved when sufficient heat energy is provided, and typically single phase particles are produced at high sintering temperature where particle growth is unavoidable.
\nWe would like to dedicate this chapter and show our gratitude to the late Assoc. Prof. Dr. Mansor Hashim from Universiti Putra Malaysia, Malaysia for sharing his pearls of wisdom with us during the course of this research.
\nIn the 20th century, Laser surface alteration played a major role in enhancing the material surface properties. Among the number of ways to enhance the material properties, laser based surface alterations are used to enhance a better physical property in the machined surface and improved the component performance. The high power Neodymium Yttrium-Aluminum-Garnet (Nd: YAG) laser, carbon-di-oxide (CO2) laser and excimer lasers are used to perform the laser surface treatment which is expensive, popular and operate at pulsed mode or continuous wave mode. These lasers are used to heat the near-surface area of the finished components for enhancing the properties. The laser surface modifications have the ability to control the amount of heat energy to work material with high directionality. The purpose of a surface hardening by laser is to improve the component wear properties. The laser surface hardening is defined as the heat energy from the laser beam that directly heated the component surface at a very short interval period without melting the work material. The heat input to the component surface is the reason for creating the tough and fine-grained structure in the hardened surface. The risk of crack forming is very low due to the self-quenching process. The laser surface melting (LSM) is heated to its melting point through a high power laser beam and rapidly solidified. The aim of LSM is to refine the surface microstructure, homogenization of composition, dissolution of precipitates. The LSM is also used to improve the corrosion resistance of steel and iron. The minimization of intergranular corrosion is possible through LSM by avoiding the carbides formation during subsequent homogenization and sensitizing treatment. The laser surface alloying (LSA) is defined as the high heat energy used to melt the metal coating through laser and a portion of underlying substrate. This technique is used to form highly resistant gradient layers on the metal surface. The major benefit of this technique is sudden heating followed by cooling and the surface properties are improved. The laser cladding (LC) is a coating method that the surface melting and new material layer formation by addition of material are simultaneously processed in the substrate at the same time by using the laser power. The desired surface properties are achieved after solidification. The large component surface properties are easily increased by using LC. The complete metallurgical bond is necessary between the melting of substrate and forming of a new material layer at the interface. The laser surface texturing (LST) is defined as the process in which the change of material surface properties by modifying its texture and roughness. The laser beam is used to create the micro patterns on the surface by laser ablation. The micro patterns are created on the surface in various shapes such as dimples, grooves and free forms with precise dimension. This process is mostly used in biomedical applications.
The different types of laser have different abilities to perform the process on materials. All the lasers are producing the heat energy and the laser beam wavelength is majorly affecting the performance of materials. Generally, the total laser heat energy is supplied to work material in which can be divided into two ways such as the fraction of heat energy is observed by work material and remaining heat energy is reflected to the environment. This happens during the surface hardening by laser. The supply of heat energy to polished metal surface components is depending upon the heat absorbability of work material and wavelength of irradiation. Generally, the short wavelength has higher absorptivity. Hence, the Nd: YAG laser (λ = 1.064 μm) has produced the higher absorbing ability beam to work material than the CO2 laser (λ = 10.6 μm) for surface hardening of steel. In order to increase the CO2 laser absorbility (high wavelength) to work material, the coating or painting is required in the work material prior to the CO2 laser surface hardening. Therefore, the Nd: YAG laser surface hardening better than CO2 laser surface hardening because the Nd: YAG laser has short wavelength and produces a high absorbing rate to work material. The Nd: YAG laser produces heat energy to work material which is transferred through fiber cable whereas CO2 laser is impossible. The inert gases, helium, neon and argon are used to eliminate the atmospheric contamination. In order to reduce the wavelength of a laser, an excimer laser is developed with very short wavelength. This laser can be used to micromachining on medical parts. In this chapter, laser surface hardening, laser surface melting, laser surface alloying, laser surface cladding and laser surface texturing have been discussed to improve the microstructure, hardness and wear resistance of mechanical components.
The laser surface hardening is defined as the heat energy from the laser beam which is directly impacted to the finished component surface for improving the wear resistance. The component life is increases without affecting the bulk material. During the hardening process, the surface layer is heated up to hardening temperature under the short period of time. The quenching is a necessary process to achieve the hard martensite phase in the heated surface. Thereby, the component surfaces are hardened by laser and achieve the high wear resistant surface with desired bulk properties. The components such as gear teeth, gears, shafts, camshafts, axles, cylinder liners, valve guides and exhaust valves showed with higher stresses due to laser surface hardening. The type of work materials, cast iron, die steel and medium-carbon steel are also required the laser surface hardening for better performance. The mass-production industries, automobile components and electronic parts are performed the laser hardening on the component surfaces [1]. The desired component performances are mainly depending upon the selection of laser process parameters such as power, scanning speed, pressure, beam shape and material properties. Now-a-days, in order to improve the surface quality of components, the number of surface treatment are commercially available to obtain the unique material properties. For example, the I-section rail (railway) is fabricated by hot rolled processes which have non-uniform properties in the flange and web. The I-section beam is shown in Figure 1. The flanges have been designed to withstand high stress whereas the web designed to withstand the least stress. The flange thickness is greater than the web thickness and stress developed in the I-section is within the allowable limit. The point is the different cross section of flange and web has produced the non-uniform properties. Hence, the laser surface hardening is required for achieving the uniform properties over the flange and web.
Schematic of I-section beam used in rail.
The laser surface transformation hardening process is performed to obtain the required depth and width for steel material. The accurate parts are made of medium carbon steels which require the laser surface hardening. The small and complex components are easily surface hardened by laser. This is because of the high rate of cooling effects to increase the hardness rate in the quenching process [2]. Therefore, LSH is a better process compared to flame and induction hardening processes. The quenching process is suddenly reducing the work material temperature by using water, oil or air to get certain material properties through the phase transformation. Therefore, a comparative study is made between the laser quenching and conventional quenching on steel to study the hardness and wear rate. The conventional quenching and tempering is carried out by using the temperature of 1198 K for 4.5 h and temperature of 523 K for 4 h respectively. The air, 10 kW CW diode laser, 3.5 mm spot diameter and 168 mm/s linear speed are used in the laser treatment. The laser quenched and conventional quenched sample for 25 μm distance from the surface, the produced hardness is 600 HV0.1 and 625 HV0.1 respectively. The laser quenched sample has 0.4 mm3/N-m wear rate which is lesser than the conventional quenched sample of 0.6 mm3/N-m wear rate at 500 m sliding distance [3]. The wear and microhardness studies are performed on 40CrNiMoA steel by using laser quenching and high-frequency quenching. A 2 kW CW CO2 laser, 1400 W laser power, 35 mm/s traverse speed, 60 degree incident angle, black organic absorbent coating, 0.9 m3/h gas flow rate and 10 mm defocusing distance are used in the laser treatment. The hardness of the quenched groove surface reached 750 HV and is substantially higher than that resulting from the high-frequency quenching method. The results of wear testing showed that the wear resistance of laser quenched specimens is 1.3 times higher than that of a high-frequency quenching specimen [4]. Comparisons were made between the gray cast iron (GCI), laser hardened quench-tempered GCI and conventional austempered GCI specimens based on the hardness and wear loss. The air, CW Nd: YAG laser, 2 mm laser spot, 22 mm defocused distance, 2 mm/s scanning speed, 6 Hz frequency, 120 A current and 8 ms pulse duration is used for laser hardening. The hardness of the laser hardened zone with ledeburitic structure is approximately 68 HRC. The quenching-tempered GCI specimen showed higher wear resistance than untreated GCI specimen [5].
The advantage of laser surface hardening is listed below
The lower level of heat energy is used to work material compared to conventional surface heat treatment.
The input laser energy is controlled by varying the process parameters such as power, scanning speed, defocus, different shapes of lenses and mirrors.
The hardened surface is obtained through self-quenching of the heated surface layer.
The work material is made under the hardening and quenching process resulting in cleaning of work material is not required.
The beam guidance is automatically controlled over the work material.
The surface heat treatment is specifically performed on small parts and complex parts.
The disadvantage of laser surface hardening is listed below
High initial capital cost
Skilled operators are needed
Surface preparations are required in difficult areas.
Radiation protection is required
Material hardness and wear
The performance of the components such as hardness and wear resistance of work materials are mainly focused in the laser surface hardening. This is depending upon the material type, material properties, and types of processing on materials. The desired properties of work materials are obtained through proper selection of laser surface treatment and optimization. In order to improve the durability of mechanical components namely gears, engine valve, brake drums and camshaft are highly needed the LSH. The induction hardening is one of the surface hardening process which is shown in Figure 2. It is performed to achieve the uniform microstructure and good wear resistance which is higher implementation cost compared to laser surface hardening.
Schematic of induction hardening.
In this induction hardening, the depth of hardening is mainly depending upon the resistivity (ρ), frequency (v) and magnetic permeability (μ). The work material is placed inside the coil and supplies the high frequency. The surface is hardened by skin effect.
The laser surface hardening can be performed on the components either partially or fully depending upon the application of the components. Specifically, the load bearing component is subjected to high surface wear. Hence, the laser surface hardening is required on the load bearing component surface. Therefore, the load bearing component is hardened by laser, the surface has produced a high hardenability and fine microstructure [6]. The service life of crankshaft and camshaft are made on EN18 steel in which properties are improved by diode laser surface hardening with beam diameter of 3 mm, velocity of 1 m/min and power of 1.5 kW. The argon gas is used as shield gas [7]. The advantages of induction hardening are localized areas heat treated, minimal surface decarburization, surface oxidation, slight deformation, improved fatigue strength and low operating cost. The disadvantages of induction hardening are high capital investment. The advantages of laser hardening are described as non-hardenable steels are surface hardened, higher hardness obtained than conventional hardening, eliminating dimensional distortion, no protective atmosphere required and very long and irregular shapes easily hardened. The disadvantages of laser hardening are high initial and working cost and difficult to harden the high alloy steel. The schematic diagram of substrate and laser processed materials are shown in Figure 3(a) and (b). The parent substrate has coarse and uneven equiaxed grains. The laser processed work material showed the hardened depth varying from top surface to 200 μm depth. The depth of hardening increases with grain size increases from finer to coarser. The curved surface is formed at top surface due to the low scanning speed produces more evaporation in the laser melted surface. The laser process parameters, power of 1.5 kW, beam diameter of 3 mm, scan speed of 1 m/min and interaction time of 0.18 s are used to obtain the desired hardness. The Nd: YAG laser and argon gas with flow rate of 20 L/min is used in the laser surface hardening. The hardness decreases from 955 HV to 236 HV which is obtained by varying distance from top to 200-micron depth and it is shown in Figure 4. This is due to the grain size refinement [8]. The 5 kW CW CO2 laser, power ranging from 1.1–2.5 kW, traverse speed ranging from 6 to 15 mm/s and spot size of 6.3 mm, 2.27 mm, 4.63 mm and 1.2 mm are used to harden the various carbon steel. The argon gas is used as shielding gas. The traverse speed has mostly affecting the hardness. The carbon percentage increases, the average hardness value also increases. The C-45 steel has produced higher hardness. The hardness of the material was improved by minimizing the diameter of spot size [9]. Further, conventional type laser surface treatment is performed on large surface areas and irregular hardness was observed on the machined component. In order to overcome irregular hardness, a laser overlapping method is used in the laser transformation hardening which is presented in Figure 5.
(a) Schematic of; (a) as received tool steel microstructure, (b) laser surface hardened tool steel with modified structure.
Microhardness variation from top surface to substrate through LSH.
Schematic of laser transformation hardening.
After the laser treatment, the laser hardened zones are divided into three sections such as hardened zone, transition zone and heat affected zone which is shown in Figure 6. A study on the effect of process parameters on surface hardness splined shafts is performed by using laser surface hardening. The fiber laser, power varying from 1900 to 2500 W, scanning speed varying from 2 to 6 mm/s, rotation speed varying from 1500 to 2500 rpm, the flank tilt angle of spline tooth varying from 15 to 20 and tooth depth of spline shaft varying from 2.5–3.5 are used in the laser hardening of spline shaft. The result found that the maximum hardness is observed by using the power of 2500 W, scanning speed of 2 mm/s, rotational speed of 2500 rpm, the flank tilt angle of spline tooth of 20° and tooth depth of spline shaft of 3.5 mm [10]. An investigation on the underwater hardening of AISI 1055 steel is carried out using lasers. A 250 W CW Ytterbium based fiber laser, focal length of 300 mm, defocus distance of 10 mm and traverse speed varying from 1 to 100 mm/s are used in the laser surface hardening. The result found that the higher surface roughness is obtained in the underwater welding compared to conventional laser hardening due to the additional cooling effect in the underwater [11].
Schematic of different zones of laser transformation hardening.
Laser surface melting is one of the surface alteration processes that the surface of the substrate is melted and rapidly solidified to form the fine microstructure and improving the mechanical properties without changing the bulk properties and without addition of any metallic elements. The piston, valve and sliding parts are made of magnesium alloys, which are used in the automobile components and energy saving material. The application and limitation of magnesium alloy is decided by properties. In order to improve the tribological and mechanical properties, the laser surface melting process is focused on magnesium alloy. In the conventional heat treatment of HSS materials are presented the retained austenite, which transforms into brittle martensite during service. But, the life of high-speed tool steel is increased by using LSM. The schematic view of LSM is shown in Figure 7. The LSM treatment are carried out using a 2 kW fiber laser with 1.06 μm wavelength, laser power of 1500 W, the laser scanning speed of 600 mm/min and the distance between the laser head, spot size of 3 mm, shielding gas pressure of 0.3 MPa and the specimen surface of 12 cm are used in the LSM. The microhardness and corrosion resistance of magnesium alloy is also improved by using LSM with electromagnetic stirring [12]. In order to enhance the microhardness of melted substrate, the LSM process parameters effect of hardness of magnesium alloy is studied. The CW CO2 laser, beam diameter of 4 mm, argon gas of 6 l/min, speed varying from 100 to 400 mm/min and power varying from 1.5–3.0 kW are used in the process. The result showed that the melt depth of magnesium alloy is directly proportional to the laser power and inversely proportional to the scan speed. Laser surface melting enhances the microhardness of the melted zone by 2–3 times than the substrate [13]. The laser processed hardness of high speed tool steel and magnesium alloy is decreased from as-received substrate by increasing distance from the melting surface which is shown in Figure 8. This is due to the refined, solid solution strengthening and uniform microstructure. The LSM is also performed in electric contact material of Cu-50Cr. The 1 kW CW Nd: YAG laser, power density varying from 106 to 107 W/cm2, scanning speed of 6000–10,000 mm/min and argon gas are used in this process. From the analysis found that the microhardness and withstanding voltage of Cu-50Cr are significantly improved by using LSM [14]. The effects of LSM process parameters are affecting the microstructure and hardness of AZ31B magnesium alloy substrate. The result found that the grain size in the fused layer increases by increasing power. The schematic diagram of as-received magnesium alloy is shown in Figure 9a. The effects of different power on microstructure of layer fused layers are shown in Figure 10 b-e. The Nd: YAG laser power varying from 1600 to 2200 W, laser beam scanning velocity of 900 mm/min, laser beam spot diameter of 4 mm, number of superimposed tracks of 9, overlap ratio of 15%, and argon flow rate of 25 mL/min are used in the process. The depth of the metal pool and grain size is increased by increasing the power. This is due to the grain growing freely in the higher metal pool depth compared to smaller metal pool depth. The reason for increasing the hardness and wear resistance are due to the grain refinement, high dislocation density and dispersive distribution of β- Mg17Al12 phase in the fused layer. [15].
Schematic view of laser surface melting.
Microhardness variation of magnesium alloy.
Schematic diagram of (a) As received AZ31B magnesium alloy, microstructure of laser fused layer of (b) laser melted at 1600 W, (c) laser melted at 1800 W, (d) laser melted at 2000 W.
The effect different heat treatment on weight loss of AISI M2 tool steel.
The LSM method produced the higher surface roughness of AZ80 magnesium alloys compared to MB26 due to the variation in cooling rate. A nanosecond pulsed fiber laser with the wavelength of 1060 nm is used for the LSM process. The process parameters such as pulse duration, repetition rate, and spot size are 220 ns, 500 kHz, and 44 μm, respectively. Alloys are irradiated with a laser power density of 1.20 × 107 W/cm2 and at a scanning speed of 200 mm/s with 50% beam bath overlapping. The higher microhardness was observed for MB26 than the AZ80 due to the higher melting layer thickness. [16]. The LSM is also used to study the grain size, microhardness of hybrid composites. The laser power is varied from 1.8 to 2.0 kW, the laser beam diameter range is 4.72–6.07 mm, standoff distance range is 35–45 mm and a constant scan speed of 400 mm/s is maintained. Argon shielding gas is used during the laser melting process to prevent the oxidation. The study found that the LSM treated hybrid metal matrix composite has lower grain size compared to untreated composites due to rapid solidification after LSM. The LSM produces the higher hardness of composites compared to untreated composite [17]. The effect of different laser power on microhardness and wear of AISI M2 high speed steel is studied by using LSM. The Nd: YAG laser, stand of distance varying from 1 to 2 cm, power varying from 600 to 1800 W, argon gas of 0.5 bar, laser spot varying from 2 to 4 mm and speed varying from 50 to 100 cm/min are used in this process. The results found that the maximum hardened depth of 0.85 mm is achieved by using power of 1400 W. The wear resistance of tool steel is nearly equal to conventionally hardened work material and it is shown in Figure 10. The reason for LSM produces high wear resistance and high hardened surface is due to the fine dendrites with dissolved carbides [18]. The LSM is also used to improve the hardness and wear resistance of Hastelloy C-276. The CW CO2 laser with the parameters of 2 mm beam diameter, 0.6 MPa argon pressure, power varying from 1.25–1.75 kW, speed of 300 mm/min and interaction time of 400 ms are used in the work. The result found that the maximum hardness of 447 HV is achieved by using the power of 1.5 kW and scanning speed of 300 mm/min. The hardness is improved by 1.8 times compared to parent metal. The wear resistance of hastelloy is high in the sample laser treated at 1.5 kW of power and 300 mm/min speed and it is shown in Figure 11. This is due to the significant effect of grain refinement on hardness [19].
The effect of LSM on wear resistance of Hastelloy C-276.
The laser surface melting is carried out on nodular cast iron (NCI) [20]. The laser parameters, power of 1.5 kW, scan speed of 600 mm/min, overlapping of 30% and defocus of 15 mm and argon gas are used to melt the NCI surface. The microstructure of as received nodular cast iron showed with more ferrite and less pearlite as shown in Figure 12a. The γ-phase dendrites and an interdendritic carbide structure were observed in the laser treated region and it is shown in Figure 12b. The reason for forming dendrite in the laser treated region is due to the rapid heating and solidification. The needle shape interdendritic structure of Fe3C and M-phase is also observed due to the higher cooling rate. The convection is also the reason for forming of homogeneous dendritic. The small diameter of nodules is also observed in the bottom layer with partial dissolution of nodular graphite due to the heat treatment and self-quenching. The uneven martensite and dendrite phases are observed in the intermediate layer due to the rapid re-solidification of the melt pool. Finally, fine martensite is observed in the bottom region. Moreover, no cracks and no voids are observed in the processed depth.
Microstructure of; (a) as-received nodular cast iron, and (b) laser surface melted nodular cast iron.
The worn out surface of as received and laser melted surface is shown in Figure 13a and b. The LSM specimen wear track showed with smooth, minor grooves and delamination. The wear depth and pile-up of laser processed specimens are lesser than untreated specimens. The laser treated surfaces have fine grooves resulting in improving the wear resistance of specimens due to the microstructure changes. The root causes for improving the wear resistance of laser processed materials are fine M-phase and retained γ-phase with Fe3C phase. The length of depth of hardness is increased by increasing the melted depth. The reasons are due to the precipitation hardening, residual stress by refinement of grains through rapid re-solidification. The cooling rate and thermal gradient also support the refinement of grains resulting in increased the hardness of the laser treated zone. Compared to hardness of substrate material, the laser processed depth has four time higher hardness due to the uniform grain structure. The partially melted zone shows the higher hardness due to the graphite nodules and fine ledeburite microstructure with the graphite interface. The wear loss is calculated for both the laser processed sample and untreated sample. The laser processed samples showed less wear than substrate.
Worn out surface of; (a) base metal, (b) laser melted specimen.
Laser surface alloying is a material processing technique that utilizes the focused laser sources and produces the high power density to melt the metal coating and a portion of the underlying substrate. The schematic view of laser surface alloying is shown in Figure 14. The schematic diagram of shape and dimensions of laser surface alloyed zone is shown in Figure 15. Here, W = width, T = thickness, B = build-up and D = melted depth. Aluminum alloys are widely used in automobile and aerospace applications due to the availability and low cost, ductility, good strength-to-weight ratio and lightweight. These alloys have low hardness and poor tribological properties which leads to wear problem. Hence, the additional protection is required to enhance the wear resistance properties to localized areas. So, LSA can be used to improve the surface properties of aluminum alloys, titanium alloys, magnesium alloys, copper alloys and nickel-copper alloys. The laser alloyed component properties are depending upon the selection of alloy material, composition and elemental surface distribution. These factors are affecting the microstructural development in the alloyed surface. The ceramic alloys, carbide, oxide and boride (SiC, WC, TiO2, TiB2 and TiC) are widely used as the coating material on aluminum alloys due to the low density, high hardness, good wear, high melting temperature and corrosion resistance. The hybrid ceramics, a component coating on aluminum produces better wear resistance than the single ceramics component coating. Titanium is added to the carbon resulting in forming TiC to improve the surface properties and by the same to prevent the formation of Al4C3 carbides. A study on FeCoCrAlCuNix high entropy alloy coating on pure copper is carried out using LSA to evaluate the microhardness and wear. The laser power 1.7 kW, laser spot diameter 1.2 mm, scanning speed 2.0–3.0 mm/s, argon as shielding gas and flow rate 12 L/min are used in this process.
Schematic view of laser surface alloying.
Schematic diagram of shape and dimensions of laser surface alloyed zone.
Figure 16a shows the microstructure of HEA FeCoCrAlCuNix. The HEA coating have high density, little holes and adequate metallurgical bonds to substrate. It is noticed that the dilution ratio of the tested HEA coating is higher than 20%. Typical dendrite and interdendrite structures are clearly observed in Ni05 and Ni10 HEAs (Figure 16b and c), while only one phase was observed for Ni15 HEA (Figure 16d). Compared to hardness of copper, coated copper produces higher hardness and it is shown in Figure 17 [21]. The effect of addition of Ni–Cr–Si–B alloy to brass substrate was studied through LSA. The 2 kW CW Nd-YAG laser with a spot diameter of 3 mm, the laser power density varied between 141 and 212 W/mm, while the scanning speed is kept constant at 5 mm/s. Argon with a flow rate of 15 l/min is used as the shielding gas to prevent the oxidation. Laser surfacing is achieved by overlapping of adjacent tracks, with an overlapping ratio of 50%.The hardness of the modified layers increased slightly from the surface to a maximum and sharply fell to the value of the substrate at the interface between the treated layer and the substrate. The increases in hardness observed for the modified layer is attributed to the formation of hard borides [22]. The effects of addition of SiC and TiO2 to aluminum alloy are studied by continuous mode CO2 laser. The CO2 laser with the parameters of 1.7 kW, scan speed of 400 mm/min, standoff distance of 40 mm and laser beam diameter of 7.4 mm are used for SiC alloying. The CO2 laser with the parameters of 1.8 kW, scan speed of 300 mm/min, standoff distance of 30 mm and laser beam diameter of 5.8 mm are used for TiO2 alloying. The result found that the ceramic nature of SiC and TiO2 improved microhardness of alloyed zone from 30 HV0.3 substrate material to 180 HV0.3 with SiC and 220 HV0.3 with TiO2 [23].
Microstructure images of (a) FeCoCrAlCuNix HEA coatings on cross sectional view, (b) high magnifications image of Ni05 HEA (c), Ni10 HEA (d) and Ni15 HEA.
Microhardness of FeCoCrAlCuNix HEA coatings.
A study on the effect of addition of WC + Co + NiCr to AISI 304 stainless steel through Nd: YAG laser. The 5 kW Nd: YAG with beam diameter of 4 mm, power varying from 1 to 3 kW, scan speed from 0.005–0.1 m/s and argon gas of 5 L/min are used in the alloying process. The experimental result found that the LSA has been performed to form a defect free and uniform alloy zone. Compared to hardness of substrate, laser alloying produces the higher hardness due to the grain refinement [24].
The laser surface alloying is carried out on nodular cast iron by adding Ni-20%Cr alloy [20]. The laser parameters, power of 1.5 kW, scan speed of 600 mm/min, overlapping of 30% and defocus of 15 mm and argon gas are used to alloying the NCI surface. The microstructure of the laser alloyed specimen, worn out surface of substrate and laser alloyed specimen is shown in Figure 18a–c respectively. The ledeburite and pre-eutectic austenite are observed in the LSA surface. In addition, γ-phase (austenite) to M-phase (martensite) is transformation observed. The laser alloyed surface has produced the defect free and fine microstructure. The γ-phase has a higher percentage of Ni than cementite, whereas the Fe3C phase has Cr more and Ni less element. Hence, the presence of Fe3C on the laser-alloyed surface is rich in Cr and the γ-phase was supported through the solid solution of both alloy powders of Ni and Cr. The rapid solidification is the reason for obtaining the fine microstructure in the laser alloyed surface. The laser processed worn out surfaces have severe plastic deformation, wear track, delamination, grooves and adhesive particles. The NiCr alloying is also observed by using the LSA. The length of depth of hardness is increased by increasing the melted depth. The reasons are due to the refinement of grains through rapid re-solidification. The rate of cooling rate and thermal gradient also support the refinement of grains resulting in increased the hardness of the laser treated zone. Compared to hardness of substrate material, the laser processed depth has 2.62 time higher hardness due to the uniform grain structure. The wear loss is calculated for laser processed sample and untreated sample. The laser processed samples are produced lesser wear rate than substrate due to the improved hardness.
Microstructure of LSA specimen (a), worn out surface of substrate (b), and worn out substrate of LSA (c).
Laser cladding is similar to arc welding. The laser is used to melt the clad material coated on the substrate. The powder, wire and strip form of clad materials are commercially available to perform by different laser processes. The major benefits of LC have low porosity, good surface uniformity and low dilution. The clad materials have rapid quench and cooling down after deposition resulted in a fine grained microstructure. The laser is used to deposit clad material on substrate through the interaction of powder with laser. The substrate permits the melt pool to solidify and form the solid track. The schematic of laser cladding process is shown in Figure 19. Compared to other different surface processing used to enhance the wear and corrosion resistance of substrate, LC is an attractive alternative method. This is due to the intrinsic properties of laser radiation. The LC benefits are high input energy, low distortion, and minimum dilutions observed between the substrate, processing flexibility and cladding on small areas. The LC can be used in surface alloys and composites in order to achieve the required properties. The LC produces desired properties are obtained by varying the process parameters such as laser beam power density, laser beam diameter at the workpiece surface and laser beam travel speed.
Schematic of laser cladding process.
The laser solution strengthening, laser surface alloying and laser cladding have highly correlation to corrosion and erosion resistance. The laser solution strengthening and laser surface alloying are used to improve the erosion and corrosion resistance of old components without changing their sizes whereas laser cladding is used to repair wasted components by restoring their size. The high entropy alloy of CoCrFeNiNbx is coated to a pure titanium sheet by using laser cladding to study the hardness of the material. The laser cladding parameters such as power of 100 W, scanning speed of 8 mm/s, defocusing amount of +2 mm, pulse duration of 5 ms, frequency of 20 Hz, beam diameter of 1 mm power density of 127.4 W/mm2 and linear energy density of 12.5 J/mm are used in this process. The result found that the CoCrFeNiNbx HEA coated on titanium sheet produces higher hardness compared to the pure titanium. The Nb coating produces significant improvement in hardness compared to pure titanium due to the consisted phase of BCC solid solution with equiaxed bulk grain morphology and Cr2Ti Laves phase [25]. A comparison is performed between the thermal spray coating and laser cladding performance on steel. The laser cladding conditions, power of 780 W, cladding speed of 4.3 mm/s, powder feed rate of 6 g/min and argon gas are used. The thermal spray conditions, distance of 200 mm, acetylene (0.7 bar) and oxygen (4 bar) gas are used. The Metco 15E powder is used in both the processes. The result found that the cladded layer produced the high hardness, crack free, and good adherence to substrate whereas flame coating produces high porosity, minimum dilution and oxides inclusions [26]. The Inconel 625 coating performance on steel is evaluated by arc welding and laser cladding based on the microstructure, wear resistance and hardness. The parameters, power of 1200 W, scan speed of 2 mm/s, powder feed rate of 5 g/min, shielding gas flow rate of 5 L/min and powder feeding gas flow rate of 8 L/min are used. The result found that the arc welded and laser cladded Inconel 625 coatings have Ni (fcc) solid solution phase, and fine microstructure. The arc welded coating to Inconel 625 is produced slightly lower hardness compared to laser cladding coating. This is due to the microstructure developed in the arc welding. The laser cladded Inconel 625 coating is preferred due to its better mechanical performance such as hardness and wear resistance at both room and elevated temperature [27]. The 316 stainless steel powders coated on EN3 mild steel is to evaluate clad geometry and distribution of elements by laser cladding. The 2 kW continuous wave CO2 with laser power 1.8 kW, beam spot diameter 2–5 mm, powder feed rate 0.160–0.220 g/s, substrate traverse speed 7–40 mm/s are used. The stainless steel powder coating provides the sound coating and no porosity [28]. The Fe-Cr-Si-B alloy powder coating is performed on low carbon steel using laser cladding to evaluate the microstructure, hardness, wear resistance and corrosion resistance. The result identified that the Fe-Cr-Si-B alloy powder coating provides higher wear resistance, high hardness and high corrosion resistance compared to substrate [29]. The CPM 15 V, CPM 10 V, CPM 9 V, D2 and M4 coatings are provided on AISI 1070 carbon steel by laser cladding. The laser cladding conditions, power varying from 2.5–2.75 W, laser beam diameter varying from 2 mm, substrate traverse speed varying from 7.6–8.6 mm/s, powder feed rate varying from 20 to 9 g/min and overlap varying from 30 to 50% are used in the process. The abrasive wear resistance of the laser-clad CPM 15 V and CPM 10 V coatings is superior performance than D2 steel, whereas the wear resistance of the CPM 9 V and M4 coatings is inferior to that of the D2 [30].
Figure 20a shows the microstructure of Colmonoy 6 cladding on Inconel 625 [31]. The laser cladding parameters are 400 mm/min speed, feed rate of 4 g/min, power of 1000 W, argon pressure of 1 bar with flow rate of 25 lpm and 150 degrees preheating used in this process. The clad surfaces have no defects, uniform dendrite eutectic phases observed. There are two regions represented in the cladded surface such as darker region for boride content and lighter region for γ-nickel. The high quantity of intermetallic lave phase is observed in the cladded surface. Figure 20b shows the worn out surface of substrate Inconel 625. Compared to wear intensity of sample, laser cladded surfaces have lesser wear. The plow marks are also observed in the worn out surface substrate due to the less wear resistance and high plastic deformation. The higher material removal rate of the sample is observed than the cladded surface. Figure 20c shows the laser cladded worn out surface. The few debris particles, few depth of wear track and few grooves are observed in the cladded surface. This is due to the high hardness of the clad layer. Therefore, better protection is provided by the clad layer over the untreated surface. The more hardness is observed in the clad surface than the base metal. The reasons for increasing the hardness of clad surface is due to the defect free cladding, proper fusion and laves phase presented. The reason for decreasing the hardness of base material is due to weak intermetallic phases.
Microstructure of Colmonoy 6 clad (a), worn out surface of substrate (b) and worn out surface of laser cladding (c).
The coefficient of friction (CoF) and wear behavior of coated and substrate found that the CoF is increased with increased sliding distance due to the reduced adhesion resistance and increasing heat between points of contact. The more CoF is observed in the substrate sample than clad sample due to the adhesion effect. The less CoF is observed in the clad sample due to the hard laves phases. It is found that low mass loss is observed in the clad sample compared to base material. The wear loss is highly related to the hardness and base material produces poor wear resistance when compared to clad surface.
Laser texturing is a process that alters a material surface property by modifying its texture and roughness. The laser beam creates micro patterns on the surface through laser ablation, removing layers with micrometer precision and perfect repeatability. Typical patterns include dimples, grooves, and free forms. Laser surface texturing can be used to improve properties like adherence, wettability, electrical and thermal conductivity, and friction. For example, the method can increase surface adherence before applying common coatings like adhesives, paint or ceramic. Laser texturing can also be used to prepare surfaces for thermal spray coating and laser cladding as well as to improve the performance of mechanical seals. Surface treatments like abrasive blasting and chemical etching processes need consumables like steel grits and acid to texture surfaces. Unlike those treatments, the laser texturing process functions without consumables. This results in low operating costs, low maintenance, and improved health and safety in the workplace. Operators will not need to handle chemicals, wear protective equipment, and stop operations to replace consumables. Laser texturing uses laser ablation to selectively remove materials from specific surface areas. By adjusting the laser’s parameters, the surface is removed as well as creates different patterns. This typically increases roughness, creating surface textures that can easily lodge adhesives and provide additional anchoring surface. To reach the material’s ablation threshold, pulsed lasers concentrate energy to reach a high peak power. Typically, the pulse duration is 100 nanoseconds, and each pulse contains between 0.5 and 1 millijoules. The time required to texture a surface depends on the material, the desired roughness level, and the laser system’s output power. The application of laser texturing is in adhesive bonding, mechanical seals, painting and coatings. The laser texturing process is shown in Figure 21. The circle and oval shape dimple texturing on metal can be made using a laser and the schematic diagram is shown in Figure 22 a-b. Where, a = pitch, b = diameter, and c = height.
Schematic of laser texturing process.
Schematic of laser surface texture dimensions: (a) circle, (b) oval.
The new materials have been developed every day to meet the demand of competitive situations. The surface properties of substrate can be improved by a number of methods such as laser surface alterations such as surface hardening, melting, alloying, cladding and texturing in order to improve the mechanical performance and tribological behavior. In this work, the effect of laser process parameters on microstructure, hardness and wear rate of materials have been presented. The laser surface hardening is needed to high stressed components namely gear teeth, gears, shafts, camshafts, axles, cylinder liners and exhaust valves. The laser surface melting can be adopted in biomedical alloys, sport cars and power plants made of stainless steel, magnesium alloy and superalloys. The locomotive, aerospace and structural components made of aluminum alloys, titanium alloys and magnesium alloys have required the laser surface alloying to improve the surface properties of metals. The repaired and refurbishment components such as internal combustion engine parts, gas turbine, turbine blades and tools are highly needed the laser surface cladding to improve the surface properties of metals. The texturing on material is used to increase the tribological characteristics of materials resulting in improved surface roughness, wettability, improve load capacity, wear rates, lubricating lifetime and reduce friction coefficient. Hence, the laser based surface modification techniques can be adopted to improve the performance of the components.
The authors wish to thank the Ministry of Science and Technology, Taiwan ROC for the financial support to carry out this work.
The authors declare that they have no conflicts of interest in the work.
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\n\nOur reputation – Everything we publish goes through a two-stage peer review process. We’re proud to count Nobel laureates among our esteemed authors. We meet European Commission standards for funding, and the research we’ve published has been funded by the Bill and Melinda Gates Foundation and the Wellcome Trust, among others. IntechOpen is a member of all relevant trade associations (including the STM Association and the Association of Learned and Professional Society Publishers) and has a selection of books indexed in Web of Science's Book Citation Index.
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\n\n"In developing countries until now, advancement in science has been very limited, because insufficient economic resources are dedicated to science and education. These limitations are more marked when the scientists are women. In order to develop science in the poorest countries and decrease the gender gap that exists in scientific fields, Open Access networks like IntechOpen are essential. Free access to scientific research could contribute to ameliorating difficult life conditions and breaking down barriers." Marquidia Pacheco, National Institute for Nuclear Research (ININ), Mexico
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Today his focus is on defining the growth and development strategy for the company.",institutionString:null,institution:{name:"TU Wien",country:{name:"Austria"}}},{id:"19816",title:"Prof.",name:"Alexander",middleName:null,surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/19816/images/1607_n.jpg",biography:"Alexander I. Kokorin: born: 1947, Moscow; DSc., PhD; Principal Research Fellow (Research Professor) of Department of Kinetics and Catalysis, N. Semenov Institute of Chemical Physics, Russian Academy of Sciences, Moscow.\r\nArea of research interests: physical chemistry of complex-organized molecular and nanosized systems, including polymer-metal complexes; the surface of doped oxide semiconductors. 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