\r\n\tSome studies should be linked to the late-stage tumorigenesis promoting metastasis in cancer. In addition, deregulated cellular processes such as cell proliferation, apoptosis, and differentiation as related to different tumor types should be investigated in this book. Besides tumorigenesis, spontaneous tumor regression and its potential formation mechanisms should be reviewed or researched. In addition, the role of the deregulated immunity in tumorigenesis should be explored. The drug targets and treatment alternatives in various cancer types should be described or investigated in some studies. The studies relating to the laboratory tests used as diagnostic and prognostic in cancer patients should also be presented. Consequently, this book may include but is not limited to these topics.
",isbn:null,printIsbn:null,pdfIsbn:null,doi:null,price:0,priceEur:null,priceUsd:null,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"46d3363b21f482c9a22ba72cca9ec4c0",bookSignature:"Dr. Nevim Aygun",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/6919.jpg",keywords:"Tumorigenesis,clinical significance, biological/genetic features, genomic/chromosomal instability, prognosis, prognostic factors, tumor suppressor genes, promotion of metastasis, spontaneous regression, tumor stages, tumor types/subtypes, signaling pathways, signaling networks, deregulated cellular processes, immunity, diagnosis, laboratory tests, treatment , oncogenes, primary tumor progression",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"March 26th 2018",dateEndSecondStepPublish:"April 16th 2018",dateEndThirdStepPublish:"June 15th 2018",dateEndFourthStepPublish:"September 3rd 2018",dateEndFifthStepPublish:"November 2nd 2018",remainingDaysToSecondStep:"3 years",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"195365",title:"Dr.",name:"Nevim",middleName:null,surname:"Aygun",slug:"nevim-aygun",fullName:"Nevim Aygun",profilePictureURL:"https://mts.intechopen.com/storage/users/195365/images/system/195365.jpeg",biography:"Nevim Aygun received her Medical Biology and Genetics Ph.D. in Health Sciences. She is interested in cancer, molecular biology, human genetics, cytogenetics, molecular cytogenetics, genomics, and bioinformatics. She has participated in many research projects on neuroblastoma, human gross gene deletions, non-B DNA-forming sequences, solid tumors, HCV, and leukemia, resulted in six articles, one book chapter, and numerous reports. She performed many molecular biological methods: PCR, real-time PCR, bacterial transformation, plasmid vector transfection, RNA interference, fluorescence in situ hybridization (FISH), cytogenetic, DNA sequencing, and cell culture. She also performed genomics and biostatistics analyses using some bioinformatics tools and SPSS program. She reviewed several manuscripts for some medical, genetics, and genomics journals. She is the Managing Editor of a special issue in Frontiers in Bioscience now.",institutionString:"Independent Scientist",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"0",institution:null}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"6",title:"Biochemistry, Genetics and Molecular Biology",slug:"biochemistry-genetics-and-molecular-biology"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"177731",firstName:"Dajana",lastName:"Pemac",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/177731/images/4726_n.jpg",email:"dajana@intechopen.com",biography:"As a Commissioning Editor at IntechOpen, I work closely with our collaborators in the selection of book topics for the yearly publishing plan and in preparing new book catalogues for each season. 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. I am responsible for developing and maintaining strong relationships with all collaborators to ensure an effective and efficient publishing process and support other departments in developing and maintaining such relationships."}},relatedBooks:[{type:"book",id:"6694",title:"New Trends in Ion Exchange Studies",subtitle:null,isOpenForSubmission:!1,hash:"3de8c8b090fd8faa7c11ec5b387c486a",slug:"new-trends-in-ion-exchange-studies",bookSignature:"Selcan Karakuş",coverURL:"https://cdn.intechopen.com/books/images_new/6694.jpg",editedByType:"Edited by",editors:[{id:"206110",title:"Dr.",name:"Selcan",surname:"Karakuş",slug:"selcan-karakus",fullName:"Selcan Karakuş"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"1591",title:"Infrared Spectroscopy",subtitle:"Materials Science, Engineering and Technology",isOpenForSubmission:!1,hash:"99b4b7b71a8caeb693ed762b40b017f4",slug:"infrared-spectroscopy-materials-science-engineering-and-technology",bookSignature:"Theophile Theophanides",coverURL:"https://cdn.intechopen.com/books/images_new/1591.jpg",editedByType:"Edited by",editors:[{id:"37194",title:"Dr.",name:"Theophanides",surname:"Theophile",slug:"theophanides-theophile",fullName:"Theophanides Theophile"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3092",title:"Anopheles mosquitoes",subtitle:"New insights into malaria vectors",isOpenForSubmission:!1,hash:"c9e622485316d5e296288bf24d2b0d64",slug:"anopheles-mosquitoes-new-insights-into-malaria-vectors",bookSignature:"Sylvie Manguin",coverURL:"https://cdn.intechopen.com/books/images_new/3092.jpg",editedByType:"Edited by",editors:[{id:"50017",title:"Prof.",name:"Sylvie",surname:"Manguin",slug:"sylvie-manguin",fullName:"Sylvie Manguin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3161",title:"Frontiers in Guided Wave Optics and Optoelectronics",subtitle:null,isOpenForSubmission:!1,hash:"deb44e9c99f82bbce1083abea743146c",slug:"frontiers-in-guided-wave-optics-and-optoelectronics",bookSignature:"Bishnu Pal",coverURL:"https://cdn.intechopen.com/books/images_new/3161.jpg",editedByType:"Edited by",editors:[{id:"4782",title:"Prof.",name:"Bishnu",surname:"Pal",slug:"bishnu-pal",fullName:"Bishnu Pal"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"72",title:"Ionic Liquids",subtitle:"Theory, Properties, New Approaches",isOpenForSubmission:!1,hash:"d94ffa3cfa10505e3b1d676d46fcd3f5",slug:"ionic-liquids-theory-properties-new-approaches",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/72.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"1373",title:"Ionic Liquids",subtitle:"Applications and Perspectives",isOpenForSubmission:!1,hash:"5e9ae5ae9167cde4b344e499a792c41c",slug:"ionic-liquids-applications-and-perspectives",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/1373.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"57",title:"Physics and Applications of Graphene",subtitle:"Experiments",isOpenForSubmission:!1,hash:"0e6622a71cf4f02f45bfdd5691e1189a",slug:"physics-and-applications-of-graphene-experiments",bookSignature:"Sergey Mikhailov",coverURL:"https://cdn.intechopen.com/books/images_new/57.jpg",editedByType:"Edited by",editors:[{id:"16042",title:"Dr.",name:"Sergey",surname:"Mikhailov",slug:"sergey-mikhailov",fullName:"Sergey Mikhailov"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"371",title:"Abiotic Stress in Plants",subtitle:"Mechanisms and Adaptations",isOpenForSubmission:!1,hash:"588466f487e307619849d72389178a74",slug:"abiotic-stress-in-plants-mechanisms-and-adaptations",bookSignature:"Arun Shanker and B. 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"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"39988",title:"New Perspectives for Magnetic Fluid-Based Devices Using Novel Ionic Liquids as Carriers",doi:"10.5772/51398",slug:"new-perspectives-for-magnetic-fluid-based-devices-using-novel-ionic-liquids-as-carriers",body:'Magnetic materials, that is to say, materials which respond to external magnetic fields, have attracted great interest since around 5th century BC. The ability of materials such as iron or magnetite to be attracted by permanent magnets has always involved some kind of mystery, although magnetism principles are well understood nowadays, especially after J.C. Maxwell stated the basis of electromagnetism in 1865. Magnetism plays a crucial role in our lives these days, being present in many technological applications surrounding us. Nevertheless, only solid magnetic materials can be found in nature. In the search for new ones that could be used in novel technological applications, scientists in the 18th centurytried to prepare field-responsive liquids by dispersing particles of magnetic materials in liquid carriers. Actually,the first attempt can be attributed to G. Knight (1779), who suspended iron filings in waterthat quickly settled (Popplewell, 1984). The preparation of magnetic fluids has undergonegreat development since then, and magnetic fluids with particles of different nature, size or shape and a wide range of liquid carriers have been reported in the literature.
In this chapter an overview of magnetic fluids and their applications is made, focusing on the latest developments in the field. More specifically, the use of novel ionic liquids as carrier fluids is described. The interest in doing so lies in the fact that ionic liquids may give rise to a new generation of magnetic fluids with promising technological applications.
As it has been pointed out above, the term “magnetic fluids” (MFs) is used to describe a group of smart materials whose properties can be controlled by means of external magnetic fields. They all are suspensions of magnetisable particles dispersed in a liquid carrier. Basically, two kinds of MFs can be defined according to the size of the dispersed phase: magnetorheological fluids (MRFs) and ferrofluids (FFs).
MRFs consist of micron-sized ferro- or ferrimagnetic particles dispersed in a liquid carrier. Traditionally, organic solvents such as kerosene or mineral oil are used as carriers. With regards to the dispersed particles, they can be considered as multi-domain from the magnetic viewpoint, since their size is much higher than the one of a single magnetic domain for the constituent material in question (Bossis et al., 2002). For example, typical MRFs can be composed ofiron particles with diameters around 1 μm, while the size of one magnetic domain in this material is approximately 30 nm (Herpin, 1968). As a result, MRFs strongly respond to external magnetic fields, giving rise to considerable changes in their flow (rheological) behaviour. More specifically, they behave as Newtonian fluids in the absence of magnetic field application, while their behaviour becomes that of a non-Newtonian plastic fluid when a magnetic field is applied. In this latter case, the MRF only flows when the shear stress applied to the suspension overcomes a finite value, the so-called yield stress. Therefore, it could be said that their rheological behaviour changes from a liquid-like to a solid-like one due to the application of external fields. This change, known as magnetorheological (MR) effect is a consequence of the formation of magnetically-induced structures by the dispersed particles, that have to be broken by the hydrodynamic forces to make the suspension flow (Bossis et al., 2002). Figure 1 shows typical MRF rheograms (shear stress vs. shear rate curves) both in the absence of and upon magnetic field application; the appearance of the yield stress (σy) can be clearly observed. The field-induced structures and their evolution as the shear rate is increased are schematized too.
Rheograms for a MRF consisting of 30 vol % of iron microparticles in mineral oil at magnetic field strengths (H) of 0 and 250 kA/m (circles andsquares respectively). The evolution of the field-induced structures is showed.
The strong magnetic interaction between the dispersed particles in MRFs, responsible for the MR effect, has its disadvantages too. Actually, it makes them agglomerate and settle down if no stabilizing additives are used. Since complete avoidance of sedimentation in MRFs is almost impossible, the efforts in formulation have focused on trying to reduce it and making particle redispersion easy. Different additives such as surfactants (oleic acid,lecithin, aluminum stearate) or thixotropic agents (organoclay particles) have been used for this purpose (de Vicente et al., 2003; López-López et al., 2005a, 2008).
FFs, on the other hand, are ultrastable suspensions of magnetic nanoparticles (size around 10 nm) dispersed in a liquid carrier. From the magnetic point of view, these particles are single-domain and therefore, FFs behave as superparamagnetic systems (Charles, 2002; Rosensweig, 1985). The term superparamagnetism is used to describe the magnetic behaviour of systems that exhibit high saturation magnetization values (i.e. typical of ferromagnetic materials),and no magnetic remanenceor hysteresis as it happens in paramagnetic materials. FFs only undergo slight changes of viscosity in the presence of external magnetic fields. This phenomenon, known as magnetoviscous (MV) effect is very interesting from the technological viewpoint (Odenbach et al., 2002).
Nevertheless, the most important feature related to FFs is their so-called ultrastability: ideally, true FFs should not settle either when subjected to strong magnetic field gradients or in the presence of gravitational forces during their lifetime (Rosensweig, 1985). As a result, they really behave as magnetic liquids, since no phase separation appears. Figure 2 shows how a FF climbs the tube walls in order to move towards the zones where the magnetic field provided by the magnet is higher.
FF (5 vol % of magnetite) subjected to magnetic field application by a powerful rare-earth magnet. It can be seen that the liquid moves as a whole towards the zone where the field is more intense.
Ultrastability in FFs is usually achieved as follows (Charles, 2002; Rosensweig, 1985): (i) particle size is low enough so that Brownian motion prevents from possible particle aggregation induced by the magnetic interaction between the particles; (ii) particle aggregation by means of van der Waals attraction (short range forces) must also be avoided by imposingsome kind of repulsion between the particles. Such repulsion is usually obtained by adsorbing surfactants or polymerson the surface of the particles, and thus providing with a strong enough barrier (steric repulsion) to overcome van der Waals interactions.In polar media (i.e. water-based FFs), this can be alternatively achieved by electrostatic repulsion between the particles derived from their surface charge (Charles, 2002; Rosensweig, 1985).
The efforts made in order to improve MFs in terms of stability, durability, MR andMV effects have led to the development of a new generation of MFs. This group would include inverse FFs, bimodal suspensions, and MRFs consisting of anisotropic particles. In the first case, non-magnetic microparticles are dispersed in a concentrated enough FF. These particles behave as non-magnetic holes in apractically continuous magnetic medium, and, as a result,are able to orientate and form magnetic structures when a magnetic field is applied (figure 3). This sort of MR effect is stronger than in the case of FFs, but it is still far from that of MRFs (de Gans et al., 1999; Ramos et al., 2011).
Microscopic picture upon magnetic field application of an inverse FF consisting of PMMA microparticles dispersed in a FF (5 vol % of magnetite in mineral oil). It can be seen that the non-magnetic particles (white spots) form chains in the direction of the magnetic field. Bar length: 100 μm.
In the case of bimodal suspensions, micron-sized particles are again dispersed in a FF, but this time, the dispersed particles are magnetic. These MFs have proved to be more stable against sedimentation than conventional MRFs due to the stabilization achieved by the formation of nanoparticle clouds around each micron-sized particle. The formation of such clouds can be observed in figure 4(López-López et al., 2005b, 2006, 2010).
Finally, the anisotropic nature of fibrillar particles leads to an increase of the MR effect in MRFs consisting of them (Kuzhir et al., 2009; López-López et al., 2007, 2009, 2012). Figure 5 shows magnetic fibrillar particles, with a longitudinal axis of about 50 nm, which have been used in the preparation of stable FFs.
Optical microscope picture of a diluted bimodal suspensionconsisting of ferromagnetic microparticles dispersed in a FF. Note the halo around each microparticle formed by the magnetite nanoparticles of the FF carrier. Bar length: 20 μm.
High resolution TEM image of CoNifibrillar particles for the preparation of MFs. Bar length: 50 nm.
The possibility of controlling the physical properties of MFs by external magnetic fields makes them versatile smart materials that can be employed in numerous technological applications, ranging from fields as different as civil and mechanical engineering, aerospace, biomedicine or optics (Carlson et al., 1996; Durán et al., 2007; Jeong et al., 2007; Jolly et al., 1999; Klingenberg, 2001; Park et al., 2010; Popplewell, 1984; Raj et al., 1990; Tran et al., 2010).
The best known application for MRFs is their useas lubricants with field-dependent viscoelasticity in shock absorbers or dampers. It was in the early 1990s when Lord Corporation
The technological applications of MR dampers are not only restricted to vehicles. For example they are also used as shock/vibration absorbers in structures (i.e. seismic control of buildings or bridges). In this particular case, the stability against sedimentation plays a very important role, since the damper is expected to remain inactive most of its lifetime (Jolly et al., 1999; Klingenberg, 2001; Park et al., 2010). In addition, MR shock absorbers can also be used in semi-active human prosthetic legs.
In the case of FFs, many biomedical applications have been described, which take advantage not only of their superparamagnetic behaviour, but also of their high surface-volume ratio, high reactivity, etc. Medical applications includecell labeling and targeting, separation and purification of cell populations, tissue repair, targeted drug delivery, magnetic resonance imaging or hyperthermia for cancer treatment (Durán et al., 2007; Tran et al., 2010). In all these applications biocompatibility and non-toxicity are of crucial importance. For this reason, iron oxides are preferred as the material for the dispersed phase and, in addition, they are often made biocompatible by means of surface coating by polymers (PEG, dextran, polyvinyl alcohol) or functional groups (thiols, amines, and carboxyls). All these additives prevent from particle aggregation too, which should be almost completely avoided so that particle size does not increase (Tran et al., 2010).
From a more engineering point of view, the control of both the position and the physicochemical properties of FFs by using magnets or solenoids makes them very interesting too. In fact, FFs have been used as lubricants, heat transfer agents or integrated in devices such as dynamic seals, dampers, magnetic inkjets or optic devices. As an example, companies like Ferrotec
Sketch of a FF-based seal. Reprinted fromJournal of Magnetism and Magnetic Materials, 85/1-3, K. Raj and R. Moskowitz, Commercial applications of ferrofluids, 233-245, Copyright (1990), with permission from Elsevier.
Finally, as it has been pointed out above, FFs can also be used as heat transfer materials, provided that their thermal conductivity increases when applying a magnetic fieldin a directionparallel to the temperature gradient. In this way,magnetically-induced particle chains, able to transfer heat by conduction, are formed in the field direction. When the field is removed, thermal conductivity reaches its original value (Shima et al., 2011). This working principle is used to dissipate heat from devices such as high power loudspeakers. In this application, the use of FFs has additional advantages like the absorption of undesirable vibrations and avoiding resonances without disturbing the quality of the sound (due to their liquid condition), or the possibility of fixing their position by magnets (as it happens in dynamic seals)(Popplewell, 1984; Raj et al., 1990).
All the applications mentioned in this section are quite well known, and some of them have already been developed at the industrial scale. However, it is quite clear that the range of technological applications of MFs will expand as progress in their dynamics and preparation is made.
Traditionally, organic carriers (mineral oil, kerosene, etc.) have been used in the preparation of MFs, although in some cases (i.e. medical applications) water-based MFs are needed too. These conventional MFs have proved to be useful for many applications as pointed out above. However, the use of novel ionic liquids (ILs) as carriers may promote further improvements in the performance of MFs, especially in ultra-high vacuum applications, in which organic solvents would easily evaporate. But the preparation of IL-based MFs is not only interesting from an applied, technological approach, but also from the fundamental one. For example, their use as carriers allows studying phenomena involving MFs in environmental conditions that conventional carriers would not withstand. But, what are ILs and why do they appear as promising candidates in the preparation of MFs? These and other questions are discussed in next sections.
ILs are substances composed entirely of ions that are liquids at room temperature (Endes et al., 2008). While common salts, such as table salt (i.e. sodium chloride), have melting points around 800 °C, the upper limit for the meltingpoint so that they can be classified as ILs is usually set at 100 °C. Therefore, they can be considered as room-temperature molten salts (Keskin et al., 2007). Such behaviour is obviously related to their chemical composition: ILs are usually composed of bulky and asymmetricorganic cations and smaller inorganic or organic anions. This feature makes their lattice energy quite lowand, therefore, so does their melting point (Keskin et al., 2007). There are many of them depending on their chemical composition, but almost every IL can be classified, according to its cationic structure, into one of the seven families reported by Torimoto et al. (Torimoto et al., 2010).
Connected to their composition, one of the most interesting properties concerning ILs is their tunability. As a matter of fact, by changing the nature of the constituent ions it is possible to obtain ILs with very different physical and chemical properties (Endes et al., 2008). Theoretically, the combination of cations and anions would lead to a number of ILs as high as 1018(Chiappe et al., 2005). In practice, however, this number would be much smaller, but it gives an idea about the broad range of physicochemical properties that can be obtained. For instance, ILs with the same imidazoliumcation, [BuMeIm][1] -, can be either hydrophilic (combined with [BF4] or [AlCl4]) or hydrophobic (if the anion is [PF6] or [Tf2N]) (Torimoto et al., 2010). Here it is worth mentioning the fact that some ILs with magnetic properties have also been prepared by using [FeCl4] anions.Tunability is especially interesting in the case of MFs, since it would allow synthesizing tailor-made MFs specifically designed for every single application.
Nevertheless, there are two common features for many of them that are ratherinteresting from the technological viewpoint. These are their negligible vapour pressure and flammability, at least when compared to those of conventional solvents such as volatile organic compounds (VOCs). Both characteristics ensure, first of all, thermal stability and vacuum resistance and, what is more, aninsignificant contribution to air pollution. As a matter of fact, they have been labelled as “green solvents” due to their negligible impact on atmospheric pollution (Keskin et al., 2007; Torimoto et al., 2010). Finally, it is possible to recycle them, which would contribute to reduce their release to the aquatic environment and lead to more efficient and economic industrial processes (Haerens et al., 2010; Wu et al., 2009).
Since the academic world began to become interested in ILs in the 1990s, the number of scientific articles and patents related to the topic has incredibly increased. For example, in 2000 about 100 patent applications had been reported, while in 2004 this number increased to 800 (Keskin et al., 2007). Nowadays, about 28200 patents related to ILs can be described.
Some applications arise from the fact that many ILs are powerful solvents,able to dissolve salts, fats, proteins, amino acids, surfactants or sugars. For instance, [(MeOEt)MeIm][BF4] can dissolve glucose 100 times better than acetone (Park et al., 2001). They caneven dissolve crude oil, inks, plastics or DNA. For this reason, they can be used as reaction media for electrochemical and chemical syntheses (Torimoto et al., 2010), giving rise to reaction rates similar or even better than those obtainedwhen usingaqueous or organic solvents. Another advantage of using them with this aim is the ease in recovering the resulting products from the reaction medium, especially in those cases in which distillation is not practical,for example, because the reaction products are thermally sensible(Keskin et al., 2007).In addition, it has been reported that ILs can be used as solvents for insoluble bio-related materials like cellulose, which is easily dissolved by strong hydrogen bond-acceptor ILs (like chloride anion-based ones) (Keskin et al., 2007; Torimoto et al., 2010).
Another typical application is their use in gas purification because many gases are soluble in ILs (for example CO2 is highly soluble in [BuMeIm][PF6]) (Anthony et al., 2002). This feature also makes them excellent candidates to be employed in gas absorption applications, together with the fact that gas separation from the IL stream would be very easy (i.e. by simple flash distillation) (Keskin et al., 2007).
Related to materials science, ILs have been widely used in chemical synthesis of nanoparticles, with self-evident advantages like the fact that almost no stabilizing agents that prevent from particle coalescence are needed (requisite almost indispensable in the case of aqueous or organic solvents) (Torimoto et al., 2010). For example, it is possible to synthesize particles for the preparation of MFs such as magnetite (Wang et al., 2009) or cobalt (Behrens et al., 2012) nanoparticles. This would allow an in situ synthesis of the dispersed particles.
As a final point, the preparation of IL-based MFs would allow the use of some of the devices mentioned in section 3under extreme environmental conditions (ultra-high vacuum or high temperature applications).This would be particularly interesting in the case of space technology such as dampers, dynamic seals or hydrodynamic bearings in gyroscopes for mini-satellites. As a matter of fact, the first MF patent was aimed to prepare controlling fluids for space applications (Papell, 1965).
In this section the research highlights in the field of IL-based MFs are described both in the case of MRFs and FFs. Some details about our group contributions to the field are given too.
Guerrero-Sánchez et al. (Guerrero-Sánchez et al., 2007) were pioneersin the preparation of IL-based MRFs. More specifically, they prepared several suspensions consisting of either micron- or nanosized magnetite particles dispersed in eight different ILs. The most stable MRF was obtained for a composition of 10 vol % of magnetite microparticles suspended in [BuMeIm][PF6]. As a matter of fact, this MRF only exhibited a sedimentation ratio of 0.95 after two months of preparation. Having prepared a highly stable IL-based MRF was important, but even more important was the fact that colloidal stability was achieved without the addition of any stabilizing agents. The enhancement of stability was attributed to the physical adsorption of the IL ions on magnetite surface (for which they had strong affinity) that gave rise to steric repulsion between the dispersed particles. In the same work, the rheological behaviour of the samples upon magnetic field application was also studied concluding that the MR effect of the IL-based MRFs was comparable to those obtained for conventional MRFs, and high enough for practical purposes.
In a different work, Guerrero-Sánchez et al. (Guerrero-Sánchez et al., 2009) also used IL-based MRFs to study the influence of temperature on their MR behaviour. Here, ILs allowedextendingsuch study to a broader range of temperature than in the case of conventional MRFs, due to their thermal stability and low vapour pressure. Something similar was pointed out by Dodbiba et al. (Dodbiba et al., 2007) who also took advantage of the good performance of ILs at high temperature to study the rheological behaviour upon magnetic field application of a mixture of two types of carbonyl iron powders dispersed in an IL. Therefore, these works make evident that the preparation of IL-based MFs is important from the fundamental point of view too.
Our group has also studied IL-based MRFs, especially for what concerns their stability. With this aim, Gómez-Ramírez et al. (Gómez-Ramírez et al., 2011) prepared IL-based MRFs differing both in the disperse phase material (pure iron and silica-coated iron particles) and in the liquid carrier ([EtMeIm][EtOSO3] and ([EtMeIm][Et2OPO3]). Additionally, conventional MRFs with mineral oil as liquid carrier were also synthesized. The particle volume fraction of all the samples was kept as 10 vol %. The most stable MRF was obtained by the combination of silica-coated iron particles and [EtMeIm][Et2OPO3]; for example, the viscosity of such MRF for shear rates over 100 s-1 almost coincided with the theoretical predictionof Batchelor equation, what means that only two-body hydrodynamic interactions existed between the particles, and, therefore, almost no magnetic aggregates were present. In fact, microscopic observations of the suspensions upon magnetic field application showed that field-induced particle chains had a more regularstructure in the case of the most stable MRF (see figure 7). The worst results were obtained for mineral oil-based MRFs in which the particles were strongly aggregated and the resulting structures became more irregular. An intermediate behaviour was found for the suspensions with [EtMeIm][EtOSO3] as liquid carrier.
Field-induced particle structures in MRFs consisting of silica-coated iron microparticles dispersed in [EtMeIm][Et2OPO3] (a) and mineral oil (b). Bar length: 200 μm.
The improvement of MRF stability when using ILs as carriers, with respect to the ones prepared in mineral oil, was also explained by the adsorption of the IL ions on the surface of the dispersed particles. In a first approximation, such stability appears to be related to the electric conductivity of ILs, which, on its part, is also connected to the anion volume, being the first lower when the latter increases. Accordingly, if the adsorbed ions are larger, the steric repulsion between the particles is stronger too, leading to a decrease in particle aggregation.This is the reason for which a low conductivity-IL like [EtMeIm][Et2OPO3] gave rise to better results than the high conductivity-one [EtMeIm][EtOSO3]. The explanation for the higher stability in the case of MRFs consisting of silica-coated iron particles was the interaction between silica and the constituentIL ions. In fact, the wettability of both ILs was better in the case of silica-coated iron than for bare iron (Gómez-Ramírez et al. 2011).
The direct consequence of the improved stability of IL-based MRFs is a simpler MRF formulation, since no stabilizing additives are needed. This makes easier their preparation at larger scale given that no additional mixing steps are needed, for example. Therefore, stable MRFs with adequate MR response that can be subjected to ultra-high vacuum or very high/low temperatures are obtained, just by using ILs as carrier fluids.
As it has been pointed out above, one of the advantages of using ILs as carriers is the stability that the physical adsorption of their constituent ions provides with. In the case of MRFs it has been seen that this improvement may be good enough for practical purposes. But what happens in the case of FFs that, by definition, need to be ultrastable? What are the mechanisms involved in the stabilization of IL-based FFs?
The first reference to IL-based FFs appeared in 2009, when Oliveira et al. prepared suspensions of bare maghemite(γ-Fe2O3) and cobalt ferrite (CoFe2O4) nanoparticles dispersed in [BuMeIm][BF4] (Oliveira et al., 2009). Such suspensions were said to be stable in the presence of an external magnetic field, even without the addition of stabilizing agents. The authors attributed such stability to the formation of a semi-organized protective layer by the IL ions around the dispersed particles. Nevertheless, when water was added to the suspensions, they became completely unstable, apparently due to the destruction of such a protective layer. The authors also tried to prepare suspensions using hydrophobic ILs (namely [BuMeIm][PF6] and [BuMeIm][Tf2N]), but these suspensions were not stable at all.
Jain et al. (Jain et al., 2011) also attempted to synthesize IL-based FFs using maghemite nanoparticles, but with particle concentrations much higher than in the case of Oliveira et al. They succeed when using [EtMeIm][Ac] and [EtMeIm][SCN] as carriers, without needing any stabilizers, but they did not in the case of the protic IL [EtN][NO3] and [BuMeIm][BF4]. In the latter case, they failed even at lower concentrations in contrast with the results of Oliveira et al. As a matter of fact, there is still some controversy related to the stabilization of bare magnetic nanoparticles in IL media, although the stabilization provided by the IL ions has been pointed out to work quite well for metal nanoparticles in general (Pârvulescu et al., 2007). This is the case of positively charged Pt nanoparticles dispersed in [BuMeIm][BF4]and [BuMeIm][PF6],for example (Scheeren et al., 2006). However, in some other cases it is not high enough, and additional stabilization is needed (Pârvulescu et al., 2007; Torimoto et al., 2010).
In most of the suspensions mentioned above, the material for the dispersed phase is maghemite. At this point it is important to mention that both Guerrero-Sánchez et al. (Guerrero-Sánchez et al., 2007) and Oliveira et al. (Oliveira et al., 2009) failed to synthesize ultrastableIL-based suspensions when using magnetite (Fe3O4) nanoparticles. [BuMeIm][BF4] that, according to Oliveira et al., had given rise to good results for maghemiteand cobalt ferrite, did not work at all in the case of magnetite. This could be due to the fact that magnetic interaction between magnetite nanoparticles is higher than in the case of maghemiteones, since the saturation magnetization of the first (90 Am2kg-1) is higher than the one of the latter (80 Am2kg-1). Given that both iron oxide surfaces must be composed of the same Fe-OH groups, the formation of the protective layer around magnetite nanoparticles could have taken place, but probably was not protective enough to overcome the magnetic attraction between the particles. An additional stabilization mechanism seemed to be needed.
In 2011 our group reported a true IL-based magnetite FF (Rodríguez-Arco et al., 2011a). In this work, emphasis was made in the fact that only strong steric repulsion was useful to obtain an ultrastable suspension of magnetite in [EtMeIm][EtOSO3]. This was achieved by adsorbing surfactants with long tails on the surface of magnetite nanoparticles that gave rise to such strong steric repulsion (more details about this IL-based FF are given below). In fact, we also tried to prepare suspensions of bare magnetite nanoparticles in the same IL and failed. Later, something similar was pointed out by Jain et al., who observed that bare maghemite nanoparticles were unstable in the protic IL [EtN][NO3], but they became highly stable (even at highly particle concentration) when coated by a layer of short acrylic-acid-b-acrylamide copolymer (Jain et al., 2012). As a result, steric repulsion seems to be the best stabilization mechanism for the preparation of IL-based FFs.
In view of the results presented above a question may arise: how can we explain that in some cases stabilization is ensured without the addition of stabilizing agents (i.e. surfactants) while in others it is strictly necessary? Here, it is particularly interesting to mention the work by Ueno et al. in which they prepared suspensions of bare and PMMA-grafted silica particles dispersed in imidazolium-based ILs (Ueno et al., 2008). Given that ILs are non-volatile, the in situbehaviour of these suspensions was studied by means of transmission electron microscopy (i.e. no escapes of the liquid to the vacuum system took place). They observed that strong aggregation, which appeared for bare silica particles, was almost absent in the case of PMMA-grafted ones (figure 8). They concluded that electrostatic repulsion, that was the only possible stabilization mechanism in the case of bare silica, did not work. They attributed this to the screening effect of the high ionic atmosphere surrounding the particles, since ILs are actually room-temperature molten salts. They also corroboratedsuch affirmation by estimating the interaction potential energy between the dispersed particles and checking that the electrostatic repulsion component was negligible when compared with the steric repulsion one (Ueno et al., 2008).
In situ TEM picture of dilute suspensions of bare (a) and PMMA-grafted (b) silica particles in [EtMeIm][Tf2N]. Reprinted (adapted) with permission from (Ueno et al., 2008). Copyright (2008) American Chemical Society.
If the results of Ueno et al. (Ueno et al., 2008, 2009) are taken into account, there are two points that seem clear: (i) electrostatic repulsion does not work in IL media because of the highly ionic environment; (ii) only steric repulsion gives rise to long-term stability. On its part, the protective layers formed by the adsorption of the IL ions (i.e. physically or by coordination compounds) could provide with steric repulsion. However, in some cases (as for magnetite suspensions), it is not strong enough to ensure long-term stability and other additives (i.e. surfactants) have to be used.
As it has been pointed out above, our group succeeded in the preparation of true magnetite IL-based FFs. This was only achieved when the surface of the particles was coated with some stabilizing agents, but not all additives worked (Rodríguez-Arco et al., 2011b). For example, citric acid, that had been previously used to stabilize water-based FFs, did not work properly in [EtMeIm][EtOSO3], since the samples consisting of citric acid-coated magnetite slightly settled when subjected to a magnetic field gradient of 10 mTmm-1, and gave rise to strong phase separation after 5 min of centrifugation at 8000g. This was due to the fact that citric acid molecule is very short and, therefore, the resulting steric repulsion was quite weak. As a consequence, it seems that only long enough molecules should be used.
In addition, compatibility between the tails of the surfactant and every particular IL must exist. For example, if magnetite particles were just coated with a single layer of oleic acid, the resulting suspension was as unstable as those consisting of bare magnetite. Nevertheless, if a second layer of oleic acid molecules was formed when an excess of oleic acid was added, a true IL-based FF was obtained. The ultrastability of such FF was accurately proved, since it did not settleeither upon magnetic field gradient application or after 30 min of centrifugation at 8000g. The differences between both particle coatings can be easily observed in figure 9.
It can be seen that the tails facing the IL in figure 9a are non-polar, while the situation is just the opposite when the oleic acid-double layer is formed (figure 9b). In the first case, there is not compatibility between the surfactant tails and the IL (highly polar), whereas in the second one there is. As it has been previously pointed out, Jain et al.(Jain et al., 2012) were able to stabilize maghemite nanoparticles in [EtN][NO3] by coating them by a layer of short acrylic-acid-b-acrylamide copolymer; however, they were not in the case of [BuMeIm][BF4] and [EtMeIm][SCN] just because the polyacrylamide block of the acrylic-acid-b-acrylamide copolymer is not soluble in these ILs, and therefore, no compatibility exists. Therefore, as it has beensaid above, the best way to ensure long-term stability is the use of surfactants with long enough, carrier liquid-compatible tails adsorbed on the surface of magnetite nanoparticles.
Monolayer of oleic acid molecules adsorbed on the surface of magnetite nanoparticles (a). Oleic acid-double layer formed when adding an excess of oleic acid (b).
Finally, some results about the rheological behaviour upon magnetic field of the samples mentioned above are shown (Rodríguez-Arco et al., 2011b). In particular, figure 10 shows the yield stress obtained for all of them.
Yield stress for IL-based suspensions consisting of bare (triangles), citric acid-coated (circles) and oleic acid-double layer-coated (squares) magnetite. Full and open squares correspond to this latter sample before and after centrifugation respectively (see text).
With regards to the results presented in figure 10 it is important to remind that, theoretically, a true FF should not display considerable yield stresses, since its response to magnetic field is too weak for this to happen. However, in the case of the suspension of bare magnetite, the yield stress is quite high, likely due to the strong particle aggregation, and therefore, to the formation of field-induced structures by the aggregates. When the particles are coated by citric acid, the aggregation degree decreases, and so does the yield stress. In the case of the oleic acid-double layer two different situations appear. The first one corresponds to the original sample, which displays similar values (a little bit lower) than the sample of citric acid-coated magnetite. However, when this sample is subjected to centrifugation, although the supernatant itself is still magnetic, the yield stress of the supernatant becomes negligible. This can be explained because particle aggregates that could be present in the original sample wereremoved by centrifugation. Similar results were found for the MV effect (Rodríguez-Arco et al., 2011b). In fact, the MV response of these new IL-based MFs was theoretically fitted by a model that was originally proposed by Zubarevet al. (Zubarev et al., 2005) for oil-based FFs, showing that the MV effect increases with both the volume of the largest particles and their concentration and when the distancebetween the magnetic cores of the particles decreases.
In conclusion, it could be said that much work is being done in the field of IL-based FFs. Thanks to such studies our understanding of the phenomena involving them (i.e. stability) is improving, and it is very likely that better IL-based FFs will be prepared in the future. However, more applied studies are needed, which, for example, analyze their real performance in technological devices like those of section 3.
Many of the future challenges in the field of IL-based MFs are related to ILs in general. One of the most important disadvantages of ILs, for instance, is their cost, that can be much higher than that of conventional organic solvents. However, in some specific applications, it is probably worth using them (i.e. space applications). Nevertheless, their price will decrease if they begin to be produced at a larger scale.
Another disadvantage of ILs when compared with traditional carriers is the lack of enough data about their physicochemical properties and toxicity (Keskin et al., 2007). In the same direction, a thorough analysis of the relationship(e.g. adsorption, wettability) between the particle surface and the constituent ions in MFs would be of the utmost importance,in order to gain a better understanding of the stability mechanisms.
Since ILs could be used to preparetailor-made MFs for each specific application, it would be interesting to broaden their preparation by changing the IL carrier, the nature of the dispersed phase or its concentration. But before this is accomplished, it is necessary to determine which solid materials (or surfactants in the case of FFs) fit best each particular IL. As a result, deeper studies on the compatibility among all the MF constituents may be needed in the future. Additionally, further research has to be done, not only with regards to the formulation of IL-based MFs, but also to their performance in each particular application. As a consequence, detailed magnetization and magnetorheological studies should be faced too.
The final step for IL-based MFs would need a much more applied study which could result in a number of patents susceptible of being exploited. For example, they should be included in prototypes before developing any industrial device. This would allow additional industrial implementation and commercialization of this new breed of MFs. Here it is worth mentioning the work by companies like Ioniqa Technologies
In this book chapter an overview of the latest advances and research highlights in the field of MFs has been done, especially concerning the use of room-temperature ILs as fluid carriers. As it has been described, there are numerous MF applications that could benefit from IL features such as low flammability, negligible vapor pressure and tunability. However, although a lot of work has been done, there are still problems that have to be overcome if a wider commercialization of IL-based MFs is desired. Therefore, these new horizons broadened by their potential uses are, at the same time, encouraging and challenging.
AppendixHere we list the IL nomenclature abbreviations used in the chapter.
Cations | [EtMeIm] | 1-ethyl-3-methylimidazolium |
[BuMeIm] | 1-butyl-3-methylimidazolium | |
[(MeOEt)MeIm] | 1-methoxyethyl-3-methylimidazolium | |
[EtN] | Ethylammonium | |
Anions | [Ac] | Acetate |
[Tf2N] | Bis(trifluoromethylsulfonyl) imide | |
[Et2OPO3] | Diethylphosphate | |
[EtOSO3] | Ethylsulphate | |
[PF6] | Hexafluoroborate | |
[NO3] | Nitrate | |
[AlCl4] | Tetrachloroaluminate | |
[FeCl4] | Tetrachloroferrate | |
[BF4] | Tetrafluoroborate |
This work is supported by projects P08-FQM-3993 andP09-FQM-4787 (Junta de Andalucía, Spain) and FIS2009-07321 (MICINN, Spain). L.R.-A. and M.T.L.-L.also acknowledge financial support by the Secretaría de Estado de Educación, FormaciónProfesional y Universidades (MECD, Spain) through its FPU Program and University of Granada (Spain), respectively.
Human evolutionary studies or paleoanthropological research are constantly yielding new information and thus revising previously assumed hypotheses as well as generating new ones. While Africa and Europe have dominated the bulk of our knowledge on human evolution over the last century, various parts of Asia are yielding new and unexpected paleoanthropological surprises. One of these vital Asian regions is South Asia or the Indian Subcontinent, its prehistory being known and regularly highlighted since the nineteenth century [1] and predominantly includes stone tool assemblages from various time periods ranging from the Lower Paleolithic to the Neolithic [2]. Prehistoric evidence is known from throughout the Subcontinent with specific geographic pockets as being exceptions due to various factors including research bias as well as other natural attributes. Lithic assemblages belonging to all prehistoric phases have been reported including Lower Paleolithic (Oldowan and Acheulean), Middle Paleolithic, Upper Paleolithic and microlithic/Mesolithic. Despite this large body of known evidence, very few sites have been properly dated using absolute dating techniques. The earlier results, though obtained through different dating methods [3, 4], should be viewed as provisional until verified by newly-available dating techniques. For example, some U-Th dates (between <390 Ka and < 131 Ka) processed a few decades ago at a multi-period site in Rajasthan have now been revised to younger estimates using the luminescence method e.g. [5], leading to a re-interpretation of that cultural sequence [6]. The persistent marginal profile of hominin fossils continues to afflict Indian prehistory and more systematic surveys are required to identify new areas with vertebrate fossil preservation. The only known pre-modern hominin fossils in the subcontinent, which may be contemporary with the Late or terminal Acheulean phase, come from Hathnora and nearby localities in the central Narmada Valley. They include a partial calvarium, possibly female, and possibly associated clavicles and a rib fragment, all recovered over a decade [7, 8]. The calvarium, originally identified as an “advanced” Homo erectus, was later reclassified as an archaic or early form of H. sapiens [9, 10]. Phylogenetic reevaluation of the calvarium reveals that it shares key morphological features with both H. heidelbergensis and H. erectus [11]; it has been most recently classified as Homo sp. indet. [12]. The oldest fossil evidence for Homo sapiens is dated to ~38 Ka and currently comes from Sri Lanka, while all younger evidence comes from multiple sites across India [13, 14].
What is also largely missing is direct evidence for butchery in the form of cut-marked fossil bones; some possible exceptions include Isampur [15] and Masol [16], both of which require further verification and substantiation through more evidence. Additionally, use-wear analyses and other scientific methods such as residue analysis are also required on well-preserved lithic assemblages. Other types of evidence that are poorly known is the age and nature of symbolic behavior (see [17]) as well as the nature of technological transitions. Indeed, there has been a recent global movement to decolonize earlier interpretations of hominin dispersals and population replacements across the Old World [18]. This also includes India, where earlier historical interpretations defined the Upper Paleolithic and modern human behavior based on the then-known European evidence [19]. Numerous reviews of the South Asian region’s prehistoric records have been published elsewhere (e.g. [3, 4, 20, 21, 22, 23, 24, 25, 26, 27, 28]). Over three dozen Paleolithic and early microlithic sites have been dated in Pakistan [29, 30, 31, 32, 33], India [5, 14, 16, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58], Nepal [59] and Sri Lanka [60, 61, 62, 63] since the 1980s onwards, using different relative and absolute dating methods including biochronology, palaeomagnetism, stratigraphic correlation, U-Th, U-series, K-Ar, Ar-Ar, luminescence, electron spin resonance, radiocarbon (calibrated and uncalibrated) and AMS. These various ages range from ~2.6 Ma to ~35 Ka, and include geographically random sites belonging to various prehistoric technologies including Oldowan-like, Acheulean, Middle Paleolithic, Upper Paleolithic and the earliest microlithic assemblages (Figure 1 and Table 1). While broad summaries are provided here, the primary goal of this paper is to highlight the most salient attributes of this zone, provide specific updates to previously known data and discuss possible implications of new discoveries from surrounding regions outside the Subcontinent.
Map of dated Paleolithic technologies across the Indian subcontinent including Pakistan, India, Nepal and Sri Lanka (LP: Lower Paleolithic; a: Acheulean; EA: Early Acheulean; LA: Late Acheulean; MP: Middle Paleolithic; UP: Upper Paleolithic; M: Microlithic; MC: Multi-cultural; OES: Ostrich eggshell).
Site | Age | Techno-chronology |
---|---|---|
Masol | 2.6 Ma? | pre-Acheulean |
Riwat (Pakistan) | ~2 Ma | Pre-Acheulean |
Pabbi Hills (Pakistan) | 2.2–0.9 Ma | Pre-Acheulean |
Attirampakkam | 1.5 Ma & 385–73 Ka | Acheulean & Middle Paleolithic |
Isampur | 1.27 Ma? | Acheulean |
Singi Talav | ~800 Ka? | Acheulean |
Dhansi | >780 Ka | Undiagnostic |
Morgaon | >780 Ka & 41 Ka | Acheulean |
Dina & Jalapur | ~700–400 Ka | Acheulean |
Chirki Nevasa | >350 Ka | Acheulean |
Sadab | 290 Ka | Acheulean |
Teggihalli | 287 Ka | Acheulean |
Umrethi | >190 Ka | Acheulean |
Kaldevanhalli | 174 Ka | Acheulean |
Patpara & Bamburi 1 | 140–120 Ka | Acheulean |
Bori | 1.38 Ma to 23 Ka | Acheulean |
Adi Chadi Wao | 190 to 69 Ka | Acheulean |
16R (Didwana) | 187 Ka - 6 Ka | Multi-period |
Sandhav | 114 Ka | Middle Paleolithic |
Bhimbetka Rockshelter III-F23 | >106 Ka & >41 Ka | Multi-period |
Nakjhar Khurd | >100 Ka | Acheulean |
Durkadi | <100 Ka | Multi-period |
Kataoti | 95 Ka | Middle Paleolithic |
Dhaba | 79–65 Ka & 48 Ka | Middle Paleolithic & microlithic |
Jwalapuram | 77–38 Ka & 35 Ka | Middle Paleolithic and microlithic |
Mehtakheri | 48 Ka | Microlithic |
Fa-Hien Lena (Sri Lanka) | 48 Ka | microlithic |
Kalpi | 45 Ka | Middle Paleolithic |
Site 55 (Pakistan) | 45 Ka | Upper Paleolithic |
Kitulgala beli-Lena (Sri Lanka) | 45 Ka | microlithic |
Sanghao Cave (Pakistan) | 42 Ka | Middle Paleolithic |
Kana | 42 Ka | Microlithic |
Batadomba Lena (Sri Lanka) | 36 Ka | microlithic |
Mahadebbera | 34 Ka | Microlithic |
Arjun 3 (Nepal) | >30 Ka? | Middle Paleolithic |
Patne | 30 Ka | Multi-period |
List of dated prehistoric sites in the Indian subcontinent.
Despite numerous efforts by several researchers such as Armand in central India [64] and the British Archeological Mission to Pakistan [33], the Oldowan has continued to remain elusive in India. Instead of unequivocally deriving from well-dated excavated contexts, almost all reported occurrences (n = 12) come from surface contexts or there are other contextual and geochronological issues associated with these finds [65]. Oldowan evidence has been reported from the Siwalik Hills in Pakistan and northern India as well as from the Narmada Basin in central India. The latest evidence, from Masol near Chandigarh, was reported by an Indo-French team and includes stone tools from excavated contexts and a possible-cut-marked fossil bone from surface context [16]. The researchers have provided an age estimate of 2.6 Ma for this material, however the contexts are disparate and the cut-marks are not properly verified [66] as they could have been produced from other processes also, such as animal teeth or fluvial transport prior to fossilization (e.g. [67]). The Lower Paleolithic of South Asia is basically dominated by (Large Flake) Acheulean assemblages that currently range in age from 1.5 Ma to 120 Ka [40, 57]. Acheulean sites are known to occur almost throughout the Subcontinent with some exceptions - the Gangetic plains, northeastern India and surrounding areas, Kerala, the extreme southern tip of India and Sri Lanka [4]– owing to various factors such as topography, geology, ecology, climate, high sea-levels and the absence of suitable raw materials. Acheulean assemblages variably include handaxes, cleavers, miscellaneous bifaces, picks, giant and small cores, polyhedrons, large and small flake blanks, flake tools such as scrapers and debitage at some primary-context factory sites (for examples, see Figures 2–7). The site with the oldest-known Acheulean evidence (Attirampakkam) also happens to preserve the oldest-known early Middle Paleolithic at 385 Ka [58]. This indicates that the full transition from the Lower Paleolithic to the Middle Paleolithic in South Asia was lengthy, geographically and chronologically uneven and behaviorally complex. This is evident from the lengthy overlap between the earliest Middle Paleolithic at Attirampakkam and the Late Acheulean dated to 140–120 Ka in the Son Valley of north-central India [40]. In addition, such a lengthy transition is making it difficult for archeologists to often separate terminal Acheulean assemblages from early Middle Paleolithic ones. For example, the Son Valley evidence was respectively classified as Middle Paleolithic and Late Acheulean by two different groups of researchers over time (see supplemental data in [58]). It is also possible that the specific hominin groups during this transition made and used different technologies in differing contexts for diverse functional purposes: e.g. assemblages with Late Acheulean handaxes for heavy-duty tasks verses Levallois dominated flake assemblages for light duty tasks, a hypothesis that can only be resolved through chronologically-targeted landscape archaeology.
Diverse handaxes, picks and trihedral elements from the Narmada Basin, Central India.
Handaxe and miscellaneous bifacial elements from Son Valley, north-central India (pic courtesy: Shashi Mehra).
Diverse cleavers from the site of Pilikarar in the central Narmada Basin.
Cleavers and cleaver-like flake blanks from the central Narmada Basin.
In situ or stratified handaxes in quaternary fluvial sections of the central Narmada Basin.
Find-spots of cleavers in surface context with diverse sedimentary types from the central Narmada Basin (pic courtesy: Vivek Singh).
Key issues that are yet to be properly understood for the South Asian Acheulean include the nature of change within this techno-chronological phase as well as understanding factors to understand regional variations in assemblage compositions, artifact and site densities, timings of regional transitions, some geographic absences of occurrence and lack of absolute ages for most of the stratified assemblages. Broader aspects that remain to be properly understood include the number and directions of Acheulean dispersals into and out of the Subcontinent, the hominin species that were associated with that technology and the diverse subsistence strategies that took place across the region. In addition, specific regions have ambiguous features for which factors are currently unclear: for instance, the Gujarat zone (westernmost India) has not yet yielded Early Acheulean sites and while Maharashtra has numerous Early Acheulean sites on Deccan Trap basalt, no Late Acheulean sites have yet been reported. While future surveys may refine such observations, we need to explore additional explanations for such discrepancies. For example, lack of assemblage burial during specific fluvial and depositional cycles and associated sub-aerial weathering processes may have affected assemblages with smaller basalt specimens than in the Early Acheulean (see [68, 69]). However, this explanation may not be equally applicable to the entire zone of Maharashtra – perhaps basalt was not deemed suitable for Late Acheulean hominins or populations shifted to other regions to target different raw materials such as quartzite, and so forth. Based on preliminary counts from compiled data, a minimum of 1560 Acheulean/Early Stone Age sites and site-complexes have been reported and there are major differences in the geographic patterns of occurrences.1 While one factor may be research bias (i.e. lack of surveys in some zones), broad observations may still hold for most regions despite future survey efforts. For example, the northern zone, northeastern zone and the southernmost tip of India have the least number of Acheulean sites totaling to 51. The remaining zones have yielded significantly higher numbers of sites, especially central, eastern and peninsular India; for example, compiled data for central India alone yielded 305 published Lower Paleolithic sites out of which 17 have been excavated [70]. The virtual lack of Lower Paleolithic sites in southern Tamil Nadu and Kerala suggests that Lower Paleolithic hominins may have never reached the southernmost Indian coastal tip; this fact, along with a probable lack of a land bridge, may explain why no Acheulean evidence is known from Sri Lanka. This may further suggest that hominins first entered Sri Lanka after about 100 Ka when large bifaces ceased being made throughout India. In any case, more intensive surveys are required in Sri Lanka to confirm a true absence as well as recover, excavate and date potential Middle and Upper Paleolithic sites [71].
Other key anomalies for the Lower Paleolithic include ‘missing contexts’ and ‘missing evidences’. For instance very few Early Pleistocene deposits, contexts and lithic assemblages have been identified south of the Siwalik Hills and the few known ones have been identified through limited but diverse methods such as palaeomagnetic dating, cosmogenic dating, electron spin resonance, associated stratigraphic correlation and microtremor readings [35, 50, 53, 57, 72, 73, 74, 75]. This is probably due to a multitude of factors including the lack of focused surveys, lack of geochrononological applications and geological processes which may have both deeply buried such contexts as well as destroyed them (e.g. cut-and-fill regimes). These may explain why legitimate or unequivocal Oldowan assemblages have yet to be discovered, excavated and dated. In the same vein, Middle Pleistocene contexts and sites have also not been adequately identified, primarily owing to the earlier lack of suitable geochronological methods. Reliable Middle Pleistocene dates have started to be reported only recently as some of the sites have been studied and known for many decades to yielded important stratified lithic assemblages: the multicultural sequence at the 16R dune at Didwana in Rajasthan [5] now dated to between ~187–6 Ka [5]2, the Late Acheulean occurrences of Patpara and Bamburi in the Son Valley in Madhya Pradesh dated to between 140 and 120 Ka [40] and multiple early and later Middle Paleolithic assemblages from Attirampakkam in Tamil Nadu dated to between 385 and 73 Ka [58]. However, despite these investigations as well as stratigraphically and geochronologically identifying some Middle Pleistocene sites and contexts, they have not yet yielded any vertebrate fossil material. This temporal and contextual pattern of fossil preservation also applies to the known Early Pleistocene sites in central and peninsular India [50] which have yet to yield adequate vertebrate fossil evidence. Some rare exceptions of vertebrate fossils found in contexts older than the Late Pleistocene in India include Isampur [15] and Attirampakkam in southern India ([76, 77]) and Dhansi in central India [44]. While the older contexts appear to be largely devoid of fossil preservation, it is highly probable that some or most of those older fossils have been redeposited in younger depositional contexts during landscape rejuvenation cycles. This probably also applies to some of the known fossil hominin material from the central Narmada Basin [7, 8] as associated mammalian teeth from Hathnora yielded variable absolute ages indicating chronologically-mixed fossils and probably artifacts as well [44]. Therefore, it is vital to date well-preserved vertebrate fossils directly using such methods as electron spin resonance and uranium-series, to obtain exact ages of the specimens rather than ages of their burial or minimum ages.
The early Middle Paleolithic appears to begin before 385 Ka [58] and is characterized by a gradual transition from large bifaces to small bifaces, before they disappear completely during the later Middle Paleolithic. In fact, the region allegedly preserves the youngest diminutive bifaces in the world (see [37, 78]), although this requires verification through more contextual and geochronological research across the Subcontinent as earlier U-Th dates need to be revised (e.g. [5]). The changing toolkit also includes the introduction of different reduction strategies and the emergence of prepared cores, points and blade elements (Figures 8 and 9). In fact, Middle Paleolithic points, which are first evident at 385 Ka at Attirampakkam, continue to occur in younger (Late Pleistocene) contexts as well [34, 36]. Late Pleistocene contexts and sites are more widespread but also remain inadequately dated. Recent examples of new and previously-known sites that were dated for the first time include Attirampakkam in Tamil Nadu where the later Middle Paleolithic ends at 73 Ka [58], Dhaba in Madhya Pradesh ([41, 79]), the Middle Paleolithic site of Sandhav in Gujarat [36] and Fa-Hien Lena in Sri Lanka [62]; the Sri Lankan evidence has been reported as the oldest known bow-and-arrow technology outside Africa at 48 Ka, making it contemporary with the microliths at Dhaba (also 48 Ka) and Mehtakheri which is 45 Ka [45]. The primary reason for the increase in such dates is the growing application of refined or new luminescence techniques as well as radiocarbon methods. The youngest Middle Paleolithic evidence has been dated to 38 Ka in southern India [56] and as with the Acheulean, Middle Paleolithic assemblages have been reported from throughout the Subcontinent with (more or less) the same geographic exceptions.
Multiple perspectives of three Levallois flakes from the Son Valley, north-central India (pic courtesy: Shashi Mehra).
Dorsal and ventral sides of three Levallois and Levallois-like points from the Son Valley, north-central India (pic courtesy: Shashi Mehra).
Preliminary compilation of published data shows a minimum of 750 occurrences of Middle Paleolithic/Middle Stone Age sites and site-complex across India. While earlier researchers have identified Middle Paleolithic sites based on the absence of bifaces, dominance of flake-based assemblages and the presence of Levallois elements, some regions do not preserve a clear signature of this phase. For example, most of the enigmatic ‘Soanian’ evidence (Figure 10) in the Siwalik Hills region appears to variably comprise contemporaneous Mode 1 and Mode 3 technologies [4]. No absolute dates for that tradition/adaptation are yet available from excavated or stratified contexts and the only two earlier-dated occurrences in the Siwalik Hills of Pakistan [31] and Nepal [59] have not been classified as Soanian. Likewise in other regions, the Middle Paleolithic evidence may be equally undiagnostic or ambiguous and not necessarily absent. Based on current evidence, specific diagnostic attributes such as preferential Levallois elements and points do not appear to be as abundant or geographically widespread as expected. That being said, most of the earliest dispersals of Homo sapiens may not be typo-technologically diagnostic as seen with the younger technologies in the archeological record. In fact, the initial arrival of Homo sapiens continues to be debated based on archaeology (advanced Middle Paleolithic vs. microlithic) and genetic studies on indigenous groups [80]. Future surveys aimed at filling key geographic and stratigraphic contexts may gradually change this pattern. Over the last few decades, this technology has been increasingly thought to be associated with the initial arrival of Homo sapiens by various researchers, some of the most recent being the Jwalapuram evidence from southern India dated to ~77 [55], the Kataoti and Sandhav evidence from western India respectively dated to 95 Ka [34] and 114 Ka [36], and the Dhaba evidence in north-central India dated to between 79 Ka and 65 Ka [41].
Diverse artifact types from the Soanian site of Toka in Siwalik Hills of northern India.
This prehistoric phase is the most enigmatic in the Subcontinent as it lacks absolute dates, is geographically irregular and temporally overlaps with the terminal Middle Paleolithic and early microlithic in several regions. Due to the latter attribute, the South Asian Upper Paleolithic has been replaced with or incorporated within the ‘Late Paleolithic’ by some researchers (see [81]). Preliminary counts from published data has revealed a minimum of 530 reported Upper Paleolithic/Late Stone Age sites across India. It is interesting that classic and diagnostic Upper Paleolithic sites have not yet been reported (or classified as such) from Pakistan, Nepal and Sri Lanka. The dominating and defining features of this techno-chronological phase include a notable increase in the production of more specialized laminar tools such as blades and burins (Figure 11). Additional tool types during this techno-chronological period include flakes, knives, awls, borers, scrapers, cores including cylindrical types, choppers, and bone tools. Unfortunately, and surprisingly, there are still no absolute dates available for any exclusive (i.e. without a microlithic component) Upper Paleolithic assemblages in India, though numerous sites have been reported. The only date currently available for a blade-dominated assemblage in the entire Subcontinent is 45 Ka for Site 55 in Pakistan [31], making it contemporary with the young Middle Paleolithic assemblages in northern India [38] and old microlithic assemblages in central India and Sri Lanka [41, 62].
Laminar elements (blades) from the Son Valley, north-central India (pic courtesy: Shashi Mehra).
Besides chronology and ecological adaptations, a key issue that remains to be understood is the nature of the transitions between the Middle Paleolithic, Upper Paleolithic and early microlithic in South Asia (Figures 12 and 13). What is also lacking in association with these technologies is comparatively abundant symbolic behavior (see [82]), the main explanation for which may be the lack of adequate research and preservation. Given the geographic mosaic of ecological diversity across the Indian subcontinent, it is likely that only some regions do contain classic/typical Upper Paleolithic technologies as distinct techno-chronological entities. In the other geographic zones, their absence may be explained by the lack of suitable raw materials such as siliceous rocks (e.g. chert, fine-grained quartzite) and other factors such as a lack of geographic movements into some zones due to various climatic, ecological and adaptive constraints. Slightly younger evidence which was dated using the AMS method has also yielded new paleoanthropological insights including the youngest dated (~16 Ka) hippo fossils in India [83] and a new microlithic-faunal-pollen association (~18 Ka) from Odisha in eastern India [84], a poorly known but promising region for Indian palaeoanthropology. Such data demonstrate the broad temporal interface between fauna, environments and/or humans. Both studies span not only the end of the Last Glacial Maximum but also perhaps indirectly reflect major transformations within the microlithic phase including the beginning of geometric microliths, human burials and other symbolic behaviors, i.e. the beginning of the Mesolithic proper. Increased human-fauna interactions and rapid colonization of the Subcontinent may have led to the beginning of long-term eco-geographic marginalization of some species (e.g. lion, rhino) as well as their subsequent extinctions (e.g. hippo, ostrich). Only high-resolution multidisciplinary studies including robust chronological frameworks from across India can, however, verify or reject such broad multi-proxy relationships.
Diverse microlithic artifacts from the site of Bayan in the Central Narmada Basin (pic courtesy: Nupur Tiwari).
Diverse microlithic cores and microblades/bladelets on different raw materials from the Son Valley (top row; pic courtesy: Shashi Mehra) and Patne (bottom row) in west-central India.
In addition to the observations and brief summaries provided above, additional key paleoanthropological discoveries in recent years include the first-ever recovery of Sivapithecus fossils outside the Siwalik Hills [85], extraction of DNA from ostrich eggshells and protohistoric human bones [86, 87] and the report of tool-use and object manipulation by the macaque populations of Andaman and Nicobar Islands [88, 89]. The Sivapithecus find comes from the western region of Gujarat and clearly demonstrates how little we know about past faunal distributions at the pan-Indian level. More systematic surveys of key sedimentary contexts in targeted locations across India may yield additional faunal surprises including the much-needed hominin fossils. The successful extraction of DNA from two diverse materials – human bone and ostrich eggshell - also demonstrates that there is now greater potential for further such studies despite earlier failed attempts which were attributed to tropical environmental conditions [90]. The observation of tool-use in monkeys further highlights the critical need for more primate studies in South Asia at various levels including primate archaeology, cognitive studies, ecological adaptations, social relationships, subsistence patterns, conservation strategies and so forth. One arguably important conclusion from the review of known data is that, with the exception of the Pabbi Hills in the Pakistan Siwaliks, no clear evidence currently exists for the presence of Oldowan evidence in the entire Indian subcontinent [65]. Based on the current lack of diagnostic Paleolithic (e.g. Acheulean, Levallois, Upper Paleolithic) and microlithic technologies in the northeastern part of the Indian Subcontinent (i.e. northeast India, Bhutan, Bangladesh, Myanmar), it does not appear to have been used as a biogeographic corridor during hominin dispersals to Southeast Asia. However, intensive surveys are required in the concerned areas as well as Southeast Asia to confirm whether the Subcontinent was a bio-cultural cul-de-sac. In that respect, Pakistan and surrounding border areas also require further surveys to increase the number of Paleolithic sites there, especially due to their significance as the geographic entry point into the Subcontinent. Numerous known sites require re-investigation through multidisciplinary methods including excavations, geological analyses, palaeoenvironmental reconstructions and absolute dating. This is especially critical as some previously-known sites are gradually getting destroyed through various geological and anthropogenic processes (e.g. Chirki-on-Pravara; Personal communication: Sheila Mishra).
Unfortunately, broad hypotheses/theories have been made for South Asian prehistory without adequate evidence, such as the innovation of microlithic technology following environmental deterioration soon after 40 Ka [46]. Not only is there no clear evidence for environmental degradation across the Subcontinent, but later discoveries have demonstrated that microlithic technology was well established in central India and Sri Lanka, respectively, between ~50 Ka and 45 ka. Though the source and nature of their origin remain ambiguous (innovated vs. introduced), it may be possible that specific evolutionary milestones converged at roughly the same time: arrival of Homo sapiens into South Asia with microlithic technology and the arrival of the ostrich into South Asia, possibly reflecting shared arid environments [66, 91]. On a related note, the nature of biological transition(s) between the archaic populations and incoming Homo sapiens has also not been theoretically explored. Was this replacement process gradual or rapid? Did the replacement of archaic populations include interbreeding, and what was its temporal rate and geographic pattern at the pan-Indian level? Did the technologies of both respective hominin groups mix and influence each other at any point in time and space? These and other questions require serious multidisciplinary attention at both empirical and theoretical levels.
Another example is the ongoing debate of the impact of 74 Ka Toba super-eruption on hominin behavior and lithic technology [55, 92, 93, 94, 95, 96]. While the Jwalapuram evidence in southern India yielded a problematic wide age range for the Toba-tephra-associated Middle Paleolithic evidence (77 Ka and 38 Ka), a similar investigation at the site of Dhaba in north-central India chronologically narrowed that gap to 79 Ka and 65 Ka [41]. Nonetheless, the lengthy time gap of 10,000 years between the eruption and the post-Toba archeological evidence makes it challenging to draw major conclusions regarding true occupational continuity and it is not clear if fluvial or other processes facilitated occupational/technological continuity by minimizing the ecological impact of the Toba tephra in the immediate region. In short, we have yet to identify a reliable site or area which preserves stratified and dateable lithic assemblages in primary chrono-stratigraphic contexts immediately prior to and following the Toba tephra [97], especially when considering that the impact of Toba was probably geographically variable across the Subcontinent [96]. Only when this is done in multiple ecological contexts across the Indian subcontinent, will we get a more comprehensive and objectively nuanced perspective on the degrees of impact.
Due to the unique geographic location and associated features of the Indian subcontinent, factors of hominin dispersals and adaptations observed in other Old World regions cannot readily apply here. For example, the link made between the dispersals of Bos and the Acheulean [98] may be applicable only to regions with Acheulean records considerably younger than India. Likewise, the discovery of a considerably older Homo sapiens presence in Europe at ~210 Ka [99] does not necessarily reflect a similar time of their arrival in Asia. However, new discoveries reported in the last few years within Asia may be more applicable and relevant to the Subcontinent. For example, the new decrease (to between 1.5 and 1.3 Ma) in the arrival date of Homo erectus in Southeast Asia [100] and the geographic extension of the Denisovans on the Tibetan Plateau in China [101] indirectly suggest the possibility of their presence in the Indian Subcontinent. Likewise, the chronological extension of Homo sapiens’ arrival into Southeast Asia between 73 Ka and 63 Ka [102] and Australia to ~65 Ka [103] as well as the age of Sulawesi rock art [104] at par with Europe at ~44 Ka has major implications for the Indian zone. The oldest dated rock art from Europe is >64 Ka and has been attributed to Neanderthals [105]. Firstly, the complexity and skill reflected in these paintings suggest the global origin of figurative art is probably much older. Secondly, these discoveries indirectly hint of a possible biogeographic dispersal of Homo sapiens from west to east through tropical rainforest and coastal contexts across Southern Asia [106, 107]. While it is possible that the SE Asian and Australian hominin populations reached there via mainland China, the areas representing northeastern India, Bangladesh and Myanmar need to be intensively surveyed to confirm the routes of dispersal. It is also possible that both southern Asian and central Asian routes were used by various species over time to reach Southeast Asia and Australasia.
From a broader research level, the most important palaeoanthropological accomplishments in South Asia in the last few years include the chronological extension of the Middle Paleolithic to 385 Ka and of microlithic technology to ~48 Ka and the beginning of decolonization of past interpretations and conceptual frameworks regarding human dispersals and population replacements [66]. Nonetheless, much more palaeoanthropological research is required to make more holistic and meaningful comparisons with not only surrounding Asian regions but also with human evolutionary records in other parts of the Old World. The current lacunae suggest that more surveys are required to locate Oldowan sites and Early Acheulean sites to understand their pan-Indian distribution, possible demographic implications, and potential relationships (if any) with East and Southeast Asian lithic records. In light of the fact that the South Asian prehistoric record is poorly known when compared to other parts of Asia, Africa and Europe, and because much more empirical data is required (priorities being hominin fossils and absolute dates), it is premature and unnecessary to propose hypotheses or theories based on preliminary evidence. At this stage in our research in South Asian prehistory, we should perhaps focus on generating abundant empirical data and simply reporting it in a neutral manner without any specific hypothesis-building.
I thank Yogesh Mallinathpur, Yezad Pardiwalla and Martina Narzary for providing preliminary minimum counts of Lower, Middle and Upper Paleolithic sites respectively, as discussed in this paper. Photographs of some of the lithic specimens were generously provided by Nupur Tiwari, Vivek Singh and Shashi Mehra. Comments from the reviewers helped improve the paper and are appreciated.
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