",isbn:"978-1-83968-760-0",printIsbn:"978-1-83968-759-4",pdfIsbn:"978-1-83968-761-7",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"cc49d6034d85f8f2e2890c6acc3cc629",bookSignature:"Dr. Abhijit Biswas",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10285.jpg",keywords:"Mott Insulators, Semi Metals, Polycrystals, Single Crystals, Electronic Properties, Magnetic Properties, PLD, MBE, Topological Insulators, Topological Hall Effect, Devices Applications, Catalysis",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 9th 2020",dateEndSecondStepPublish:"October 7th 2020",dateEndThirdStepPublish:"December 6th 2020",dateEndFourthStepPublish:"February 24th 2021",dateEndFifthStepPublish:"April 25th 2021",remainingDaysToSecondStep:"5 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"A pioneering researcher in the field of tailoring metal oxide crystal surfaces and growth as well as engineering of thin films for various emergent phenomena and energy applications. Dr. Biswas received his Ph.D. from POSTECH, South Korea.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"194151",title:"Dr.",name:"Abhijit",middleName:null,surname:"Biswas",slug:"abhijit-biswas",fullName:"Abhijit Biswas",profilePictureURL:"https://mts.intechopen.com/storage/users/194151/images/system/194151.png",biography:"Dr. Abhijit Biswas is a research associate at the Indian Institute of Science Education and Research (IISER) Pune, in India. His research goal is to design and synthesize highest quality epitaxial heterostructures and superlattices, to play with their internal degrees of freedom to exploit the structure–property relationships, in order to find the next-generation multi-functional materials, in view of applications and of fundamental interest. 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Currently, he is also serving as a reviewer of several reputed peer-review journals.\nDr. Biswas received his B.Sc. in Physics from Kalyani University, followed by M.Sc in Physics (specialization in experimental condensed matter physics) from Indian Institute of Technology (IIT), Bombay. His Ph.D., also in experimental condensed matter physics, was awarded by POSTECH, South Korea for his work on the transport phenomena in perovskite oxide thin films. 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1. Introduction
A battery generally consists of three important parts namely, anode, cathode and electrolyte. The batteries further classified into primary and secondary batteries. Among the different kinds of batteries, Li-ion batteries are plays a very important role in the development of modern technologies especially in the portable electronic device industries and in heavy electrical vehicles because of its advantages such as high theoretical capacity, improved safety, lower material costs, ease of fabrication into flexible geometries, and the absence of electrolyte leakage. In the battery system different kinds of electrolytes were used for promoting the ions from anode to cathode (during charge) and cathode to anode (during discharge). For this purpose, liquid electrolyte is identified as suitable electrolytes which facilitate higher ionic conductivity (10-2 Scm-1) than other electrolyte systems. However, it has several disadvantages namely gas formation during the operation, leakage, difficult to utilise for portable applications and etc. To overcome these difficulties, many attempts were made on solid polymer electrolyte systems. The main objective of the researchers is to improve the ambient temperature ionic conductivity, mechanical stability, thermal and interfacial stability of the electrolytes. However, it is difficult task for the researchers, inorder to improve these basic requirements of the electrolytes simultaneously because the ionic conductivity and mechanical strength of a polymer electrolyte are disparate to each other, i.e., mechanical strength of the electrolyte decreases as conductivity increases.
In recent years, Polymer electrolytes have been attracted scientific and technological importance because of their potential applications in many areas such as Li-ion polymer batteries, super capacitor, electro chromic devices and etc. The idea of preparation of polymer electrolytes was first proposed by Wright and Fenton et.al in 1973 [wright et al., 1973] but their technological significances are fulfilled and appreciated by Armand et.al few years later [Armand et al., 1998]. Poly (ethylene oxide) was the first solvating polymer to be proposed and studied in solid polymer electrolyte (SPE) Li-rechargeable batteries. Most of the solid polymer electrolytes (SPEs) are prepared by dissolving lithium salts in a solvating polymer using common solvent or by diffusion in the solid (or) molten state. An effort is also made to fix or immobilize the anion on the polymer matrix by covalent bonding (or) another chemical or physical process.
In general, Polymer electrolytes are plastic materials that can be modified and processed by conventional techniques. If the polymer chains are helped for a charge transport of the ionic type, often called “polymer electrolyte”. Solid polymer electrolytes (SPEs) afford two important roles in Li-ion battery. 1) It is used as a separator in the battery system because of it rigid structure, at the same time to avoid the electrical contact between the anode and the cathode; 2) it is the medium in which the ions are transported between the anode and cathode during the cell operations. As a result, the polymer electrolyte should act as good electrical insulator but at the same time it should has high ionic conductivity.
1.1. Classification of polymer electrolyte systems
The polymer electrolyte systems could be classified into three categories, namely, i) Polyelectrolyte, ii) Solvent swollen polymer electrolyte and iii) solvent free polymer electrolytes.
1.2.1. Polyelectrolyte’s
Polyelectrolytes are polymers which have their own ion-generating groups chemically bound to the macromolecular chain and the presence of a counter-ion maintains the electroneutrality of the salt. This class of materials either positively or negatively charged ions covalently attached to the polymer backbone and therefore only the unattached counter ion has long range mobility. The conductivity of these polymers is very low (10-10-10-15 Scm-1) in dry conditions but hydrated polyelectrolytes achieve high conductivity in the presence of high dielectric constant solvent (e.g. Water). In hydrated polyelectrolytes, ionic transport takes place through the aqueous medium in which the polymer is dispersed. Slade et.al. [Slade et al., 1983] reported high ambient temperature conductivity of 10-2 Scm-1 in hydrated Nafion.
1.2.2. Solvent swollen polymer electrolytes
In solvent swollen polymers, solvents (aqueous/non-aqueous) swell the basic polymer host [like poly(vinyl alcohol) or poly(vinyl pyrrolidone)]. The dopant ionic solutes like H3PO4 are accommodated in the swollen lattice which permits the ionic motion in solvent rich swollen region of the polymer host. These materials are, in general, unstable and their conductivity depends on the concentration of the solvent in the swollen region. The properties of such polymers depend on the pre-treatment, structure of the sample, temperature, relative humidity, etc.
The polymer –salt complexes are formed by complexes between salts of alkali metals and polymer containing solvating heteroatoms such as O, N, S, etc. The most common examples are complexation between poly (ethylene oxide) (PEO) and alkali metal salts. The polymer salt complexes are further classified into: i) Solid polymer electrolytes ii) Blend polymer electrolytes iii) Gel polymer electrolytes iv) Composite polymer electrolytes. Among the various polymer electrolytes which are used in Li-ion batteries, solvent free polymer electrolytes are the most favourable for device fabrications. The solvent free polymer salt complexes are further classified into: i) Solid polymer electrolytes ii) Gel polymer electrolytes iii) Composite polymer electrolytes.
a) Solid polymer electrolytes
Solid polymer electrolytes (SPEs) have an ionic conductivity when modified by dissolving alkali salts in suitable polymer matrix. SPEs are typically thin films, which have a wide range of electrochemical applications such as batteries and electrochromic devices. They have several advantages when used in a battery and can be formed into thin films of large surface area giving high power levels. The flexibility of the films allows space-efficient batteries to be constructed [Quartarone et al., 1998].
b) Gel polymer electrolytes
Plasticizers incorporated polymer- salt complex is called gel polymer electrolytes. The addition of plasticizers into the polymer matrix softens the polymers and they increase free volumes which are used for ion migration. Addition of plasticizer also increases the chain flexibility, reduces crystallinity, decreases the glass transition temperature and hence increases the ionic conductivity. The conductivity of PEO: LiBF4 is of the order of x10-6 Scm-1 which has been increased to the order of x10-4Scm-1 when the complex is plasticized at 25ºC [Chiodelli et al., 1988] this is mainly due to the specific nature of the plasticizers and the prepared gels has both the cohesive properties of solids and the diffusive property of liquids. Even though the gel polymer electrolyte exhibits high ionic conductivity, its thermal and mechanical stability are poor and it has higher reactivity towards the electrode. Gel electrolytes may undergo solvent exudation upon long storage, especially under open atmosphere conditions. This phenomenon is known as ‘Synerisis effect’, and has been encountered in many systems such as PAN: EC: PC: LiClO4, PAN: EC: PC: LiAsF6 [Groce et al., 1994 and Slane & Salomon et al., 1995].
c) Composite polymer electrolytes
This is another approach in which both the ionic conductivity and the mechanical stability of the electrolytes were considerably enhanced simultaneously. Composite polymer electrolytes are prepared by the addition of high surface inorganic fillers such as Al2O3, SiO2, MgO, LiAlO2, TiO2, BaTiO3 and Zeolite powders. The mechanical strength and stiffness of the complex systems were improved appreciably when the fillers are incorporated into the polymer matrix. However the main advantages of the composite electrolyte is the enhancement of room temperature ionic conductivity and an improved stability at the electrode electrolyte interface. The inert fillers due to its large surface area prevent the local chain reorganization with the result of locking in at ambient temperature, a high degree of disorder characteristic of the amorphous phase, which is more favour for the high ionic transport [G. Nagasubramanian and S. Di Stefano, 1990, Peter P Chu,P.P. Reddy, M.J., 2003]. The nano sized BaTiO3 incorporated PEO composite electrolytes exhibits ionic conductivity of the order of x10-3 Scm-1 and good electrochemical stability (4.0V).
1.3. Blend polymer electrolytes
Blend is a mixture of two or more polymers. Mixing of two polymers is a well established strategy for the purpose of obtaining materials with combined superior properties or avoiding the need to synthesize novel structures constitutes an attractive research area. As many emerging applications are of limited volume and require specific property profiles not suitable for broad application utility, polymer blend technology is often the only viable method to deliver the desired material. These polymer blends have some unique properties that are different from the basic polymers from which these have been produced. To improve the processing behaviour for end use, one polymer blending with another polymer is a common practice. The exploitation of certain unique set of properties of individual polymer for the benefit of the overall properties of a multi component system forms the basis of polymer blending. Hence blending of polymers has resulted in the development of polymeric materials with desirable combination of properties. Polymer blend electrolytes are developed in such a way that they remain structurally stable during manufacturing, cell assembling, storage and usages as well as to prevent leakage from the cell container or without the cell.
1.4. Some commonly available polymer electrolytes for lithium ion batteries
1.4.1. PEO based electrolytes
PEO is a crystalline polymer. The oxygen in PEO acts as a donor for the cation and the anion generally of large dimension stabilizes the PEO alkali salt complex.
The polymer electrolytes composed of a blend of poly (ethylene oxide) (PEO) and poly (vinylidenefluoride-hexa fluoropropylene) as a host polymer, mixture of EC and PC as plasticizer and LiClO4 as a salt were prepared by Fan et al. [Fan et al., 2002]. The ionic conductivity of various compositions of blend polymers was found to be in the order of x10-4 Scm-1 at 30ºC. On increasing the PEO content in the matrix, the conductivity decreased due to its high crystalline nature. The mechanical strength of the polymer electrolytes was measured from stress-strain tests. The electrolytes were also characterized by SEM, XRD and thermal analysis techniques. Xi et al. [Xi., 2006] aimed to improve ionic conductivity with a novel approach using PEO and PVdF as host polymers by phase inversion technique. The room temperature conductivity was measured as a function of PEO content. As the weight ratio of PEO was increased from 40 to 50%, the ionic conductivity increased more than one magnitude from 0.15 to 1.96 x10-1Scm-1 which is mainly due to the increasing of pore connectivity. This is very important for the transport of charge carriers in microporous polymer membrane. The plasticizer effect on PEO-salt complex was studied by Fan et al [Fan et al., 2008] using succinitrile (SN) as a plasticizer, LiClO4, LiPF6 and LiCF3SO3 as lithium salts. They found that the addition of plasticizer was responsible for high ionic conductivity which could be attributed to the high polarity and diffusivity of succinitrile. This, in turn, decreased the crystallinity of PEO polymer. Activation energy of the electrolytes was also estimated from Arrhenius plot. Itoh et al. [Itoh et al., 2003] prepared the composite polymer electrolytes using poly(ethylene oxide)/ poly(triethylene glycol) benzoate, BaTiO3 and lithium imides. They estimated the ionic conductivity value as 1.6x10-3 Scm-1 at 80ºC and the electrochemical stability window as 4.0V. The membrane was also characterized by TG/DTA and it is thermally stable upto 307ºC. Novel effect of organic acids such as malonic, maleic and carboxylic acids on PEO/LiClO4/Al2O3 complexes was studied by Park et al. [Park et al., 2006]. It was noted that the ionic conductivity of the film consisting of PEO/LiClO4: Citric acid (99.95:0.05 wt%) was 3.25x10-4Scm-1 at 30ºC and it was further improved to 3.1x10-3 Scm-1 at 20ºC by adding 20wt% of Al2O3 filler. The prepared membranes were also characterized by Brewster Angle Microscopy (BAM), thermal analysis and cyclic voltametry.
1.4.2. PVC based electrolytes
PVdF/PVC blend composite polymer electrolyte was prepared by Aravindhan et al. [Aravindhan et al., 2007] incorporating lithium bis(oxalate) borate and ZrO2. All the prepared membranes were subjected to SEM, XRD and ac impedance studies. The maximum ionic conductivity (1.53x10-3 Scm-1) was obtained for 2.5wt% of ZrO2 at 343K. The ionic conductivity and FTIR studies on plasticized polymer electrolyte based on PVC and PMMA as host polymer were studied by Manuel Stephan et al. It was found that LiBF4 based PVC/PMMA/EC/PC complexes exhibited higher ionic conductivity compared to that with LiClO4. The thermal stability of the films was also ascertained using TG/DTA analysis.
1.4.3. PAN based polymer electrolytes
Kim et.al [Kim,D.W. Sun,Y.K. 2001] prepared highly porous polymer electrolyte employing P(VdF-co-HFP) and PAN with a view to attain high ionic conductivity and good mechanical strength. Lithium-ion polymer battery using these gel polymer electrolytes was assembled, and its charge-discharge characteristics were also reported. Panero et al. [Panero et al., 2002] studied the characteristics and the properties of a polymer electrolyte formed by trapping LiPF6-PC solution in a poly(acrylonitrile) matrix with the addition of Al2O3. They reported the ionic conductivity value as 0.8x10-2Scm-1 at 25ºC. The performances of the electrolyte were found to be promising in terms of cycle life and basic energy density content. Very recently, Moreno et.al [Moreno et al., 2010] reported a series of composite electrolytes basically constituted by poly(acrylonitrile), Clay and montmorillonite as filler. The structural and complex formations of the CPEs were also studied. However, the composite based on PAN system showed poor ionic conductivity of the order of x10-6 Scm-1.
Tsutsumi and Kitagawa [Tsutsumi and Kitagawa et al., 2010] synthesized a new type polymer electrolyte films based on poly(acrylonitrile), and Cyanoethylated poly(vinyl alcohol) (CN-PVA) and its conductivity behaviour was also investigated. They found the ionic conductivity value as 14.6x10-3Scm-1 at 30ºC for PAN (10)-CN-PVA (10) - LiClO4 (8)-PC (4) complex system. The interactions of Li+-ion and nitrile groups of PAN in the matrix were confirmed by FTIR analysis. The ionic conductivity and FTIR studies were carried out on PAN based gel electrolytes with EC: PC and EC: DMC mixtures as plasticizers, LiClO4 or LiBF4 as the salt by Amaral et al [Amaral et al., 2007]. The high ionic conductivity (1.47x10-3 Scm-1) was estimated for 20:28:45:7 molar ratio of PAN-PVA: EC: DMC: LiBF4 system. Charge/discharge performance of the maximum ionic conductivity complex was also studied. The practical performance and thermal stability of Li-ion polymer batteries with LiNi0.8Co0.2O2, mesocarbon microbead-based graphite, and poly (acrylonitrile) (PAN) based gel electrolytes were reported by Akashi et al. [Akashi et al., 2002].
1.4.4. PVdF based polymer electrolytes
PVdF is a semicrystalline polymer and the electrolytes based on PVdF are expected to have high anodic stabilities due to strong electron withdrawing functional groups (-C-F). It also has high permittivity, relatively low dissipation factor and high dielectric constant (ε=8.4) which assist in high ionization of lithium salts, providing a high concentration of charge carriers. Choe et al. [Cheo et al., 1995] reported that the PVdF based electrolytes plasticized with a solution of LiN(SO2CF3)2 in PC had a conductivity of 1.74x10-3 Scm-1 at 30ºC and has a oxidatively stable potential limits between 3.9 and 4.3V vs Li+/Li. Nicotera et al. [Nicotera et al., 2006] measured the ionic conductivity and the lithium salt diffusion coefficient of PMMA/PVdF based blend electrolytes with EC/PC as plasticizers and lithium perchlorate as salt by the PFG-NMR method, which revealed maximum lithium mobility for the composition PMMA 60%-PVdF 40%. Raman spectroscopic study confirmed the change of interaction between the lithium cations and the plasticizer molecules for different PMMA/PVdF ratios. Wang et al. [Wang et al., 2007] prepared the nanocomposite polymer electrolytes comprising of poly (vinylidene fluoride) (PVdF) as a host polymer, lithium perchlorate (LiClO4) as salt and TiO2 used as a filler by solvent-casting technique. The prepared films were characterized by XRD, DSC and SEM. The conductivity value was found to be of the order of 10-3 Scm-1 for the sample with 10% TiO2.
1.4.5. PMMA based electrolytes
Ali et al. [Ali et al., 2007] reported the electrical properties of polymer electrolytes comprising PMMA, PC, EC as plasticizer and different lithium salts LiCF3SO3 and LiN(CF3SO2)2. The polymer electrolytes exhibited high ionic conductivity at room temperature in the range of 10-6 to 10-4 Scm-1. The temperature dependence studies confirmed that the conduction in electrolyte is only by ions and seemed to obey the VTF rule. FTIR spectroscopy studies confirmed the polymer-salt interactions. FTIR spectroscopic investigations coupled with ionic conductivity and viscosity measurements on lithium imide LiN(CF3SO2)2–propylene carbonate (PC)–poly(methyl methacrylate) (PMMA) based liquid and gel electrolytes over a wide range of salt (0.025–3 M) and polymer (5–25 wt.%) concentration were reported by Deepa et al. [Deepa et al., 2004] and found that the high ionic conductivity occurs at salt concentrations ≥1.25 M.
1.4.6. PVdF-co-HFP based polymer electrolytes
In recent years, the studies on PVdF-co-HFP based systems are electrochemically stable and indispensable for the electrode properties. The PVdF-co-HFP based electrolyte system shows high electrochemical stability in the range 4V. Fan et al. [Fan et al., 2002] studied the thermal, electrical and mechanical properties of EC/PC/LiClO4 based PEO/P(VdF-co-HFP) blends. They concluded that the polymers have good compatibility and PVdF-HFP hinders the crystallinity of PEO. Saika and Kumar [Saika and Kumar, 2004] made systematic studies on the ionic conductivity and transport properties of polymer electrolytes comprising of co-polymer PVdF-co-HFP/ PC/ DEC/ LiClO4 and PVdF/ PC/ DEC/ LiClO4 separately. The co-polymer complex showed higher ionic conductivity and transport number compared to PVdF system. The higher conductivity of the polymer electrolyte based on copolymer was attributed to its higher amorphousity. Wang et.al [Wang et al, 2004] reported that the polymer electrolyte composed of poly(methyl methacrylate-co-acrylonitrile-co-lithium methacrylate) (PMAML) and poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-co-HFP) exhibited high ionic conductivity and good electrochemical stability. The ionic conductivity was about 2.6×10-3 Scm−1 at ambient temperature and the electrochemical window of the polymer electrolyte was about 4.6V. Charge –discharge test results revealed that lithium ion batteries with these gel polymer electrolytes have good electrochemical performance.
Manuel Stephan et.al [Manuel Stephan et al., 2006] prepared the composite polymer electrolyte membranes, comprising Poly(vinylidene fluoride–hexafluoropropylene), Aluminum Oxyhydroxide of two different sizes 7nm/14 nm and LiN(C2F5SO2)2 as lithium salt and they found that the incorporation of the inert filler not only reduces the crystallinity of the polymer host but also acts as ‘solid plasticizer’ capable of enhancing the transport properties and also provides a better interfacial property towards lithium metal anode. Nam-Soon Choi et.al [Choi et al., 2001] reported that the interfacial stability between the polymer electrolyte and the lithium electrode was enhanced by blending PVAc with P(VdF-co-HFP)(Kynar 2801). The ionic conductivity of the polymer electrolyte based on the Kynar 2801: PVAc (7:3, w:w) blend was 2.3×10-3 S cm-1 at 25 C. Kim et.al [Kim et al., 2005] prepared and characterized gel polymer electrolytes consisting 25wt% PVdF-co-HFP/65 (EC+PC)/10 wt% LiN(CF3SO2)2.They reported the ionic conductivity value as 1.2x10-3Scm-1. The electrochemical stability window of the membrane was obtained at around 4.8V Vs Li/Li+ using linear sweep voltametry technique. The Charge – discharge behaviour of the membrane was also studied and they estimated the specific discharge capacity as 140 mAhg-1 for upto 20 cycles at different current densities.
1.4.7. PVAc based polymer electrolytes
Though variety of polymer electrolytes were characterized for the fast four decades, a limited number of studies were made on PVAc based polymer electrolytes. PVAc polymer has a large dipole moment and high relaxation time. Baskaran et al [Baskaran et al., 2006] prepared the polymer electrolyte comprising of PVAc-PMMA and reported the conductivity value as 1.76x10-3Scm-1 at 303K. The DSC thermograms of the blend electrolytes showed two Tg’s and they decreased with an increase of LiClO4 concentration. The structural and complex formations of the electrolytes were confirmed by X-ray diffraction analysis. They established that the optimized blend ratio of PVAc: PMMA: LiClO4 is suitable for lithium battery applications. Structural, thermal and transport properties of PVAc-LiClO4 base complexes were studied by Baskaran et al [Baskaran et al., 2007]. The bulk conductivity of PVAc: LiClO4 system was found to vary between 7.6x10-7Scm and 6.2x10-5 Scm-1 at 303K with an increase in the salt concentration. The amorphous nature of the polymer complexes was confirmed by XRD and SEM analysis.
Surface morphology and ionic conductivity of the membrane based on P(EO)/PVAc /LiClO4 were studied by Animitsa et al [Animitsa et al., 1998]. They reported the conductivity value as 10-5 Scm-1 for lower concentration of PVAc at 25ºC. Baskaran et al. [Baskaran et al., 2006] studied the ac impedance and dielectric properties of PVdF/PVAc blend electrolytes. They reported that the blend ratio (75:25) of PVAc/PVdF exhibited a maximum ionic conductivity value of the order of 6.4x10-4Scm-1 at 343K. The ionic transference number of mobile ions was also estimated by Wagner’s polarization method. The complex formation and thermal behaviour of the electrolytes were also studied by FTIR and DSC analysis respectively.
2. Basic requirements of polymers and the salt for polymer electrolytes
Atoms or groups of atoms with sufficient electron donor power to form coordinate bonds with cations.
Low barriers to bond rotation so that segmental motion of the polymer chain can take place readily.
A suitable distance between coordinating centres for the formation of multiple intrapolymers ion bonds appears to be important
Low glass transition temperature to increase the segmental motion.
The polymer should have amorphous phase which lowers the barrier for ionic movement and yields high ionic conductivity.
The lattice energy of the salt should be low.
High electrochemical reduction potential
Electron pair donicity (DN)
\n\t\t\t
DN measures the ability of the solvent to donate electrons to solvate the cations considered as a Lewis acid. So the polymer host should have high DN number.
Acceptor number (AN)
The acceptor number quantifies the possibility of anion salvation. It should be less for an inorganic salt so that cationic salvation is high compared to anionic salvation.
Entropy term
The entropy term depends on the optimal spatial disposition of the solvating units which should be high for the polymer host.
2.1. Importance of Li+ cation
Last four decades, many alkali salts consisting Li+, Na+, K+, Ag+, Mg+, NH4+ cations were mixed with the polymers (PEO), (PPO) etc in the preparation of polymer electrolytes. Among the various cations in the periodic table, Li+ is the most electropositive. Lithium easily gives up electrons to form a positive Li+ which has small ionic radii (0.6Å). Lithium is promising candidate for high energy density batteries because of its high specific capacity of 3860 Ah/Kg, its light weight and high electrochemical reduction potential [Scrosati et al., 1994; Abraham et al., 1993; Dell, 2000].
2.2. Preparation of polymer blend electrolytes
Polymer blend electrolytes have been prepared using various approaches namely, Phase inversion method, Hot pressed method, Solvent casting method and etc. Each method has own advantages and disadvantages. Among the various method of preparation solvent costing is the cost effective one and easier to control the moistures during the preparation of electrolytes as well as in the cell assembling. However, when assembling the cells, these membranes show poor cyclic behaviour. As a result many research groups have been mainly focused on phase inversion method for preparing the suitable electrolytes. Preparation of polymer electrolyte system is explained using the following flow chart (Fig.1.).
Figure 1.
Preparation of Polymer electrolyte
In the present study, all the electrolytes were prepared using solvent casting technique. The polymers PVAc, PVdF-co-HFP, and the salt LiClO4 were dissolved in a common solvent (tetrahydrofuran) separately. All three solutions were mixed together and starrier continuously using magnetic stirrer until got a homogeneous mixture. The low molecular weight plasticizer and the inorganic fillers were added into the matrix inorder to get the gel and composite polymer electrolytes systems. In the present study, ethylene carbonate(EC) and barium titanate (BaTiO3) were used a plasticizer and fillers respectively. Thus the obtained homogenous slurry was degassed to remove air bubbles for about five minutes and the slurry was poured on a well cleaned glass plate. The casted slurry was allowed to evaporate the solution at room temperature about 5h followed by the electrolyte membranes were heated using hot air oven at a temperature of 60 ºC for 6h in order to removing the residual solvent present in the electrolyte films. Finally, the harvested electrolyte films were stored in highly evacuated desiccators to avoid the moistures absorption.
3. Characterization of polymer blend electrolytes
Ac impedance analysis was carried out with the help of stainless steel blocking electrodes by using a computer controlled micro auto lab type III Potentiostat/Galvanostat of frequency range 1 Hz–300 KHz in the temperature range 303–373 K. The XRD equipment used in this study was X\'pert PRO PANlytical X-ray diffractometer. FTIR spectroscopy studies were carried out using SPECTRA RXI, Perkin Elmer spectro-photometer in the range 400–4000 cm−1. FTIR spectroscopy studies were carried out for confirming the complex formation using SPECTRA RXI, Perkin-Elmer spectro-photometer in the range 400–4000 cm−1. TG/DTA thermal analysis of the film having maximum ionic conductivity was studied using PYRIS DIAMOND under air atmosphere with the scan rate of 10 ◦C min−1. The electrolyte film having maximum ionic conductivity was subjected to atomic force microscopy [model Veeco-diCP-II]. The pore size and the root mean square (rms) roughness of the film were measured from the topography image. Secondary electron images of the sample were examined by using JEOL, JSM-840A scanning electron microscope
3.1. FTIR analysis
Infrared spectral (IR) analysis is a powerful tool for identifying the nature of bonding and different functional groups present in a sample by monitoring the vibrational energy levels of the molecules, which are essentially the fingerprint of different molecules [Nagatomo et al., 1987]. Fig.2. depicts the FTIR transmittance spectra in the range 400-4000 cm-1 for polymers, the LiClO4 salt, the blend electrolyte with the incorporation of plasticizer ethylene carbonate and the filler BaTiO3.
The vibrational bands observed at 2933 cm-1 and 2465 cm-1 are ascribed to –CH3 asymmetric and symmetric stretching vibrations of PVAc respectively. The strong absorbance at 1734 cm-1 represents the C=O stretching vibration mode of PVAc polymer. The existence of C-O band has been confirmed by the strong absorbance band at around 1033 cm-1. The strong band at 1373 cm-1 is ascribed to -CH3 symmetric bending vibration of pure PVAc. The band at 1243 cm-1 is assigned to C-O-C symmetric stretching mode of vibration. The peak at 947 cm-1 is ascribed to CH bending vibration and the peak at 609 cm-1 is assumed to be linked with CH3 (C-O) group. The C-H wagging mode of vibration has been confirmed by the presence of a band at 799 cm-1 [Baskaran et al., 2004]. The vibrational peaks at 502 and 416 cm-1 are assigned to bending and wagging vibrations of –CF2 of PVdF-co-HFP polymer respectively. Crystalline phase of the PVdF-co-HFP polymer is identified by the vibrational bands at 985, 763, and 608 cm-1 and the amorphous phase of the co-polymer is confirmed by the presence of vibrational band at 872 cm-1 [Rajendran et al., 2002].
The strong absorption peak appeared at 1173 cm-1 is assigned to the symmetrical stretching of –CF2 group. The peak appeared at 1390 cm-1 is assigned to the CH2 groups [Rajendran et al., 2002; Singh Missan et al., 2006]. Table.1. shows the comparison of band spectra of pure polymers and their blends with different blend ratios. From the table, it is clear that the band assignments of FTIR spectra of blend samples are shifted from their pure spectra. For all the blends, some peaks are found above 3000 cm-1, which correspond to the C-H stretching vibration modes of blend electrolytes.
In addition, some new peaks are present and some of them are absent in the blend electrolytes. Thus the spectral analysis confirms the complexation of these two polymers and lithium salt.
Figure 2.
FTIR analysis of LiClO4, PVAc, PVdF-co-HFP and their complexes
3.2. X-ray diffraction analysis
XRD patterns of LiClO4, PVdF-co-HFP, PVAc and their complexes A, B, C are shown in Fig. 3. The presence of characteristic peaks corresponding to the lithium salt reveals the high crystalline nature of the salt. Three peaks found at 2θ = 17.3, 18.59 and 38.78 for PVdF-co-HFP confirms the partial crystallization of PVdF units present in the copolymer, to give an overall semi-crystalline morphology for PVdF-co-HFP [Saika, Kumar, 2004]. Presence of broad humps in the XRD pattern of PVAc confirms the complete amorphous nature of the polymer. It is observed that the characteristic peaks corresponding to the lithium salt in their respective electrolyte systems (A, B and C) were absent and it confirms the complete dissolution of the lithium salts in the complex matrix which implies that the salt do not have any separate phase in the electrolytes. The addition of plasticizer in the blend complex enhances the amorphous region thus permitting the free flow of ions from one site to another site; hence the overall ionic conductivity of the electrolyte has been significantly improved. According to Hodge et al. [Hodge et al., 1996] the ionic conduction in the polymer electrolytes occurs mostly in the amorphous region and it has been achieved by the addition of low molecular weight plasticizer. Further addition of inorganic filler into the polymer salt matrix would increase the dissolution of the charge carriers in the matrix; hence, the ionic conductivity was improved. The XRD pattern of the sample contains the filler BaTiO3 shows a broad hump confirms the further enhancement of the amorphous region in the polymer electrolyte complex systems.
Figure 3.
X-ray diffraction analysis of LiClO4, PVdF-co-HFP, PVAc and their complexes.
3.3. Ac impedance analysis
Ac studies are similar to the DC techniques in that the ratio of voltage to current is measured. For DC, this ratio provides the value of the resistance, R, measured in ohms. For AC the ratio gives an analogous quantity, the impedance, Z, also measured in ohms. The impedance contains four main contributions; these are from resistance, capacitance, constant phase elements, and inductance. The induction is not an important factor for the polymer electrolytes although it can play a role in other electrochemical applications of polymers.
Measurement of the impedance as a function of frequency is called impedance spectroscopy. In general, impedance is complex quantity, in which the real and the imaginary parts are labelled Z’ and Z” respectively. In the complex impedance plot, the real quantity Z’ (X-axis) is plotted against Z” (Y-axis) which displayed the polymer electrolytes characteristics as an arc followed by the linear spike is straight line inclined to the real axis. From the plotted graph, we can easily read the bulk resistance of the electrolyte system.
The complex impedance plot of the PVAc/PVdF-co-HFP/LiClO4 electrolyte is shown in Fig.4a. Figure shows the semicircular portion which is mainly due to the parallel combination of the geometrical capacitance, Cg and the bulk resistance, R. When adding the plasticizer and the filler (Fig.4b.) into the electrolyte matrix, the impedance spectra shows only a linear spike which corresponds to the lower frequency region. It confirms the idea that the current carriers are ions and the majority of the conduction only by the ions not by the electrons. And the disappearance of the semicircular portion is may be due to the fact the corresponding characteristic frequency is higher than the frequency 300kHz and it is mainly depends on the instrument limit. From the obtained bulk resistance value, we can estimate the ionic conductivity value of the electrolyte system using the relation σ = l/Rb A, where, Rb is the bulk resistance of the electrolyte film, A is the area of the electrode surface and is the thickness of the electrolyte medium and σ is the ionic conductivity.
It is noted from the spectra that the addition of plasticizer (ethylene carbonate) in to the polymer salt matrix greatly being reduced the bulk resistance of the system; this is because of the high dielectric nature of the low molecular weight plasticizer. The addition of plasticizer would considerably enhance the amorphous phase of the polymer electrolyte which will improve the ionic conductivity of the system. However, the gain in conductivity is adversely associated with a loss of the mechanical properties and by a loss of the compatibility with the lithium electrode, both effects resulting in serious problems since they affect the battery cycle life and increase the safety hazard. So it is necessary to identify the solid additives which would not affect the mechanical stability and interfacial stability of the electrolyte, at the same time will enhances the ionic conductivity. The addition of solid additives should improve the amorphicity of the electrolyte at room temperature. The addition of solid additives in the present study, such as nano filler BaTiO3 highly being enhanced the amourphicity of the electrolyte medium, hence the room temperature ionic conductivity and the interfacial stability of the electrode-electrolyte interface is increased. The ceramic dispersed electrolyte shows good thermal stability. The BaTiO3 incorporated sample is thermally stable up to 320 ºC. The temperature dependence of the conductivity is given by the Vogel–Tamman–Fulcher (VTF) equation σ = σ0 exp (-B/T-T0), where σ0 is the pre-exponential factor, B should not be confused with an activation energy in the Arrhenius expression and T0 is related to the so called thermodynamic Tg. Plots of logs vs 1/T are curved because of the reduced temperature (T-T0).
Figure 4.
Room temperature complex ac impendance spectra
3.4. TG/DTA analysis
Thermo gravimetric analysis /differential thermal analysis have been used widely to study all physical processes involving the weight changes. It is also used to investigate the thermal degradation, phase transitions and crystallization of polymers. Fig.5(a-c) shows the TG/DTA curves of PVAc/PVdF-co-HFP/LiClO4, PVAc/PVdF-co-HFP/LiClO4/EC and PVAc/PVdF-co-HFP/LiClO4/EC+PC/BaTiO3 polymer electrolytes. From the thermogram, it is observed that the sample A is thermally stable up to 238ºC. The sample starts to decompose at 238ºC, beyond which, there is a gradual weight loss of 20% in the temperature range 240-280ºC. DTA curve of the sample shows an exothermic peak at 265ºC, which is well correlated with the weight loss of the sample observed in TG curve. It is also observed that the complete decomposition of the sample takes place between 490-510ºC with the corresponding weight loss of about 80-90%. After 520ºC, there is no appreciable weight loss (Fig.5a). The remaining residue around 15% may be due to the formation of impure crystalline metal oxide and lithium fluoride. It is also observed from DTA curves that the exothermic peaks at 90, 225, and 445 ºC are concurrent with the weight losses observed in the TG trace. The sample (Fig.5b.) exhibit gradual weight loss of about 10-15%, which is due to the removal of the residual solvent and the moisture from the electrolyte sample in the temperature range 90-115 ºC. From the TG curve of the sample PVAc/PVdF-co-HFP/LiClO4/EC, it is observed that the decomposition occurred at 229ºC with the weight loss of about 20%. After the second decomposition, there is sudden weight loss of 40-45% in the temperature range 446-460 ºC for the electrolyte. The thermogram of the sample having BaTiO3 inert filler is shown Fig.5c. From the themogram, it is observed that the sample is thermally stable up to 320ºC. The sample exhibits gradual weight loss of about 8% in the temperature range 100-110 ºC, which is due to the removal of the residual solvent and the moisture. DTA curve of the sample shows an exothermic peak at 320ºC, which is well correlated with the weight loss of the sample observed in the TG curve. The remaining residue around 30% may be due to the presence of BaTiO3. It is noted from the above analysis that the additions of plasticizer into the polymer blend-salt matrix slightly influence the thermal stability of the electrolyte medium; however it has enhanced the ionic conductivity of the electrolyte. But, the addition of nano composite in to the matrix greatly being increased the thermal stability and the room temperature conductivity simultaneously. It is concluded that the incorporation/dispersion of inorganic filler in the electrolyte significantly increased the thermal stability of the electrolyte membrane.
3.5. SEM analysis
The scanning electron microscope (SEM) is one of the most versatile instruments available for the examination and analysis of the microstructure morphology of the conducting surfaces. Scanning electron microscope (SEM) image of PVAc-LiClO4, PVdF-co-HFP-LiClO4, PVAc/PVdF-co-HFP/LiClO4, PVAc/PVdF-co-HFP/LiClO4/EC and PVAc/PVdF-co-HFP/LiClO4 /EC+PC/BaTiO3 electrolyte films are shown in Fig.6(a-e). Fig.6a clearly shows smooth and uniform surface morphology of the PVAc- LiClO4. This smooth morphology confirms the complete amorphous nature of PVAc polymer and complete dissolution of the lithium salt, which also coincides with the XRD result. Fig.6b shows the photograph of PVdF-co-HFP-LiClO4 salt complex with maximum number of pores giving rise to high ionic conductivity. Presence of the spherical grains in the microstructure image
Figure 5.
TG/DTA Thermal analysis of a) PVAc/PVdF-co-HFP/LiClO4; b) PVAc/PVdF-co-HFP/LiClO4/EC; c) PVAc/PVdF-co-HFP/LiClO4/EC+PC/BaTiO3
of the samples A and B (Fig.6b and d) are belongs to the co-polymer and it means that the copolymer do not dissolve completely in the matrix which results, the membrane gets brittle nature. The appearance of number of uniform tracks of few micrometer sizes is responsible for the appreciable ionic conductivity of the electrolyte (Fig.6c). The maximum ionic conductivity of the polymer blend electrolyte also depends on the segmental motion of the PVAc and PVdF-co-HFP. The better miscibility of these two polymers can be depicted from the microstructural photograph. Fig.6d shows the scanning electron micrographs of PVAc/PVdF–co-HFP/LiClO4/EC-based electrolyte system. The micrograph shows the spherical grains, and they are uniformly distributed in the electrolyte system. It is observed that the numerous pores (dark region) with the size of 1–10μm are responsible for the high conductivity of the sample, i.e., the membrane shows highly porous structure. This increased number of porosity leads to entrapment of large volumes of the liquid in the pores accounting for the increased conductivity. The interconnected microspores in the membrane helped in absorbing liquid electrolytes and hence the ionic conductivity of the membrane is enhanced. The presence of pores in the microstructure is mainly due to the solvent removal and increased amorphous region and solvent retention ability in the electrolyte system. Surface images of the samples BaTiO3 is shown in Fig.6e. The pores in the complexes are responsible for entrapping the large volume of the solution (plasticizer +salt) in the cavities accounting for the enhanced ionic conductivity. It is observed from image that the membrane has numerous number of randomly distributed spherical grains and shows maximum number of pores with very small size of the order of 50-100nm. The smooth surface of the sample reveals that the polymers and salt used in this study have a good compatible nature and the light gray region indicates the presence of plasticizer rich medium which assists for ionic motion. It is also studied that the content BaTiO3 increases beyond certain percentage the film surface becomes rough above the optimum level the grain size increases, with a reduction in the number of grain aggregates, that tend to restrict the ionic movement. Finally, the SEM photograph of the polymer electrolyte indicates good compatibility of these two polymers and the other constituents which are used in the electrolyte preparation. The enhancement of the amorphous region in the matrix has also been confirmed from the images. The miscibility of these two polymers has also been confirmed from FTIR analysis.
3.6. AFM analysis
An AFM is a mechanical imaging instrument, which is used to obtain the three dimensional topography images of the samples. In the present study, the scanning probe spectroscopic method was used to measure the pore size of the prepared sample as well as the roughnees factor of the sample. The two dimensional and three dimensional topography images of PVAc/PVdF-co-HFP/LiClO4 complex are shown in Fig.7a. This image clearly shows the presence of pores within the scanned area of 3x3µm and the measured pore size of the sample is approximately 600nm. The size of the chain segment is also obtained and it is in the order of 688 nm. The root mean square (rms) roughness of the topography image over the scanned area is found to be 122 nm. The topography image of the sample PVAc/PVdF-co-HFP/LiClO4/EC is shown in Fig.7b. The two dimensional image shows smooth surface. The modified surface image of the sample is mainly due to the addition of plasticizer which increases the amorphous phase of the matrix and hence the ionic conductivity. In addition, small pores are also observed in the surface entrapping the liquid solution, which are responsible for easy ionic movement. From the topography image we have determined the pore size of the order of 100nm which is in close agreement with the value obtained from SEM photograph. In addition, the rms roughness of the sample over the scanned area 1.4x1.4μm has been estimated and it is of the order of 53nm, it is quiet low when compare with sample without plasticizers. The micropores, amorphous phase and the chain segments of the plasticized polymer electrolytes are responsible for the enhancement of ionic conductivity. Two and three dimensional topographic images of the sample having BaTiO3 are shown in Fig.7c. The image shows the dispersion of the fillers and it also contains small pore with a size of 100nm entrapping the ionic liquid which assists for fast ionic motion. In addition, the rms roughness of the sample over the scanned area 1x1μm has been obtained and it is of the order of 4nm. It is noted that the sample contains BaTiO3 showed lower roughness value than the other two samples which means that the incorporation of the fillers and the plasticizers are significantly improve d the amorphous phase in the matrix is helpful for the ionic movement.
Figure 6.
SEM images of a) PVAc/LiClO4; b) PVdF-co-HFP-LiClO4; c) PVAc/PVdF-co- HFP/LiClO4;d) PVAc/PVdF-co-HFP/LiClO4/EC; e) PVAc/PVdF-co-HFP/LiClO4/EC+PC
Figure 7.
AFM images of a) PVAc/LiClO4; b) PVdF-co-HFP-LiClO4; c) PVAc/PVdF-co- HFP/LiClO4; d) PVAc/PVdF-co-HFP/LiClO4/EC; e) PVAc/PVdF-co-HFP/LiClO4/EC+PC
4. Conclusion
All the polymer electrolytes were prepared using solvent costing technique. The specific interactions of the constituents were confirmed using FTIR analysis. The enhanced amorphous region of the polymer electrolyte has been identified from X-ray diffraction analysis. The porous natures of the samples were identified using scanning electron microscope. The Atomic force microscope study was used to estimate the roughness factors of the scanned area. The thermal stability of the electrolyte samples were estimated using TG/DTA analysis. It is concluded that the addition of plasticizer (Ethylene Carbonate) and the dispersion of inorganic filler into the PVAc/PVdF-co-HFP/LiClO4 electrolyte system significantly improve the amourphicity of the medium, which will helped for easy ionic motion. These enhanced regions have been confirmed from the impedance and the surface image studies. The change in bulk resistance of the electrolytes mainly due to the interactions of the basic constituents which cause produce more amorphous phase in the matrix. It is no doubt about that the addition of plasticizers and the fillers are greatly enhanced the amorphous phase of the electrolyte, hence the ionic conductivity is improved. To conclude, polymer electrolyte for possible applications as in high energy density batteries has been identified in terms of parameters such as conductivity, thermal stability.
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Rajendran",authors:[{id:"102326",title:"Dr.",name:"M",middleName:null,surname:"Ulaganathan",fullName:"M Ulaganathan",slug:"m-ulaganathan",email:"nathanphysics@gmail.com",position:null,institution:null},{id:"102329",title:"Prof.",name:"S",middleName:null,surname:"Rajendran",fullName:"S Rajendran",slug:"s-rajendran",email:"sraj54@yahoo.com",position:null,institution:{name:"Alagappa University",institutionURL:null,country:{name:"India"}}}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_1_2",title:"1.1. Classification of polymer electrolyte systems",level:"2"},{id:"sec_1_3",title:"1.2.1. Polyelectrolyte’s ",level:"3"},{id:"sec_2_3",title:"1.2.2. Solvent swollen polymer electrolytes",level:"3"},{id:"sec_3_3",title:"1.2.3. Solvent free polymer electrolytes",level:"3"},{id:"sec_5_2",title:"1.3. Blend polymer electrolytes",level:"2"},{id:"sec_6_2",title:"1.4. Some commonly available polymer electrolytes for lithium ion batteries",level:"2"},{id:"sec_6_3",title:"1.4.1. PEO based electrolytes",level:"3"},{id:"sec_7_3",title:"1.4.2. PVC based electrolytes",level:"3"},{id:"sec_8_3",title:"1.4.3. PAN based polymer electrolytes",level:"3"},{id:"sec_9_3",title:"1.4.4. PVdF based polymer electrolytes",level:"3"},{id:"sec_10_3",title:"1.4.5. PMMA based electrolytes ",level:"3"},{id:"sec_11_3",title:"1.4.6. PVdF-co-HFP based polymer electrolytes ",level:"3"},{id:"sec_12_3",title:"1.4.7. PVAc based polymer electrolytes",level:"3"},{id:"sec_15",title:"2. Basic requirements of polymers and the salt for polymer electrolytes",level:"1"},{id:"sec_15_2",title:"2.1. Importance of Li+ cation",level:"2"},{id:"sec_16_2",title:"2.2. Preparation of polymer blend electrolytes",level:"2"},{id:"sec_18",title:"3. Characterization of polymer blend electrolytes",level:"1"},{id:"sec_18_2",title:"3.1. FTIR analysis",level:"2"},{id:"sec_19_2",title:"3.2. X-ray diffraction analysis",level:"2"},{id:"sec_20_2",title:"3.3. Ac impedance analysis",level:"2"},{id:"sec_21_2",title:"3.4. TG/DTA analysis",level:"2"},{id:"sec_22_2",title:"3.5. SEM analysis",level:"2"},{id:"sec_23_2",title:"3.6. AFM analysis ",level:"2"},{id:"sec_25",title:"4. Conclusion",level:"1"}],chapterReferences:[{id:"B1",body:'AbrahamK. M.BrummerS. B.\n\t\t\t\t\t1983 “Secondary Lithium Cells”: “Lithium Batteries”Editor, Gabano, J.P. Academic Press, London\n\t\t\t'},{id:"B2",body:'AkashiH.ShibuyaM.OruiK.ShibamotoG.SekaiK.\n\t\t\t\t\t2002 Practical performances of Li-ion polymer batteries with LiNi0.8Co0.2O2, MCMB, and PAN-based gel electrolyte, J.Power Sources, 112\n\t\t\t\t\t2 (November 2002), 577582 , 0378-7753'},{id:"B3",body:'AliA. M. M.YahyaM. Z. A.BahronH.SubbanR. H. Y.HarunM. K.AtanI.\n\t\t\t\t\t2007 Impedance studies on plasticized PMMA-LiX [X: CF3SO3−, N(CF3SO2)2−] polymer electrolytes, Mater.Lett.\n\t\t\t\t\t61\n\t\t\t\t\t10 (April 2007), 20262029 , 0016-7577X\n\t\t\t'},{id:"B4",body:'AmaralF. A.DalmolinC.CanobreS. C.NerilsoB.Rocha-FilhoR. C.BiaggioS. 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D.\n\t\t\t\t\t2007 Crystallinity, morphology, mechanical properties and conductivity study of in situ formed PVdF/LiClO4/TiO2 nano composite polymer electrolytes, Electrochimi.Acta, 52\n\t\t\t\t\t9 (February 2007), 31813189 , 0013-4686\n\t\t\t'},{id:"B49",body:'WangZ.L.TangZ.Y.\n\t\t\t\t\t2004 A novel polymer electrolyte based on PMAML/PVDF-HFP blend, Electrochimi.Acta,\n\t\t\t\t\t49\n\t\t\t\t\t7 (March 2004), 10631068 , 0013-4686'},{id:"B50",body:'XiJ.QiuX.LiJ.TangX.ZhuW.ChenL.\n\t\t\t\t\t2006 PVDF-PEO blends based microporous polymer electrolyte: Effect of PEO on pore configurations and ionic conductivity, J.Power Sources, 157\n\t\t\t\t\t1 (June 2006), 501506 , 0378-7753'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"M. Ulaganathan",address:null,affiliation:'
Energy Research Institute @ NTU, Nanyang Technological University, Singapore, Singapore
School of Physics, Alagappa University, Karaikudi, Tamil Nadu, India
Energy Research Institute @ NTU, Nanyang Technological University, Singapore, Singapore
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1. Introduction
Teeth are a topic of interest to paleontologists because they are very well preserved. As a matter of fact, the dental remains have made it possible to study the evolution of mammals by analyzing their morphology. In developmental biology, the mouse model is an interesting model for studying dental development.
Humans have two dentitions (temporary and permanent) and different types of teeth, incisor, canine, premolar, and molar with different morphologies, whereas mice only have two types (incisor and molar) separated by a diastema from which the incisors have unlimited growth. Despite these differences, the dental development process is similar in humans and mice, and regulatory phenomena have been maintained over the evolution.
Teeth, such as mammary glands, hair, and feathers, develop from two adjacent tissues: the epithelium and the mesenchyme, although they all have different morphologies. Indeed, during development, the specific shape of each organ is defined in relation to epithelial-mesenchymal proliferation and to all the changes that the epithelium undergoes [1].
The embryological aspect of the molars was addressed in order to clarify the etiopathogenic aspect and to adapt therapeutic attitudes according to the diagnosis.
The objective of this chapter is to address the embryology of human molars by focusing on its molecular and morphological characteristics.
2. Phylogenetic aspects
Teeth represent a new morphological feature of mammals [2, 3]. Molars are complex teeth able to become occluded. Interlocking intercuspation between upper and lower molars allows food to be crushed [4]. Evolutionary dietary radiations are related to the great diversity of the current mammalian molars. They are clarified in the fossil record, where new molar organizations are often related to significant line diversifications. Several theories have been advanced to explain the evolution of molars. Like all primates, Man is a placental mammal, and the ancestor of contemporary humans is Homo sapiens. For 200 million years, in Therian mammals, the molars have trigonodontal morphology; in other words, the three tubercles are arranged in a triangle [5].
In 1965, the discovery of a fossil of a lower molar made it possible to show that on this Therian branch around 135 million years ago, these molars already existed. They were called tribosphenic by Simpson in 1936 [6]. These mandibular molars have six tubercles, three of which are pointed, high, sharp, and are arranged in a triangle and distal position. The three others tubercles are lower and are arranged in a central basin to receive the main palatal tubercle of the opposite teeth that have only three cusps. The fact of having six tubercles is of physiological interest when taking food.
Nearly 110 million years ago, the oldest placental mammals had a dental formula with 52 teeth, including 3 molars in a decreasing series, the first being the largest. This primitive disposition is found in modern man.
Around 75 million years ago, with the dinosaurs extinction, other species invaded space, and the dental formula was reduced to 44 teeth for all placental mammals including the man.
In the Catarrhini, the loss of one incisor and two premolars leads to a dental formula with 32 teeth found in monkeys of the ancient world (Afro-Eurasia), the Hominids, and the contemporary Men. It has been recognized for 45 million years [7].
In the genus Homo, the 32-teeth morphology does not differ much from the modern men, except for the great variability in size. Root morphology may vary from one group to another. The reduction in the number of cusps observed in humans can be considered as a specialization trait and not as a step backward. However, the reduction in the dental formula in the placentals and primates mainly affected the incisors, premolars, and even canines but not the molars.
Wisdom tooth agenesis, especially mandibular agenesis, is often considered as a sign of evolution. On the other hand, the presence of supernumerary teeth or hypergenesis is explained as a return to ancestral forms
3. Morphological aspects
3.1 Formation of the odontogenic epithelium
The odontogenic epithelium is formed from the oral epithelium that lines the primary oral cavity called the “stomodeum.” It appears as a localized thickening of the oral epithelium, and it is formed by several cellular layers resulting from a series of localized mitoses affecting the oral epithelium. The mitotic spindle of dividing cells is oriented perpendicular to the basal membrane that separates the epithelium from the ectomesenchyma.
3.2 Placement of the vestibular and primary dental blades
Epithelial thickening continues to proliferate and sinks into the underlying ectomesenchymal tissue forming a plunging wall (also called a primitive dental blade). This latter splits into two blades: vestibular and dental. The vestibular blade determines the formation of the buccal vestibule, which is the space between the cheek/lip and the dental arch.
3.3 Evolution of dental placodes
In humans, as in rats and mice, the dental blade will give birth to the dental placodes that will be at the origin of the formation of future dental germs. Dental placodes are cellular clusters attached to the dental blade by a net of epithelial cells called the primary dental blade. Each dental arch initially contains 10 dental placodes. From the primary dental blade develops the secondary dental blade, which is at the origin of the 16 permanent teeth per arch.
Each placode will undergo morphological changes that are described as three successive stages: bud stage, cup stage, and bell stage [1].
4. Placement of molar dental germs
Since the three molars are not preceded by temporary teeth, they evolve from the distal end of the initial dental blade, which proliferates in a posterior direction. The primary dental blade of the second temporary molar will cause the formation of four secondary dental blades. For each half of the arch, starting from the anterior area toward the posterior area, each of these four secondary dental blades will give the permanent germ of the following teeth: the first permanent molar, the second permanent molar, and the third permanent molar.
The secondary dental blades that are at the origin of the formation of the 1st and 2nd molar will orient themselves vertically as long as they have space that allows them to orient themselves in the mesenchyma. On the other hand, in most cases for the 3rd molar, orientation problems arise because there is not enough space for its secondary dental blade to be parallel to the other two blades [8].
All dental buds, with the exception of the second and third permanent molars, are present and begin to develop before birth [9]. The chronology of the appearance of molar germs remains variable according to the authors; however, it is often found that the germ of the first molar appears around the 4th or 5th month of intrauterine life. The one of the second molar appears around the 9th month or 1 year after birth.
The germ of the third molar does not appear until around 4 or 5 years of age. Mineralization begins between 7, 9, and 10 years, and the crown is completed between 12 and 16 years. The emergence in the oral cavity is between 17- and 21-year-olds; the tooth will then slide along the distal surface of the second molar to reach the occlusion level. Root building ends between the ages of 18 and 25 years. The place it has depends on the growth in the posterior region of the arch. The main activity of the dental blade is spread over a period of about 5 years. However, the dental blade near the third molar continues to be active until about 15 years of age [9].
A number of anomalies can occur during the development of the tooth. The development of excess dental blade can lead to an increase in the number of dental buds, resulting in too many teeth (supernumerary). A deficient dental blade can lead to a reduction in the number of teeth (hypodontia) [9].
5. Root formation
Molars are multiradiculated teeth. Indeed, the vast majority of the first maxillary molars have three roots. The second maxillary molar has more frequent variations in the number of roots than the first maxillary molar, and the first mandibular molar and the second have two roots in the majority.
Root formation or radiculogenesis or rhizagenesis is the development of the root pulpo-dentinary organ in close relationship with cemenesis, the outline of the dentoalveolar ligament and the construction of the alveolar bone. It begins when the final dimensions are acquired. The Hertwig epithelial sheath is at the origin of root formation, depending on their number, shape, and size [10].
As for the crown, root development is governed by interactions involving the Hertwig epithelial sheath, basement membrane, mesenchymal papilla, and dental follicle.
5.1 Formation of the Hertwig epithelial sheath
The Hertwig epithelial sheath originates from the reflection zone or cervical loop which is the place where the external and internal adamantin epitheliums (EAE and EAI) meet to form a double epithelial layer. Hertwig epithelial sheath has an annular structure surrounded by a basal membrane that separates it from the pulpal and follicular mesenchyma. This basement membrane has anchoring fibrils on the pulp side. The internal epithelium faces the papilla and the external epithelium faces the dental follicle. The Hertwig epithelial sheath will emit tongues in the centripetal direction that will fuse in the central region of the papilla and form rings from which the roots can be identified. The number of strips emitted is proportional to the number of roots that each molar can have. For example, for the molar which will have two roots, two tongues are formed, and after fusion of two rings, each of the two will be at the origin of the formation of a root. These two leaves remain attached and progress in the underlying connective tissue in the apical direction defining the future shape of the dental root [11].
Root elongation and tissue formation are related to the coordinated proliferation of sheath epithelial cells and surrounding mesenchymal cells [12].
5.2 Formation of root dentin, cement, and apex
Root dentin forms in parallel with the proliferation in the apical direction of the Hertwig sheath. The latter gradually induces odontoblastic differentiation. The pulp parenchyma cells close to the anchor fibrils differentiate into odontoblasts. These odontoblasts produce preentine, which mineralizes to form dentin. The cells of the outer dental epithelium forming the outer layer of the sheath do not differentiate into ameloblasts as is the case for the crown. Then, the basement membrane degrades, and the epithelial blade involutes and gradually dissociates.
Developmental defects of the Hertwig sheath at the apical third of the root are at the origin of the formation of the lateral canals following a stop of dentinogenesis at this site due to the nondifferentiation of pulp fibroblasts into odontoblasts.
The cells of the sheath can undergo three spells: some can form the “Malassez epithelial debris,” others can die by apoptosis, while others can undergo epithelial-mesenchymal transformation.
As the sheath disintegrates, follicular cells near the surface of the root dentin differentiate into cementoblasts. These synthesize and deposit the cement matrix in contact with the dentin.
As the root development progresses, the epithelial ring forming the Hertwig epithelial sheath gradually shrinks as a result of a reduction in mitosis, thereby reducing the size of the root tube. This narrowing allows the development of one or more orifices (or foramina), which are the place where vascular and nervous elements intended for the pulp to pass through.
The development of the root ends with the construction of the apex, which is a slow process. In humans, for example, for the 1st permanent molar, this operation is performed until the age of 9–10 years. In the case of permanent teeth, this phenomenon lasts longer and requires more time than the development of the root itself.
6. Molecular aspects
6.1 Epithelial-mesenchymal interactions
In humans, dental development includes the morphogenesis of crowns and roots and results in the formation of the enamel organ, odontoblastic, ameloblastic, and cementoblastic differentiation. Huge advances in research have made it possible to understand the phenomena of molecular regulation of dental development.
Dental development follows a precisely controlled and regulated genetic program. The dental organ consists of an epithelial part that derives from the ectoderm and a mesenchymal part that derives from mesodermal cells on the one hand and cells from neural ridges on the other hand [13, 14, 15, 16].
The dental organ develops from a communication between the epithelium and the underlying mesenchyma. The communication language has been preserved throughout the evolution. This communication between the epithelium and the mesenchyma is done through signaling molecules and growth factors [17, 18, 19].
The studies carried out on the mouse molar have enabled us to gather a body of knowledge with many similarities to those of humans. However, the experimental data obtained in animals can be extrapolated relatively reliably to understand what is actually happening in humans.
Several families have been described, including:
TGF-beta (transforming growth factor beta) including BMP (bone morphogenetic proteins) activins and follistatin;
FGF (Fibroblast growth factors);
Hedgehog (only Sonic hedgehog (Shh) is known for its role in odontogenesis);
These molecules send their message to the nucleus through the signaling pathways and receptors on the cell membrane surface. Transcription factors will then modulate the expression of different target genes and induce changes in cell response and behavior (Figure 1) [25].
Figure 1.
Signaling in tooth development [25].
Genes represented in “light blue” colored squares or rectangles are responsible, when inactivated, for stopping dental development.
6.2 Determination of the dental region
It should be remembered that the odontogenic epithelium is formed at the first gill arch. The latter undergoes pharyngeal regionalization, resulting in the expression of Fgf8 and 9 (fibroblast growth factors 8 and 9) and Lhx-6 and -7 (LIM homeobox 6 and 7) in the oral part (rostral) and Gsc (goosecoid) in the aboral part (caudal). Indeed, the expression of Fgf8 in the odontogenic epithelium in the oral part of the first pharyngeal arch causes the expression of Lhx-7 in the underlying ectomesenchyma. In the aboral region, there is an important expression of Gsc in the ectomesenchyma. Gsc expression in the caudal region is not responsible for inhibiting Lhx-7 expression in this area; however, Lhx-7 expression in the rostral region will result in blocking Gsc gene expression in this.
In addition to Fgf8, a second BMP4 signaling molecule (bone morphogenetic protein 4) is expressed in the epithelium in the distal and therefore in the median region of the 1st arc.
The activation and inhibition of transcription factors allows the delimitation of the odontogenic territory by BMP4 and Fgf8a double signalling. (Figure 2) [19].
Figure 2.
Pattern of gene expression in the developing tooth [19]. (a) Signaling within the epithelium and between the epithelium and the mesenchyme at embryonic day (E) 10.5. The diagram shows an isolated mandibular arch. Positive autoregulatory loops and mutual repression within the epithelium lead to the formation of strict boundaries of gene expression, which sets up the presumptive incisor and molar fields. Members of the bone morphogenetic protein (BMP) and fibroblast growth factor (FGF) families of protein in the epithelium induce and inhibit the expression of various homeobox genes. This results in a complex pattern of gene expression in the mesenchyme, across both the proximal–distal and oral–aboral/rostral–caudal axes. (b) The odontogenic homeobox code model of dental patterning. The nested expression pattern of homeobox genes in the mandible produces a homeobox code that defines tooth type. Bapx1 (bagpipe homeobox gene 1 homolog); Barx1 (BarH-like homeobox 1); Dlx (distalless homeobox); Gsc (goosecoid); Lhx (LIM homeodomain genes); Msx (homeobox, msh-like); Pitx (paired-related homeobox gene).
6.3 Determination of dental identity
Mammalian teeth are meristic series. The determination of different morphology was explained by two theories:
The gradient theory proposed by Butler [26] which stipulates the presence of morphogenetic fields and that the determination of the shape of the tooth is a function of its position in the field independent of local factors.
The theory of clones proposed by Osborn [27] which stipulates that ectomesenchyma is already differentiated into three cellular clones, incisal, canine, and molar clones, before its migration. The proposal of this second concept suggested that the two theories are competing.
In 1995, the theory of odontogenic homeocode was developed by Sharpe [22], which represents a synthesis of the two theories: gradients and clones and shows that the latter two are complementary. These two concepts were explained in the light of the discovery of new genes and signaling molecules (Figure 3) [26, 27, 28].
The identity of each tooth, including the molars, is characterized by its homeocode, which represents the combination of homeogens that defines the position and identity of the tooth. Indeed, different homeogens are expressed by the neural crest cells of the ectomesenchyma under the instructive induction of the oral epithelial cells. These homeogens are divergent and therefore of the nonhox type.
This odontogenic homeocode theory involves four homogenous genes: muscle segment homeodomain-homeobox 1 (Msx-1), muscle segment homeodomain-homeobox 2 (Msx-2), distal-less homeobox 1 (Dlx1), and goosecoide. In the molar sector, Msx-1 and Dlx-1 are expressed and Msx-2 and goosecoide are not expressed. In the canine sector, Msx-1, Msx-2, and goosecoide are expressed, and Dlx-1 is not expressed; in incisal sector, Msx-1 and goosecoide are expressed, Msx-2 and Dlx-1 are not expressed.
In the concept of morphogenetic fields, the consideration of various genetic factors and their epigenetic modulation influences dental development [29].
According to Mitsiadis’ work in 2006, the three models, gradients, clones, and homeocodes, could be grouped into a single model to explain dental identity. Indeed, dental identity, including molars, is given by the presence of morphogenetic fields defined by the diffusion of growth factors. The odontogenic epithelium expresses gradients of signaling molecules that are mainly Fgf, Bmp, Shh, and Wint that will diffuse to the underlying mesenchymal tissue containing neural peak cells. Depending on the location and instruction received by these cells, they will express a set of divergent genes in relation to concentrations of signaling molecules. The locally defined tooth type is related to the locally expressed divergent homeogen combinatorics of these ridge cells (Figure 4) [30].
Figure 4.
Dental identity determination (adapted from Ref. [30]).
The Mitsiadis model combines the three concepts: morphogenetic fields, clone, and odontogenic homeocode.
These three models should be viewed as complementary rather than contradictory and propose that this unifying view can be extended into the clinical setting using findings on dental patterning in individuals with missing teeth. The proposals are compatible with the unifying etiological model developed by Brook in 1984 based on human epidemiological and clinical findings. Indeed, this new synthesis can provide a sound foundation for clinical diagnosis, counseling, and management of patients with various anomalies of dental development, as well as suggesting hypotheses for future studies.
6.4 Molecular factors involved in root formation
The root development process involves a set of signaling cascades. Various growth factors, including BMPs (bone morphogenetic proteins), EGF (epidermal growth factor), IGF (insulin-like growth factor), FGF (fibroblast growth factor), transcription factors Msx1, Msx2, Runx-2, Sonic Hedgehog (Shh), enamel proteins (secreted by HGH cells), and other proteins such as follistatin and activin A, are involved in the root development process. Indeed, they are involved in the growth and/or differentiation of odontoblasts and cementoblasts and/or in the mineralization of dentin and/or cementum [21, 31, 32, 33, 34, 35, 36].
7. Signaling center (primary and secondary enamel knots)
Dental morphology is controlled by an epithelial signaling center called the enamel node. The node of the enamel is a particular and transient histological structure formed by a cellular cluster that appears at the basal part of the internal dental epithelium. The node of the primary enamel is present in the dental germs of all types of teeth including incisors.
Because the enamel nodes link cell differentiation to morphogenesis, Thesleff suggests that the latter can be considered as central regulators of dental development [37].
During molar development, the node of the secondary enamel is formed during the bell stage at the location of future cusp areas. At this point, the expression of signaling molecules precedes the folding and growth of the dental epithelium [38, 39].
The Slit1 gene is expressed in the nodes of the primary and secondary enamel during the formation of molar cusps [40].
8. Genes and dental problems
The approaches provided by Line and Mitsiadis have advanced the clinic’s understanding of dental identity establishment based on gradient, clone, and homeocode theories [29, 30].
The multifactorial model involving genetic, epigenetic, and environmental determinants has provided better explanations and helped to understand missing and supernumerary teeth in monozygotic twins [41].
In humans, dental problems are observed during pathologies of dental development or syndromes.
Mutations in genes known as divergent homeobox genes encoding transcription factors such as MSX1 and PAX9 (paired domain box gene 9) are at the origin of oligodontia. Indeed, a mutation in the homeobox of the MSX1 gene (substitution of an arginine by a proline in the homeodomain region) is associated with the agenesis of third molars, indicating the involvement of MSX1 in the dentition pattern [42, 43, 44].
Also, mutations in the PAX9 gene cause oligodontia characteristic of molars [45, 46, 47, 48]. The severity of dental agenesis appears to be correlated with the ability of the mutated PAX9 protein to bind to DNA [49].
A misdirection mutation during the sequencing of the PAX9 gene may explain a different phenotype of hereditary oligodontia observed in humans, which affects not only molars but also other tooth lines; and is characterized by tooth small size in both types of dentition. This mutation is characterized by a replacement of the amino acid arginine by tryptophan in a region entirely preserved in all genes of the matched sequenced box [50].
In humans, Pitx2 expression deficiency associated with Rieger syndrome is characterized by oligodontia [51].
9. Conclusion
The biological process is the same for all teeth, including molars, regardless of their identity, but epithelial signaling and homeogenic combination differ from one tooth type to another.
The study of first molar of the mouse has allowed us to better understand and follow the stages of dental development in humans. The general pattern remains the same, unlike the training time, the complexity of the dental system, the presence of two types of teeth in humans, and unlimited incisors growth in mice.
The multidisciplinary approach between fundamental and clinical research is essential to clarify the relationship between molecular involvement and clinical manifestations.
Understanding the molecular mechanisms of dental anomalies, including those affecting human molars, helps to propose diagnostic hypotheses and thus to improve patient management.
Future research should focus on synergizing molecular and genetic approaches to further analyze the action mechanisms of key genes involved in the development of human molars.
Conflict of interest
The authors declare that they have no conflicts of interest with the contents of this article.
\n',keywords:"tooth development, molar, morphological appearance, molecular regulation, epithelial-mesenchymal interaction",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/66644.pdf",chapterXML:"https://mts.intechopen.com/source/xml/66644.xml",downloadPdfUrl:"/chapter/pdf-download/66644",previewPdfUrl:"/chapter/pdf-preview/66644",totalDownloads:456,totalViews:0,totalCrossrefCites:0,dateSubmitted:"December 5th 2018",dateReviewed:"March 7th 2019",datePrePublished:"May 8th 2019",datePublished:"January 22nd 2020",dateFinished:null,readingETA:"0",abstract:"Dental development is a complex process by which teeth from embryonic cells grow and erupt into the mouth. It is governed by epithelio-mesenchymal interactions. The biological mechanism is the same for all teeth; however, epithelial signaling and homeogenous combinatorics are different from one type of tooth to another. The primary dental blade splits into the vestibular and primary dental blades opposite to the mesenchymal condensation. During dental development, three successive stages are described: bud, cup, and bell. The secondary dental blade responsible for the formation of germs in permanent teeth is formed from the primary dental blade in the bell stage. For the central incisor, lateral incisor, canine, first temporary molar, and second temporary molar, each primary dental blade gives rise to a single secondary dental blade for the corresponding permanent tooth. On the other hand, the primary dental blade of the second temporary molar will cause the formation of four secondary dental blades that will cause the formation of permanent germs of the second premolar, the first permanent molar, the second permanent molar, and the third permanent molar. The objective of this chapter is to focus on the cellular and molecular mechanisms explaining the normal development of molars by presenting the different current data and theories of science illustrating the human molar embryological development.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/66644",risUrl:"/chapter/ris/66644",signatures:"Fatiha Rhrich and Hakima Aghoutan",book:{id:"8837",title:"Human Teeth",subtitle:"Key Skills and Clinical Illustrations",fullTitle:"Human Teeth - Key Skills and Clinical Illustrations",slug:"human-teeth-key-skills-and-clinical-illustrations",publishedDate:"January 22nd 2020",bookSignature:"Zühre Akarslan and Farid Bourzgui",coverURL:"https://cdn.intechopen.com/books/images_new/8837.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"171887",title:"Prof.",name:"Zühre",middleName:null,surname:"Akarslan",slug:"zuhre-akarslan",fullName:"Zühre Akarslan"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:[{id:"172240",title:"Prof.",name:"Hakima",middleName:null,surname:"Aghoutan",fullName:"Hakima Aghoutan",slug:"hakima-aghoutan",email:"hakimadental@yahoo.fr",position:null,institution:null},{id:"288550",title:"Prof.",name:"Fatiha",middleName:null,surname:"Rhrich",fullName:"Fatiha Rhrich",slug:"fatiha-rhrich",email:"fatiharhrich@hotmail.com",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Phylogenetic aspects",level:"1"},{id:"sec_3",title:"3. Morphological aspects",level:"1"},{id:"sec_3_2",title:"3.1 Formation of the odontogenic epithelium",level:"2"},{id:"sec_4_2",title:"3.2 Placement of the vestibular and primary dental blades",level:"2"},{id:"sec_5_2",title:"3.3 Evolution of dental placodes",level:"2"},{id:"sec_7",title:"4. Placement of molar dental germs",level:"1"},{id:"sec_8",title:"5. Root formation",level:"1"},{id:"sec_8_2",title:"5.1 Formation of the Hertwig epithelial sheath",level:"2"},{id:"sec_9_2",title:"5.2 Formation of root dentin, cement, and apex",level:"2"},{id:"sec_11",title:"6. Molecular aspects",level:"1"},{id:"sec_11_2",title:"6.1 Epithelial-mesenchymal interactions",level:"2"},{id:"sec_12_2",title:"6.2 Determination of the dental region",level:"2"},{id:"sec_13_2",title:"6.3 Determination of dental identity",level:"2"},{id:"sec_14_2",title:"6.4 Molecular factors involved in root formation",level:"2"},{id:"sec_16",title:"7. Signaling center (primary and secondary enamel knots)",level:"1"},{id:"sec_17",title:"8. Genes and dental problems",level:"1"},{id:"sec_18",title:"9. Conclusion",level:"1"},{id:"sec_22",title:"Conflict of interest",level:"1"}],chapterReferences:[{id:"B1",body:'Pispa J, Thesleff I. Mechanisms of ectodermal organogenesis. Developmental Biology. 2003;262:195-205. DOI: 10.1016/S0012-1606(03)00325-7'},{id:"B2",body:'Tims HWM. The evolution of the teeth in the mammalia. Journal of Anatomy and Physiology. 1903;37(2):131-149. PMC1287046'},{id:"B3",body:'Luo ZX. Transformation and diversification in early mammal evolution. 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