\r\n\tIn sum, the book presents a reflective analysis of the pedagogical hubs for a changing world, considering the most fundamental areas of the current contingencies in education.
",isbn:"978-1-83968-793-8",printIsbn:"978-1-83968-792-1",pdfIsbn:"978-1-83968-794-5",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"b01f9136149277b7e4cbc1e52bce78ec",bookSignature:"Dr. María Jose Hernandez-Serrano",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10229.jpg",keywords:"Teacher Digital Competences, Flipped Learning, Online Resources Design, Neuroscientific Literacy (Myths), Emotions and Learning, Multisensory Stimulation, Citizen Skills, Violence Prevention, Moral Development, Universal Design for Learning, Sensitizing on Diversity, Supportive Strategies",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 14th 2020",dateEndSecondStepPublish:"October 12th 2020",dateEndThirdStepPublish:"December 11th 2020",dateEndFourthStepPublish:"March 1st 2021",dateEndFifthStepPublish:"April 30th 2021",remainingDaysToSecondStep:"4 months",secondStepPassed:!0,currentStepOfPublishingProcess:4,editedByType:null,kuFlag:!1,biosketch:"Dr. Phil. Maria Jose Hernandez Serrano is a tenured lecturer in the Department of Theory and History of Education at the University of Salamanca, where she currently teaches on Teacher Education. She graduated in Social Education (2000) and Psycho-Pedagogy (2003) at the University of Salamanca. Then, she obtained her European Ph.D. in Education and Training in Virtual Environments by research with the University of Manchester, UK (2009).",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"187893",title:"Dr.",name:"María Jose",middleName:null,surname:"Hernandez-Serrano",slug:"maria-jose-hernandez-serrano",fullName:"María Jose Hernandez-Serrano",profilePictureURL:"https://mts.intechopen.com/storage/users/187893/images/system/187893.jpg",biography:"DPhil Maria Jose Hernandez Serrano is a tenured Lecturer in the Department of Theory and History of Education at the University of Salamanca (Spain), where she currently teaches on Teacher Education. She graduated in Social Education (2000) and Psycho-Pedagogy (2003) at the University of Salamanca. Then, she obtained her European Ph.D. on Education and Training in Virtual Environments by research with the University of Manchester, UK (2009). She obtained a Visiting Scholar Postdoctoral Grant (of the British Academy, UK) at the Oxford Internet Institute of the University of Oxford (2011) and was granted with a postdoctoral research (in 2021) at London Birbeck University.\n \nShe is author of more than 20 research papers, and more than 35 book chapters (H Index 10). She is interested in the study of the educational process and the analysis of cognitive and affective processes in the context of neuroeducation and neurotechnologies, along with the study of social contingencies affecting the educational institutions and requiring new skills for educators.\n\nHer publications are mainly of the educational process mediated by technologies and digital competences. Currently, her new research interests are: the transdisciplinary application of the brain-based research to the educational context and virtual environments, and the neuropedagogical implications of the technologies on the development of the brain in younger students. Also, she is interested in the promotion of creative and critical uses of digital technologies, the emerging uses of social media and transmedia, and the informal learning through technologies.\n\nShe is a member of several research Networks and Scientific Committees in international journals on Educational Technologies and Educommunication, and collaborates as a reviewer in several prestigious journals (see public profile in Publons).\n\nUntil March 2010 she was in charge of the Adult University of Salamanca, by coordinating teaching activities of more than a thousand adult students. She currently is, since 2014, the Secretary of the Department of Theory and History of Education. Since 2015 she collaborates with the Council Educational Program by training teachers and families in the translation of advances from educational neuroscience.",institutionString:"University of Salamanca",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"University of Salamanca",institutionURL:null,country:{name:"Spain"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"23",title:"Social Sciences",slug:"social-sciences"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"301331",firstName:"Mia",lastName:"Vulovic",middleName:null,title:"Mrs.",imageUrl:"https://mts.intechopen.com/storage/users/301331/images/8498_n.jpg",email:"mia.v@intechopen.com",biography:"As an Author Service Manager, my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"6942",title:"Global Social Work",subtitle:"Cutting Edge Issues and Critical Reflections",isOpenForSubmission:!1,hash:"222c8a66edfc7a4a6537af7565bcb3de",slug:"global-social-work-cutting-edge-issues-and-critical-reflections",bookSignature:"Bala Raju Nikku",coverURL:"https://cdn.intechopen.com/books/images_new/6942.jpg",editedByType:"Edited by",editors:[{id:"263576",title:"Dr.",name:"Bala",surname:"Nikku",slug:"bala-nikku",fullName:"Bala Nikku"}],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:"38715",title:"Application of Ionic Liquids in Hydrogen Storage Systems",doi:"10.5772/50154",slug:"application-of-ionic-liquids-in-hydrogen-storage-systems",body:'In the present world, individual mobility is mainly based on fossil hydrocarbons as transportable energy medium. Since there is a wide agreement on the future depletion of fossil resources, an alternative energy carrier, that can be transported efficiently, has to be found. One material, which is in many considerations suitable to fill this gap, is hydrogen.(Hamilton et al., 2009; Schlapbach & Zuttel, 2001) The major advantages of hydrogen for these purposes are the low weight, the high abundance of the oxide, i.e. water, and the environmental benignity of the waste oxidation product, also water. The major hindrance for a widespread application of hydrogen in mobile applications is its low density in the gaseous state. Since the compression or liquefaction of hydrogen respectively the transportation of the denser forms of hydrogen is accompanied by a manifold of problems, i.e. severe disadvantages in especially gravimetric efficiency, alternatives are sought after.(Eberle et al., 2009; Felderhoff et al., 2007; Hamilton et al., 2009; Marder, 2007; Staubitz et al., 2010)
Since there are some materials that consist of an amount of hydrogen, that is high enough to compete with the aforementioned physical storage solutions, the storage of hydrogen in a chemical compound is discussed intensively lately. One important compound with one of the highest hydrogen contents possible is ammonia borane. The application of ammonia borane and its derivatives for hydrogen storage is matter of research in the last decade as well as a compound as simple as formic acid, which is in this sense the hydrogenation-product of carbon dioxide.(Fellay et al., 2008; Loges et al., 2008; Scholten et al., 2010; Stephens et al., 2007)
The application of ammonia borane itself is more efficient than elemental hydrogen, but nevertheless accompanied by some problems as well. Since there is a worldwide infrastructure suitable for the deployment of liquid fuels, a solid fuel bears certain disadvantages competing with a liquid fuel. Another important aspect of fuels is the applicability, and here liquid fuels are also advantageous in comparison to solid fuels.
In conclusion it seems reasonable to search for a liquid fuel (-system). Regarding this assumption ionic liquids (ILs) promise advantages owing to their tunable physico-chemical properties.(Dupont & Suarez, 2006) Hydrogen-enriched materials or blends are as well in the focus of current research as catalytic decomposition.(Groshens & Hollins, 2009; Hugle et al., 2009; Jaska et al., 2003; Mal et al., 2011; Wright et al., 2011) ILs are investigated for their ability of supporting decomposition as well as solution of certain materials, including in some cases spent fuel products.(Bluhm et al., 2006; Wright et al., 2011) In some extent these approaches can be applied in combination.(Wright et al., 2011)
In the last two decades ionic liquids (ILs) have become very popular in various fields in chemistry.(Dupont et al., 2002; Dupont & Scholten, 2010; Dupont et al., 2011; Migowski & Dupont, 2007; Prechtl et al., 2010; Prechtl et al., 2011; Scholten et al., 2012) Their physico-chemical properties, i. e. non-flammable, non-volatile, highly solvating, in general weakly-coordinating, tunable polarity and good thermal stability make them highly attractive for various applications.(Dupont, 2004; Dupont & Suarez, 2006) Low melting (organic) salts are defined as IL if the melting point is below 100 °C.(Dupont et al., 2002; Hallett & Welton, 2011; Welton, 1999)
Selected examples for IL-cations: (a) imidazolium, (b) pyrrolidinium, (c) pyridinium, (d) ammonium, (e) phosphonium and (f) guanidinium. The side-chains are alkyl groups, which can also carry functionalities like alcohols, ethers, nitriles, etc. Usually weakly coordinating anions are used as counter-parts such as BF4-, PF6-, bistrifluoromethanesulfonylimide (NTf2-) etc.
The low melting points are a result of the reduced lattice energy originating from large ion-pairs and low symmetry of the cations (Figure 1).(Dupont, 2004; Dupont & Suarez, 2006; Krossing et al., 2006) Ionic liquids have been known since the early 20th century, though their predicted potential and wider application developed rapidly in the last two decades. For a more detailed historic introduction see the article by Wilkes. (Wilkes, 2002)
For different applications the physico-chemical properties of ILs can be modified by tailoring the cation and/or anion structures.(Chiappe et al., 2006; Cui et al., 2010; Fei et al., 2007; Yang et al., 2008; Zhao et al., 2004) It is possible to design the hydrophilicity or hydrophobicity, the viscosity as well as the coordinating properties, especially those implied by the anion. Another important aspect one has to keep in mind is the pKa value, since especially in imidazolium-ILs the C2-proton is fairly acidic(Dupont, 2011; Dupont et al., 2002; Prechtl et al., 2010; Welton, 1999) and metal ions form carbene complexes in some cases.(Xu et al., 2000) This can be avoided by protecting the C2-position with a methyl group. Some ILs are able to stabilize certain homogenous and heterogeneous catalysts against decomposition or agglomeration, which can be of great benefit.(Prechtl et al., 2010)
The outcome of a reaction is strongly influenced by the solubility of the reactants, intermediates and products. In the particular case of dehydrogenation reactions, the reaction is influenced by the rather low solubility of hydrogen gas in ILs driving the equilibrium to the desired side.(Anthony et al., 2002; Jacquemin et al., 2006) In recent research ionic liquids have been employed not only as solvent in dehydrogenation reactions, but also as storage materials (vide infra).
Suitable molecules for the storage of hydrogen have to fulfill several requirements. Since hydrogen is storable in elemental form as a gas or liquid, these molecular systems must bear certain advantages over storage as elemental hydrogen. The most impractical properties of elemental hydrogen are the low density of gaseous hydrogen and the high requirements to the storage system in case of compressed or liquid hydrogen. The amount of hydrogen (atmospheric pressure) required for a 500 km travel (6 kg) would require a tank volume of nearly 67 m³! To overcome this problem one is able to compress hydrogen into a reasonable volume. A 700 bar hydrogen storage tank is able to store the same amount of hydrogen in the volume of only 260 liters.(Eberle et al., 2009) Due to the severe pressure the tank has to withstand, the fuel including the tank weights 125 kg. This corresponds to a gravimetric efficiency of 4.8 %. Concerning liquid storage the losses due to boil off are considered too high for practical application, since they add up to the problems of a strongly isolated tank, i.e. gravimetric inefficiency. Since molecular hydrogen has these severe disadvantages, it seems reasonable to store hydrogen in a chemical way, where higher volumetric hydrogen density in the condensed phase is an obtainable target.
One important molecule in the focus of research is the simple adduct of ammonia and borane (AB). (Ahluwalia et al., 2011; Al-Kukhun et al., 2011; Basu et al., 2011; Bluhm et al., 2006; Staubitz et al., 2010; Stephens et al., 2007) This solid Lewis pair is stable towards air and water and consists of 19.6 % hydrogen. When heating this compound to 130 °C it loses 14 % of its weight as hydrogen.(Eberle et al., 2009) Undesired side-products in the decomposition-reaction can be ammonia, diborane and borazine, where the last is a standard decomposition product, that is only critical due to its high volatility contaminating the gas stream and lowering efficiency due to incomplete hydrogen release. For the complete dehydrogenation of AB temperatures of over 500 °C are required. The dehydrogenation of this compound leads via oligoamino boranes and polyamino boranes to insoluble polyborazylene (Figure 2), which is significantly stable in mechanical, chemical and thermal means.
Decomposition Pathway of Ammonia Borane.
Since the temperature to decompose ammonia borane completely is so high and the according product is remarkably stable, complete dehydrogenation is undesired. As above mentioned, partial dehydrogenation leads to a capacity of around 14 wt% which is still enough to be considered as efficient hydrogen storage material.
Regarding the regeneration of spent fuel Sutton and co-workers recently presented meaningful results.(Sutton et al., 2011) The solution of AB spent fuel in liquid ammonia could be quantitatively reduced by hydrazine to yield AB, with gaseous nitrogen as the only by-product.
Several derivatives of AB have been studied recently. The most important are: hydrazine borane (HB),(Hugle et al., 2009) guanidinium borohydride (GBH),(Groshens & Hollins, 2009) ethylenediamine bisborane (EDB),(Neiner et al., 2011) methylguanidinium borohydride (Me-GBH)(Doroodian et al., 2010) and different alkyl amine boranes (Figure 3).(Bowden et al., 2008; Mal et al., 2011) On the frontier between molecular and metal hydride storage materials are the metal amido borane compounds, which are not in the scope of this chapter.(Chua et al., 2011)
A derivative of AB with a comparable weight efficiency has been studied by Lentz and co-workers recently: hydrazine borane (HB).(Hugle et al., 2009) Much of the hydrogen content of pure HB is thermally available, but the efficiency of release could be significantly improved by combining HB with the hydride-donor LiH: Though blending with LiH in 1:1 molar ratio lowers the theoretical gravimetric hydrogen density from 15.4 wt% to 14.8 wt% the actual release of hydrogen reached nearly 12 wt% at 150 °C in 4.5 h. The idea of combining HB with a hydride-donor arose from the fact that HB has an excess acidic hydrogen atom, since it consists of four acidic but only 3 hydridic hydrogen atoms. The released gas stream showed to consist of mainly hydrogen with an impurity of ammonia present in the range of <1%. The solid residue showed to be reactive towards water and completely insoluble in organic solvents. Hydrazine bisborane, a molecule very similar to HB, with a hydrogen content a little higher than HB, is not considered due to stability problems. The authors reported that rapid heating or temperatures above 160 °C lead to explosive decomposition.
Structures of selected molecular hydrogen storage materials.
Guanidinium borohydride (GBH) and blends containing GBH were investigated by Groshens and co-workers showing remarkable results.(Groshens & Hollins, 2009) The material consists of the guanidinium ion contributing acidic protons and borohydride for hydridic hydrogen atoms. As this material consists only of light weight atoms and hydrogen, the theoretical capacity is 10.8 wt%. The exothermic reaction results in a self-sustaining decomposition when initiated by a heat source. Nearly quantitative release of hydrogen was observed with a distinct impurity of ammonia of about 5 %. The imbalance of acidic and hydridic hydrogen atoms is a factor susceptible to improvement by blending. The material of choice for blending was ethylene diamine bisborane, which contributes two excess hydridic hydrogen atoms to the mixture. As shown in figure 4 the blending results in the maintenance of hydrogen yield, while suppressing the formation of undesirable ammonia. This effect is exceptionally strong in the mixtures containing approximately equimolar amounts of both materials.
GBH-EDB Self-Sustaining-Thermal-Decomposition. Mixture containing 60 wt% EDB is not self-sustaining.(Groshens & Hollins, 2009)
In comparison to pure GBH, that decomposes with an impurity of ammonia of 4.1 mol% in the gas stream, resulting in a hydrogen yield of 10.6 wt%, the 40:60 wt% mixture of GBH and EDB releases 10.1 wt% of hydrogen with an impurity of ammonia as low as 0.026 mol%. The solid state of this material(-blend) is one major drawback.
The decomposition of pure EDB is comparably efficient to that of the blend mentioned above.(Neiner et al., 2011) The characteristics in decomposition are especially interesting due to the purity of released hydrogen without additives. No volatile by-products are released up to a temperature of 200 °C. In addition the decomposition achieves release rates comparable to AB.
In recent years catalytic splitting of formic acid into hydrogen and carbon dioxide has drawn some interest (Figure 4). (Boddien et al., 2011; Enthaler et al., 2010; Johnson et al., 2010; Scholten et al., 2010; Tedsree et al., 2011; Yasaka et al., 2010; Zhao et al., 2011)
Reversible splitting of formic acid.
Though the hydrogen storage capacity of 4.4 wt% stays behind that of several other materials, the simplicity and wide availability of carbon dioxide as educt make formic acid attractive for hydrogen storage. In chemical means formic acid can be utilized as hydrogen source for catalytic hydrogenation reactions. (Blum et al., 1972; Bulushev & Ross, 2011; Kawasaki et al., 2005)
The unique physico-chemical properties of ILs make it possible to use them for different applications in hydrogen storage systems. The most simple one is to use a low molecular weight, hydrogen rich IL as hydrogen storage material. This approach has been realized in two different ways, which are presented below. Other possible applications are as inert solvent, as a catalytically active solvent, as a co-catalyst or as a stabilizing agent e.g. for nanoparticles, as presented afterwards.
Introducing one methyl group into a GBH molecule results in the first reported IL that can be efficiently dehydrogenated (Figure 6).(Doroodian et al., 2010)
Structure of methyl guanidinium borohydride.
Me-GBH has a storage capacity slightly reduced in compraison to GBH. Rieger and co-workers modified GBH by introducing a methyl group. As the methyl group lowers the cation’s symmetry and, consequently, lowers the melting point,(Mateus et al., 2003) this salt is an IL, i.e. liquid below 100 °C. Furthermore with a melting point of -5 °C Me-GBH is the first room temperature IL that can be readily dehydrogenated with a reasonable gravimetric efficiency having a theoretical capacity of 9.0 wt%. Kinetic investigations by Rieger and co-workers about the thermal decomposition (75 °C) showed the decomposition of this material to be insufficiently slow and too inefficient for application. In the course of the decomposition some mass loss exceeding the theoretical capacity of the substrate is observed and consequently cannot be assigned to hydrogen evolution. Temperatures above 120 °C result in a detectable ammonia amount in the gas stream. The authors reported around 9 wt% hydrogen yield determined by TGA and volumetric quantification. The dehydrogenation product is solid and insoluble in the IL. To improve the rate and extent of hydrogen generation Wilkinson’s catalyst ((PPh3)3RhCl) and FeCl2 were employed with moderate success.
Initial attempts using an imidazolium IL containing a cyclohexyl moiety as hydrogen carrier were reported by Dupont and co-workers.(Stracke et al., 2007) This group used commercial palladium on charcoal catalyst and rather harsh conditions in the dehydrogenation/hydrogenation cycles. Despite the theoretical storage capacity of this system being insignificant, this was the first report of an IL being employed as hydrogen storage material. Chemically this procedure is based on the reversible dehydrogenation of a cyclohexyl group (Figure 7).
Structure of cyclohexyl-ILs for hydrogen storage by Dupont and co-workers.(Stracke et al., 2007)
The strong thermal stress (300 °C), required for fast dehydrogenation, and low weight efficiency are the most severe drawbacks of this system. The thermal stability of some of the employed ILs is remarkable.
Dimethyl amine borane (DMAB) is another derivative of AB able to decompose releasing hydrogen. It has been studied for mechanistic investigations, since the two additional methyl groups inhibit further dehydrogenation after the first equivalent of hydrogen. The group of Manners investigated catalytic dehydrocoupling of different disubstituted amine boranes for the selective formation of cyclic dimers and trimers at ambient temperatures.(Jaska et al., 2003) These investigations were found to be important for mechanistic considerations in the dehydrogenation of amine boranes (see section 2.2.1). The dehydrogenation of DMAB proceeds via the diammoniate of diborane to the cyclic dimer.(Zahmakiran & Ozkar, 2009) The group of Özkar found DMAB to reduce the dimeric rhodium(II)-hexanoate to rhodium(0) forming Rh-clusters and dimethyl ammonium hexanoate (Figure 8).
The formed nanoclusters (~2 nm) were tested for catalytic activity in the dehydrogenation of dimethyl amine borane and found to be highly active. The in-situ generated IL dimethyl ammonium hexanoate was found to act as protecting agent for the nanoparticles.
Another interesting option is the employment of an ionic liquid (IL) as active solvent supporting the dehydrogenation of AB.(Bluhm et al., 2006; Himmelberger et al., 2009)
Rhodium nanoparticle formation and catalytic decomposition of dimethyl amine borane. Reprinted with permission from (Zahmakiran & Ozkar, 2009). Copyright (2009) American Chemical Society.
Structures of employed ILs by Sneddon and co-workers.(Himmelberger et al., 2009)
Figure 10 displays the hydrogen release results from Toepler pump measurements of the decomposition reactions of 50 wt% of AB in different ILs at 85 °C. Whereas the decomposition in pmmimTf3C is comparable to the decomposition of neat AB (compare Figure 11(left)), every other tested IL improves the hydrogen yield significantly, though initial rates of hydrogen release do not relate strictly to the amount of overall released hydrogen.
Deeper investigations were conducted on the decomposition of AB in 1-butyl-3-methyl-imidazolium chloride ([BMIM]Cl). The application of this IL results in enhanced kinetics (Figure 11) and improved hydrogen yield. As shown in figure 11 (left) the hydrogen yield at a temperature as low as 85 °C can be more than doubled by addition of [BMIM]Cl implicating that a 50 wt% mixture of AB and [BMIM]Cl has a better weight-efficiency than pure AB.
H2-release measurements (Toepler pump) of the reaction of 50 wt% AB (250 mg) at 85 °C in 250 mg of (A) [BMMIM]Cl, (B) [BMIM]Cl, (C) [EMMIM][EtSO4], (D) [BMIM]BF4, (E) [MMIM][MeSO4], (F) [BMIM]OTf, (G) [EMMIM]OTf, (H) [BMIM]I, (I) [BMIM]PF6, and (J) [PMMIM]Tf3C. Reprinted with permission from (Himmelberger et al., 2009). Copyright (2009) American Chemical Society.
Left) H2-release measurements at 85 °C of: (A) 50-wt% AB in [BMIM]Cl and (B) solid-state AB (Right) H2-release measurements of 50-wt % AB in [BMIM]Cl at (A) 110 °C, (B) 105 °C, (C) 95 °C, (D) 85 °C, and (E) 75 °C. Reprinted with permission from (Himmelberger et al., 2009). Copyright (2009) American Chemical Society.
Only trace amounts of volatile borazine are identified in the gas stream indicating that its formation is suppressed or borazine is soluted readily by the IL. As can be seen, the addition of [BMIM]Cl prevents induction times and promotes dehydrogenation. This effect persists, if the amount of IL is reduced to 20 wt%. In direct comparison, the promoted dehydrogenation at 75 °C releases an equal amount of hydrogen as neat AB at 85 °C but without the induction time. An increase in temperature leads to a slight increase in quantity of hydrogen and an intense acceleration: The dehydrogenation at 85 °C results in a release of about 2.1 equivalents of hydrogen in 250 minutes and at 110 °C approximately 2.3 equivalents are released in less than 30 minutes.
Employing a metal complex as catalyst is an option to improve reaction kinetics and optimize low temperature application for the demands of hydrogen-storage materials for transportation applications.(Alcaraz & Sabo-Etienne, 2010; Jaska et al., 2003) This idea was combined with the idea of using ILs as supporting solvents. Sneddon and co-workers reported that ILs, loaded with different precious metal (Rh, Ru, Pd) or Ni-based pre-catalysts, decrease the onset temperature (45–85°C) of AB-decomposition significantly improving hydrogen yield at the same time (Figure 12).(Wright et al., 2011)
Hydrogen evolution from AB-decomposition at 65 °C catalyzed by different metal catalyst-precursors. Reproduced from (Wright et al., 2011) with permission of The Royal Society of Chemistry.
Though there were no deeper investigations concerning the active species, many of the precursors are known to form nanoparticles when being treated with a reducing agent.(Migowski & Dupont, 2007) This leads to the assumption that metal(0)-nanoparticles are involved in at least some of the catalyses. It is clearly visible that many of the employed precursors evoke a severe acceleration of hydrogen release as well as improving yield significantly as well. The shown results were obtained in experiments with 5 mol% of the respective catalyst.
In recent work Baker and co-workers employed another substrate blend for catalytic decomposition in IL.(Mal et al., 2011) The utilized mixture consisted of AB and sec-butyl amine borane (SBAB). The decomposition of this blend in the IL 1-ethyl-3-methylimidazolium ethyl sulfate ([EMIM][EtSO4]) leaves only a solution of products behind. The formation of insoluble polyamino borane is effectively hindered. Instead the formation of the cyclic (formal trimeric) borazine derivative is observed (Figure 13).
Observed decomposition products of SBAB decomposition.(Mal et al., 2011)
The alkyl group decreases the gravimetric efficiency to 5 wt%. This value was achieved by a metal catalyzed dehydrogenation reaction at 80 °C employing 1% RuCl2(PMe4)3 as catalyst-precursor. Concerning the purity of the released hydrogen no investigations have been reported yet.
A very interesting application of ILs is the utilization as solvent and base at the same time. In the decomposition of formic acid this can be realized by the employment of the amine-functionalized imidazolium-IL 1 (Figure 14). (Li et al., 2010; Scholten et al., 2010)
Structure of amino-functionalized IL 1.(Li et al., 2010; Scholten et al., 2010)
While the Dupont group reported only about the application of the chloride IL 1, the Shi-group used various anions, i.e. BF4-, OTf-, NTf2- and HCOO-. Both groups used the catalyst (-precursor) [(p-Cymene)RuCl2]2, investigations of the Dupont group suggested the formation of hydrogen bridged and hydrogen/formate bridged Ru(p-Cymene)-Dimers. The group of Shi, Deng and co-workers reported varying TOFs up to 36 h-1 without additional base and up to 627 h-1 with additional base. The group of Dupont and co-workers reported TOFs of up to 1684 h-1 without additional base.
In investigations of the Dupont group the amount of IL in the system seemed to play an important role, since after a required amount additional IL decreases the efficiency of the system remarkably. Addition of more formic acid proved the durability of this easy system in 6 recycling experiments. The high activity of the first run could not be sustained in subsequent runs. Nevertheless the slightly reduced activity remained constant for the subsequent runs except the 5th (Figure 15).
Reaction profiles for formic acid decomposition catalyzed by [(p-cymene)RuCl2] in IL 1 (Cl-) at 80 °C for 6 cycles. Reprinted with permission from (Scholten et al., 2010). Copyright (2010) John Wiley and Sons.
The same catalyst (-precursor) was investigated in another context: The solubilization and decomposition of biomass especially cellulose-based ones. Different ILs can be employed to solvate the carbohydrate feedstock and the [(p-Cymene)RuCl2]2 complex (-precursor) is suitable for dehydrogenation.(Taccardi et al., 2010) Detailed investigations by Wasserscheid et al. showed that this reaction proceeds via the thermal decomposition of glucose to formic acid and subsequent catalytic decomposition of formic acid by the Ru complex. Some ILs, in this case for example 1-ethyl-3-methylimidazolium methyl-methylphosphonate, are able to solute wood. The soluted biomass can be thermally decomposed at 180 °C and the resulting formic acid can be split into hydrogen and CO2 by the Ru-complex (Figure 16).
Thermal decomposition pathway of glucose and subsequent catalytic splitting of formic acid in IL.(Taccardi et al., 2010)
The thermal stability of the employed IL is remarkable and important in this application.
In the field of molecular hydrogen storage materials, ILs add interesting aspects in different meanings. Besides the application of ILs as (molecular) hydrogen storage materials, they can act in several other ways: They can be utilized as inert solvents, as solvents which support dehydrogenation, i.e. active solvents, as promoting agent/base or as a combination of these aspects. Especially the unique solubilization properties of ILs show considerable promise to find a liquid hydrogen storage system that remains liquid after dehydrogenation. One important aspect one has to keep in mind, when considering the application of ILs, is the addition of weight into the system, which, in general, lowers the gravimetric efficiency. This ‘weight penalty’ is the most severe drawback in the discussed applications of ILs.
The PID (Proportional Integral Differential) algorithm is the most popular feedback controller used within the process industries. It has been successfully used for over 50 years. It is a robust easily understood algorithm that can provide excellent control performance despite the varied dynamic characteristics of process plant. It is designed to generate an output that causes some corrective effort to be applied to a process so as to drive a measurable process variable towards a desired value, known as the set point. The concept is based (as shown in Figure 1) on the re-input of the system own output according to certain laws (hence the name “feedback”). It is desired for the system output to follow the set point. All feedback controllers determine their output by observing the difference, called error, between the set point and the actual process variable measurement. The PID looks at (a) the current value of the error, (b) the integral of the error over a recent time interval, and (c) the current derivative of the error signal to determine not only how much of a correction to apply, but for how long. Each of those three quantities are multiplied by a (tuning constant) and added together. Thus the PID output is a weighted sum. Depending on the application one may want a faster convergence speed or a lower overshoot. By adjusting the weighting constants, Kp, Ki, and Kd, the PID is set to give the most desired performance.
Typical closed loop control system.
As a result of enormous development in microcomputer technology, analog controllers have been replaced by digital controllers either in small or large industry. It is now a common practice to implement PID controllers in its digital version, which means that they operate in discrete time domain and deal with analog signals quantized in a limited number of levels. The trend toward digital rather than analog control is mainly due to: (1) versatility where programs can be easily modified or completely changed, (2) sophistication where advanced control laws could be implemented, (3) cost effectiveness where microcontrollers are available at very low costs compared to PLCs, industrial computers, RTUs or DCS. A typical digital feedback control system is shown in Figure 2. In digital feedback systems, the controller input and output are digital (sampled) rather than continuous signals. Thus, the continuous signal from the measurement device (sensor/transmitter) is sampled and converted periodically to a digital signal by an analog-to-digital converter (ADC). A digital control algorithm is then used to calculate the controller output as a digital signal. Because most final control elements are analog devices, the digital output signal is usually converted to a corresponding analog signal by a digital-to-analog converter (DAC).
Digital closed loop based on a microcontroller.
In feedback control, the objective is to reduce the error signal to zero where
where
The three-term PID controller.
where
A straightforward way of deriving a digital version of the parallel form of the PID controller is to replace the integral and derivative terms by finite difference approximations,
where
There are two alternative forms of the digital PID control equation, the position form and the velocity form. Substituting Eqs. (3) and (4) into (2) gives the position form:
where Pk is the controller output at the Kth sampling instant. Eq. (5) is referred to as the position form of the PID control algorithm because the actual value of the controller output is calculated [3, 4].
In the velocity form, the change in controller output is calculated. The velocity form can be derived by writing the position form of Eq. (5) for the (k − 1) sampling instant:
Note that the summation still begins at j = 1 because it is assumed that the process is at the desired steady state for j ≤ 0, and thus ej = 0 for j ≤ 0. Subtracting Eq. (6) from (5) gives the velocity form of the digital PID algorithm:
In this study, velocity form is chosen because of the following advantages:
It does not need initialization. The position form requires the initial value of the controller output
It is protected against integral windup. The integral mode of a controller causes its output to continue changing as long as there is a nonzero error. Often the errors cannot be eliminated quickly enough and given enough time they produce larger and larger values for the integral term, which in turn keeps increasing the control action until it is “saturated” (e.g., the valve completely opens or closes). This condition is called integral windup. Then, even if the error returns to zero, the control action will remain saturated. The position form with its continuous summation of errors will produce integral windup and special attention will be required. The velocity form, on the other hand, is protected from integral windup for the following reason: The control action changes continuously until it becomes saturated. But then as soon as the error changes sign, the control action can return within the control range in one sampling period.
It protects the process against computer failure. With the velocity algorithm one can send out a signal which is used to drive an integrating amplifier or a stepper motor. These devices will retain the last calculated position of the control valve (or other final control element) in case the computer fails, thus avoiding total loss of control of the process.
As mentioned earlier, the implementation is based on a Microchip PIC18F452 microcontroller, where the controller plays the role of the brain of the control system [5]. The right choice of the microcontroller is essential, as it will be the core of the final design. The PIC18F452 from Microchip has been chosen for the following advantages:
Speed: with its maximum internal clock rate of 20 MHz and its 16-bit-wide instruction bus, the CPU can execute most of its instructions at a single machine cycle of four clocks which is equivalent to a 0.2 μs.
Math support: unlike classical microprocessors, the controller in hand has got a hardware multiplier and divider for multiple-bytes, fixed-point numbers and for floating-point numbers so multiplication is carried out in a single instruction.
Flexible timer resources: four independent timers modules support timing measurements and output interval control with a timing resolution as fine as 0.1 μs. Those timers could be used to produce up to three pulse width modulations which could be used for electrical motor control.
Free software tools: Microchip’s Development Package MPLAB® (consisting of assembler, simulator, and user interface) as well as all manuals and application notes are available at no cost from their Web site (
Development tool versatility: it supports in-circuit debugger which permits the loading and execution of a user program as well as the use of breakpoints, memory/ register modification, and single stepping.
Build-in ADCs: it has analogue-to-digital converters with 10 bits resolution.
Built-in serial peripheral interface: it has a variety of serial bus interfaces like USART, I2C & SPI.
C programmable: it could be programmed using C language with the use of a variety of built in C libraries developed by microchip.
The PIC18F452 microcontroller is a 40 or 44-pin depending on the package, where in the 40 pins configuration, a dual inline package is used; whereas in the 44 pins configuration, either thin quad flat package or dual flat no leads package is used. Its design is based on Harvard technology where the program and data have different buses. This type of microcontrollers is very cheap, small in size, and could be customized. It could be easily programmed on-line using either assembly language, BASIC or C language. In fact, it is ideal for small application such as the one in hand. The controller has a 24 kbytes of flash memory and 2048 bytes of SDRAM. It also has a 8 × 10 bits analog to digital channels. It also has 5 bidirectional digital ports with 33 inputs/outputs, configured as follows: 3 × 8 digital I/O ports (PORTB, PORTC and PORTD), one six digital I/O port (PORTA) and one three digital I/O port (PORTE). Unfortunately, one of the drawbacks of microcontrollers, it is very seldom to find one with a digital to analog converter. Luckily, they are few manufacturers around including microchip, which make serial DACs which could be programmed through Serial Port Interface (SPI) using only three wires. The PIC18F452 has four timer/counters which could be programmed either as 8 or 16 bit timers/counters. It also has two ports which could be configured either as capture, compare or pulse width modulation (PWM). It has two serial peripheral interfaces: (SPI) and an inter-integrated circuit (I2C). An asynchronous port (USART) is also provided. For the microcontroller to output analogue data, an MCP4921 device is used. The device is a 12-bit buffered single voltage output Digital-to-Analog Converter (DAC). The device operates from a single 2.7 V to 5.5 V supply with an SPI compatible Serial Peripheral Interface. The user can configure the full-scale range of the device to be VREF or 2*VREF by setting the gain selection option bit (gain of 1 of 2). The user can shut down the device by setting the Configuration Register bit. In Shutdown mode, most of the internal circuits are turned off for power savings, and the output amplifier is configured to present a known high resistance output load (500 kΩ, typical). The device includes double-buffered registers, allowing synchronous updates of the DAC output using the LDAC pin. The device also incorporates a Power-on Reset (POR) circuit to ensure reliable powerup. The device utilizes a resistive string architecture, with its inherent advantages of low Differential Non-Linearity (DNL) error and fast settling time. The device is specified over the extended temperature range (+125°C). It provides high accuracy and low noise performance for consumer and industrial applications where calibration or compensation of signals (such as temperature, pressure and humidity) is required. The MCP4921 device is available in the PDIP, SOIC, MSOP and DFN packages. Figure 4 shows the chip pin configuration. The MCP4921 device is designed to interface directly with the Serial Peripheral Interface (SPI) port, which is available on the PIC18F452 microcontroller and supports Mode 0,0 and Mode 1,1. Commands and data are sent to the device via the SDI pin, with data being clocked-in on the rising edge of SCK. The communication is unidirectional; this means the data cannot be read out of the MCP4921. The CS (chip select active low) pin must be held low for the duration of a write command. The write command consists of 16 bits and is used to configure the DAC’s control and data latches. Register shown in Figure 5, details the write command which is loaded into the input register that is used to configure and load the DAC register [6].
MCP4921 pin configuration.
Write command register for MCP4921 (12-bit DAC).
The write command is initiated by driving the CS pin low, followed by clocking the four Configuration bits and the 12 data bits into the SDI pin on the rising edge of SCK. The CS pin is then raised, causing the data to be latched into the DAC’s input register. The MCP4921 utilizes a double-buffered latch structure to allow the analog output to be synchronized with the LDAC pin, if desired. By bringing the LDAC pin down to a low state, the content stored in the DAC’s input register is transferred into the DAC’s output register (VOUT), and VOUT is updated. The write to the MCP4921 device is 16-bit words. Any clocks past the 16th clock will be ignored. The Most Significant 4 bits are Configuration bits. The remaining 12 bits are data bits. No data can be transferred into the device with CS high. This transfer will only occur if 16 clocks have been transferred into the device. If the rising edge of CS occurs prior to that, shifting of data into the input register will be aborted. The most four significant bits are defined as follows:
bit 15 0 = Write to DAC register
1 = Ignore this command
bit 14 BUF: VREF Input Buffer Control bit
1 = Buffered
0 = Unbuffered
bit 13
1 = 1x (VOUT = VREF * D/4096)
0 = 2x (VOUT = 2 * VREF * D/4096)
bit 12
1= Active mode operation. VOUT is available.
0 = Shutdown the device. Analog output is not available.
VOUT pin is connected to 500 kΩ (typical).
This module is designed to display the value of the temperature detected by the temperature sensor and to guide the user in changing the parameters of the controller. The LCD is a 16 × 2 alphanumeric display with the built-in Hitachi 44780 controller and LED backlighting. It works with an 8-bit data bus, which means it will require a total of 11 data lines. Three control lines (connected to port E) plus the 8 lines for the data bus (connected to port D) [7].
The system is design around a stand-alone PIC18F452 controller, where the measured variable (MV) is read through channel0 (pin 2). The MV is subtracted from the set point automatically by the controller. The error is treated by the PIC PID and produces a digital control variable. This control variable is outputted through PIC serial data output pin (SDO pin 24) together with serial clock pin (SCK pin 18) to synchronize the conversion process. For the conversion to take place, the serial DAC chip select (CS) has to be pulled low. The CS is connected to pin RC0. The positive reference voltage is connected to +5 V (pin 6) and the negative reference voltage (pin 7) is tied to zero volt. The analog output is read through pin8 (Vout). This voltage is small to drive an electric motor. This voltage is pulled up to +12 V through the non-inverting operational amplifier (LM358). The Darlington transistor 2SD1409 is used to bust the current. The motor is connected to the emitter follower so that the driving current is sufficient enough to drive the motor. Needless to say that the diode 1N4148 is used to protect the Darlington transistor against any spike due to the change of current. Figure 6 shows the schematic of the system. The LCD is used to display the measured temperature. To manipulate the setting of different parameters, six push buttons are used as follows:
System schematic circuit showing all the connection to the microcontroller, as well as the liquid crystal display and the final control element.
Six push buttons were used in the project to allow the user to change the setting and the controller parameters. Their functions are as follows:
Reset: To reset the microcontroller.
Stop: interrupt the program to allow the user to change the controller settings
Run: To run the program
Mode: To allow the user to change between setting modes.
Increment: To increment the controller variables by 1 or 0.1.
Decrement: To decrement the controller variables by 1 or 0.1.
These switches are connected to PIC PORTB to allow the user to use the internal build-in pull up resistors to prevent floating instead of using external pull-down resistors. The reset has got a separate button connected to MCLR pin. A buzzer is used as an alarm to indicate that the temperature is more than what the user specifies. Three LEDs were used to show the user the status of the microcontroller program. The three colors green, yellow, and orange were used as follows:
Green: means that the PID controller is working properly.
Yellow: means that the program is interrupted by (STOP) push button.
Red: means that the alarm is triggered.
To implement the control program, three major routines are used; the main routine along with the timer and external interrupts. The program starts with the main routine which contains all the configurations of the external pins whether outputs or inputs. It also contains the configurations of timer and external interrupts, so when one of these interrupts is triggered, the microcontroller will stop its current execution and perform another action. The trigger will be caused by either an overflow in timer register or a change on an external pin (RB0/INT0).
Because the time is a crucial element in digital control, the PID algorithm is controlled through a timer interrupt. This choice allows the user the ability to calculate the sampling time accurately. On the other hand, an external interrupt (INT0) is used to interrupt the program in order to allow the user a chance to modify the controller parameters. In the following we discuss in some details about the functions of each routine.
This routine, as mentioned earlier, is dedicated to configure the direction of external pins as well as interrupt sources. It also allows the user to choose the measured variable (temperature, flow, level or others). The flow chart of this routine is shown in Figure 7.
Main routine.
First PORTA (pin RA0) is configured as an analog input channel0 and PORTB as input digital port which is connected to the push button switches; while all other pins are configured as outputs.
The configuration of the LCD was performed by separate software from Microchip called Application Maestro [8]. With the aid of this software, a configuration code was produced after modifying the module parameters. It was then incorporated into the project. Once incorporated, the LCD is configured and ready to work. One feature of using Application Maestro is its ability to use the prewritten code that this software provides to initialize or to write to the LCD.
Timer0 can operate as a timer or as a counter. In Timer mode, the Timer0 module will increment with every instruction cycle (without prescaler). It is configured by setting a special function register called T0CON (timer0 control byte). This register is a readable and writable register that controls all the aspects of Timer0, including the prescale selection. In the design in hand, T0CON register is set to 0x85 (0b10000101) as shown below [9, 10].
This value will configure the timer0 as follows:
● | TMR0ON | = 1 | : Timer0 is enabled | ||
● | T08BIT | = 0 | : Timer0 is configured as a 16-bit timer | ||
● | T0CS | = 0 | : Internal instruction cycle clock | ||
● | T0SE | = 0 | : This bit is used only with external clock | ||
● | PSA | = 0 | : Timer0 prescaler is assigned | ||
● | T0PS2 | = 1 | : Bit2: T0PS2 =1: | } | 1:64 prescaler value |
● | T0PS1 | = 0 | : Bit1: T0PS1 =0: | ||
● | T0PS0 | = 1 | : Bit0: T0PS0 =1: |
There are ten registers which are used to control internal and external interrupt operations to accommodate a variety of interrupts [11]. In the project in hand, only two interrupts are required INT0 and timer0 interrupt. To do so, only three control registers are required. These registers are INTCON, INTCON2, and RCON. INTCON register contains various enable bits as well as several interrupt flags. RCON is the Reset Control register which contains flag bits that allow differentiation between the sources RESET. Timer0 interrupt is enabled by setting TMR0IE bit (<5>) while external interrupt is enabled by setting INT0IE (INTCON<4>). Note that the interrupt flags are reset before enabling the interrupt in order to avoid unwanted interruptions.
To start the interrupt, the global interrupt bit GIE/GIEH (INTCON<7>) must be set. If set, it enables all unmasked interrupts, so if more than one interrupt source is used (as in our case) the Interrupt Priority Enable bit IPEN (RCON<7>) must be set and the interrupt sources should be specified either as high or low priority interrupt. The interrupt priority bit TMR0IP (INTCON2<2>) is used to specify the interrupt priority for Timer0. This bit is reset so timer0 interrupt is set to low priority. On the other hand, no need to specify the priority of the external interrupt (INT0), because it is already set to high priority by default.
After configuring the interrupts, the program will enter an infinite loop until one of the interrupt sources is triggered.
The main purpose of this routine is to calculate the controller output and send it to the DAC serially through the synchronous SPI module [12]. Figure 8 shows the routine function.
Timer interrupt routine.
Because of the importance of time in calculating the timed controller output, timer0 is used as an accurate hardware timer. The source clock of the timer is the crystal oscillator which is fed to the clock pin of Timer0 internally. The clock used is a 20 MHz derived from a stable crystal oscillator. This frequency is automatically divided by 4 because the controller machine cycle is 4 clocks to give a 5 MHz which is fed to the timer. The timer is exactly clocked every 0.2 μs and takes 13107.2 μs (16-bit mode) to count from zero to zero again. However, by loading the timer with a suitable value, a smaller time interval could be obtained. For example, by loading the timer with the value 4095 (0xFFF), the overflow would occur after 12288.2 μs. Alternatively, the time period can be extended by using a prescaler as was done in the main routine. If a divide by 64 prescaler is selected, timer0 only overflows after 838.848 ms. This is obtained as follows:
This time period is less than one second, while a one second sampling time is required for the design in hand. To obtain a one second sampling time, the timer should count 78,125 pulses.
Because timer0 register is only 16 bit wide, it is only limited to count up to 65,535 pulses. The interruption is trigged several times to obtain one second timing, after which the controller computes the control action and sends it to the DAC. By using MPLAP simulator, it was found that 5362 cycles are required to calculate the controller output and send it to the DAC besides 51 extra cycles needed to reload the timer with time constant. If the interruption is required to repeat itself five times before calculating the controller output, one needs 5362 + 51 × 5 = 5617 cycles (1.1234 ms). Thus, in order to get exactly one second sampling time, the timer register (TMR0) has to be reloaded with a value that interrupts the program every 998.8766 ms (1 s–1.1234 ms). The following shows how this value is obtained:
By using a timer with 64 prescaler:
When we repeat the interrupt for 5 times:
But because the timer counts in ascending order (from 0x0000 to 0xFFFF):
However, the timer register accepts only integer numbers, thus the final value that should be added to the timer register is 49918. Because we omitted the numbers after the decimal point, our error will be ± 1 count which is equal to 64 cycles. Therefore, our error in calculating the sampling time will be:
This calculation is for getting 1 s sampling time. To expand the calculation in order to enable the user to change the sampling time, one defines two integer variables (repeat and cycle). The first variable repeat is to determine how many times we need to repeat the interrupt, while the second one cycle is the final value that should be added to the timer register. The following pseudo code shows the general formula used to reload the timer register.
The ADC module normally operates at 10-bits resolution, giving output digital values 0–1024 [13]. It needs a reference voltage to set the maximum and minimum values for the input conversion. This reference can be provided internally as Vdd and Vss (supply values) or externally through Vref+ and Vref− pins. To configure this module, OpenADC function from Microchip C library is used. This function performs a bitwise AND operation (“&”) between its arguments which are defined in the file adc.h. The parameters of this function along with their meaning of each argument are discussed below [1]
ADC_FOSC_32: FOSC/32.
A clock divider to allow the minimum specified conversion time (about 20 μs). A 32 prescaler was chosen because the clock source is 20 MHz
ADC_RIGHT_JUST: Right justified.
Because the ADRES register pair (where the converted values are loaded) is 16-bit wide. But the ADC is only 10bit wide. The ADC module could either be configured as right or left justified. In this project, right justified is chosen as shown in Figure 9. This sets the 6 most significant bits of register ADRES to zeros.
ADC_8ANA_0REF: VREF+ = VDD, VREF− = VSS
The supply values are chosen as the voltage references to the ADC.
ADC_CH0: Channel0 (AN0) is selected
ADC_INT_OFF: Interrupts of ADC interrupts are disabled.
Once the A/D conversion is completed, the result is stored in an integer variable called result. After reading the analog value by the ADC module, the result will be compared with the variable alarm-trigger which was previously specified. If the result is greater than this value, the microcontroller triggers the buzzer and lights the red LED.
Choosing right justified for data input.
Due to the limitation in the microcontroller’s memory, the PID equation is divided into three terms (term_1, term_2, and term_3) and after calculating each term separately, they are added together along with the previous output to give the controller output which will be sent to the DAC. The following code shows how to calculate the controller output
To send the control variable to the final control element, the serial DAC, which is interfaced to the Serial Peripheral Interface (SPI) port, is used. The SPI is initiated using Microchip C library called OpenSPI. This function also performs a bitwise AND operation between its arguments which are defined in the file SPI.h according to the following formula.
SPI_FOSC_16: Master mode and the clock = FOSC/16
MODE_00: Mode 0,0 (change takes place on the rising edge)
SMPEND: Input data sample at end of data out
After configuring the module, it is time to write a command to the DAC in order to convert it into analog signal. The write command is initiated by driving the CS pin low, followed by clocking the four configuration bits and the 12 data bits into the SDI pin on the rising edge of SCK. The CS pin is then raised, causing the data to be latched into the DAC’s input registers and when the LDAC pin is pulled down through RC1, the values held in the DAC’s input registers are transferred into the DAC’s output registers to provide the analog signal. It is important to mention here that we wrote the write command in two steps (as shown in the following code) because the SPI module send only 8 bit at a time.
To write characters to the LCD, required prewritten functions are provided by Application Maestro. Some of These functions are listed in following table:
It is used to initialize the LCD module according to the Application Maestro options | |
It sends the clocking signal and data to be displayed to the LCD | |
Points to the first address location of line one of the LCD | |
Points to the first address location of line two of the LCD | |
Clears the DDRAM content of the LCD and points to the 00 address location | |
Displays String in Program memory | |
Displays String in Data memory | |
It sends clocking signal and instructions to the LCD |
For numbers to be displayed, they are first converted into strings (characters) before being sent to the LCD, since the latter only accepts strings. To do so a C function called sprintf is called upon. This function saves the number in an array after converting it into string. The subroutine to do so is shown below [4]:
The main function of this routine is to allow the user to change the controller parameters. The routine is initiated by pressing the push button (STOP) which is connected to the external interrupt pin (RB0/INT0). Once initiated, the user is able to change all the parameters of the controller (KC, τI, τD, sampling time, alarm trigger and sensitivity) by using three push buttons (MODE, INCREMENT and DECREMENT [11].
To determine which action the microcontroller should take if any push button is pressed, we defined two integer variables (present_button and present_mode) to be used as statuses. That is, each bit of them has specific meaning as described below:
present_button
Np | ____ | ____ | ____ | ____ | ____ | ____ | ____ | ____ | ____ | ____ | ____ | ____ | dec | inc | Mod |
bit15 | bit0 |
● | Np: set if there are no push buttons pressed |
● | Unimplemented |
● | dec: set if the DECREMENT push button pressed |
● | inc: set if the INCREMENT push button pressed |
● | mod: set if the MODE push button pressed |
present_mode
____ | Srt | Spt | KC | TI | TD | Stm | Sen | Alm | Tun | Dp | Tp | Kp | ____ | ____ | ____ |
bit15 | bit0 |
● | Unimplemented |
● | Srt: set in the starting mode |
● | Spt: set in the set point mode |
● | KC: set in the controller gain mode |
● | TI: set in the integral time mode |
● | TD: set in the derivative time mode |
● | Stm: set in the sampling time mode |
● | Sen: set in the sensitivity mode |
● | Alm: set in the alarm mode |
● | Tun: set in the tuning mode |
● | Dp: set in the process delay mode |
● | Tp: set in the process time constant mode |
● | Kp: set in the process gain mode |
● | Unimplemented |
Initially, before pressing any push button, present_button variable is loaded with 0x8000 (no push button pressed), and present_mode with 0x2000 (starting mode).Then if any push button is pressed, the corresponding bit of that push button will be set, giving a specific value of present_button which indicates the push button that was pressed by the user. So by performing a bitwise OR operation between the two variables (present_button and present_mode) we will come up with a number indicates the push button pressed and the present mode and based on that number we can decide the proper action to be taken by the microcontroller. The following code shows how to perform the OR operation after checking which of the push buttons was pressed. Beside changing the controller variables, this routine has another feature, it gives the user preliminary values of the controller parameters after entering the process variables. The result is derived based on Cohen-Koon tuning method. However, this feature is impractical if the sampling time is big [14].
To test the system, a first order system given by the equation below was used. To run the control action, the system was converted into a difference equation given by Eq. (10).
The process transfer function is first order, thus the discrete transfer function obtained using Zero-Order Hold will be:
where:
If kp = 10, τp = 5, and Ts = 1, The discrete transfer function will be:
Therefore the difference equation of the output is:
After getting the difference equation, the control scheme was tested and the output of Figure 10 was obtained with the parameters set to: Kc = 0.2, Ti = 4.0 and Td = 0.0. The parameters were then changed to: Kc = 0.1, Ti = 3.0 and Td = 0.2. The response is shown in Figure 11.
Controller response with Kc = 0.2, Ti = 4.0 and Td = 0.
Controller response with Kc = 0.1, Ti = 3.0 and Td = 0.2.
By referring to the previous graphs, it could be concluded that the response tracks the set point as expected. In addition, the increase in controller gain (Kc) does speed up the response but at the expense of the overshoot. Based on these results, it could be concluded that the three-term controller is working according to plan. Because of the flexibility of the microcontroller and its programming, any control scheme could be developed and implemented in the manner as described in this chapter. Not only that, the scheme could be transferred to several high range microcontrollers from the same company such as 16 or 32 bits with the use of the benefits those types of controllers offer.
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