PHYSICAL AND ELECTRICAL ANALYSES OF SOLID POLYMER
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.comPHYSICAL AND ELECTRICAL ANALYSES OF SOLIDPOLYMER ELECTROLYTESM. F. Hassan1,2 and H. K. Ting31Advanced Nano Materials (ANoMa) Research Group, Universiti Malaysia Terengganu, Kuala Nerus, Terengganu, Malaysia2School of Fundamental Science, Universiti Malaysia Terengganu, Kuala Nerus, Terengganu, Malaysia3School of Ocean Engineering, Universiti Malaysia Terengganu, Kuala Nerus, Terengganu, MalaysiaE-Mail: mfhassan@umt.edu.myABSTRACTIn this work, we prepared a solid polymer electrolyte based on starch and sodium hydroxide via a simple castingmethod. The hybrid starch sodium hydroxide film formed the belts morphology. Such belt structure is believed to be ableto improve ionic mobility and electrochemical reaction effectively. The highest ionic conductivity was achieved at 3.93 x10 3 S/cm for 25 wt% of sodium hydroxide. A comparative investigation on sodium hydroxide as an ionic dopant in starchproved that the sodium hydroxide addition is an effective way to increase ionic conductivity and electrochemical activity.Keywords: solution casting technique, solid polymer electrolyte, starch, sodium hydroxide, ionic conductivity, physical analyses,electrical conductivity.INTRODUCTIONSolid polymer electrolyte (SPE) systems arepromising candidates for all solid state storage devices.These SPEs are known to have a lot of advantages such asno possibility of leaks, ability to strengthen devices due toits all solid state construction, shape flexibility, lowdevice weight as all solid state devices do not need heavymetal casing, prevention of dendrite development, betteroverheat, wider operating temperature ( 40oC to 150oCcompared to liquid electrolyte at 15oC to 60oC), andimproved cell safety. The materials used in solid tal friendly and exist in abundance in nature.However, its conductivity at room temperature is not highenough for application in batteries. A highly resistivelayers formation at the anode electrolyte interfaceprovides another disadvantage.Many researchers have been implemented SPEsas one of the components in their all solid state devices[1 8]. Singh et al. had tested the performance of asolid state battery with a Zn/ZnSO4.7H2O/I2configuration[1]. The cell was given an open-circuit voltage of 1.1V, ashort circuit current of more than 10mA and an energydensity of 13.8Whkg 1 at a constant current drain of100 A. The cells based on the Zn/PVA KOH/MnO2configuration conducted by [4] claimed that its opencircuit potential had reached above 1.5 V. A plateau ofcell voltage was shown in the discharge curves rangingfrom 1.3 to 1.1 V. The cell discharge capacity of ca. 210mAh g 1 was obtained per gram of MnO2 mass for 1mAconstant discharge current and exhibited good dischargecharacteristics and stability of the electrolyte. Hiralal etal. studied the mechanical stressed conditions of theall solid state and flexible zinc carbon batteries [2]. Byusing a solid polymer electrolyte in the batteryfabrication, the results showed that improvements interms of battery shelf life and solid state mechanicalflexibility can be achieved. Similar results were alsoobtained by Fu et al. on a flexible solid state electrolyteused in a rechargeable zinc air battery system [3]. Thesystem which used a nano porous alkaline-exchangeelectrolyte membrane from natural cellulose nano fiberexhibited high ionic conductivity and water retention aswell as high bending flexibility. These advantages renderthe membrane as a promising solid state electrolyte forrechargeable zinc–air batteries in lightweight and flexibleelectronic applications. All of these novel works provideproof that the SPEs have potential in solid state batteryapplications. Hence, SPEs based on starch complexedwith sodium salts would be the next new system to beexplored.Starch is a carbohydrate extracted fromagricultural raw materials which extensively exist infactually thousands of daily food and non foodapplications. Since it is renewable and biodegradable, it isalso an impeccable raw material to be used as a substitutefor fossil fuel components in various chemicalapplications such as plastics, detergents, glues etc. Itspotential as one of the components of interest inelectrochemical storage devices provides extra advantagesfor advanced exploration [9-13].NaOH is known as a caustic soda. It is aninorganic compound with the formula NaOH. It is a whitesolid ionic compound consisting of sodium cations Na and hydroxide anions OH . It is used in many industries,including electrochemical applications [14-17]. Earlierstudies have revealed that NaOH could improve someelectrochemical properties of the energy storage systemsin terms of its energy density and voltaic efficiency.To the best of our knowledge, studies on astarch NaOH solid polymer electrolyte hybrid are veryrare. Therefore, this study is focused on the evaluation ofthe microstructure, crystallization behavior and electricalproperties of the starch NaOH films. Moreover, thisstudy is based on our recent reports on poly (sodium 4styrenesulfonate) LiClO4 and poly (sodium 4styrenesulfonate) NH4NO3 films [18, 19]. The material8189
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.comproduced involves degradable polymers, and thus is morebiodegradable.The solutions were poured into different plastic Petridishes and left for thin film formation. The films werethen kept in desiccators for a certain period to ease watercontent. All the experimental steps were conducted atroom temperature. To note here, the weight in gram ofNaOH was calculated using Equation 1 as follows:MATERIALS AND EXPERIMENTAL METHODSSample preparationStarch (derived from corn) and NaOH werepurchased from Aldrich and Sigma Aldrich, respectively.Concisely, two different solvents (25 ml distilled waterand 0.6 ml glycerin) were mixed together under atemperature of 70 oC. Starch powder (1g) was added tothe prepared solution under vigorous mechanical stirring.Next, NaOH concentrations (varied from 0 to 30 (inweight percentage, wt.%)) were added to the solution asscheduled in Table-1. The mixtures were stirredcontinuously until homogenous solutions were achieved.𝑤𝑡. % 𝑥𝑥 𝑦 100(1)where x is the amount of dopant in gram (g), y isthe amount of starch, and weight percentage is the varyingvalues of dopant in percentage form. All the experimentalsteps were carried out at room temperature and describedin Figure-1.Table-1. The compositions of starch and NaOH powders.Solvent 250.333F250.61300.429SampleIonic salt(wt.%)Ionic salt (g)Figure-1. A schematic diagram to prepare starch-NaOH complex films.8190
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.comCharacterizationsAn X ray diffraction (XRD) analysis wasperformed using a MiniFlex II diffractometer equippedwith an X’ celerator using CuKα operated at 40 kV and 30mA to record diffractogram in the range of 2θ 10 o to80o.Fourier transform infrared (FTIR) spectra of thepure starch and hybrid starch NaOH were recorded usinga Thermo Nicolet Avatar 380 FT IR spectrometer at aresolution of 4 cm 1 in the wave number range of 675 to4000 cm 1.Micrographs of film surfaces were investigatedusing scanning electron microscopy (SEM) at anacceleration voltage of 20kV using JEOL JSM 6360LAunder magnifications of x300 to x10000, accordingly.Prior to the SEM observations, the samples were coatedwith a fine gold layer.Impedance analysis was measured using a HIOKI3532 02 LCR Hi Tester interfaced with a computer overa frequency range of 50Hz to 1MHz. The preparedsamples were cut to 2 cm diameter size and positionedbetween two stainless steel electrodes on a sample holderwhich were connected via lead to a computer. Theimaginary impedance (Zi) versus the real impedance (Zr)was plotted using the same scale for both vertical andhorizontal axes in order to obtain the bulk resistance, Rb.A micrometer screw gauge was used to measure thesample thickness, and the sample conductivity wascalculated using the Equation (2) as follows:𝜎 𝑡(2)𝑅𝑏 𝐴where t is the thickness of the thin film (in cm),and A is the area of the contact and Rb is bulk resistance.RESULTS AND DISCUSSIONSIntensity 0405060 deg. 708090100Figure-2. XRD patterns for starch and hybrid starch NaOH films.The XRD patterns of the starch and hybridstarch NaOH films are shown in Figure-2. The purestarch diffraction pattern can be acknowledged with abroad peak of 2θ (15o to 27o). As discussed by someresearchers, this peak is a combination of several peakslocated at 2θ 15.19o, 17, 23o, 18.13o, 20.10o and 23.10o.According to Ramirez et al., with the addition of glycerin,the starch grains were restructured, causing modificationsto the crystallographic profile [20]. In other words, thecrystallinity of starch was significantly reduced, andtended to exist in highly amorphous conditions. Similarresults were also reported in literature [20 26]. The otherXRD patterns refer to the starch NaOH complex films.No major alterations were spotted with the addition ofNaOH up to 20 wt.%, and the diffractograms definitelyhave a similarity and exist in an amorphous state. Severalpeaks at 17.8o, 28.6o, 33.5o, 39.8o and 44.3o were clearlyvisible after the addition of 25-30wt.% of NaOH. Thepeaks at 17.8o, 39.8o and 44.3o corresponded to NaOHpeaks, and the rests were probably matched with Na2Oand Na2O2[27]. From the XRD analyses, two conclusionscan be made; first, the complex films were present inamorphous rather than crystalline condition, and NaOHdid not wholly influence the crystallographic profile dueto the incredibly amorphous nature of polymer and itsincomplete crystalline structure, and second, the presenceof a variation of peaks of the studied materials on the8191
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.comcrystallographic patterns had confirmed that thepolymerization process had taken place in the solidpolymer electrolyte preparation [28 30].30 wt.%25 wt.%Intensity (a.u.)20 wt.%15 wt.%10 wt.%5 wt.%0 wt.%5001000 1500 2000 2500 3000 3500 4000 4500 5000-1Wavenumber (cm )Figure-3. This FTIR patterns for starch and hybrid starch-NaOH films.The FTIR spectra for the starch andstarch sodium hydroxide complex films are illustrated inFigure-3. In the figure, the IR spectrum of films showscharacteristic absorption bands at 1036 cm 1, 1382 cm 1,1643 cm 1, 2916 cm 1 and 3304 cm 1, respectively. TheIR spectrum of films showed a CO stretching in the planeat 1036 cm 1 and an –OH bending vibration band at 1382cm 1. The FTIR spectrum of the as-prepared films alsoshowed the band at 1643 cm 1 which was attributed towater adsorbed in the amorphous state and has beendescribed to diverge based on crystallinity. The other peaklocated at 2916 cm 1 corresponds to the methyl group (CH2 stretching vibration). The prepared film also showedan –OH stretching peak at 3304 cm-1 due to waterabsorption. As can be seen in the complexed spectra, thereare significant changes for all films, particularly in termsof their intensity. Specifically, the peak intensityincreased as the amount of NaOH increased (1382 cm 1)and decreased with respect to the addition of NaOH (2916cm 1 and 3304 cm 1, respectively). All of thecorresponding bands have been summarized in Table-2. Itwas undoubtedly confirmed that significant modificationshad taken place in the chemical structure due to thedoping of NaOH into the starch chains. These resultsverified that NaOH has been embedded into starch in thepolymerization process.Table-2. FTIR absorbance, functional groups and references of starch–NaOH complex films.V(cm-1) related to thecrystal system1036Absorbance changeFunctional groupReference (CO stretching)[31]1382 1643 2916 3304 ( OH bendingvibration)Hydroxyl ( OHbending)Methyl ( CH2stretching vibration)Hydroxyl ( OHstretching)[32][33][33][34]**indicator: - not change; increase; decrease8192
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights (f1)Figure-4. SEM micrographs for (a,) starch film, (b) 5 wt.% of NaOH (sample A), (c) 10 wt.%of NaOH (sample B), (d) 15 wt.% of NaOH (sample C), (e) 20 wt.% of NaOH (sample D),(f) 25 wt.% of NaOH (sample E) and (g) 30 wt.% of NaOH (sample F).The morphologies of starch and hybridstarch NaOH films are illustrated in Figure-4. A withoutdopant film had a smooth surface morphology (Figure4a). The morphology had been altered with the presenceof small quantities of round shapes on certain areas of thefilm after the addition of 5wt.% of NaOH. With theaddition of 10wt.% of NaOH, the film did not change toomuch, but the round shape morphology had tripled inquantity compared to the previous film. The surfacecontour of the following samples (15, 20 and25wt.%NaOH) was extremely modified with the presenceof very tiny particles on top of the film surface (25wt.%NaOH). Remarkably, the tiny particles observed at highmagnification were attributed to the belt shapemorphology probably because the belt shape can beconsistently found in the whole area of film. The beltshape structure had the width and length of around of 250nm and 1.50 m (Figure-4f1), respectively. With furtheradditions of NaOH (25wt.%), the contour had changed toaccommodate a bigger belt size (width 1 m and length 2.5 m) as shown in Figure 4g.Table-3. The bulk resistance and ionic conductivity ofstarch–NaOH complex films.PureBulk resistance,Rb (Ω)8.21 x 103Conductivity, (S cm 1)1.20 x 10 6A1.18 x 1021.14 x 10 4B4.80 x 1012.09 x 10 4C1.50 x 1017.36 x 10 4D6.00 x 1001.93 x 10 3E2.70 x 1003.93 x 10 3F3.00 x 1015.24 x 10 4Sample8193
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.com-2-1(Conductivity, (S cm ))10-310-410-510-61005101520wt.% NaOH253035Figure-5. The conductivity variation as a function of salt content at room temperature.The values of bulk resistance and conductivityare listed in Table-3, whereas the trend of conductivityversus salt content of prepared films is depicted in Figure5. The measured thicknesses of the films were in between0.009 to 0.049 cm. The bulk resistance of starch was 8.21x 103 Ω with an ionic conductivity of approximately 1.20x 10 6 S cm 1. With the addition of 5 wt.% of NaOH tothe polymer, the bulk resistance decreased to 1.18 x 10 2 Ωand the ionic conductivity increased to 1.14 x 10 4 S cm 1.The bulk resistance (4.80 x 101 Ω) decreased after that,given the ionic conductivity of 2.09 x 10 4 S cm 1 for thefilm containing 10 wt.% of NaOH. With the addition of15 wt.% of NaOH, the bulk resistance increased to 2.30 x102 Ω and the ionic conductivity achieved was 4.80 x 10 5S cm 1). The measured resistance decreased to 5.10 x 10 1Ω, while the ionic conductivity increased to 2.27 x 10 4 Scm 1 for the film with 20 wt.% of NaOH. The increasingtrend of ionic conductivity continued for the filmcontaining 25 wt.% of NaOH and its value was 1.07 x10 3 S cm 1 with a bulk resistance of 2.7 Ω. With theaddition of 30 wt.% of NaOH, the bulk resistance wasincreased; as a result, the ionic conductivity of filmdecreased (5.24 x 10 4 S cm 1). With further additions ofNaOH, the solution experienced low rigidity, thus causingthe film to be hard to form. It was anticipated that thevariation in ionic conductivity was attributed to themobile free ion associations occurring at low and highsalt concentrations. At the medium salt concentrations, thedissociation and redissociation of salt had taken place [35,36]. The drop in conductivity could be because of theincrease in crystallinity as confirmed by the increase inintensity and the few peaks which emerged on the X raydiffractogram. Besides that, another factor whichcontributed to the high ionic conductivity was themodification on the of film morphology to a belt shapestructure. According to literature, materials withbelt shape structures are well known to have specialproperties such as effective improvisation of electricalconductivity, good mechanical strength, high catalyticactivity and good electrochemical stability. We believedthat this second factor might be the alternative side thatcontributed to the high ionic conductivity in the studiedfilm [37, 38].For comparison purposes, the method ofsynthesis, morphology and conductivity values of ourprepared starch-NaOH microbelt films in this work andthose of starch based materials reported in the literatureare summarized in Table 4. The results presented hereshow that the prepared starch NaOH microbelt filmspossesses a fascinating structure and exhibit high ionicconductivity which is rarely documented in previousreports.8194
VOL. 13, NO. 20, OCTOBER 2018ISSN 1819-6608ARPN Journal of Engineering and Applied Sciences 2006-2018 Asian Research Publishing Network (ARPN). All rights reserved.www.arpnjournals.comTable-4. Comparison of the conductivity value of hybrid starch NaOH film prepared in this work with thoseof starch produced with different shapes and by different methods, as reported in literature.SampleCorn starch-NaOHPotato Starch-Mg(C2H3O2)2Corn Starch-LiPF6Starch-KIPotato Starch/ChitosanLiCF3SO3Potato starch-Sodium SaltsRice Starch-LiISago starch-KISolventdistilled water glycerolacetic acid glyceroldistilled waterdistilled waterdistilled water ethanoicaciddistilled water glutaraldehyde polyethylene glycol 300distilled waterdistilled waterMorphologybelts shape 8 4 3ReferenceThis work[39][40]7.02 10-7.11 10 7[42]-1.12 10 4[43]-4.68 10 5[44]entangled matrixwatergranulesCorn tilled waterACKNOWLEDGEMENTSThe financial and facilities supports from Schoolof Fundamental Science and School of Ocean Engineeringare greatly appreciated.1.47 10 3--CONCLUSIONSIn summary, a highly ionic conductingstarch NaOH polymer electrolyte film was prepared via asolution casting technique. Interestingly, this simplepreparation method had an important effect on theformation of a uniform dimension and a highlyamorphous belt structure. The 25 wt.% starch NaOHmicro belt film exhibited the highest ionic conductivity atas high as 3.39 10 3 S cm 1. Two main factors werethought to contribute to the high conductivity values. Firstis the amorphous structure (belts-shape structure) of thecomplex film which acts as a supportive medium for fastionic movement. The second factor is related to theinorganic salt which supplied free mobile ionicconductors to the closed system until a saturated conditionwas achieved. Combined with its unique characteristics ofmentioned above, it is therefore expected that the presentreported starch NaOH micro belt polymer electrolytefilm can be a promising candidate material for applicationin energy storage devices.2.44 10-glycerolacetic acid deacetylation3.39 10-Cassava StarchCassava thiumPerchlorateCorn starch–chitosan-NH4IConductivity (S/cm)2.91 104.90 10 4 5[41][45][46]1.6 10 6 8.1 10 3[47]1.28 10 2[48]3.89 10 5[49]aggregate andtail like chainparticlesgranules3.04 10 4[50]REFERENCES[1] Sing K., Tiwari R. U. and Deshpande V. K. 1993.Performance of a solid-state battery with a protonconducting electrolyte.J. Power Source. 46, 65-71.[2] Hiralal P., Imaizumi S., Unalan H. E., Matsumoto H.,Minagawa M., Rouvala M., Tanioka A., AmaratungaA. J. 2010. Nanomaterial-Enhanced All-Solid FlexibleZinc-Carbon Batteries. ACS Nano. 5, 2730-2734.[3] Fu J., Zhang J., Song X., Zarrin H., Tian X., Qiao J.,Rasen L., Li K. and Chen Z. 2016. A flexible solidstate electrolyte for wide-scale integration ofrechargeable zinc-air batteries. Energ. Environ. Sci. 9:663-670.[4] Zhang G. Q. and Zhang X. G. 2003. A novel alkalineZn/MnO2 cell with alkaline solid polymer electrolyte.Solid State Ionics. 160: 155-159.[5] Kotobukia M., Lua L., Savilovc S. V. and Aldoshin S.M. 2017. Poly(vinylidene fluoride)-Based Al IonConductive Solid Polymer Electrolyte for Al Battery.J. Electrochem. Soc. 164: A3868-A3875.8195
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2School of Fundamental Science, Universiti Malaysia Terengganu, Kuala Nerus, Te rengganu, Malaysia 3School of Ocean Engineering, Universiti Malaysia Terengganu, Kuala Neru s, Terengganu, Malaysia E-Mail: mfhassan@umt.edu.my ABSTRACT In this work, we prepared a solid polymer electrolyte based on starch an d sodium hydroxide via a simple casting
Electrical Infrastructure includes an electrical installation, electrical equipment, electrical line or associated equipment for an electrical line. 1.9 Electrical installation As per the Electrical Safety Act 2002 (s15) (a) An electrical installation is a group of items of electrical equipment that—
Dynamic analyses can generate "dynamic program invariants", i.e., invariants of observed execution; static analyses can check them Dynamic analyses consider only feasible paths (but may not consider all paths); static analyses consider all paths (but may include infeasble paths) Scope Dynamic analyses examine one very long program path
P100 Partial Plumbing Plan ELECTRICAL E001 Electrical Notes E002 Electrical Symbols E003 Energy Compliance ED100 Electrical Demo Plan E100 Electrical Lighting Plan E200 Electrical Power Plan E300 Electrical One-Line E400 Electrical Schedules The Addenda, if any, are as follows: Number Date Pages . .
Export Content from Analyses and Dashboards 2-8 Export the Results of Analyses 2-9iii. Preface. Audiencexiv. Documentation Accessibilityxiv. Diversity and Inclusionxiv. Related Resourcesxv. Conventionsxv. Introduction to Oracle Transactional Business Intelligence . Get Started with Creating Analyses and Dashboards. About Oracle Transactional .
local (e.g., gap opening) behavior of the walls reasonably well.7 The fiber wall model was used to conduct nonlinear static lateral load analyses and nonlinear dynamic time history analyses of prototype walls. The typical behavior of the walls ob tained from static analyses is dis cussed below. Dynamic analyses of the walls are described .
physical education curriculum table of contents acknowledgements 2 district mission statement 3 physical education department mission statement 3 physical education task force 3 physical education and academic performance 4 naspe learning standards 8 new york state physical education learning standards 8 physical education high school curriculum guide 15 physical education curriculum analysis .
Layout the electrical circuit Clean/maintain the work place Carry Out Electrical Fittings and Fixtures Installation (SEIP-LIG-ELE-3-O) Install electrical circuit protection components Gather tools, equipment and electrical materials Install electrical fittings and fixtures Fix Electrical component holders and ceiling rose Clean/maintain the
26 00 00 Electrical General Requirements 26 01 00 Basic Electrical Systems Testing By Electrical Contactor 26 05 00 Basic Electrical Materials and Methods 26 08 00 Commissioning of Electrical Systems 26 10 00 Medium-Voltage Electrical Distribution 26 20 00 Electrical Service & Distribution 26 29 00 Variable Speed Drives 26 30 00 Standby Power .
