The textural properties of the samples of mesoporous TiW oxides.
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More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
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Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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T1D is a classic autoimmune disease. Genetic factors are clearly determinant but cannot explain the rapid, even overwhelming expanse of this disease. Understanding etiology and pathogenesis of this disease is essential. The complications associated with T1D cover a range of clinical obstacles. A number of experts in the field have covered a range of topics for consideration that are applicable to researcher and clinician alike. This book provides apt descriptions of cutting edge technologies and applications in the ever going search for treatments and cure for diabetes.",isbn:null,printIsbn:"978-953-307-788-8",pdfIsbn:"978-953-51-6584-2",doi:"10.5772/1539",price:139,priceEur:155,priceUsd:179,slug:"type-1-diabetes-complications",numberOfPages:494,isOpenForSubmission:!1,isInWos:1,hash:"b7ba654e889d323762cc9fb4a014cdbf",bookSignature:"David Wagner",publishedDate:"November 25th 2011",coverURL:"https://cdn.intechopen.com/books/images_new/1035.jpg",numberOfDownloads:56421,numberOfWosCitations:28,numberOfCrossrefCitations:3,numberOfDimensionsCitations:14,hasAltmetrics:0,numberOfTotalCitations:45,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"November 9th 2010",dateEndSecondStepPublish:"December 7th 2010",dateEndThirdStepPublish:"April 13th 2011",dateEndFourthStepPublish:"May 13th 2011",dateEndFifthStepPublish:"July 12th 2011",currentStepOfPublishingProcess:5,indexedIn:"1,2,3,4,5,6",editedByType:"Edited by",kuFlag:!1,editors:[{id:"45994",title:"Dr.",name:"David",middleName:"H",surname:"Wagner",slug:"david-wagner",fullName:"David Wagner",profilePictureURL:"https://mts.intechopen.com/storage/users/45994/images/1976_n.jpg",biography:"Dr. David Wagner, PhD is an Associate Professor in the Department of Medicine, Division of Pulmonary Sciences at the University of Colorado, Denver. 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To achieve mesoporous inorganic oxide powders with high surface area, uniformity and even mesoporous structures, there are many protocols have been implemented [1, 2] and the most important ones are: mesoporous silica materials as a host [3, 4], sol-gel precipitation, solution co-precipitation, thermal solid state, and surfactant self-assembled templates [5, 6, 7, 8]. Generally, the sol-gel precipitation, co-precipitation, and surfactant self-assembled templates were the most widely used methods for preparation of mesoporous ion exchange materials.
The synthesis of nonsiliceous nanostructured mesoporous materials with high surface area using surfactant self-assembled templates has been recognized as a method for controlling the phase structure, ordering and pore size of these functional materials [9, 10, 11, 12]. A wide range of mesoporous oxides, metals and semiconductors materials with regular geometries have been successfully prepared by direct templating from liquid crystalline phases [13]. Nevertheless the synthesis of nonsiliceous mesostructured still lags behind the synthesis of mesoporous silica materials, particularly for complex and multi-components inorganic materials. The reasons for this come from the complexity, reactivity, chemical stability and interaction of the surfactant with the inorganic precursor. Establishment of synthetic routes for multi-component metal oxide mesostructured those are effective, applicable, reproducible and suitable for large-scale production still remains a challenge.
Inorganic ion exchange materials are widely used for water treatment, in the semiconductor industry, and in nuclear technology. Multi-component ion-exchange materials, such as titanium tungstosilicate (TiWSi) and tungstophosphate (TiWP) mixed oxides have better chemical and thermal stability and exchange capacity compared to Ti (IV) tungstate, Ti (IV) silicate and Ti (IV) phosphate. The crystalline phases of these materials have been utilized for separating heavy metals in aqueous media. The adsorption, separation and exchange properties of these systems could potentially be enhanced significantly if the materials were obtained with mesoporous structures.
In this work, the solvent evaporation-induced self-assembly (EISA) template method is adapted to produce a selection of mesoporous ion exchange materials such as titanium tungstate (meso-TiW) titanium tungstosilicate (meso-TiWSi) and tungstophosphate (meso-TiWP) mixed oxides with the high surface area and controlled porous structures that similar to mesoporous silica. Using this method mesoporous ionic exchange materials can be synthesized with homogeneous and uniform structures in the form of powders, amenable to mass production, or as membranes depending on the conditions employed during the synthesis. The characterization and adsorption capacity of the resulting nanostructured mesoporous materials is investigated for water demineralization and the removal of heavy metal ions from water solution.
Using the template strategy to synthesize nanostructured mesoporous materials with a different shape, size and morphology was firstly introduced by Mobil scientists [14] and Martin et al. [15, 16]. In this template method, the desired materials are chemically formed using self-assembled surfactant templates (sol-gel) or electrochemically deposited inside the pores of a nanoporous membrane that subsequently dissolves away leaving a replica of nanomaterials structures. The templates are divided into two different types: hard and soft templates. The commonly used hard templates include anodic aluminum oxide [16], silica [17], and polystyrene spheres [18] and mesoporous carbon [19]. The soft templates are formed from surfactant molecules that are self-assembled into organized mesophases (soft matter) that are intermediate in order between crystalline solids and isotropic liquids.
In recent years, the sol-gel process is widely utilized concurrency with organic-directed assembly to synthesize a variety of non-siliceous mesostructured materials such as transition metals, metal oxides, semiconductors, carbons, and polymers. Such mesostructured materials have attracted significant attention because of the application of these materials in nanoscale devices, sensors, microelectronic devices, catalysts, energy storage media, and adsorbent materials. Mesoporous silica-based materials, for example, have been widely attracted an attention for heavy metal ions adsorption from wastewater [20, 21, 22, 23]. This because they exceptionally have the large specific surface area, regular pore structure, and tunable pore sizes. Consequently, the mesoporous materials are expected to exhibit better heavy metal ions adsorption due to improved accessibility to the adsorption sites and/or speeding up the diffusion process within the mesopores. Toward this end and very recently, mesoporous silica materials were prepared by microwave assistant heating using silica fume as silica source and evaluated as adsorbents for the removal of Cu2+, Pb2+, and Cd2+ from aqueous solutions [24]. The results showed that the produced mesoporous silica could efficiently confiscate the heavy metal ions from aqueous solution within pH range of 5–7 and the maximum removal capacities of the mesoporous silica for Cu2+, Pb2+, and Cd2+ were 36.3, 58.5, and 32.3 mg/g, respectively.
In addition, mesoporous silica modified with suitable organic functional groups have shown enhanced heavy metals adsorbents capacity due to combining the open porous structure of mesoporous silica with suitable organic compounds that exhibit high binding affinity toward the target metal ions. As an example, Lee et al. [22] reported the adsorption of Pb(II) and Cu(II) metal ions on mesoporous silica modified with organic amine and thiol functional groups and results reveal that the thiol-functionalized mesoporous silica adsorbents exhibit enhanced adsorption affinity for Pb2+ than the amino-mesoporous silica. Moreover, other studies reported an excellent Hg removal efficiency on thiolated mesoporous silica compared to the aminated ones [23, 25].
Sol-gel process using polyethylene oxide (PEO) as well as low molecular weight surfactants have been adapted for the preparation of thermally stable, ordered and large pore size mesoporous non-silica materials of metal oxides including MnO2, TiO2, ZrO2, Nb2O5, Ta2O5, Al2O3, SnO2, WO3, HfO2, and mixed oxides of Al2TiOy, ZrTiOy, ZrW2Oy [26, 27, 28]. The pore topology and pore size of the mesoporous oxides can be controlled by varying the surfactant or by the addition of hydrophobic swelling agents to the template mixture. However, the nature of the inorganic precursors of transition metals plays a critical for this process and it has to be compatible with organic co-assembly [29]. Therefore the evaporation-induced self-assembly (EISA) was introduced for the synthesis of non-silica mesostructured materials and has shown to be the very useful approach for both controlling macroscopic form (powder, thin films, and membranes) and mesostructured [30, 31]. In this EISA process, the mixture of volatile solvent, (commonly ethanol) surfactant and inorganic precursors are exposed to evaporation which drives the co-assembly of surfactant molecules and inorganic precursors to form the ordered mesophases. Subsequently using aging, chemical or heat treatments induce the formation of the desired mesostructures. Recently mesostructures of titanium tungstate with the high surface area, large pore volume, uniform pore size, and tunable W/Ti ratios were successfully fabricated by using (EISA) strategy [32]. Also, mesoporous zirconium phosphotungstate with large specific surface area ~170 m2/g, large pore volume, uniform pore size distribution, and tunable W/Zr ratios were prepared by adopting this EISA method [33]. In another template strategy, mesoporous TiO2/WO3 hollow fibers and interconnected nanotubes are prepared by hollow fibers as a framework, in addition, to block copolymer as a template. The mesostructures showed a surface area of ∼130 m2/g with improved photodegradation activity [34].
Earlier studies on the synthesis of inorganic ion-exchangers are well documented by Amphlet [35] and Clearfield [36]. A comprehensive review of inorganic ion-exchangers with layered structures [37] has been published which suggests that group IV phosphates, molybdates, tungstates, etc. possess interesting cation-exchange properties. Silicates of Ti(IV) have been shown to have porous properties and are being used as molecular sieves [38]. Two new crystalline phases of α-titanium phosphates with layered structures have been reported [39]. Siddiqui et al. [40] have synthesized crystalline phases of titanium tungstosilicate (TiWSi) and titanium tungstophosphate (TiWP) with better ion exchange capacity and better chemical and thermal properties as compared to titanium phosphate, titanium tungstate, and titanium silicate. Furthermore, ion-exchange materials with the amorphous state, crystalline state, and hybrid organic-inorganic states have been recently synthesized and studied for environmental applications [41, 42].
Triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly-(ethylene oxide) copolymer Pluronic® P123 (EO20PO70EO20, Mw = 5800, Sigma-Aldrich) was used as the structure-directing agent (SDA) and titanium tetraisobutoxide (Ti(OBu)4, 98%, Aldrich), tungsten hexachloride WCl6, phosphorus pentachloride PCl5 (reagent grade, 95%, Sigma-Aldrich) and tetraethyl orthosilicate (TEOS, 98%, AnalaR) were used as Ti, W, P and Si source respectively. n-Propanol (n-C2H8O, BDH AnalaR) was used for dissolve the surfactant and hydrochloric acid HCl (37 wt. %, Analar) were all supplied by Shanghai Chemical Corp. Copper(II) nitrate hydrate, lead(II) nitrate (ACS reagent, ≥99.0%) and mercury(II) nitrate monohydrate (ACS reagent, ≥98.0%) are purchased from Sigma-Aldrich. All other chemicals were used as received without further purification and all aqueous solutions were prepared using Milli-Q (Millipore, Inc.) high quality deionized (DI) water (resistance 18.2 MΩ cm).
Mesoporous bi-components titanium tungstate (meso-TiW-x) oxides were synthesized with different composition through a modified evaporation-induced self-assembly (EISA) method. Typically, with a total Ti-W molar content of 18 mmol, Ti(OBu)4 and WCl6 were first dissolved in a mixture containing 20 g of n-propanol and 2.0 g of Pluronic 123 (EO20PO70EO20). Then, the mixture was allowed for stirring for 2.0 hours at room temperature in a sealed vial. The obtained sol was cast into Petri dishes and kept under ambient conditions for 1 hour as shown in Scheme 1. Subsequently, the as-made gel was cured at 40°C for 2 days and then calcined in flowing air at 400°C for 4 hours with a ramping rate of 1°C min−1. The obtained samples of meso-TiW were denoted as meso-TiW-x, where X equals 20, 30, and 40 wt. % the percentage of W in the original template mixture.
Schematic diagram for the synthesis of mesoporous materials of titanium tungstate (meso-TiW) titanium tungestophosphate (meso-TiWP) and titanium tungstosilicate (meso-TiWSi) by EISA.
Specifically, for the synthesis of meso-TiW-20, meso-TiW-30 and meso-TiW-40, a 4.90, 1.43, 4.28 g of Ti(OBu)4 were added to 2.14, 3.68, 2.86 g of WCl6, respectively. In order to further moderate the hydrolysis rate, a 1.20 g of hydrochloric acid (37 wt. %) was added to the solution for synthesizing meso-TiW-20 oxides. A control experiment was performed to prepared pure meso-TiO2 using EISA approach for comparison purpose.
The mesoporous titanium tungstosilicate oxides (meso-TiWSi-x, where x is equal 5, 10, 15, 20, 40, 60 wt. % the percentage of Si in the original template mixture) and titanium tungstophosphate mixed oxides (meso-TiWP-x, where x is the wt. % of P in template mixture equal 5, 10, 15, 20 and 30 wt. %) were synthesized through adopted (EISA) method as shown above in Scheme 1. In a typical experiment, 2.86 g of WCl6 was dissolved in 10 g of n-propanol, this mixture was mixed by stirring until getting the clear solution then 3.68 g of Ti(OBu)4 was added to this solution to obtain a solution (A). Then 2.0 g of nonionic surfactant (triblock copolymer templates (P®123), was dissolved in 10 g n-propanol and stirred for 10 min and different amounts of TEOS (5, 10, 15, 20, 40, 60 wt. %) were added to this solution and stirring for another 5.0 min to obtain a solution (B). In case of titanium tungstophosphate 5, 10, 15, 20 and 30 wt. % of PCl5 was added to this solution and stirring for 5 min to obtain solution B. The solution (A) was added dropwise to (B) then the mixture was stirred for 2.0 hours at room temperature in a sealed vial. In order to further moderate the hydrolysis rate, 1.20 g of hydrochloric acid (37 wt%) was added to the solution for all prepared mixtures of mesoporous meso-TiWSi oxides. The obtained dark-blue colored homogeneous solution (shown in the inset in Scheme 1) was cast into Petri dishes and kept under ambient condition for 1.0 hour. Subsequently, the as-made gel was cured at 40°C for 2 days to completely remove solvents. Finally, the blue deposit was scraped and crushed into powder and then calcined in flowing air at 400°C for 4.0 hours with a ramping rate of 1.0°C/min.
X-ray powder diffraction (XRD) and Small-angle X-ray (SAXS) measurements were recorded respectively on a Bruker D4 powder X-ray diffractometer (Germany) and Nanostar U small-angle scattering system (Bruker, Germany) by using Cu Kα radiation (40 kV, 40 mA). The BET surface area, pore volume, and the pore size distributions were measured by nitrogen adsorption/desorption using a Micromeritics Tristar 3020 analyzer (USA). Prior to the measurements, the samples were degassed at 180°C for at least 6.0 hours. The Brunauer-Emmett-Teller (BET) method was utilized to calculate the specific surface area. By using the Barrett-Joyner-Halenda (BJH) model, the pore volumes and pore size distributions were derived from the adsorption branches of isotherms. Transmission electron microscopy (TEM) analysis was conducted on a JEOL 2011 microscope (Japan) operated at 200 kV and equipped with an energy dispersive X-ray (EDX) detector. Field-emission scanning electron microscopy (FESEM) images were collected on the Hitachi Model S-4800 field-emission scanning electron microscope. The heavy metals analysis was performed using an inductively coupled plasma optical emission spectroscopy (ICP-OES) system (Thermo Scientific; UK, Model ICAP 6000).
The standard procedure for the removal of heavy metal ions from water using the produced mesoporous materials was performed by mixing a weighted amount of the mesoporous absorbent with 3.0 mL solutions containing 0.2 mg/L Cu(II), Cd(II) or Pb(II) nitrate salt in polypropylene tubes. The samples were placed in a shaking water bath at 25°C for 2.0 hours and then the solution was separated by centrifuge at rpm 7000 for 10 min in each run. Each solution was then diluted by taking 100 μl and transferred into 10 mL conical polypropylene flask for analysis by ICP. The amount of metal ion adsorbed at the mesoporous adsorbents was calculated by the difference of the initial concentration (Co) and the equilibrium concentration (Ce). The removal efficiency and equilibrium adsorption capacity of Cd(II), Pb(II), and Hg(II) ions from the solution was calculated using the following equations:
Where, E, Q e, Co, Ce, V, and m are the removal efficiency, equilibrium adsorption capacity (mg/g), initial concentration (mg/L), equilibrium concentration (mg/L), solution volume (L) and adsorbent mass (g) respectively. To investigate metal ion loss during the adsorption due to the glassware or any of the experimental equipment a parallel experiment was performed in the absence of the mesoporous adsorbents and it was regarded as a standard solution.
In this section, we present the result for the synthesis of bi-components meso-TiW with various ratios using modified solvent evaporation-induced self-assembly (EISA). Firstly the synthesis of bi-components of mesoporous titanium tungstate (meso-TiW) with various compositions was executed. In EISA process the mixture of volatile solvent, (commonly ethanol), copolymer surfactant and inorganic precursors are mixed together and exposed to evaporation which drives the co-assembly of surfactant molecules and inorganic precursors to form the ordered mesostructures. The W content was varied between 20 and 40 moles and the meso-TiW powder after annealed at 400°C for 4.0 hours shows the light yellow color crystal as such shown in the inset of Scheme 1 which indicating on the precipitation of TiW oxide while pure meso-TiO2 exhibits white color.
Figure 1 shows the wide-angle XRD patterns for meso-TiW-20 and for pure meso-TiO2 prepared using EISA approach for comparison purpose. The XRD pattern of pure meso-TiO2 displayed a well-crystallized anatase phase (JCPDS Card No. 01-083-2243), while for meso-TiW-20 the XRD peaks intensity is slightly decreased in addition to the disappearance of some other peaks. This can attribute to the addition of 20 wt. % of W precursor hinders the crystallization of anatase phase and instead an amorphous composite of Ti▬W oxides were formed.
X-ray diffraction patterns for meso-TiW-20 and pure meso-TiO2 prepared by EISA approach and annealed at 400°C, 4.0 hours.
The nitrogen adsorption-desorption isotherms and the plot for pore size distribution of the mesoporous TiW-x oxides are shown in Figure 2. From the isotherms we can see that the meso-TiW oxide showed typical type IV isotherms with sharp capillary condensation steps at a relative pressure (P/Po) of 0.35–0.85 that characteristic for mesoporous materials.
(a) Nitrogen adsorption-desorption isotherms, (b) the corresponding pore size distribution curves of the meso-TiW oxide.
The average pore size, surface area (BET), pore volume for the meso-TiW oxide sample in comparing with pure mesoporous TiO2 (prepared using EISA approach but without adding WCl6) are shown in Table 1. Obviously, the meso-TiW-30 oxide shows the highest surface area; lower pore volume and a narrow pore size distribution which demonstrates the formation of highly ordered and uniform mesoporous structure. On the other hand, the pure mesoporous TiO2 prepared in absence of WCl6 shows lower surface area (81 m2/g) and higher pore volume with bimodal pore diameters. This can be attributed to the incorporation of W precursor effectively improve the order of mesoporous structure and because of the tungsten oxide has a high density (7.16 g/cm3) the incorporation of W leads to slightly reduce the pore volume of meso-TiW oxide.
Samples | SBET (m2/g) | Pore volume (cm3/g) | Pore size (nm) |
---|---|---|---|
meso-TiW-20 | 189 | 0.27 | 6.1 |
meso-TiW-30 | 206 | 0.21 | 3.9 |
meso-TiW-40 | 188 | 0.37 | 9.5 |
meso-TiO2 | 81 | 0.33 | 6/12.5 |
The textural properties of the samples of mesoporous TiW oxides.
Figure 3 shows the TEM image of the mesoporous meso-TiW samples. Clearly, the fine structure of the meso-TiW oxides shows typical morphologies of the highly ordered 2D hexagonal mesostructures with highly orderly channels extended over large domains which are consistent with high surface area obtained by N2 adsorption results and confirms the successful production of bi-components mesoporous TiW oxides by EISA approach.
TEM images of the samples (a) meso-TW-20, (b) meso-TW-30, and (c) meso-TW-40.
Here we investigate the possibility of synthesis more complicated mesoporous materials of tri-components mesoporous oxides of Ti, W, and Si. Because the bi-components meso-TiW-30 showed the highest surface area (206 m2/g) and ordered pore structure we used its composition of mole ratio (Ti70W30) as start material for the synthesis of tri-component mesoporous titanium tungstosilicate meso-TiWSi-x and tungstophosphate (meso-TiWP-x) materials with various compositions of silica (x = 10, 15, 20, 40 and 60 wt. %) via the facile EISA method employing P®123 surfactant, Ti(OBu)4, WCl6 and TEOS as described in Section 2 above and shown in Scheme 1. Optical images of the produced meso-TiWSi materials with Si ratio of 10, 15, 20, 40 and 60 wt. % after annealing at 400°C in the air are shown in the inset of Scheme 1.
Figure 4 shows the low-angle and wide-angle X-ray diffraction patterns of mesoporous meso-TiWSi-x calcined at 400°C in the air. As shown in Figure 4a, there’s a distinct peak at 2θ = 0.53°can be observed which is indexed as (100) reflections characterize of the 2D hexagonal mesostructure [32, 43]. Furthermore, another one broad and weak diffraction peak can clearly observe at 2θ = 1–1.5° indicates the long-range order of the mesopores structure. An increase in the Si ratio up to 60 wt. % result in one broad peak can be seen in the SXRD diffraction pattern, suggested that an excessive increase in Si incorporation decreased the ordering of the mesoporous structure. For the TiWSi-10, the first scattering peak shifts from a 0.53 nm−1 to a larger q value of a 0.56 nm−1, corresponding to the framework shrinkage during the removal of the template. The wide angle X-ray diffraction (WXRD) patterns of these samples are shown in Figure 4b. All the patterns kept consistent with each other and only exhibited two broad peaks in the 2θ range of 20–40° and 40–60°, indicating the existence of an amorphous or semicrystalline mesoporous TiWSi wall structure. No individual crystalline peak of titanium tungstate or titanium was observed.
(a) Low-angle and (b) wide-angle X-ray diffraction patterns of mesoporous meso-TiWSi-x calcined at 400°C in the air for 4.0 hours.
Meanwhile, there were no peaks of tungsten oxide in the patterns, illustrating the high dispersion of tungsten and silicon oxide among the mesoporous framework even in meso-TiWSi-0, which had silica ratio of 0 wt. %. This might be accounted to the silica atoms in the materials were segregated by titanium and tungsten atoms due to the advantage of using the one-pot EISA method [44]. We presumed that the presence of W and Si species somehow retarded the crystallization of TiO2 during the calcination and hence benefited the preservation of the ordered mesostructured which is consistent with Figure 4b and the previous studies [45, 46].
In order to further confirm the presence of mesopores in meso-TiWSi-x materials, the SEM and TEM characterizations were performed and Figure 5 shows the SEM images of the meso-TiWSi-x samples with different Si ratios after the annealing process. For the meso-TiWSi-10 (Figure 5a) and meso-TiWSi-20 (Figure 5b), the SEM images clearly show the highly ordered mesopores uniformly exist through the TiWSi framework over a wide micrometer area. However for meso-TiWSi-40 and meso-TiWSi-60, the SEM images in Figure 5c and d show wormlike mesoporous structure indicating on less order pore arrangement when Si ratio is increased to 60 wt. %.
SEM images of (a) meso-TiWSi-10 (b) meso-TiWSi-20 (c) meso-TiWSi-40 (d) meso-TiWSi-60.
Figure 6 shows the TEM images for different composition of meso-TiWSi after calcination and obviously, the TiWSi framework exhibits a 2D hexagonal mesostructured with ordered mesopores of about 10 nm in diameter. It also clearly observes the existence of ordered pores along the [110] and [001] directions in Figure 6b of meso-TiWSi-20. Nevertheless by further increasing the Si ratios to 60 wt. % (Figure 6d), the structure showed wormlike mesoporous channels rather than the long-range ordered hexagonal pores. The results of SEM and TEM agreed quite well with the results of the SXRD characterization, which predicted the presence of ordered mesoporous structure for samples with Si ratio from 0 to 20% and wormlike mesopores structure for meso-TiWSi-60.
TEM images of (a) meso-TiWSi-10 (b) meso-TiWSi-20 (c) meso-TiWSi-40 (d) meso-TiWSi-60.
For the elemental composition analysis, the backscattering SEM image and energy-dispersive X-ray (EDX) analysis of the elemental composition of the meso-TiWSi-20 materials are shown in Figure 7. The backscattering SEM image (Figure 7a) obviously shows very and highly order channels running through the meso-TiWSi framework confirming the formation of long-range and ordered mesopores. The EDX elemental analysis in Figure 7b shows evidently the existence of Ti, W, O and Si elements approving that all the elements were successfully introduced into the framework of the mesoporous structure. The Si wt. % derived from the EDX analysis were very close to the target composition set up in the template mixture as shown in Table 2.
(a) Backscatter SEM image of meso-TiWSi-20 (b) EDX elemental profile of meso-TiWSi-20.
Samples | Si wt. % |
---|---|
meso-TiWSi-10 | 7.4 |
meso-TiWSi-20 | 18.4 |
meso-TiWSi-60 | 54.3 |
EDX analysis of the Si wt. % in the meso-TiWSi samples.
The textural properties and the surface area of the ordered meso-TiWSi-x with different Si ratios were characterized by the N2-physisorption technique. Nitrogen adsorption and desorption isotherms and the corresponding pore size distributions of the meso-TiWSi materials are shown in Figure 8. For all the materials, the isotherms exhibited typical type IV isotherms and well-defined H2 shaped hysteresis loops with sharp capillary condensation steps at a relative pressure (P/Po) of 0.4–0.8, that characteristic of mesoporous materials [45, 47]. Besides, all the capillary condensation steps of the hysteresis loops for all the samples were very steep, pointing to the presence of a uniform and ordered pore size in the framework of meso-TiWSi. The average pore size of these samples was narrowly distributed at around 4–10 nm, implying the existence of the uniform mesoporous channels within the obtained materials. The details textual parameters including specific surface area, pore size and volume of meso-TiWSi-x obtained from the N2 adsorption-desorption isotherms, are summarized in Table 3. Clearly, all the samples had excellent textural properties with large specific surface area (131–188 m2 g−1), uniform pore size (4–10 nm) and pore volume (0.17–0.37 cm3 g−1).
(a) Nitrogen adsorption isotherms and (b) the corresponding pore size distribution curves of the meso-TWSi materials.
Samples | Specific surface area ± 5 (m2 g−1) | Pore size ±0.5 (nm) | Pore volume (cm3 g−1) |
---|---|---|---|
meso-TiWSi-0 | 188 | 9.5 | 0.37 |
meso-TiWSi-5 | 131 | 7.0 | 0.20 |
meso-TiWSi-10 | 164 | 5.5 | 0.19 |
meso-TiWSi-15 | 138 | 7.0 | 0.20 |
meso-TiWSi-20 | 142 | 7.5 | 0.22 |
meso-TiWSi-40 | 151 | 6.0 | 0.17 |
meso-TiWSi-60 | 156 | 5.0 | 0.19 |
Textural properties of the meso-TWSi-x materials derived from nitrogen adsorption and desorption analysis.
Tri-components mesoporous titanium tungstophosphates meso-TiWP-x materials were fabricated via the facile EISA method employing P®123 surfactants as a template and Ti(OBu)4, WCl6 and PCl5 as precursor for Ti, W and P respectively. Starting with Ti: W mole ration of 70:30, various compositions of P (5, 10, 15, 20 and 30 wt. %) were incorporated into the meso-TiW-30 and an optical image of the produced meso-TiWP-x samples is shown in the inset of Scheme 1.
Figure 9 shows the small and wide angle X-ray diffraction pattern of meso-TiWP-x samples after annealing at 400°C for 4 hours. As indicates in Figure 9a there’s a broad scattering peak in the 2θ range 0.5–1° which indicates on the formation of less ordered mesoporous TiWP structures. However, the meso-TiWP-10 shows rather well-defined peak among the other samples; presumably, due to better order pores have been formed. The wide-angle X-ray diffraction patterns of the TiWP samples shown in Figure 9b are consistent with each other and only exhibited two broad peaks in the 2θ range of 20–30° and 40–60° which is evidence for the existence of an amorphous or semi-crystalline framework of mesoporous TiWP. Based on the above results it can be concluded that the produce meso-TiWP-x samples have amorphous and less order porous structures than in the case of TiWSi.
X-ray diffraction patterns for meso-TiWP-x materials, (a) low angle and (b) high angle.
Figure 10 reveals the surface morphology of the meso-TiWP-x samples and by examining the SEM images, the formation of the pores are evidently observed within the TiWP framework and generally, the pores order seems to be irregular. However, for the meso-TiWP-10 sample, it shows some degree of ordered pores domains is formed. In addition the X-ray mapping and EDX composition analysis (not shown here) demonstrate the presence of Ti, W, P and oxygen elements which are uniformly distributed through the mesoporous TiWP materials.
SEM images of meso-TiWP-X: (a) meso-TiWP-5 (b) meso-TiWP-10 (c) meso-TiWP-15 (d) meso-TiWP-20.
The transmission electron microscope characterization of the meso-TiWP-x materials is illustrated in Figure 11. The TEM images of the mesoporous TiWP-x materials display large domains of the porous structure obtained after direct calcination at 400°C in the air due to the removal of templates. Clearly, the pores arrangement is rather random presumably due to the source of phosphor (PCl5) affected the formation of the ordered mesostructured during the self-assembly process. However the TEM image for meso-TiWP-10 with phosphor content of 10 wt. % shows the pores are arranged in the highly ordered structure. It implies that adding phosphorus with 10 wt. % retains the pore order of the titanium tungstophosphates.
TEM images of (a) meso-TiWP-5, (b) meso-TiWP-10, (c) meso-TiWP-15, (d) meso-TiWP-20 after annealing at 400°C in air for 4 hours.
The N2 adsorption/desorption isotherms of meso-TiWP-x materials after annealing at 400°C in the air are shown in Figure 12a. Evidently, the N2 adsorption/desorption isotherms for meso-TiWP-x materials show typical type IV curves with a sharp capillary condensation step at P/Po = 0.8–0.9 and an H2-type hysteresis loop, which is typical of large-pore mesoporous materials with cylindrical channels. The pore size derived from the adsorption branches of the isotherms by using the Barrett-Joyner-Halenda method is shown in Figure 12b. Generally, the pore diameter for the meso-TiWP-x materials shows a narrow distribution and a gradual decrease as the phosphorus content increases, with a pore diameter of 9.6 nm for meso-TiWP-0 and 4.3 nm for meso-TiWP-30 as reported in Table 4. The Brunauer-Emmett-Teller surface area and pore volume of the meso-TiWP-x materials are calculated from the N2 adsorption/desorption isotherms and reported in Table 4. The BET surface area of the meso-TiWP-x materials is varied between 188 m2/g for no phosphorus and a 128 m2/g for meso-TiWP-15 which presumably due to the formation of the more crystalline mesoporous wall as the phosphorus is added to titanium tungstate. However, it can conclude that mesostructured of titanium tungstate can be retained during the addition of phosphorus and annealing treatment which confirms the versatility of EISA soft template approach to producing multi-components mesoporous oxides with various compositions.
(a) Nitrogen adsorption/desorption isotherms of meso-TiWP-x and (b) the corresponding pore size distribution curves.
Material | Pore diameter/nm | Pore volume/cm3 g−1 | Specific surface area/m2 g−1 |
---|---|---|---|
meso-TiWP-0 | 9.5 | 0.37 | 188 |
meso-TiWP-5 | 7.5 | 0.232 | 140 |
meso-TiWP-10 | 7.6 | 0.220 | 129 |
meso-TiWP-15 | 5.6 | 0.200 | 128 |
meso-TiWP-20 | 4.5 | 0.150 | 153 |
meso-TiWP-30 | 4.3 | 0.120 | 154 |
Textural properties of the meso-TiWP-x materials derived from nitrogen adsorption/desorption analysis.
This section reports the preliminary evaluation of the produced mesoporous materials for heavy metal ions removal from synthetic water solution. The ability of mesoporous titanium tungstosilicate to enrich the metals ions absorption from water was tested by adding aliquots of metal ions solution to a known weight of meso-TiWSi-x absorbent. Figure 13 shows the effect of the meso-TiWSi-x loading on the removal efficiency of Cd(II), Hg(II) and Pb(II) ions at pH equals 7 and 25°C. It is observed that the Cd(II) ion uptakes are independent on absorbent loading of meso-TiWSi-10 (Figure 13a) and the removal efficiency stabilized at around 92%. On the other hand, for Hg(II) ion uptakes gradually increase as the meso-TiWSi-10 absorbent load increases reaching about 92% at 200 mg meso-TiWSi-10 loading. However, for Pb(II) ion adsorption at meso-TiWSi-10 is inconsistent and unexpectedly shows a decrease in absorption efficiency as the absorbent loading increased. Figure 13b shows with the addition of meso-TiWSi-20 adsorbent in the range of 50–200 mg, no significant variation in the metal ions uptakes were observed for Hg(II), whereas slight decrease in Cd(II) ions removals was maintained. In contrast, the Pb(II) ions uptakes show a remarkable increase in a number of meso-TiWSi-20 adsorbent increases and 80% removal efficiency was achieved at 200 mg adsorbent. Effect of meso-TiWSi-40 adsorbent dose on the adsorption of Cd(II), Pb(II) and Cd(II) are shown in Figure 13c. The removal efficiency of Hg(II) and Pb(II) gradually increases with increasing the adsorbent dose and record about 90 and 85% respectively. This can attribute to the greater availability of the exchangeable sites or surface area at a higher concentration of the adsorbent. While increasing the meso-TiWSi-40 adsorbent dose gave rise to a remarkable decrease in adsorption of Cd(II).
Effect of the adsorbent dose of (a) meso-TiWSi-10, (b) meso-TiWSi-20, (c) meso-TiWSi-40 on the adsorption of Pb(II), Cd(II) and Hg(II) from aqueous solution at pH of 7, a contact time of 2 hours and a metal ion concentration of 20 ppm, (d) effect of contact time on the adsorption of Pb(II), Cd(II) and Hg(II) from aqueous solution by m-TiWSi-20 at pH of 5, 0.15 g m-TiWSi-20/3 mL solution and a metal ion concentration of 0.2 mg/L.
Figure 13d shows the effects of agitation time on the removal efficiency of Hg(II), Cd(II) and Pb(II) using 150 mg of meso-TiWSi-20 adsorbent at pH = 6. It was noted that the adsorption of Cd(II) and Pb(II) gradually increases with an increase in agitation time and attains an equilibrium adsorption of 95 and 89% respectively within 40 min. Then the removal efficiency gradually decreases at longer agitation time. This result is important as the equilibrium time is a key parameter for economical wastewater treatment applications. On the other hand, the adsorption equilibrium time for Hg(II) takes about 2 hours to reach adsorption efficiency of 90%.
The mesoporous titanium tungstophosphate (meso-TiWP) adsorbent was also evaluated for the adsorption of heavy metal ions from water. Figure 14a shows the effect of the meso-TiWP-15 and meso-TiWP-20 adsorbent dose of on the uptakes of Hg(II) ions from water at pH 6. At a fixed Hg(II) ion concentration, it can be observed that the removal % of Hg(II) ion slightly increases with increasing weight of the adsorbents. This is attributed to the high surface area and greater availability of adsorption active sites of meso-TiWP-15 and meso-TiWP-20 adsorbents. For 95% removal of Hg(II) ion a maximum of 100 mg is required from meso-TiWP-15 or meso-TiWP-20 adsorbent. Figure 14b shows the effect of adsorption time on the removal efficiency of Hg(II), Cd(II) and Pb(II) ions using 150 mg of the meso-TiWP-15 absorbent. It is seen that for meso-TiWP-15 absorbent exhibited a rapid adsorption for Cd(II) and Pb(II) ions with a removal efficiency reaching about 90% within the first 10 min while it takes about 1.0 hour to achieve 80% for Hg(II) adsorption.
(a) Effect of the meso-TiWP-15 and a meso-TiWP-20 dose of on the adsorption of Hg(II) from aqueous solution, experimental conditions included a solution pH of 6, a contact time of 2 hours and a metal ion concentration of 20 mg/L, (b) effect of contact time on the adsorption of Pb(II), Cd(II) and Hg(II) from aqueous solution by m-TiWP-15. Experimental conditions included a solution pH of 5, 0.15 g m-TiWP-15/3 mL solution and a metal ion concentration of 0.2 mg/L.
Finally, Table 5 shows a comparison of the heavy metal ions removal efficiency of the best performance of our mesoporous titanium tungstophosphate and tungstosilicate materials with some of the modified mesoporous silica-based material widely reported in the literature at similar experimental conditions. Mesoporous meso-TiWP-20 showed a good performance for removing Cu2+, Pb2+, and Cd2+ in the pH region of 5.0–7.0 which is comparable to the performance, for example, mesoporous silica modified with amine functional group and magnetic iron oxide. This metal ion adsorption enhancement can be apparently attributed to the higher surface area and active sites available to metal ion binding at the surface of meso-TiWP and meso-TiWSi adsorbents [7].
Adsorbent | Cu | Pb | Cd | Hg | Ref. |
---|---|---|---|---|---|
SBA-15-3-aminopropyl trimethoxy-silane | 98.0 | 99.0 | 90.0 | — | [48] |
KIT-6-ethylenediaminetetraacetic acid (EDTA) | 99.5 | 98.0 | 99.0 | — | [49] |
SBA-15-ethylenediaminetetraacetic acid (EDTA) | 99.0 | 98 | 99.5 | — | [49] |
SBA-15-aminopropyl (SBA/NH2) | — | 96 | 50 | — | [50] |
Magnetic MCM-48 mesoporous silica amine (▬NH2) | 91 | 96 | 90 | — | [51] |
meso-TiWP-20 | 95.9 | 95.5 | 95.8 | — | This work |
meso-TiW-20 | 50 | 76 | — | — | This work |
meso-TiWSi-10 | — | 82 | 91 | 92 | This work |
A comparison of the heavy metal ions removal efficiency of the best performance meso-TWSi-x and meso-TiWP-x materials with some of the modified mesoporous silica-based material reported in the literature.
In this work we investigate the synthesis of new bi- and tri-component of mesoporous oxides of titanium tungstate (TiW), titanium tungstosilicate (TiWSi) and titanium tungstophosphate (TiWP) oxides. For the mesoporous titanium tungstosilicate, the silica content was varied between 10, 15, 20, 40 and 60 wt. % using TEOS precursor, while for mesoporous titanium tungstophosphates the ratio of phosphorus was varied as 5, 10, 15, 20 and 30 wt. % by adding PCl5 into the EISA template mixture of P®123 surfactants, Ti(OBu)4 and WCl6 precursors. Subject to silica and phosphorus content, the obtained meso-TiWSi-x and meso-TiWP-x exhibits high surface area, ordered 2D hexagonal mesostructure with orderly channels extended over a large domain. The EISA approach demonstrates a successful synthesis approach for the synthesis of new complex inorganic nanostructured and mesoporous materials for potential application in environmental and catalysis. The produced meso-TiW, meso-TiWSi, and meso-TiWP adsorbents exhibit good adsorbent efficiency for the removal of Pb(II), Cd(II) and Hg(II) ions from water due to the presence of high surface area and accessibility of surface active sites. The adsorption of these metal ions is found to be dependent on contact time and adsorbents dose.
This work was funded by The National Plan for Science, Technology, and Innovation (MAARIFAH) King Abdulaziz City for Science and Technology, Kingdom of Saudi Arabia, Award number AT34-203. The authors appreciate Dr. Yuhui Li and Prof. Dongyuan Zhao from Fudan University for their cooperation in the SEM and TEM analysis.
There is no any conflict of interest can be declared.
Voltammetry is an electrochemical technique for current-voltage curves, from which electrode reactions at electrode-solution interfaces can be interpreted. Since current-voltage curves, called voltammograms, include sensitive properties of solution compositions and electrode materials, their analysis provides not only chemical structures and reaction mechanisms on a scientific basis but also electrochemical manufacture on an industrial basis. The voltammograms vary largely with measurement time except for steady-state measurements, and so it is important to pay attention to time variables. Voltage is a controlling variable in conventional voltammetry, and the current is a measured one detected as a function of applied voltage at a given time.
\nThe equipment for voltammetry is composed of electrodes, solution, and electric instruments for voltage control. Electrodes and electric instruments are keys of voltammetry. Three kinds of electrodes are desired to be prepared: a working electrode, a counter one, and a reference one. The three will be addressed below.
\nLet us consider a simple experiment in which two electrodes are inserted into a salt-included aqueous solution. When a constant current is applied to the two electrodes, reaction 2H+ + 2e− → H2 may occur at one electrode, and reaction 2OH− → H2O2 + 2e− occurs at the other. The current is the time variation of the electric charge, and hence it is a kind of reaction rate at the electrode. Since the applied current is a sum of the two reaction rates, one being in the positive direction and the other being in the negative, it cannot be attributed to either reaction rate. A technique of attributing the reactions is to use an electrode with such large area that an uninteresting reaction rate may not become a rate-determining step. This electrode is called a counter electrode. The current density at the counter electrode does not specifically represent any reaction rate. In contrast, the current density at the electrode with a small area stands for the interesting reaction rate. This electrode is called a working electrode. It is the potential difference, i.e., voltage, at the working electrode and in the solution that brings about the electrode reaction. However, the potential in the solution cannot be controlled with the working electrode or the counter one. The control can be made by mounting another electrode, called a reference electrode, which keeps the voltage between an electrode and a solution to be constant. However, the constant value cannot be measured because of the difference in phases. A conventionally employed reference electrode is silver-silver chloride (Ag-AgCl) in high concentrated KCl aqueous solution.
\nAn electric instrument of operating the three electrodes is a potentiostat. It has three electric terminals: one being a voltage follower for the reference electrode without current, the second being a current feeder at the counter electrode, and the third being at the working electrode through which the current is converted to a voltage for monitoring. A controlled voltage is applied between the working electrode and the reference one. These functionalities can readily be attained with combinations of operational amplifiers. A drawback of usage of operational amplifiers is a delay of responses, which restricts current responses to the order of milliseconds or 10 kHz frequency.
\nVoltammetry includes various types—linear sweep, cyclic, square wave, stripping, alternating current (AC), pulse, steady-state microelectrode, and hydrodynamic voltammetry—depending on a mode of the potential control. The most frequently used technique is cyclic voltammetry (CV) on a time scale of seconds. In contrast, currently used voltammetry at time as short as milliseconds is AC voltammetry. We describe here the theory and tips for practical use of mainly the two types of voltammetry.
\nThe theory of voltammetry is to obtain expressions for voltammograms on a given time scale or for those at a given voltage. First of all, it is necessary to specify rate-determining steps of voltammograms. There are three types of rate-determining steps under the conventional conditions: diffusion of redox species in solution near an electrode, adsorption on an electrode, and charging processes at the double layer (DL). Electric field-driven mass transport, called electric migration, belongs to rare experimental conditions, and hence it is excluded in this review. When a redox species in solution is consumed or generated at an electrode, it is supplied to or departed from the electrode by diffusion unless solution is stirred. When it is accumulated on the electrode, the change in the accumulated charge by the redox reaction provides the current. Whenever electrode voltage is varied with the time, the charging or discharging of the DL capacitor causes current. Therefore, the three steps are frequently involved in electrochemical measurements.
\nA mass transport problem on voltammetry is briefly described here. The redox species is assumed to be transported by one-directional (x) diffusion owing to heterogeneous electrode reactions. Then, the flux is given by f = −D(∂c/∂x), where c and D are the concentration and the diffusion coefficient of the redox species, respectively. Redox species in solution causes some kinds of chemical reaction through chemical reaction rates, h(c, t). Then the reaction rate is the sum of the diffusional flux and the chemical reaction rate, ∂c/∂t = −∂f/∂x − h(c, t). Here the equation for h = 0 is called an equation of continuum. Eliminating f with the above equation on the assumption of a constant value of D yields ∂c/∂t = D(∂2c/∂x2) − h(c, t). This is an equation for diffusion-chemical kinetics. The expression at h = 0 is the diffusion equation. A boundary condition with electrochemical significance is the control of c at the electrode surface with a given electrode potential. If the redox reaction occurs in equilibrium with the one-electron transfer at the electrode, the Nernst equation for the concentrations of the oxidized species, co, and the reduced one, cr, holds.
\nwhere Eo is the formal potential. If there is no adsorption, the zero-flux condition in the absence of accumulation is valid:
\nThe other conditions are concentrations in the bulk (x → ∝) and the initial conditions.
\nIf the mass transport is controlled only by x-directional diffusion, cr and co are given by the diffusion equations, ∂c/∂t = D(∂2c/∂t2) for c = cr or co. An electrochemically significant quantity is not concentration in any x and t, but a relation between the surface concentrations and the current (the flux at x = 0). On the assumption of Do = Dr = D, of the initial and boundary conditions, (cr)t = 0 = c*, (co)t = 0 = 0, and (cr)x = ∞ = c*, (co)x = ∞ = 0, a solution of the initial-boundary problem is given by [1].
\nwhere j is the current density. The common value of the diffusion coefficients yields co + cr = c* for any x and t. Inserting this relation and Eq. (3) into the Nernst equation, (co)x = 0 = c*/[1 + exp[−F(E − Eo)/RT]], we obtain the integral equation for j as a function of t or E.
\nWhen the voltage is linearly swept with the time at a given voltage scan rate, v, from the initial potential Ein, Eq. (3) through the combination with the Nernst equation becomes
\nThe above Abel’s integral equation can be solved by Laplace transformation. When the time variation is altered to the voltage variation through E = Ein + vt, the current density is expressed as
\nwhere ζ = (E − Eo)F/RT and ζi = (Ein − Eo)F/RT. Evaluation of the integral has to resort to numerical computation. Current at any voltage should be proportional to v1/2, as can be seen in Eq. (5). The voltammogram for v > 0 rises up from Eo, takes a peak, and then deceases gradually with the voltage. The decrease in the current is obviously ascribed to relaxation by diffusion. The peak current density is expressed by
\nat Ep = Eo + 0.029 V at 25°C, where 0.446 comes from the numerical calculation of the integral of Eq. (5).
\nPractical voltage-scan voltammetry is not simply linear sweep but cyclic voltammetry (CV), at which applied voltage is reversed at a given voltage in the opposite direction. The theoretical evaluation of the voltammogram should be at first represented in the integral form with the time variation and then express the time as the voltage. One of the features of the diffusion-controlled cyclic voltammograms is the difference between the anodic peak potential and the cathodic one, ΔEp (in Figure 1), of which value is 59 mV at 25°C.
\nVoltammograms calculated from Eq. (5) for v = (a) 180, (b) 80 and (c) 20 mV s−1.
AC voltammetry can be performed when the time variation of voltage is given by E = Edc + V0eiωt, where ω is the frequency of applied AC voltage, i is the imaginary unit, V0 is its voltage amplitude, and Edc is the DC voltage. A conventional value of V0 is 10 mV. When this voltage form is inserted into Eq. (3) together with the Nernst equation, the AC component of the current density is represented by [2].
\nA voltammogram (j vs. Edc) at a given frequency takes a bell shape, which is expressed by sech2{(Edc − Eo)/RT}. The functional form of sech2 is shown in Figure 2. The peak current appears at Edc = Eo.
\nVoltammogram calculated from Eq. (10).
The AC-impedance technique often deals with the real impedance, Z1, = 1/2Y1 and the imaginary one, Z2 = −1/2Y1, where Y1 is the real admittance given by
\nHere Y2 is the imaginary admittance, equal to Y1. Since Z1 = −Z2, the Nyquist plot, i.e., −Z2 vs. Z1, is a line with the slope of unity. The term 1 + i in Eq. (7) has come from (Dω)1/2, originating from (Diω)1/2. Therefore, it can be attributed to diffusion. In other words, diffusion produces the capacitive component as a delay.
\nWhen the redox species with reaction R = O + e− is adsorbed on the electrode and has no influence from the redox species in the solution, the sum of the surface concentrations of R and O is a constant, Γ*. Then the surface concentration of the oxidized species, Γo, is given by the Nernst equation:
\nThe time derivative of the redox charge corresponds to the current density, j = d(FΓo)/dt. Application of the condition of voltage sweep, E = Ein + vt, to Eq. (9) yields.
\nThe voltammogram takes a bell shape (Figure 2), of which peak is at E = Eo, similar to the AC voltammogram. The current at any voltage is proportional to v. Since the negative-going scan of the voltage provides negative current values, the cyclic voltammogram should be symmetric with respect to the I = 0 axis. The peak current is expressed as jp = F2Γ*v/4RT. The width of the wave at jp/2 is 90 mV at 25°C.
\nSince a phase has its own free energy, contact of two phases provides a step-like gap of the free energy, of which gradient brings about infinite magnitude of force. In order to relax the infinity, local free energy varies from one phase to the other as smoothly as possible at the interface. The large variation of the energy is compensated with spontaneously generated space variations of voltage, i.e., the electric field, which works as an electric capacitor. The capacitance at solution-electrode interface causes orientation of dipoles and nonuniform distribution of ionic concentration, of which layer is called an electric double layer (DL).
\nWhen the time variation of the voltage is applied to the DL capacitance, Cd, the definitions of the capacitance (q = CdV) and the current lead
\nwhere Cd generally depends on the time. This dependence is significant for understanding experimentally observed capacitive currents.
\nThe DL capacitance has exhibited the frequency dispersion expressed by Cd = (Cd) 1Hz f −λ, called the constant phase element [3, 4, 5] or power law [6, 7], where λ is close to 0.1. Inserting this expression and V = V0eiωt into Eq. (11) yields
\nThis is a simple sum of the real part of the current and the imaginary one, indicating that the equivalent circuit should be a parallel combination of a capacitive component and a resistive one, both depending on frequency. Since the ratio, −Z2/Z1, for Eq. (12) is 1/λ, the Nyquist plots have slopes less than 10 rather than infinity.
\nIf the capacitive charge is independent of the time, the capacitive current should be I = d(CV)/dt = C(E − Eo)/v. Therefore, it takes a horizontal positive (v > 0) and a negative line (v < 0), as shown in Figure 3 (dashed lines). When the time dependence of C, i.e., Cd = (Cd)0t−λ, is applied to Eq. (11), for the forward and the backward scans, respectively, we have
\nCapacitive voltammograms by CV at v= 0.5 V s−1 for (dashed lines) the ideal capacitance and for Eq. (13) (solid curves) at λ = 0.2.
The variation of CV computed from Eq. (13) (Figure 3, solid curves) is similar to our conventionally observed capacitive waves.
\nVoltammograms can identify an objective species by comparing a peak potential with a table of redox potentials and furthermore determine its concentration from the peak current. Their results are, however, sometimes inconsistent with data by methods other than electrochemical techniques if one falls in some pitfalls of analytical methods of electrochemistry. For example, a peak potential is influenced by a reference electrode and solution resistance relevant to methods. Peak currents are varied complicatedly with mass transport modes as well as associated chemical reactions. Since the theory on voltammetry covers only some restricted experimental conditions, it can rarely interpret the experimental data successfully. This review is devoted to some voltammetric tips which can lead experimenters to reasonable interpretation.
\nIt is rare to observe a reversible voltammogram in which both oxidation and reduction waves appear in a symmetric form with respect to the potential axis at a similar peak potential, as in Figure 1. Frequently observed voltammograms are irreversible, i.e., either a cathodic or an anodic wave appears; a value of a cathodic peak current is quite different from the anodic one in magnitude; a cathodic peak potential is far from the anodic one. These complications are ascribed to chemical reactions and/or phase transformation after the charge-transfer reaction. A typical example is deposition of metal ions on an electrode. The complications can be interpreted by altering scan rates and reverse potentials.
\nA wave at a backward scan is mostly attributed to electrode reactions generated by experimenters rather than to species latently present in the solution. That is, it is artificial. It is caused either by the reaction of the wave at the forward scan or the reaction of the rising-up current just before the reverse potential. A source of the backward wave can be found by changing the reverse potentials.
\nSome voltammograms have more than two peaks at one-directional scan. The appearance of the two can be interpreted as a two-step sequential charge-transfer reaction. However, multiple waves appear also by combinations of chemical reactions and adsorption. The peak current and the charge for this case are quite different from the predicted ones, as will be described in Section 3.2. Change in scan rates may be helpful for interpreting the multiple waves.
\nIt is possible to predict theoretically a controlling step of voltammograms from their shape (a bell type corresponding to an adsorption wave or a draw-out type corresponding to a diffusion wave). However, the shape strongly depends on chemical complications, adsorption, and surface treatment of the electrodes. When redox species in solution is partially adsorbed on an electrode, the electrode process is far from a prediction because of very high concentration in the adsorbed state. A draw-out-shaped wave can be observed even for the adsorbed control. It is important to estimate which state the reacting species takes on the electrode. Potentials representing of voltammetric features do not express a controlling step in reality although the theory does. One should pay attention to the current. The peak current controlled by diffusion with one-electron transfer is given by Ip = 0.27 cAv1/2 μA (c, bulk concentration mM; A, electrode area mm2; v, potential sweep rate mV s−1). The microelectrode behavior sometimes comes in view at v < 10 mV s−1, A < 0.1 mm2, so the measured current is larger than the estimated value. On the other hand, the peak current controlled by adsorption is given by Ip = 1.6 Av nA when one redox molecule is adsorbed at 1 nm2 on the electrode. The voltammogram by adsorption often differs from the ideal bell shape due to adsorbed molecular interaction and DL capacity. Division of the area of the peak by the scan rate yields the amount of adsorbed electricity. Comparison of this with the anticipated amount of adsorption may be helpful for understanding the electrode process.
\nThe peak potential difference ΔEp between the oxidation wave and the reduction wave (Figure 1) has been used for a prediction of the reaction mechanism. For example, ΔEp = 60 mM suggests the diffusion-controlled current accompanied by one-electron exchange, whereas ΔEp = 30 mM infers a simultaneous reaction with two electrons. Then what would happen for 120 mV which is sometimes found? A half-electron reaction might not be accepted. Potential shift over 60 mV occurs by chemical complications. In contrast, the voltammogram by adsorbed species shows theoretically a bell shape with the width, E1/2 = 90 mV, at the half height of the peak (Figure 2). This value is based on the assumption of the absence of interaction among adsorbed species. However, adsorption necessarily yields such high concentrations as strong interaction.
\nIt is necessary to pay attention to the validity of analyzing ΔEp and E1/2. The peak potential is the first derivative of a voltammogram. Since ΔEp is a difference between the two peaks, it is actually the second-order derivative of the curves in the view of accuracy. In other words, the accuracy of ΔEp is lower than that of peak current. Furthermore, peak potentials as well as E1/2 readily vary with scan rates owing to chemical reactions and solution resistance. One should use the peak current for data analysis instead of the potentials.
\nVoltammograms of a number of redox species have been reported to be diffusion controlled from a relationship between Ip and v1/2. The redox species exhibiting diffusion-controlled current is, however, limited to ferrocenyl derivatives under conventional conditions. Voltammograms even for [Fe(CN)6]3−/4− and [Ru(NH3)6]3+ are deviated from the diffusion control for a long-time measurement. Why have many researchers assigned voltammograms to be the diffusion-controlled step? The proportionality of Ip to v1/2 in Eq. (6) has been confused with the linearity, Ip = av1/2 + b (b ≠ 0). The plot for the adsorption control (Ip = kv) also shows approximately a linear relation for Ip vs. v1/2 plot in a narrow domain of v, as shown in Figure 4B. The opposite is true (Figure 4A). Therefore, it is the intercept that determines a controlling step of either the diffusion or adsorption. Some may say that the intercept can be ascribed to a capacitive current. If so, the peak current should be represented by Ip = av1/2 + bv, which exhibits neither linear relation with v1/2 nor v.
\nPlots of Ip of (A) K3Fe(CN)6 and (B) polyaniline-coated electrode against v1/2 and v. Both plots show approximately linear relations.
There is a simple method of determining a controlling step either by diffusion or adsorption. Current responding to diffusion-controlled potential at a disk electrode in diameter less than 0.1 mm would become under the steady state after a few seconds [8]. Adsorption-limited current should become zero soon after the potential application. Many redox species, however, show gradual decrease in the current because reaction products generate an adsorbed layer which blocks further electrode reactions.
\nIt is well known that currents vary not only with applied voltage but also with the time. It is not popular, however, to discuss quantitatively time dependence of CV voltammograms. Enhancing v generally increases the current and causes the peak potential to shift in the direction of the scan. A reason for the former can be interpreted as generation of large current at a shorter time (see Eqs. (6) and (10)), whereas the latter is ascribed to a delay of reaction responses as well as a voltage loss of the reaction by solution resistance. Then the voltage effective to the reaction is lower than the intended voltage, and so the observed current may be smaller than the predicted one. Although Ip is related strongly with Ep, the relationship has rarely been examined quantitatively.
\nA technique of analyzing the potential shift is to plot Ip against Ep, [9] as shown in Figure 5. If the plots on the oxidation side (Ip > 0) and the reduction side (Ip < 0) fall each on a straight line, the slope may represent conductivity. If values of both slopes are equal, the slope possibly stands for the conductivity of the solution or membrane regardless of the electrode reaction. The potential extrapolated to the zero current on each straight line should be close to the formal potential. Since this plot is simple technically, the analytical result is more reliable than at least discussion of time dependence of Ep.
\nPlots of Ip vs. Ep by CV of the first (circles) and the second (triangles) peak of tetracyanoquinodimethane (TCNQ), and ferrocene (squares) in 0.2 M (CH3)4NPF6 included acetonitrile solution when scan rates were varied, where triangles were displayed by 0.4 V shift.
Most researchers have quoted the Randles-Sevcik equation, jp = 0.446 (nF)3/2c*(Dv/RT)1/2, for the diffusion-controlled peak current without hesitation, where n is the electron transfer number of the reaction. According to Faraday’s law, the electrolytic quantity is proportional to nc*. Why is the peak current proportional to n3/2 instead of n? Let us consider voltammetry of metal nanoparticles (about 25 nm in diameter) composed of 106 metal atoms dispersed in solution. Faraday’s law predicts that the current is 106 times as high as the current by the one metal atom. However, Randles-Sevcik equation predicts the current further (106)1/2 = 1000 times as large, just by the effect of the potential scan. The order 3/2 is specific to CV. The order of n for AC current and pulse voltammetry is 2 [10]. On the other hand, the diffusion-controlled steady-state currents at a microelectrode and a rotating disk electrode are proportional to n. Comparing the differences in the order by methods, we can predict that the time variation of the voltage increases the power of n.
\nLet a potential width from a current-rising potential to Ep be denoted by ΔE. When an n-electron transfer reaction occurs through the Nernst equation at which F in Eq. (1) is replaced by nF, the concentration-potential curve takes the slope n times larger than that at n = 1 (see co/cr ≅ nF(E − Eo)/RT near E = Eo in Eq. (1)). Then we have (ΔE)n = (ΔE)n = 1/n. The period of elapsing for (ΔE)n becomes shorter by 1/n, as if v might be larger by n times. Then v in Eq. (6) should be replaced by (nv)1/2. Combining this result with the flux j/nF, the current becomes n3/2 times larger than that at n = 1. Therefore, the factor n3/2 results from the Nernst equation. This can be understood quantitatively by replacing F in Eq. (3) by nF. There are quite a few reactions for n ≥ 2 both for Nernst equation and in the bulk as stable species. The term n3/2 is valid only for a concomitant charge-transfer reaction, i.e., simultaneous occurrence n-electron transfer rather than a step-by-step transfer. Apparent two-electron transfer reactions in the bulk, for example, Cu, Fe, Zn, and Pb, cause other reactions immediately after the one-electron transfer.
\nAn electrochemical response is observed as a sum of the half reactions at the two electrodes. In order to extract the reaction at the working electrode, a conventional technique is to increase the area of the counter electrode so that the reaction at the counter electrode can be ignored. If the counter electrode area is increased by 20 times the area of the working electrode, the observed current represents the reaction of the working electrode with an error of 5%. Let us consider the experiment in which nanoparticles of metal are coated on a working electrode for obtaining capacitive currents or catalyst currents. Then, the actual area of the working electrode can be regarded as the area of the metal particles measured by the molecular level. Then, the area will be several thousand times the geometric area so that the observed current may represent the reaction at the counter electrode. This kind of research has frequently been found in work on supercapacitors. On the other hand, if the electrode reaction is diffusion controlled, the current is determined by the projected area of the diffusion layer. Then the current is not affected by the huge surface area of nanoparticles.
\nIt is important to examine whether or not a reaction is controlled by at a counter electrode. A simple method is to coat nanoparticles also on the counter electrode. Then the current in the solution may become so high that the potential of the working electrode cannot be controlled. It is better to use a two-electrode system. Products at the counter electrode are possible sources of contaminants through redox cycling.
\nThe Ag-AgCl electrode is most frequently used as a reference electrode in aqueous solution because of the stable voltage at interfaces of Ag-AgCl and AgCl-KCl through fast charge-transfer steps, regardless of the magnitude of current density. The “fast step” means the absence of delay of the reaction or being in a quasi-equilibrium. The stability without delay is supported with high concentration of KCl.
\nWhen an Ag-AgCl electrode is inserted to a voltammetric solution, KCl necessarily diffuses into the solution, associated with oxygen from the reference electrode. Thus, the reference electrode is a source of contamination by salt, dichlorosilver and oxygen. It is interesting to examine how much amount a solution is contaminated by a reference electrode [9]. Time variation of ionic conductivity in the pure water was monitored immediately after a commercially available Ag-AgCl electrode was inserted into the solution. Figure 6 shows rapid increase in the conductivity as if a solid of KCl was added to the solution. Oxygen included in the concentrated KCl may contaminate a test solution. Even the Ag-AgxO electrode, which was formed by oxidizing silver wire, increased also the conductivity, probably because the surface is in the form of silver hydroxide. As a result, no reference electrode can be used for studying salt-free electrode reactions. If neutral redox species such as ferrocene is included in a solution, the potential reference can be taken from redox potential of ferrocene.
\nTime-variation of conductivity of water into which (circles) Ag|AgCl, (triangles) Ag|AgxO, and (squares) AgCl-coated Ag wire were inserted. Conductivity measurement was under N2 environment.
When a constant voltage is applied to the ideal capacitance C, the responding current decays in the form of exp(−t/RC), where R is a resistance in series connected with C. It has been believed that a double-layer capacitance in electrochemical system behaves as an ideal capacitor, where R is regarded as solution resistance. However, any exponential variation cannot reproduce transient currents obtained at the platinum wire electrode in KCl aqueous solution, as shown in Figure 7. The current decays more slowly than by exp(−t/RC), because it is approximately proportional to 1/t. The property of non-ideal capacitance is the result of the constant phase element of the DL capacitance, as described in Section 2.3. The dependence of 1/t can be obtained approximately by the time derivative of q = V0C0t−λ for the voltage step V0.
\nChronoamperometric curves when 0.2 V vs. Ag|AgCl was applied to a Pt wire in 0.5 M KCl aqueous solution. Solid curves are fitted ones by exp(-t/RC) for three values of RC.
The slow decay is related with a loss of the performance of pulse voltammetry, in which diffusion-controlled currents can readily be excluded from capacitive currents. The advantage of pulse voltammetry is based on the assumption of the exponential decay of the capacitive current. Since the diffusion current with 1/t1/2 dependence is close to the 1/t dependence, it cannot readily be separated from the capacitive current in reality. A key of using pulse voltammetry is to take a pulse time to be so long as a textbook recommends.
\nHigh-performance potentiostats are equipped with a circuit for compensation of resistance by a positive feedback. Unfortunately, the circuit is merely useful because voltammograms depend on intensity of compensation resistances of the DL capacitance. It should work well if the DL capacitance is ideal.
\nAC techniques have an advantage of examining time dependence at a given potential, whereas CV has a feature of finding current-voltage curves at a given time. The former shows the dynamic range from 1 Hz to 10 kHz, while the latter does conventionally from 0.01 to 1 Hz. This wide dynamic range of the AC technique is powerful for examining dynamics of electrode reactions. Analytical results by the former are often inconsistent with those by the latter, because of the difference in the time domain. The other scientific advantage of the AC technique is to get two types of independent data set, frequency variations of real components and imaginary ones by the use of a lock-in amplification. The independence allows us to operate mathematically the two data, leading to the data analysis at a level one step higher than CV. An industrial advantage is the rapid measurement, which can be applied to quality control for a number of samples. The analysis of AC impedance necessarily needs equivalent circuits of which components do not have any direction relation with electrochemical variables.
\nData of the electrochemical AC impedance are represented by Nyquist (Cole-Cole) plots, that is, plots of the imaginary component (Z2) of the impedance against the real one (Z1), as shown in Figure 8. The simplest equivalent circuit for electrochemical systems is the DL capacitance Cd in series with the solution resistance RS. The Nyquist plot for this series circuit is theoretically parallel to the vertical axis (Figure 8A-a), but experiments show a slope of 5 or more (Figure 8A-b). This behavior, called constant phase element (CPE) and the power law, has been verified for combinations of various materials and solvents [6, 7, 11, 12]. The equivalent circuit for Eq. (12) is a parallel combination of capacitance and resistance (Figure 8B). Even without an electrode reaction, current always includes a real component.
\n(A) Nyquist plots for a RC-series circuit with ideal capacitor (a) and DL capacitor (b). (B) Equivalent circuit with the power-law of Cd. (C) Randles circuit.
The equivalent circuit with the Randles type is a parallel combination of the ideal DL capacitor Cd with the ideal resistance Rct representing the Butler-Volmer-type charge-transfer resistance. Practically, the Warburg impedance (the inverse of Eq. (8)) due to diffusion of redox species is incorporated in a series into Rct (Figure 8C). Rct cannot be separated from the DL resistance because of the frequency dispersion. Since even the existence of Rct is in question (Section 3.12), it is difficult to determine and interpret Rct. The usage of a software that can analyze any Nyquist plots will provide values of R and C. Even if analyzed values are in high accuracy, researches should give them electrochemical significance.
\nResidual current varies with treatments of electrodes such as polishing of electrode surfaces and voltage applications to an extremely high domain. It can often be suppressed to yield reproducible data when the electrode is replaced by simple platinum wire or carbon rod having the same geometric area. Simple wire electrodes are quite useful especially for measurements of DL capacitance and adsorption. One of the reasons for setting off large residual current is that the insulator of confining the active area is not in close contact with the electrode, so that the solution penetrated into the gap will give rise to capacitive current and floating electrode reactions. Since the coefficient of thermal expansion of the electrode is different from that of the insulator, the residual current tends to get large with the elapse from the fabrication of the electrode. This prediction is based on experience, and there are few quantitative studies on residual currents.
\nUnexpected gap has been a technical problem at dropping mercury electrodes. If solution penetrates the inner wall of the glass capillary containing mercury, observed currents become irreproducible. Water repellency of the capillary tip has been known to improve the irreproducibility in order to reduce the penetration. A similar technique has been used for voltammetry at oil-water interfaces and ionic liquid-water interfaces at present.
\nVoltammograms are said to vary with electrode reaction rates, and the rate constants have been determined from time dependence of voltammograms. The fast reaction of which rate is not rate determining has historically been called “reversible.” In contrast, such a slow reaction that a peak potential varies linearly with log v is called “irreversible.” A reaction between them is called “quasi-reversible.” The distinction among the three has been well known since the theoretical report on the quasi-reversible reaction by Matsuda [1]. This theory is devoted to solving the diffusion equations with boundary conditions of the Butler-Volmer (BV) equation under the potential sweep. As the standard rate constant ks in the BV equation becomes small, the peak shifts in the direction of the potential sweep from the diffusion-controlled peak. Steady-state current-potential curves in a microelectrode [13] and a rotating disk electrode also shift the potential in a similar way. According to the calculated CV voltammograms in Figure 9, we can present some characteristics: (i) if the oxidation wave shifts to the positive potential, the negative potential shift should also be found in the reduction wave. (ii) Both the amounts of the shift should have a linear relationship to log v. (iii) The shift should be found in iterative measurements. (iv) The peak current should be proportional to v1/2.
\nCV voltammograms (solid curves) at a normally sized electrode and steady-state voltammograms (dashed curves) at a microelectrodes in 12 μm in diameter, calculated theoretically for v = 0.5 V s−1, D = 0.73 × 10−5 cm2 s−1, ks = (a) 0.1, (b) 0.01, (c) 0.001, (d) 0.0001 cm s−1. The potential shift of CV is equivalent to the wave-shift at a microelectrode through the relation, v = 0.4RTD/αFa2 (a: radius).
The authors attempted to find a redox species with the above four behaviors. Some redox species can satisfy one of the four requirements, but do not meet the others. Most reaction rate constants have been determined from the potential shift in a narrow time domain. They are probably caused by follow-up chemical reactions, adsorption, or DL capacitance. For example, CV peak potentials of TCNQ and benzoquinone were shifted at high scan rates, whereas their steady-state voltammograms were independent of diameters of microdisk electrodes even on the nanometer scale [14]. The shift at high scan rates should be due to the frequency dispersion of the DL capacitance, especially the parallel resistance in the DL (Figure 8B). Values of the heterogeneous rate constants and transfer coefficients reported so far have depended not only on the electrochemical techniques but also research groups. Furthermore, they have not been applied or extended to next developing work. These facts inspire us to examine the assumptions and validity of the BV formula.
\nLet us revisit the assumptions of the BV equation when an overvoltage, i.e., the difference of the applied potential from the standard electrode potential, causes the electrode reaction. The rate of the oxidation in the BV equation is assumed to have the activation energy of α times the overvoltage, while that of the reduction does that of (1 − α) times. This assumption seems reasonable for the balance of both the oxidation and the reduction. However, the following two points should be considered. (i) Once a charge or an electron is transferred within the redox species, the molecular structure changes more slowly than the charge transfer itself occurs. The structure change causes solvation as well as motion of external ions to keep electric neutrality. These processes should be slower than the structure change. If the overvoltage can control the reaction rate, it should act on to the slowest step, which is not the genuine charge-transfer process. (ii) Since a reaction rate belongs to the probability theory, the reaction rate (dc/dt) at t is determined with the state at t rather than a state in the future. In other words, the rate of the reduction should have no relation with the oxidation state which belongs to the future state. The BV theory assumes that the α times activation energy for the oxidation is related closely with 1-α times one for the reduction. This assumption is equivalent to predicting a state at t + Δt from state at t + 2Δt, like riding on a time machine. This question should be solved from a viewpoint of statistical physics.
\nDevelopment of scanning microscopes such as STM and AFM has allowed us to obtain the molecularly and atomically regulated surface images, which have been used for interpreting electrochemical data. Then the electrochemical data are expected to be discussed on a molecular scale. However, there is an essential problem of applying photographs of regularly arranged atoms on an electrode to electrochemical data, because the former and the latter include, respectively, microscopically local information and macroscopically averaged one. A STM image showing molecular patterns is information of only a part of electrode, at next parts of which no atomic images are often observed but noisy images are found. Electrochemical data should be composed of information both at a part of the electrode showing the molecular patters and at other parts showing noisy, vague images. Noisy photographs are always discarded for interpreting electrochemical data although the surfaces with noisy images also contribute electrochemical data.
\nAn ideal experiment would be made by taking STM images over all the electrodes that provide electrochemical data and by obtaining an averaged image. However, it is not only impossible to take huge amounts of images, but the averaged image might be also noisy. It may be helpful to describe only a possibility of reflecting the STM-imaged atomic structure on the electrochemical data.
\nVoltammograms by adsorbed redox species, called surface waves, are frequently different from a bell shape (Figure 2). Really observed features are the following: (i) the voltammogram does not suddenly decay after the peak, exhibiting a tail-like diffusional wave; (ii) the peak current and the amount of the electricity are proportional to the power less than the unity of v; (iii) the oxidation peak potential is different from the reduction one; (iv) the background current cannot be determined unequivocally; and (v) voltammograms depend on the starting potential. Why are experimental surface waves different from a symmetric, bell shape in Figure 2?
\nA loss of the symmetry with respect to the vertical line passing through a peak can be ascribed to the difference in interactions at the oxidized potential domain and at the reduced one. Since redox species takes extremely high concentration in the adsorbed layer, interaction is highly influenced on voltammetric form. When the left-right asymmetry is ascribed to thermodynamic interaction, it has been interpreted not only with Frumkin’s interaction [15] but also Bragg-Williams-like model for the nearest neighboring interactive redox species [16]. On the other hand, most surface waves are asymmetric with respect to the voltage axis even at extremely slow scan rates. This asymmetry cannot be explained in terms of thermodynamics of intermolecular interaction, but should resort to kinetics or a delay of electrode reactions. There seems to be no delay in the electrode reaction of the monomolecular adsorption layer, different from diffusion species. The delay resembles the phenomenon of constant phase element (CPE) or frequency power law of DL capacitance, in that the redox interaction may occur two-dimensionally so that the most stable state can be attained. This behavior belongs to a cooperative phenomenon [17]. A technique of overcoming these complications is to discuss the amount of charge by evaluating the area of the voltammogram. It also includes ambiguity of eliminating background current and assuming the independence of the redox charge from the DL charge.
\nThe simplest theories for voltammetry are limited to the rate-determining steps of diffusion of redox species and reactions of adsorbed species without interaction. Variation of scan rates as well as a reverse potential is helpful for predicting redox species and reaction mechanisms. Furthermore, the following viewpoints are useful for interpreting mechanisms:
comparison of values of experimental peak currents with theoretical ones, instead of discussing ΔEp and E1/2;
examining the proportionality of Ip vs. v or vs. v1/2, i.e., zero or non-zero values of the intercept of the linearity;
a reference electrode and a counter electrode being a source of contamination in solution;
attention to very slow relaxation of DL capacitive currents;
inclusion of ambiguity in the equivalent circuit with the Randles type.
IntechOpen publishes different types of publications
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\n\nRESEARCH CHAPTER – A research chapter reports the results of original research thus contributing to the body of knowledge in a particular area of study.
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