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Background Recently, transition‑metal oxides have represented an exciting research topic, especially their funda‑ mental and technological aspects. Here, vanadium pentoxide nanoparticles ( V O ‑NPs) were synthesized through the 2 5 thermal decomposition of ammonium meta‑ vanadate. In the current study, we investigated the photocatalytic activ‑ ity of V O ‑NPs to develop and regulate the V O structure for adsorption applications. 2 5 2 5 Results The obtained nanoparticles were inspected by X‑ray diffraction, scanning electron microscope, transmission electron microscope, and differential thermogravimetric analysis, which proved the formation of the nanorod struc‑ ture. The ultraviolet–visible absorption spectra revealed a 2.26 eV band gap for V O ‑NPs that correlates with indirect 2 5 optical transitions. The photocatalytic activity of the V O ‑NPs was investigated by methylene blue (MB) degradation 2 5 in aqueous solutions. An initial concentration of 25 ppm, a temperature of 40 °C, 40 mg of adsorbent mass, and 1 h of contact time were the optimal conditions for the efficient removal of MB that could reach up to 92.4%. The mecha‑ nism of MB photocatalytic degradation by V O ‑NPs is explained. 2 5 Conclusions The photodegradation data better fit with the Langmuir isotherm model. The thermodynamic param‑ eters indicated that the adsorption was spontaneous and endothermic. The reaction kinetics followed the pseudo‑ second‑ order model. Thermally prepared V O ‑NPs offer a simple and efficient approach for selective MB removal 2 5 from an aqueous medium. Keywords V O nanorods, Thermal decomposition, Photocatalytic degradation, Methylene blue, Dye degradation 2 5 *Correspondence: E. M. Elsehly elsahli@sci.dmu.edu.eg Full list of author information is available at the end of the article © The Author(s) 2023. Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http:// creat iveco mmons. org/ licen ses/ by/4. 0/. Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 2 of 15 Graphical abstract result of this decomposition secondary products are also 1 Background produced [4]. Recently, transition metal oxides have rep- Owing to their physiochemical features, compared resented an exciting research topic, especially their fun- to bulk materials, photocatalysis nanomaterials have damental and technological aspects. It contains atoms attracted significant attention in applied environmental with unfilled d-shells, which have numerous oxidation science [1]. Moreover, the term "photocatalysis nano- states and exhibit mixed-valence phenomena [5]. One of materials" dates back nearly 100 years ago and could these transition metals is vanadium, which generally sub- be simply defined as the change in the rate of a chemi - sists in several oxidation states such as (1) V O (e.g. cal transformation under the action of light in the pres- n 2n+1 V O ), (2) V O (e.g. V O ), and (3) V O (e.g. V O ) ence of a catalyst that absorbs light and is involved in the 2 5 n 2n−1 2 3 n 2n 2 4 [6]. Owing to its saturated oxidation state ( V ), Vana- chemical reaction. It has been widely used to mineral- dium pentoxide (V O ) is the main stable compound in ize organic compounds as environmental pollutants [2]. 2 5 these oxidation groups [7]. Owing to its structure, V O Photocatalysis appear to be promising technology with 2 5 has been incorporated into many applications, including various applications in environmental systems such as solar cells, optical, and electrical devices [8, 9]. α-V O air and water purification. The catalyst is activated by 2 5 (Orthorhombic), β-V O (tetragonal or monoclinic), and interacting with light energy larger than or in the range 2 5 γ-V O (Orthorhombic) are some of the polymorphs of of the photocatalyst’s band gap (hv ≥ E ). The band gap or g 2 5 V O [10]. Orthorhombic α-V O is the most stable phase energy gap is an energy range in a solid where no elec- 2 5 2 5 at ambient conditions [11], whereas the β and γ phases tron states can exist. This is equivalent to the energy are metastable [7]. V O has recently gained significant required to liberate an outer shell electron from its orbit 2 5 attention due to its unique features, such as catalytic to move freely within the solid material [3]. These photo- activity, outstanding semiconducting, and electrochemi- generated electron–hole particles migrate to the semi- cal qualities. Based on the oxidation states variety and conductor surface and act to accelerate the reduction and the heterogeneity of oxygen coordination geometries, oxidation of adsorbed particles individually [1]. Thermal V O is an excellent catalyst candidate. However, V O decomposition (thermolysis) is an important rapid syn- 2 5 2 5 has been the focus of numerous studies because of its thetic process to prepare nanomaterials with exceptional scientific curiosity and commercial importance. Among properties. Thermal decomposition is an endothermic its attractive applications, the photocatalytic activity of chemical disintegration that is induced by heat. As a A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 3 of 15 V O nanoparticles motivates the degradation of hydro- obtained from the thermal decomposition of ammonium 2 5 carbons and methylene blue in aqueous solutions [1]. meta-vanadate. DTA-TGA data were collected by the Industrial wastewater effluents, such as paints, leather Thermo analyzer (TGA-50 and DTA-50) in the air with tanning, and printing, contain a wide range of chemicals a 10 K/min heating rate. The initial mass of the sample that cause pollution to the environment [12–15]. One was 19.1 mg, and the annealing procedure for NH VO 4 3 of the most toxic pollutants is dyes discharged into the was conducted at 170 °C, 270 °C, and 450 °C for 1 h. environment by the textile and painting industries [16, X-ray diffraction (XRD) with monochromatic Cu Ka 17]. Once those dyes metabolize and interact with other (λ = 1.5406 Å) was conducted to investigate the crystal- contaminants in wastewater, hazardous by-products are linity. The synthesized nanoparticles morphology was produced and affect the aquatic environment and human characterized by scanning electron microscopy (SEM, health [16]. Methylene blue (MB) is commonly used to JMS-6010LV) and transmission electron microscopy dye wool and silk, as well as for medicinal purposes to (TEM, JMS -2100F). Fourier transform infrared spectros- investigate certain illnesses. However, MB-contaminated copy (FTIR; Bruker Tensor 37, FTIR spectrophotometer) water is discharged into water resources without treat- was used to detect the functional groups. Optical proper- ment. It causes serious ramifications such as vomiting, ties and the absorption spectrum were measured by the eye burns, and diarrhea [18]. As a result, developing an UV–vis spectrometer (Thermo Scientific Evolution 300) effective dye-based treatment approach has become a with wavelengths 190–1100 nm. The band gap of each major research aim [19]. sample was calculated by the following equation [27]: The photocatalytic process is described as the rate (αhv) = A hv − Eg (1) change of chemical processes in the presence of a pho- tocatalyst when exposed to light. When a photocatalyst where A is a constant where α is the absorbance, E is the absorbs light quanta, electron–hole pairs are formed, band gap energy, (hν) is the photon energy (h represents causing chemical modification in reacting materials that the Planck’s constant), A is a constant (varies from transi- make contact with them [20]. The process depends on tion to transition), and n is an index. n takes the values electron–hole recombination. The hole is large enough 1/2, 3/2, 2 and 3. The value of n depends on the nature of to oxidize a wide range of organic pollutants in the water the electronic transition causing reflection. The Tauc plot system while also creating the hydroxyl radical OH [21, 1∕2 is constructed with hν on x axis and (hνα) on y-axis. An 22]. The superoxide radical is formed when electrons in extrapolation of this linear region to (hνα) = 0 gives the the conduction band interact with oxygen in H O, which band gap energy of the studied material [3]. − • then reacts with the OH ion to form OH radical [23, 24]. Because OH is a strong oxidizer, it destroys contam- inants by oxidizing organic molecules [25, 26]. 2.2 Photocatalytic degradation experiments Herein, the photocatalyst V O -NPs were prepared, 2 5 The photocatalytic degradation of MB by the V O NPs 2 5 and the structure was controlled via the thermal decom- was used to obtain equilibrium data. The initial dye con - position technique. The obtained nanoparticles were centration, contact time, photocatalyst loading, and solu- applied as prospective catalyst for Methylene blue degra- tion temperature were examined as influences on the dation. Meanwhile, the thermodynamic studies and pho- photodegradation process. Afterward, 2 ml of degraded tocatalytic mechanism were investigated in detail. MB was collected and analyzed using the spectropho- tometer of UV–visible range at 655 nm wavelength. 2 Materials and methods The dye removal, R%, was estimated using the follow - 2.1 Methods ing equation [28]: Ammonium metavanadate (NH VO , 99%) was pur- 4 3 C − C o e chased from Sigma Aldrich (Saint Louis, MO, USA), R% = ∗ 100 (2) Methylene blue (MB, with the molecular formula C C H N SC H O; λ of 655 nm) was purchased from 18 18 3 l3 2 max C and C are the initial and equilibrium liquid phase o e Chemjet (India) and utilized to prepare the aqueous −1 concentrations, respectively, (mg l ). solution. stock solutions of MB, (50 mg/250 ml), were The following equation was used to evaluate the quan - prepared using distilled water. Double distilled water tity of the adsorbed MB, q (mg/g) [28]. was employed for the necessary dilutions to create suit- able concentrations from the stock solution. The MB (C − C )V o e q = (3) concentration before and after each experiment was determined using a UV–Visible spectrophotometer set at 655 nm. The synthesizing of V O nanoparticles was 2 5 Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 4 of 15 where C and C are the initial and equilibrium concen- dq 0 e = K (q − q ) (5) 2 e t trations of MB, respectively (mg/L), m is the weight of dt adsorbent in (g) and the solution volume is V (l). where K (g/mg.min) represents the second-order kinetic constant. 2.3 B atch study of photodegradation process Contact time is one of the most significant factors in the photodegradation process. To investigate the influ - 2.4.2 A dsorption isotherm models and thermodynamic ence of the contact time, 50 mg of the prepared photo- studies catalyst was suspended into a 50 ml aqueous solution of When the adsorption process achieves equilibrium, an MB (50 ppm, pH = 7) by magnetically stirring at 200 rpm isotherm model explains the mechanism of the adsorp- for a period ranging from 15 to 120 min with other con- tion molecules across the solid and liquid phases. The stant parameters at room temperature. The effect of con - most important isotherm models are Freundlich and centration on the MB decolorization was investigated Langmuir [23]. Adsorptions occur at predetermined at four dye concentrations (100, 50, 25, and 10 ppm) in homogeneous regions on the adsorbent, according to the presence of 50 mg of the photocatalyst. The removal the Langmuir model, which is extensively used for mon- percentage was controlled by varying adsorbent doses. olayer adsorption systems. The Freundlich model sup - The main precursor V O , varying as 10, 25, 40, 50, and 2 5 ports surface heterogeneity for different energy stages of −1 100 mg with 50 ml aqueous solution of MB dye 25 mg l adsorption sites [28]. The Langmuir isotherm equation is concentration with other constant parameters. To elu- given by [32]: cidate the temperature effect on MB dye removal, three C 1 C e e different temperatures, 25, 40, and 60°c, were examined = + (6) Q Q K Q with other previously selected parameters. All the experi- e max l max ments were carried out in triplicate and the results were −1 where C is the equilibrium concentration (mgL ), Q e e presented as mean ± SD. −1 is the amount of adsorbed dye at equilibrium (mg.g ), −1 Q (mg.g ) is the Langmuir constants that are related max 2.4 Mathematical modeling −1 to the adsorption capacity, and K (L mg ) is the adsorp- 2.4.1 The kinetic models tion rate. The first and second-order pseudo-kinetic models were The correlation coefficient, R , controls the applica- used to assess whether the reaction process is chemical bility of the isotherm [32]. R , a dimensionless constant or physical [29]. These popular models make the adsorp - named the separation factor and represented the essen- tion kinetics and the interaction between adsorbent tial property of the Langmuir isotherm. The viability and and adsorbate easier to understand [30]. These kinetic nature of adsorption were evaluated by R [33], which experiments reveal a link between the amount of adsorb- can be defined by: ate removed and the time required to remove it from an aqueous solution [31]. The pseudo-first-order model R = l (7) was proposed based on the hypothesis that the adsorp- 1 + K c l o tion rate is proportional to the number of unoccupied The R value specifies the isotherm type: favorable adsorption sites. In this model, the adsorption rate was (0 < R < 1), linear (R = 1), irreversible (R = 0), or unfa- estimated as: L L L vorable (R > 1) [32, 33]. The quantity of the metal adsorp - dq tion on a given mass of the adsorbent is described by the = K (q − q ) (4) 1 e t dt Freundlich isotherm model. This approach could apply to multi-layer sorption with quasi-adsorption energy where the equilibrium adsorption capacities at a given −1 and affinity distributions over a wide range of substrates, time are q (mg/g) and q (mg/g), respectively. K (min ) e t 1 which takes the form: is the first-order kinetic constant. The second-order pseudo-kinetic model was proposed ln q = ln K + ln C (8) e F e based on the hypothesis that the adsorption rate is pro- portional to the square of the number of unoccupied −1 where k (l. mg ) and 1/n are the Freundlich constants. adsorption sites. This model claims that the interactions The slope 1/n, which ranges from 0 to 1, is an indica - between the adsorbate and adsorbent are generated by tor of adsorption ability or surface homogeneity, and it the adsorbate’s strong binding to the adsorbent’s surface, becomes more heterogeneous as it approaches zero [28]. which can be expressed as [30]: A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 5 of 15 The thermodynamic factors can assess the probability ammonium hexavanadate (AHV) [39]. When the tem- and mechanism of adsorption [34]. The Gibbs free energy perature was increased to 450 °C, the sample did not (ΔG°), enthalpy (∆H°), and entropy (ΔS°) are utilized reveal any change in the weight, indicating that the V O 2 5 to determine the nature of the adsorption mechanism product was stable. Between 400 and 500 °C, the sample and the adsorbent suitability [35]. The energy of activa - exhibits a slight increase in weight. This weight increase +4 +5 tion (E ) is critical in establishing whether adsorption is could be attributed to the V oxidation to V , which mostly physical or chemical [36]. The thermodynamic resulted in the creation of yellow crystalline V O . 2 5 parameters were calculated using the given-below equa- Figure 2 demonstrates the XRD pattern of V O pre- 2 5 tions [37]. pared at 170 °C, 270 °C, and 450 °C for 1 h. According to the diffraction patterns, the sample at 450°c has sharp G =−RT ln K (9) peaks at the 2θ° values 15.087°, 19.944°, 20.618°, 25.317°, 30.508°, 31.023°, 33.143°, 47.01, and 50.848° that can be ◦ ◦ S H indexed with the planes (200), (001), (101), (201), (400), LnK = − (10) R Rt (301), (111), (600), and (020). These planes were char - acterized by V O orthorhombic structure (JCPDS 2 5 Card No PDF 89–2482), with a = 11.544 A°, b = 3.571 K = (11) C A°, and c = 4.383 A° cell parameters, and unit cell vol- ume = 180.7 A°. The XRD data was refined, along with at −1 −1 R is the gas constant (J mol K ), ΔG° is the free energy, reliability factors R = 10.32, R = 7.68, and χ (= 1.60). wp exp K is the distribution constant, T is the absolute tem- This shows that the observed diffraction peaks properly perature (K), q is the quantity of dye adsorbed by the matched. adsorbent at equilibrium (mol/L), C is the equilibrium To further investigate the functional groups of the syn- concentration. The E defined as the following equation thesized V O nanoparticles, FTIR spectroscopy in the 2 5 [38]: −1 range of 400–4000 cm was employed. The FTIR spectra of three investigated materials at different temperatures E = H + RT (12) are shown in Fig. 3. As we can see from Fig. 3c, V O -NPs 2 5 at 450 °C infrared spectrum has multiple bands. Three 3 Results distinct vibration modes were observed in the FTIR spec- 3.1 Characterization of V O nanoparticles 2 5 tra of V O nanoparticles. The triply coordinated oxygen 2 5 The pure NH VO (TGA–DTA) curves are shown in 4 3 atom between three vanadium atoms induces a stretch- −1 Fig. 1. The TGA-curve of this sample, as shown in the fig - ing absorption peak of around 475 cm [40]. The bond −1 ure, reveals weight loss processes in the ranges of tem- V–O–V symmetrically stretched around 590 cm [41]. peratures 170–230 °C, and 290–500 °C. The initial stage, The stretching vibration of the unshared V=O bonds was with 14.82% weight loss, was the thermal disintegration of ammonium meta-vanadate (AMV) into vanadyl chem- ical species (NH4) V O . Before the V O synthesis at 2 6 16 2 5 450 °C, the solid product bears the empirical formula of 105 4 -2 -4 -6 -8 -10 -12 TG% DTA -14 -16 80 -18 0100 200300 400500 600 T C Fig. 2 The X‑ray diffraction of V O prepared at 170 °C, 270 °C, and Fig. 1 Thermogravimetric analysis–differential thermal analysis 2 5 450 °C ( TGA–DTA) of pure ammonium vanadate TG% DTA(uv) Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 6 of 15 Fig. 3 FTIR spectra of synthesized V O at different temperatures 170 °C (a), 270 °C (b) and 450 °C (c) 2 5 Annealing at 170°c Annealing at 170°c Annealing at 270°c Annealing at 270°c Annealing at 450°c Annealing at 450°c 196296 396496 596 0500 1000 1500 Wave length (nm) wave length (nm) Fig. 4 Absorption spectra of the sample at different wavelengths on the left side. Ultraviolet–visible (UV–VIS) transmission spectra for samples with different wavelengths on the right side −1 with the sample caused absorption in the near UV area. attributed to the absorption bands at 1020 and 822 cm , A significant absorption band at 550 nm corresponded according to previous study [42]. to 2.26 eV in the UV–VIS absorption spectra. The peak Understanding the electrical nature of the optical within the range of 400–700 nm was displaced to the band gap of the material may be facilitated by a UV–VIS low-wavelength region, demonstrating a blue shift. absorption spectrum spectroscopy [43]. Figure 4 shows a Figure 5 shows the V O band gaps for the indirectly reduction in absorption with increase in the wavelength. 2 5 allowed transitions at 170, 270, and 450 °C which equaled The "band gap" refers to a dramatic drop in absorption at 3.94, 3.16, and 2.26 eV, respectively. The disturbance of low wavelengths [44]. Electronic transitions associated Absorbance T% A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 7 of 15 Fig. 5 Energy gaps for V O at temperature values of 170 °C (a), 270 °C (b), and 450 °C (c) 2 5 2 Pure MB 50 ppm 3.2.2 Influenc e of the initial dye concentration on the MB dye 1.8 10 min removal 1.6 15 min Figure 7b depicts the effect of dye concentration on the 1.4 30 min Photodegradation efficiency of MB. The effective removal 1.2 45 min of the MB dye increased with an increase in dye con- 60 min 0.8 centration during photodegradtion by the V O -NPs. 2 5 120 min 0.6 The highest removal percentage was recorded at the ini - 150 min 0.4 tial concentration of 25 ppm to reach 92.4%. Then the 0.2 removal percentage decreased at the concentrations of 50 and 100 ppm to 77.8% and 45.6%, respectively. 400 500 600 700800 Wave length(nm) 3.2.3 P hotoadsorbent dosage and removal efficiency Fig. 6 Variation in the absorption spectra of MB on V O at various 2 5 times Figure 7c shows the adsorbent mass impact on the MB removal from an aqueous solution by photocatalytic degradation. As shown in Fig. 7c, the MB removal effi - ciency increased from 48.5 to 92.4% with the addition of electrons caused by incoming light and the transition V O -NPS when the photodsorbent dose was increased 2 5 between electronic states are the sources of the optical from 10 to 100 mg, indicating that additional adsorption property of a material [45]. In V O , 3d bands of vana- 2 5 sites were accessible. For future investigations, a 40 mg dium constitute the conduction band, while 2p bands of adsorbent dosage was adopted. The transfer of dye ions oxygen form the valence band. to active adsorption sites was be constrained at large adsorbent doses, thereby lowering the removal efficiency 3.2 P hotodegradation of methylene blue [46]. 3.2.1 Effect of contact time Over 150-min time intervals; the effect of contact time 3.2.4 T emperature dependence of MB removal on the photodegradation process of MB by the V O -NPs 2 5 The solution temperature considerably impacts the pho - was examined. Figure 6 shows the change in the optical todegradation procedure, where any variation in the tem- absorption of the aqueous MB solution by V O -NPs 2 5 perature might disrupt the equilibrium research [47]. The under a light spectrum. The intensity of the absorption influence of solution temperature on MB Photodegrada - peak at 655 nm gradually decreased with an increase in tion efficiency is illustrated in Fig. 7d. It was revealed that time, indicating that MB had been photodegraded by when the temperature increased, the removal efficiency the V O catalyst. As shown in Fig. 7a, with an increase 2 5 also increased. It can be stated that when dye mobil- in contact time, the quantity of MB adsorbed increased ity increased, the interaction with the active areas on until it reached its maximum value after 45 min. It may the surface of the adsorbent improves [48]. A tempera- take up to 60 min for the dye to be completely absorbed ture of 40 °C was selected for subsequent equilibrium by the prepared material. Therefore, within 45 min, studies because of the efficient removal attained at this the maximal dye elimination by the V O powder was 2 5 temperature. achieved, and the system attained equilibrium. Absorbance (a.u) Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 8 of 15 (b) 100 (a) 0306090120 150180 initial concentration (ppm) contact time(min) 80 (c) (d) 0 70 15 25 35 45 55 65 050100 15 adsorbent doses(mg) Temperature°C Fig. 7 Degradation percentage versus contact time of V O (a). Variation in the initial concentration of methylene blue (MB) during its 2 5 photodegradation by V O (contact time = 60 min, pH = 7, and T = 25 °C ± 2 °C) (b). Influence of the dose on the adsorption of MB (initial 2 5 concentration = 25 ppm, temperature = 25 °C ± 2 °C, shaking speed = 200 rpm, and pH = 7) (c). Temperature effect on the removal at an initial concentration of MB of 25 ppm (contact time = 60 min and pH = 7) (d) Fig. 8 Pseudo‑first ‑ order kinetic reaction (a) Pseudo‑second ‑ order reaction (b) 3.3 K inetic studies of MB degradation The pseudo-second-order reaction is shown in Fig. 8b, To determine the sorption mechanism, various models which reveals a positive relationship between t/q and can demployed [49]. Here, we employed the pseudo- time. Table 1 shows the kinetic constants (q , K , and K ) e 1 2 first- and pseudo-second-order models because they are derived from the slope and intercept of the regression more widely applicable than other adsorption models. equations. Figure 8a shows the pseudo-first-order kinetic response The correlation factor was 0.996 for the pseudo-sec - as a linear relationship between log(q −q ) with time (t). ond-order model, Table 1: it was higher than those of t e Removal (%) Dye Removal % dye removal (%) Removal % A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 9 of 15 Table 1 Pseudo‑first and second‑ order kinetic constants with correlation coefficients Removal process Pseudo-first-order Pseudo-second-order −1 −1 2 −1 −1 −1 2 q , (exp)mg/g K, min q, mg g R K, g mg min q, (mg g ) R e 1 e 2 e Photodegradation 1.44 0.009 0.126 0.956 0.0645 1.663 0.996 Table 2 Isotherm parameters of the Langmuir and Freundlich of MB by V O photocatalytic 2 5 Isotherm model Isotherm parameters R −1 −1 Langmuir Q (mg g ) = 1.267 K (L mg ) = 5.320 R = 0.0019–0.018 0.9988 max l l −1 −1 1/n Freundlich K (mg g)(L mg ) = 1.321 1/n = 0.278 0.8570 the first-order model. The information obtained showed 3.4 Adsorption isotherm that the pseudo-first-order model failed to illustrate the MB adsorption was investigated using V O -photocatalysis 2 5 adsorption capacity, q , where the pseudo-second-order at various initial concentrations. Table 2 shows the param- model could describe MB adsorption upon photoca- eters and the relevant correlation coefficients of the two talysis. In addition, the adsorption capabilities estimated isotherms. The Langmuir model yielded the equilibrium using the pseudo second-order model were similar to adsorption data better than the Freundlich model, based those obtained through experiments. The adsorption on the obtained high correlation coefficients (R ). C /q is e e capabilities derived using the pseudo-first-order model, plotted versus C in Fig. 9a, providing a straight line with otherwise, did not match the experimental results. Con- R = 0.996, suggesting that the Langmuir model suited the sequently, the MB adsorption can be represented as a adsorption data well. The slope of the linear plot yielded pseudo-second-order model, indicating that the MB the value of q of 1.267 mg/g, while the intercept yielded max adsorption can be described as chemical adsorption. the value of K (Table 1). The MB separation factor (R ) L L 1.4 (b) (a) 1.2 2.5 0.8 1.5 0.6 y = -0.6235x + 0.3575 1 y = 0.789x - 0.1483 0.4 R² = 0.8517 R² = 0.9988 0.2 0.5 0 -0.5 -1 -1.5 lnce Ce 3.5 (c) (d) 2.5 y = -1138.4x + 6.761 R² = 0.9793 1.5 0.0029 0.0030.00310.00320.00330.0034 1/T(1/K) Fig. 9 Plots of MB adsorption using the Langmuir isotherm at various starting concentrations (a), the Freundlich isotherm at various beginning concentrations (b), separation factor for MB adsorption (c). lnK versus 1/T obtained for the Photodegradation of Methylene blue by V O (d) 2 5 Ce/qe Ln(Kl) lnqe Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 10 of 15 was calculated using Eq. (6) at various starting metal con- of water and ammonia during the degradation process centrations (Fig. 9c). Table 2 shows that the values of R for that led to the production of AHV. Without detecting any MB adsorption by V O photocatalytic were in the range of weight changes in the TGA-curve, the high and abrupt 2 5 0.0019–0.018. The adsorption of MB onto the V O adsor- exothermic peak, its maxima, positioned at 360 °C, was 2 5 bent was found to be favorable, with an R value ranging observed. Such a peak could be related to V O crystal- L 2 5 from 0 to 1. As shown in this table, the Langmuir isotherm lization [55]. The formations of the intermediates were data reveals the rapid filling of the material’s active sites. atmosphere-dependent stages [56]. The main weight loss The resulting data also illustrated that the chemisorption occurred because of the desertion of NH and H O dur- 3 2 and monolayer adsorption processes of sorbate on the ing the thermal decomposition of NH VO as follows 4 3 adsorbent surface were highlighted using the Langmuir [57]: isotherm. The Freundlich isotherm model has a good cor - 2NH VO → V O + 2NH + H O (13) 4 3 2 5 3 2 relation coefficient, which might imply its adaptability. Sequences of chemical processes are required to pro- duce V O from AMV. The immediate removal of water 2 5 3.5 Thermodynamic studies and ammonia represents the initial step in this process. The slope and intercept of the ln(K ) against 1/T plot, Exothermic and endothermic processes were involved in Fig. 9d, were used to calculate ΔS° and ΔH° values. the second stage of decomposition. The exothermic pro - The negative value obtained for ΔG° indicated that the cess was compatible with the degradation of ammonia on adsorption was spontaneous and favorable. With increase the surface of vanadium pentoxide, and the endothermic in temperature, the negative value of ∆G decreased, indi - reaction might be the release of water [58]. cating that the Photodegradation of Methylene blue on The material’s band gap energy (E ) is one of the essen- V O -NPs was favorable [51]. The obtained ∆G values 2 5 tial distinctive parameters regarding its properties. The were lower than 20 kJ/mol, suggesting that the adsorp- E of semiconductors or insulators reveals a marked tion rate follows a physical adsorption mechanism. The decrease with the temperature rising. The fluctuation enthalpy (∆H°) indicated whether the process is exother - in the E value is critical for basic research and practi- mic or endothermic, and distinguishes between chemi- cal applications [59, 60]. The fundamental absorption in cal and physical adsorption systems [30]. As a result, the crystalline V O is mostly due to the change from oxygen 2 5 positive value of ∆H° (9.465 kJ/mol), Table 3, indicated p-type to a vanadium 3d-type wave-function [61]. The that the removal of MB was an endothermic process, current study confirms that the band gap value of V O 2 5 whereas the low value of this energy (< 40 kJ/mole) indi- is 2.26 eV due to indirect optical transitions, as previously cates that it was physisorption [52]. The increased diffu - reported which recorded the band gap of V O in the 2 5 sion rate of adsorbate across the exterior boundary and range of 2.15–2.65 eV [62]. the interior pores of adsorbents might explain this phe- SEM images were taken at different temperatures (170, nomenon [53]. During the adsorption phase, the value 270, and 450 °C) to investigate the surface and the mor- of ∆S was positive, suggesting randomness existed in phology of thermally treated AMV (Fig. 10). It is revealed the system solid/solution interface [54]. The resulting E that ammonium Meta vanadate heated at 170 °C attained value is less than 40 kJ/mol, which confirms the inferred an average particle size of 2.06 µm (Fig. 10a). In addition, physisorption process [52]. when the temperature reaches 270 °C, the shape of the particles change from the rectangular plate with sharp 4 Discussion edge (Fig. 10a) [63]. It is assumed that the agglomerated According to the DTA curve of AMV, (Fig. 1), the sam- shape and rectangular plate may be attributed to the ple heated in air exhibited two endothermic peaks. The formation of ammonium Hexa vanadate with an aver- endothermic peak at 130 °C, could specify the loss of age particle size of 1.462 µm. The surface morphologies water. At 218 °C, a second peak corresponded to the loss of the products and structural information at different Table 3 The thermodynamic parameters for the MB removal −1 −1 −1 −1 Adsorbent Adsorbate Temp(K) Kd ∆G° (kJ mol ) E (KJmol ) ∆S° (kJ mol K) ∆H° (kJ mol ) V O MB 298 19.103 − 7.309 11.924 56.211 9.465 2 5 313 22.739 − 8.129 12.067 323 24.594 − 8.600 12.150 333 29.006 − 9.323 12.233 A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 11 of 15 Fig. 10 SEM images of thermally treated AMV at T = 170 °C (a), T = 270 °C (b), and 450 °C (c, d) magnifications are illustrated in Fig. 10c, d. The nano - enhanced with the increased surface area of the adsor- structured V O particles fabricated under thermal bent available for dye ion adsorption. Due to lower active 2 5 decomposition at 450 °C for 1 h, include nanorods of sites on the sorbent surface, only a minor increase in nonuniform V O crystals and rectangular plates. Fur- dye removal was detected after a specific duration [64]. 2 5 thermore, most agglomeration attained an average par- When a dye concentration of 50 ppm was used, the agi- ticle size of 0.153 µm. Vanadium oxide nanoparticles tation time of 60 min appeared to be sufficient to attain appear in the form of a black powder. equilibrium. TEM and HRTEM images show the morphologies of When the dye concentration increased, the photode- thermal decomposition of NH VO at 170 °C, 270 °C, and colorization, i.e., MB dye removal, increased. The gen - 4 3 the prepared V O powders treated at T = 450 °C, respec- eration of hydroxyl radicals (OH ), which might react 2 5 tively (Fig. 11). As can be seen from the figure the lattice with dye molecules, is linked to these findings. As the fringes of V O in the range of d = 0.19 nm. MB concentration increased, the catalyst’s active sites 2 5 Figure 12 shows the FTIR spectra of MB solution prior became coated with dye ions, which causes a decrease in to and after V O decomposition. The MB dye exhibited the removal efficiency. u Th s, the production of hydroxyl 2 5 a distinctive peak associated with the functional groups radicals (OH ) on the surface of catalyst was reduced, and −1 in the MB dye consisting of CH=N at 1615 cm prior the path length of photons entering the dye solution was to degradation (Fig. 12a). The FTIR spectrum exhibited reduced [65]. a new peak after photocatalytic degradation of the MB The performance of synthesized V O is compared with 2 5 dye. The V=O symmetric stretching was responsible other materials for the degradation of MB. Table 4 shows −1 for the bands at 1030 cm , whereas V–O–V stretching a comparison of the photocatalytic performance of some −1 is responsible for the bands at 850 cm , Fig. 12b [63]. photocatalysts for the degradation of Methylene blue. Furthermore, due to the absorption of MB on V O , the Compared with published results, our study offers a simple 2 5 −1 FTIR peak of CH=N changed from 1615 to 1655 cm . and efficient approach to selectively remove MB from an As indicated in Fig. 6, the proportion of MB removed aqueous medium, with a detailed thermodynamic study. raised significantly as contact time increased. The find - Three phases are generally involved in the photocata - ings imply that the initial rate of adsorbate removal lytic process. The dye molecules travel from the aqueous Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 12 of 15 Fig. 11 TEM and HRTEM images of thermally treated ammonium Meta vanadate at T = 170 °C (a), T = 270 °C (b) and at T = 450 °C (c–e) 60 solution to the external surface of the catalyst during the first diffusion layer of the dye. Intraparticle diffusion is (a) the second inner diffusion, in which dye molecules are absorbed from the external layer to inside the catalyst pores. Finally, the dye molecules connect with the active sites of the interior pores of the catalyst during the third (a )Before stage [1]. Figure 13 shows a schematic of the photodegra- (b) (b) After dation phenomena. When a photon with an energy of at least 2.3 eV interacted with the photocatalyst V O -NPs, 2 5 an electron–hole pair is formed. In this situation, elec- 400900 1400 1900 trons (e ) were stimulated from the valence band to the -1 + wave number (Cm ) conduction band whereas holes (h ) are created in the Fig. 12 The FTIR spectra for MB prior to (a) and after degradation (b) valence band [54]: Table 4 comparison of the photocatalytic performances of certain photocatalysts for the degradation of methylene blue (MB) Catalyst Photodegradation Dye initial The catalyst Light source Degradation time Temperature References efficiency (%) concentration dose (mg) (°C) V O ‑NPs 81 10 mg/l 50 Visible light 2 h 25 [47] 2 5 −5 CdS nanorods 92.5 1 × 10 M 100 Visible light 25 min 25 [48] NGP/V O 75 20 mg/l 400 Visible light 120 min 25 [61] 2 5 ZnO‑NPs 96 40 mg/l 200 Visible light 60 min 25 [49] −5 MnTiO /TiO 75 1 × 10 M 50 Sunlight irradiation 240 min 25 [50] 3 2 V O /ZnO 97 500 mg/l 500 Visible light 120 min 25 [51] 2 5 V O ‑nanorods 92.4 25 mg/l 40 Light spectrum 60 min 40 This work 2 5 T% A shery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 13 of 15 Fig. 13 The proposed mechanism involved in the photocatalytic activities of V O ‑NPs 2 5 − + correlated with the solution temperature, initial dye con- V O − NPs + hv → e + h 2 5 (14) CB VB centration, adsorbent dose, and contact duration. Under where hv denotes the energy required to transport an visible light, the V O nano-rods exhibited an efficient 2 5 electron from the VB to the CB. degradation of MB dye within 60 min. The obtained Irradiated electrons might be easily captured by O adsorption data fit the Langmuir isotherm model. The absorbed on the photocatalyst surface, resulting in super- reaction kinetics followed the pseudo-second-order •− − •− •− oxide radicals O , e + O → O . u Th s , O might model. This study offers a simple and effective photocat - 2 CB interact with H O to form the hydroperoxy radical HO alyst approach for the effective removal of various dyes 2 2 and hydroxyl radical (OH ), which are powerful oxidizing from polluted solutions. mediators that can degrade organic molecules. Simul- taneously, surface hydroxyl groups on the photocatalyst Abbreviations surface might trap the photoinduced holes, resulting in XRD X‑ray diffraction hydroxyl radicals OH . Finally, oxidizing the organic mol- SEM Scanning electron microscope TEM Transmission electron microscope ecules will produce carbon dioxide and water. Moreover, DTA Differential thermogravimetric analysis positive hole and electron recombination may occur, FTIR Fourier–transform infrared spectroscopy lowering the photocatalytic activity of the produced MB Methylene blue V O Vanadium pentoxide 2 5 nanocatalyst. αV ‑ O Orthorhombic vanadium pentoxide 2 5 AMV Ammonium metavanadate AHV Ammonium hexavanadate 5 Conclusion NPs Nanoparticles V O nano-rods were successfully synthesized by ther- 2 5 Acknowledgements mal decomposition. The TEM and SEM of V O -NPs 2 5 Thanks to the Faculty of Science, Physics department, Damanhour University, revealed its rod-like shape. V O particles were gen- 2 5 Egypt. erated by decomposition at 450 °C for 1 h had a parti- Author contributions cle size of 0.153 μm and a lattice fringe of d = 0.19 nm. MA, E. Elsehly, EME, and ME contributed to the conception and design of the According to the UV–VIS absorption spectrum, V O 2 5 study. Data collection, analysis, and manuscript preparation were performed had a band gap of 2.26 eV. The Photocatalytic activity by E. Elsehly. E. Elsehly, MA and ME wrote the first draft of the manuscript. EME and E. Elsehly revised the manuscript, participate on the discussion and of the synthesized V O nano-rods was examined by 2 5 analysis of the data. All the authors commented on previous editions of the selectively removing of MB from an aqueous medium manuscript. All authors read and approved the final manuscript. under light spectrum. The quantity of adsorbed MB is Ashery et al. Beni-Suef Univ J Basic Appl Sci (2023) 12:12 Page 14 of 15 Funding 13. Gajbhiye SB (2012) Photocatalytic degradation study of methylene blue This study was funded by the Academy of Scientific Research and Technology solutions and its application to dye industry effluent. Int J Mod Eng Res (ASRT ), Egypt, Grant No. 6735. 2:1204–1208 14. Elsehly EM, Chechenin NG, Makunin AV, Shemukhin AA, Motaweh HA Availability of data and materials (2020) Surface functionalization of multi‑ walled carbon nanotubes by All data and other supplementary materials are already included in the main ozone and the enhancement of their environmental applications. Nano manuscript. Express 1(2):020023. https:// doi. org/ 10. 1088/ 2632‑ 959X/ abaafd 15. Elsehly EM, Chechenin NG, Makunin AV, H.A. (2016) Motaweh, morpho‑ logical and structural modifications of multiwalled carbon nanotubes by Declarations electron beam irradiation. Mater Res Express 3:105013 16. Akpan UG, Hameed BH (2009) Parameters affecting the photocatalytic Ethics approval and consent to participate degradation of dyes using TiO ‑based photocatalysts: a review. J Hazard Not applicable. Mater 170:520–529 17. Houas A, Lachheb H, Ksibi M, Elaloui E, Guillard C, Herrmann J‑M (2001) Consent for publication Photocatalytic degradation pathway of methylene blue in water. Appl Not applicable. Catal B 31:145–157 18. Salehi M, Hashemipour H, Mirzaee M (2012) Experimental study of influ‑ Competing interests encing factors and kinetics in catalytic removal of methylene blue with The authors declare that they have no competing interest in this study. TiO nanopowder. Am J Environ Eng 2:1–7 19. Elsehly EM (2020) Enhanced removal of Ni(II) from aqueous solutions by Author details effective acid functionalization of carbon nanotube based filters. Egypt J Physics Department, Faculty of Science, Damanhour University, Daman‑ Chem 63:3861–3871 hour 22516, Egypt. Nanomaterials and Composites Research Department, 20. Kadhim RF (2017) Photocatalytic removal of methylene blue dye by using Advanced Technology and New Materials Research Institute (ATNMRI), City of ZnS and CdS. Iraqi J Phys (IJP) 15:11–16 for Scientific Research and Technological Applications (SRTA‑ City), New Borg 21. 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Beni-Suef University Journal of Basic and Applied Sciences – Springer Journals
Published: Jan 28, 2023
Keywords: V2O5 nanorods; Thermal decomposition; Photocatalytic degradation; Methylene blue; Dye degradation
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