Glass compositions of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
\r\n\t
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He holds 27 patents and has developed electrical equipment for machine tools, spooling machines, high power ultrasound processes and other, with the homologation of 18 prototypes and 12 zero manufacturing series.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"1063",title:"Prof.",name:"Constantin",middleName:null,surname:"Volosencu",slug:"constantin-volosencu",fullName:"Constantin Volosencu",profilePictureURL:"https://mts.intechopen.com/storage/users/1063/images/system/1063.jpeg",biography:"Constantin Volosencu is a professor at the “Politehnica” University of Timisoara, Department of Automation. He is the author of 10 books and five book chapters, the editor of nine books, the author of over 150 scientific papers published in journals and\nconference proceedings, the author of 27 patents, and a manager of research grants. He is a member of editorial boards of international journals, a former plenary speaker, a member of scientific committees, and chair at international conferences. He research is in the fields of control systems, electrical drives, power ultrasounds, fuzzy logic, neural networks, fault detection and diagnosis, sensor networks, and distributed parameter systems. 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Theophanides",coverURL:"https://cdn.intechopen.com/books/images_new/1591.jpg",editedByType:"Edited by",editors:[{id:"37194",title:"Dr.",name:"Theophanides",surname:"Theophile",slug:"theophanides-theophile",fullName:"Theophanides Theophile"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3092",title:"Anopheles mosquitoes",subtitle:"New insights into malaria vectors",isOpenForSubmission:!1,hash:"c9e622485316d5e296288bf24d2b0d64",slug:"anopheles-mosquitoes-new-insights-into-malaria-vectors",bookSignature:"Sylvie Manguin",coverURL:"https://cdn.intechopen.com/books/images_new/3092.jpg",editedByType:"Edited by",editors:[{id:"50017",title:"Prof.",name:"Sylvie",surname:"Manguin",slug:"sylvie-manguin",fullName:"Sylvie Manguin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"60870",title:"Structure and Physical Properties of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30) Glass System",doi:"10.5772/intechopen.73865",slug:"structure-and-physical-properties-of-59b2o3-10na2o-30-x-cdo-xzno-1cuo-0-x-30-glass-system",body:'\nAlkali borate systems are attractive materials from a fundamental point of view as well as technological point of view [1]. From the literature, it has been observed that certain borate glasses are of greater interest and relevance because of their suitability in the progress of waveguides, electro-optic switches and modulators, magneto-optic materials, and solid-state laser materials [2]. B2O3–ZnO glass has a high transparent window in the region from 370 nm to 2.2 μm, and these glasses are attractive host materials to incorporate rare earth elements for optoelectronics and optical fibers [3, 4]. The properties of B2O3 glass can often be altered by the addition of network modifiers. The most commonly used network modifiers are the alkali (Li2O, Na2O, and K2O) and alkaline earth oxides (MgO, CaO, SrO, and BaO) [5, 6]. When mixed with these glass modifiers, its internal structure is rearranged due to the formation of non-bridging oxygen [7]. In particular, the addition of alkali oxide to pure B2O3 causes a progressive change of the boron atom coordination number (CN), from 3 (BO3) to 4 (BO4), and results in the formation of various borate units (diborate, triborate, tetraborate groups, etc.) [1].
\nFrom the literature, it was found that with the presence of ZnO or CdO in B2O3 glass matrix, UV transmission ability could be enhanced [8]. Therefore the authors have selected Na2O, CdO, and ZnO as network modifiers. The addition of Cd and Zn oxides also results in the large glass formation domain [9]. When zinc oxide is introduced to borate glasses, there are two ways in which zinc ion can get incorporated into the glass. Zinc oxide may act as a network modifier by disrupting the bonds connecting neighboring [BO3] and [BO4] groups. On the other hand, zinc oxide can be incorporated into the glass as [ZnO4] structural units. Besides Cu2+ ions have been chosen in the present study as an EPR probe due to its EPR spectrum being sensitive enough to detect minute changes in the structure of the glasses [10]. Therefore in this article, authors have been presented the structural changes of Cu2+ ions-doped B2O3–Na2O–CdO–ZnO glass induced by addition of ZnO into B2O3 glass matrix at 10 mol% Na2O content. The various literature surveys show no evidences on structural study using FTIR, Raman spectroscopy, EPR, and optical absorption. Therefore the authors have planned to investigate the structural, optical, and physical changes in the Cu2+ ions-doped B2O3–Na2O–CdO–ZnO glass system. The authors have also studied the spin-Hamiltonian parameters and site symmetry around Cu2+ ions in these glasses using EPR and optical absorption studies. The variations in the thermal properties and other physical properties in terms of structural changes of glasses have been discussed [6].
\nGlasses with compositional formula 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (where x = 0, 7.5, 15, 22.5, and 30 mol%) were prepared using melt-quenching technique, and a series of glasses along with their codes are given in Table 1. All the chemicals used were of 99% purity from well-known companies (sd-fine, Merck, and Loba Chemie).
\nSample code | \nComposition (mol%) | \n
---|---|
BNCZ1 | \n59B2O3–10Na2O–30CdO | \n
BNCZ2 | \n59B2O3–10Na2O–22.5CdO–7.5ZnO | \n
BNCZ3 | \n59B2O3–10Na2O–15CdO–15ZnO | \n
BNCZ4 | \n59B2O3–10Na2O–7.5CdO–22.5ZnO | \n
BNCZ5 | \n59B2O3–10Na2O–30ZnO | \n
Glass compositions of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
Appropriate amounts of H3BO3, Na2CO3, ZnO, and CdO were ground with a mortar and pestle and thoroughly mixed. About 1 mol% CuO was added as a spin probe and was melted in a platinum crucible at 1000°C for 30 min in an Autoset electric furnace; a similar technique was employed by Devde et al. [6].
\nDuring the melting the crucible with homogeneous mixture was covered with a lid to avoid the volatility of the powder compounds or contamination from the furnace. Melts were stirred frequently to promote homogeneity, and the liquids were rapidly poured into a mold made with a stainless steel which was maintained at 200°C and pressed with another stainless steel plate maintained at the same temperature. The prepared glass samples were then transferred to another furnace and annealed at 300°C for 6 h to relieve thermal stress and strains of the glass samples. The prepared samples were examined, and it was found that the samples are clear, bubble free, and transparent.
\nArchimedes’ method using xylene as immersion liquid was employed for the measurement of densities of the prepared glasses at room temperature. An average of three samples of each glass code was used. Obtained density values were used to calculate the molar volume using relation Vm = M/ρ, where M and ρ are the average molecular weight and density of the glasses, respectively. Oxygen packing density (OPD) was calculated using the relation OPD = Σxini/Vm, where xi is the molar fraction of an oxide RmOn and ni is the number of oxygen atoms of this oxide [6]. The molar volume of oxygen (Vo) is the volume of glass in which 1 mole of oxygen is contained. These values were calculated using the relation Vo = (Vm)(1/Σxini).
\nVarious spectroscopic techniques were employed for structure investigation of present glass system.
\nX-ray diffraction patterns of the glass samples were recorded from Philips diffractometer (PANalytical X-pert PRO model) with Cu Kα (1.54 Å) source at room temperature.
\nThe infrared transmission spectra of all glasses were recorded at room temperature in the wave number range 400–1800 cm−1 by a Shimadzu FTIR-8001 Fourier-transform computerized infrared spectrometer. The IR transmission measurements were made using the KBr pellet technique.
\nRaman spectra of all prepared glasses were recorded at room temperature in the range 200–1800 cm−1 using a He–Ne excitation source (632.81 nm) coupled with Jobin Yvon Horiba (LABRAM HR-800) micro Raman spectrometer equipped with a 50× objective lens to focus the laser beam. The incident laser power was focused in a diameter of ~1–2 μm, and a notch filter was used to suppress Rayleigh light. Samples used for the measurement were of 1 mm thickness and 1 cm in diameter. Raman shifts are measured with a precision of ~0.3 cm−1, and the spectral resolution is of the order 1 cm−1; a similar characterization was studied by Upender et al. [11].
\nDifferential scanning calorimetry of the prepared glass powders was carried out at temperatures up to 850°C at the rate of 10°C/min using a SETARAM instrument (Model LABSYS EVO DSC; SETARAM Instrumentation, Caluire, France) to determine the thermal properties of the glasses [6].
\nJEOL-JES FE 3X EPR spectrometer was employed for recording EPR spectra of the glass samples in the X-band at room temperature with 100 kHz field modulation. Polycrystalline diphenyl picryl hydrazyl (DPPH) was used as the standard “g” marker for the determination of magnetic field; a similar technique was employed by G. Upender et al. for invention of structure of WO3–GeO2–TeO2 glasses [12].
\nUV-Visible absorption spectra of prepared borate-based glasses were recorded by using LABINDIA Analytical UV-3092 spectrophotometer in the wavelength range 350–900 nm at room temperature. The precision of wavelength measurement is about ±1 nm [12].
\nThe physical parameters of the present glasses are presented in Table 2. It is observed that the density (ρ) decreases from 3.334 to 2.815 g/cm3 with the addition of ZnO content from 0 to 30 mol% at the expense of CdO content. This could be due to the lower molecular weight of ZnO (81.38 g/mol) in comparison with CdO (128.4 g/mol). This could also be due to the lower density of ZnO (\n
Parameter | \nx = 0 | \nx = 7.5 | \nx = 15 | \nx = 22.5 | \nx = 30 | \n
---|---|---|---|---|---|
*AMW (g/mol) | \n86.589 | \n83.062 | \n79.536 | \n76.009 | \n72.483 | \n
ρ (g/cc) (±0.005) | \n3.334 | \n3.181 | \n3.033 | \n2.924 | \n2.815 | \n
†Vm (cm3/mol) | \n25.972 | \n26.112 | \n26.224 | \n25.995 | \n25.749 | \n
OPD (mol/l) | \n83.936 | \n83.487 | \n83.129 | \n83.862 | \n84.663 | \n
Vo (cm3/mol) | \n11.914 | \n11.978 | \n12.029 | \n11.924 | \n11.812 | \n
Physical parameters of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
AMW: average molecular weight.
Error in Vm is ±0.005.
The molar volume (Vm) increases from 25.972 to 26.224 cm3/mol with ZnO content up to 15 mol% then Vm starts decreasing from 26.224 to 25.995 and then to 25.749 with further addition of ZnO up to 30 mol% at the expense of CdO. This could be due to the difference between cation radii of Cd2+ ion (1.03 Å) and Zn2+ ion (0.83 Å). The nonlinear variation in Vm also suggests the dual role of ZnO content as in the present system ZnO up to 15 mol%, it plays a modifier role, and beyond it plays a glass former role. It is also observed that the oxygen packing density (OPD) decreases from 83.936 to 83.129 mol/l, while oxygen molar volume (Vo) increases from 11.914 to 12.029 cm3/mol with ZnO content up to 15 mol%. But OPD increases from 83.129 to 84.663, while Vo decreases from 12.029 to 11.812 with ZnO addition up to 30 mol%. The nonlinear variation in OPD and Vo values with the increase in ZnO content from 0 to 30 mol% could be due to the variation in density (ρ) and the dual role of ZnO in the present glass system, while the number of oxygen atoms in the glass network remains the same according to the ratio 1:1.
\nThe obtained XRD patterns of BNCZ glass system are shown in Figure 1. It is clear that a broad hump is repeatedly observed in all the samples and is the characteristic of glass, and there is no evidence of crystallization. Hence it is confirmed that the prepared samples possess glassy nature.
\nXRD patterns of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 = x = 30 mol%) glass system.
The IR transmission spectra of all the glasses were recorded in the wave number range 1600–400 cm−1 and are shown in Figure 2. The band positions and their assignments are given in Table 3.
\nIR spectra of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 = x = 30 mol%) glass system.
Band positions | \nAssignment | \n
---|---|
1360–1375 | \nSymmetric stretching vibrations of B–O bonds of trigonal (BO3)3− units in Meta, Pyro and ortho borates | \n
1260 | \nSymmetric stretching vibrations of B–O of (BO3)3− units in meta and Ortho Borates | \n
1040 | \nB–O stretching vibrations of BO4 units in tri, tetra and penta borate groups | \n
970 | \nB–O asymmetric stretching of BO4 units of diborate groups | \n
690 | \nBending vibrations of B–O–B linkages in borate network | \n
Band positions and assignments of IR bands of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
In the BNCZ glass system, significant bands are observed at about ~474, 694, 970–1040, 1250–1260, and 1360–1375 cm−1. These bands assigned to B2O3 and about 80% of the boron atoms are present in the boroxol rings, B3O6, that are interconnected by independent BO3 groups. The vibrational modes of the vitreous borate network are mainly active in three infrared regions. The IR features located in the first region that ranges between 1200 and 1600 cm−1 [13]. The second region ranges between 800 and 1200 cm−1, and the third region ranges between 600 and 800 cm−1. From Figure 2 it is evidently seen that the structure of the glass network formed by boron ions is significantly changed with the incorporation of ZnO at the expense of CdO content. The absence of IR band at ~806 cm−1 indicates that the boroxol rings are not formed in the present glass system, and hence the structure of the glasses consists of borate groups other than the boroxol rings. The weak band observed at ~474 cm−1 in all the glasses is attributed to the vibration of metal cations in their oxygen sites (RO4 groups where R = Cd, Zn) [16].
\nThe bands observed around 694 cm−1 could be attributed to the bending vibration of B–O–B linkages of various borate groups [17]. The bands near 979 cm−1 are assigned to B–O asymmetric stretching of BO4 units of diborate groups [18]. This band shifts to higher wave number side, i.e., from 979 to 1040, while the intensity of this band significantly decreased with the increase of ZnO content up to 30 mol%. The bands observed at around 1040 cm−1 are due to B–O stretching vibrations of BO4 units in tri-, tetra-, and pentaborate groups [12, 19, 20]. The bonds that appeared in the range of 1260 cm−1 are assigned to B–O symmetric stretching vibrations of (BO3)3− units in metaborate and orthoborates [21]. The intensity of this band is unaffected with the addition of ZnO content up to 30 mol%. The bands at around 1363–1375 cm−1 could be attributed due to symmetric stretching vibrations of B–O bonds of trigonal (BO3)3− units in meta-, pyro-, and orthoborates [21, 22]. The broadness of these bands was found to be more with the substitution of ZnO content up to 30 mol%. The B2O3 is built up of BO3 triangles, and upon adding ZnO, the coordination number of the boron changes from SP3 tetrahedral BO4 to form SP2 planar BO3, preserving the B–O bonding without the creation of non-bridging oxygen ions. It means that the introduction of ZnO causes a significant formation of the BO3 groups with a lower coordination number. Therefore, the progressive increase in ZnO content makes the IR bands observed at about 1040 and1373 cm−1 more pronounced. This means that the BO3 groups and hence the bridging oxygen contents are increased with increasing of ZnO content on the expenses of CdO content.
\nFigure 3 shows the Raman spectra of the present glass system in the spectral range 200–1800 cm−1 consisting of sharp, broad peaks and shoulders.
\nRaman spectra of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 = x = 30 mol%) glass system.
The Raman peak positions are summarized in Table 4.
\nSample code | \nRaman peaks (cm−1) | \n||||
---|---|---|---|---|---|
BNCZ1 | \n470 | \n697 | \n770 | \n948 | \n1420 | \n
BNCZ2 | \n464 | \n697 | \n770 | \n943 | \n1420 | \n
BNCZ3 | \n464 | \n697 | \n770 | \n942 | \n1420 | \n
BNCZ4 | \n457 | \n697 | \n770 | \n935 | \n1420 | \n
BNCZ5 | \n447 | \n697 | \n770 | \n932 | \n1420 | \n
Raman peak positions of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system, with error ±1 cm−1.
The Raman spectrum of vitreous B2O3 is dominated by a strong peak centered at ~804 cm−1. The ~804 cm−1 peak is assigned to the boroxol ring breathing vibration involving little motion of boron [23, 24, 25]. The desired peak at ~ 804 cm−1 was not appeared and therefore boroxol rings are absent in the present glass system. Therefore, boroxol ring is absent in these glasses. The Raman peak at around 447–470 cm−1 is assigned to pentaborate and diborate groups [26]. The weak Raman peak appearing at ~697 cm−1 is due to metaborate/(BO3)3− vibrations [27, 28]. The strong peak at around ~770 cm−1 is assigned to symmetric breathing vibrations of six-membered rings with both BO3 triangles and BO4 tetrahedra (tri-, tetra-, or pentaborate groups) [29, 30]. The intensity of this peak is significantly increased with the addition of ZnO content up to 30 mol%. This observation suggests more number of BO3 units instead of BO4 units in six-membered rings. No Raman peaks appeared at around ~ 834 cm−1 in any of the glass, and it indicates that there are no pyroborate groups (B2O54−) present in these glasses. The pentaborate and tetraborate groups were assigned by the peaks observed in the range ~930–950 of Raman spectrum. The broad band around 1420 cm−1 was assigned to the B–O− bonds attached to the large number of borate groups [31, 32]. The decrease in intensity of the peak at ~1420 cm−1 is due to increase of ZnO content up to 30 mol%. This shows that significant formation of Zn2+-B–O− bonds by reducing the number of non-bridging oxygen’s (NBO’s) similar finding was recorded by Upentre et al. for the glass system (90–x)TeO2–10GeO2–xWO 3 (7.5 ≤ x ≤ 30) doped with Cu2+ ions [33]. The observed slight decrease in intensity and shift in the peak ~470 toward lower wave number (447 cm−1) indicates the decrease of penta- or diborate groups in the glasses. The intensity of the peak at ~940 cm−1 decreases while shifts to lower wave number from 948 to 943, 942, 935, and then 932 with increase in ZnO content. This may indicate the presence of less number of pentaborate groups and bond lengths of B–O bonds of pentaborate groups could be increased. The above results suggest the presence of more BO3 units in the glasses with the addition ZnO as Zn2+ establishes the linkages of NBOs with BO4 units.
\nThe DSC thermograms of the present glasses are shown in Figure 4. Glass transition temperature (Tg) is always visible, and this result is in agreement with the result of XRD data as both the techniques confirm the glassy nature of the samples.
\nDSC curves of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 = x = 30 mol%) glass system. Heating rate was 10°C/min.
The values of glass transition temperature (Tg) are given in Table 5.
\nSample code | \nGlass Transigirían temperature Tg (°C) | \n
---|---|
BNCZ1 | \n497 | \n
BNCZ2 | \n494 | \n
BNCZ3 | \n488 | \n
BNCZ4 | \n492 | \n
BNCZ5 | \n496 | \n
Glass Transigirían temperature Tg (°C) for compositions of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
From this table it is observed that Tg decreases from 497 to 488°C with gradual increase in ZnO content up to 15 mol% at the expense of CdO, and thereafter Tg increases from 488 to 492 and then to 496°C with further addition of ZnO up to 30 mol%. This behavior suggests that Tg varies nonlinearly with the addition of ZnO content in place of CdO. It is well known that a higher cation radius of Cd2+ (1.03 Å) replaced with a lower cation radius of Zn2+ (0.83 Å) decreases the overall cation polarizability (polarizability is proportional to the cation size); as a result, Tg should decrease linearly with ZnO content. On the contrary to this, the bond strength of Zn–O (151 kJ/mol) is more than that of Cd–O (101 kJ/mol) [33]; as a result, Tg should increase linearly. But none of the reasons are suitable in this case. Therefore, the observed nonlinear variation in Tg with ZnO content can be understood in the following way: As it was observed clearly from FTIR and Raman that more numbers of BO4 units are present up to 15 mol% of ZnO, then with further addition of ZnO in place of CdO up to 30 mol%, most of BO4 units are converted to BO3 units. The bond strength of BO4 units (373 kJ/mol) is smaller than BO3 units (498 (kJ/mol%) [34]. Hence, Tg decreases up to 15 mol% of ZnO and then starts increasing with further addition of ZnO up to 30 mol%. Besides this the higher field strength of Zn2+ ions (0.53 cm−2) than that of Cd2+ ions (0.38 cm−2) in the glass network also causes to increase the Tg [34]. However, the ionicities of both Zn–O (51%) and Cd–O (51%) are the same, and its role could be neglected. From Figure 4 it is clearly seen that except in BNCZ1 the onset crystallization temperature (To) is not prominently observed with the incorporation of ZnO content. This indicates that the increase of ZnO in place of CdO has a tendency to prevent crystallization. Thus, the present glasses are more thermally stable against crystallization.
\nThe electron paramagnetic resonance spectra of Cu2+-doped BNCZ series are shown in Figure 5. It is essential to dope the glass samples with Cu2+ ions as this gives resonance signals; a similar work is reported in earlier literature [35, 36, 37]. The copper ions with spin 1/2 gives a nuclear spin I = 3/2 for 63Cu and 65Cu and therefore results in (2I + 1) hyperfine components, i.e., four parallel and four perpendicular components.
\nEPR spectra of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 = x = 30 mol%) glass system at room temperature.
The spectra recorded for prepared glass series exhibit three parallel components in the lower field region and one parallel component which is overlapped with the perpendicular component. The EPR spectra of copper ions in all the glass samples have been analyzed using an axial spin-Hamiltonian in which the quadrupole and nuclear Zeeman interaction terms are ignored.
\nThe symbols have their usual meaning.
\nThe solution to the spin-Hamiltonian gives the expressions for the peak positions related to the principal values of g and A tensor as follows [35, 36, 37].
\nFor parallel hyperfine peaks,
\nFor perpendicular hyperfine peaks,
\nThe symbols have the usual meaning. Using Eqs. (2) and (3), the spin-Hamiltonian parameters of all the glasses have been calculated and are tabulated as shown in Table 6 [12].
\nSpin-Hamiltonian parameters (SHP) of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
From Table 6, the
The UV-Visible absorption spectra of prepared glass series were displaced in Figure 6.
\nOptical absorption spectra of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO.
The observed absorption band around ~765 nm in BNCZ1 is assigned to the 2B1g → 2B2g transition (ΔExy) of Cu2+ ion in octahedral coordination with a strong tetrahedral distortion, and the EPR results were found to be in agreement with this assumption [36]. From Figure 6, it was found that the absorption peak firstly blueshifted, i.e., from 764 to 760 and then to 756 nm with the addition of ZnO up to 15 mol%, and then redshifted, i.e., from 756 to 760 to 763 nm with the further addition of ZnO from 15 to 30 mol%. This result is consistent with the observations made in FTIR, Raman, and DSC. As pointed out by Raman and IR analysis, the major structural changes in the present glass take place with the addition of divalent ZnO. This consequence suggests that ZnO enters the glass system in the form of network modifier. Hence, all the observations are clearly from tetragonal (BO4) to trigonal (BO3) units with the incorporation of ZnO content at the expense of CdO content.
\nThe variation in peak position with ZnO doping in glass system BNCZ (30 mol%) indicates the change in the ligand field around paramagnetic Cu2+ ions. This could be due to higher field strength of Zn2+ ions (0.53 cm−2) than that of Cd2+ ions (0.38 cm−2) [33]. The change in polarizability of oxygen ions surrounding the Cu2+ may also change the peak position [6]. This can be understood as follows. As ZnO content substitutes CdO content from 0 to 30 mol%, from IR and Raman structural analysis, it was observed that ZnO has played the dual role. Thus, during the modifier role of ZnO (up to 15 mol%), weak bonds Zn2+–O–B were formed in the place of B–O–B or Cd–O–B, whereas during the former role of ZnO (from 15 to 30 mol%), strong Zn–O–B bonds were formed. Thus the oxygen ions in Zn2+–−O–B bonds are less tightly bound than in B–O–B or Cd–O–B bonds. Thus the oxygen ions can be treated as NBOs in which electrons are loosely bound to the nucleus, and hence these NBOs are more polarized than the oxygen ions in B–O–B or Cd–O–B. These NBOs are decreased during the conversion of BO4 units into BO3 units when ZnO started playing the former role above 15 mol%. Similar observations were reported by other authors [37]. With the conversion of four coordination boron atoms [BO4] into three coordination boron atoms [BO3], the excess of oxygen converts some of Zn2+ ions into tetrahedra [ZnO4] where the structural modification in the glass network could be reason for the variation of the ligand field strength of Cu2+ ions. This may be the reason why the optical absorption maximum has showed the nonlinear variation with ZnO content.
\nThe data of EPR and optical absorption can be correlated to understand the environment around Cu2+ ions in the present glass network; in connection to this, the bonding parameters were evaluated using EPR and optical data by the following equations [6].
\nwhere ΔExy and ΔExz,yz are the energies corresponding to the transitions of 2B1g → 2B2g and 2B1g → 2Eg, respectively, and λ is the spin-orbit coupling constant (= −828 cm−1) and the bonding coefficients α2, β12, and β2 (≈1.00) characterize in-plane σ bonding 16 between the d orbital of Cu2+ and the p orbital of ligand, in-plane π bonding between the d orbital of Cu2+ and p orbital of ligand and out-of-plane π bonding between the d orbital of Cu2+ and p orbital of ligand in the glasses respectively [6]. Besides the values of ΔExy and ΔExz,yz are also calculated and presented in Table 7. In the present glasses, the bonding parameters α2, β12, and β2 were evaluated using the following equations [38, 39] and are displayed in Table 7.
\nParameter | \nx = 0 | \nx = 7.5 | \nx = 15 | \nx = 22.5 | \nx = 30 | \n
---|---|---|---|---|---|
λ (nm) (±1) | \n764 | \n760 | \n756 | \n760 | \n763 | \n
ΔExy (cm−1) | \n13,089 | \n13,158 | \n13,228 | \n13,158 | \n13,106 | \n
ΔExz,yz (cm−1) | \n20,666 | \n19,408 | \n20,017 | \n19,117 | \n19,408 | \n
α2 | \n0.798 | \n0.799 | \n0.804 | \n0.802 | \n0.803 | \n
β2 | \n0.964 | \n0.963 | \n0.957 | \n0.959 | \n0.958 | \n
β12 | \n0.793 | \n0.794 | \n0.801 | \n0.803 | \n0.797 | \n
Γπ (%) | \n41.4 | \n41.2 | \n39.8 | \n39.4 | \n40.6 | \n
Γσ (%) | \n37.33 | \n37.15 | \n36.22 | \n36.59 | \n36.41 | \n
Bonding parameters of 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (0 ≤ x ≤ 30 mol%) glass system.
Here P is dipolar hyperfine coupling parameter (=0.036 cm−1). From Eqs. (4) and (5), in order to determine Cu2+ bonding coefficients, besides the EPR parameters, the energy positions of the absorption bands of Cu2+ which indicate the values of ΔExy and ΔExz,yz are required. Since one absorption band corresponding to 2B1g → 2B2g transition (ΔExy, are presented in Table 7) was observed, the position of the second band can be estimated by using the following equation [39] and the values are presented in Table 7.
\nwhere K2 is the orbital reduction factor (K2 = 0.77) and λ is the spin-orbit coupling constant.
\nThe normalized covalency of the Cu2+–O in-plane bonding of σ and π symmetry is expressed in terms of bonding coefficients α2 and β12 as follows:
\nwhere S is the overlapping integral (Soxy = 0.076). The values of Γσ and Γπ are given in Table 6. It is clear from Table 7 that both of these values are varied with addition of ZnO content to B2O3 network. This could be due to variation of structural changes within the glasses. In general if α2 have smaller values, then the greater the covalent nature of the bonding. The calculated values of α2 for prepared glass series (the range 0.798–0.803) suggest that the in-plane σ bonding in the glasses is moderately covalent in nature, whereas the values of β12 (0.793–0.803) obtained for various glasses indicate that the in-plane π bonding is significantly ionic in nature.
\nThe changes in this parameter can be attributed to the changes in O–X bonds (where X = B, Cd, and Zn) because it reflects the competition in the Cu2+–O–X bonds, between the cupric ion and its neighboring X cations for attracting the lone pairs of the intervening oxygen ions. In the present system, the values of β2 were found to be close to unity, and it suggests that out-of-plane π bonding is more ionic in nature and the magnitudes of all bonding parameters are comparable to those found for Cu2+ in other glasses [6].
\nTransparent glasses with composition 59B2O3–10Na2O–(30 − x)CdO–xZnO–1CuO (where x = 0, 7.5, 15, 22.5, and 30 mol%) were prepared by melt-quenching technique. It was observed that the density (ρ) decreases, while OPD, molar volume (Vm), and oxygen molar volume (Vo) are nonlinearly varying with the addition of ZnO content from 0 to 30 mol% at the expense of CdO content. From FTIR studies, it is found that the glasses are composed of [BO4] and [BO3] units in various borate groups. FTIR and Raman studies revealed that more numbers of BO4 units are present up to 15 mol% of ZnO, and then with further addition of ZnO in place of CdO up to 30 mol%, most of BO4 units are converted to BO3 units. The nonlinear variation in Tg is due to the dual role of ZnO. From EPR results, it was found that
The discovery of microwave cooking by Percy Spencer marked the dawn of a new era in microwave heating technology, which has gained huge attention in the scientific areas, especially in synthetic chemistry [1]. Numerous factors enabled the microwave technique to become a breakthrough technology in the complex synthesis process [2]. The significance of microwave heating for the synthesis of high-quality semiconducting nanomaterials, pristine or doped ones, is a subject that needs to be profoundly studied and explored due to its capability to revolutionize the semiconductor industry. The synthesis of high-quality nanocrystals primarily relies on controlled reactions of molecular precursors in a liquid medium at an adequate temperature in the presence of stabilizing agents [3, 4]. Most of the synthetic methods such as wet chemical process [5], emulsion methods, anti-solvent precipitation methods [6], have studied only the impact of the chemical process and parameters, on the properties of as-synthesized nanocrystals. Of late, the effect of additional external stimulations like microwave irradiation [7, 8], ultraviolet/visible light irradiation, ultrasound, etc. is also studied [5]. Microwave heating increases the rate of reaction, thereby considerably decreasing the reaction time without altering the kinetics and chemical reaction [9, 10, 11]. The rate accelerations caused by “specific microwave effect” as well as “non-thermal effects” have to be considered in the microwave heating mechanism. Baghbanzadeh et al. propose that microwave dielectric heating can be termed as “specific microwave effects” by which one can achieve rate accelerations that cannot be attained by the conventional methods [12]. In the case of “non-thermal microwave effects”, the heating mechanism arises as a result of the direct interaction of microwaves with specific molecules or materials in the reaction medium [2, 12]. Jacob et al. report that the enhancement rate of reaction with microwave heating compared to conventional heating is mainly due to the thermal effects which arise due to three significant factors. Firstly, the localized heating effect is a consequence of superheating phenomena due to the abundant ions present in the medium. Secondly, the molecular agitation due to lag of dipole, in following the fast-moving EM wave. Thirdly, increase of diffusion rate of reactants [13].
\nEarlier, the synthesis of high-quality semiconducting quantum dots was very tough and the process of doping at this length scale makes it even more challenging. Erwin et al. reported that the difficulty in doping at nanoscale regime is due to the difference in mechanisms involved in doping at bulk and at the nanoscale, while other reports in literature claim the process of ‘self-purification’ as the leading cause for de-doping during the growth process [14]. The major daunting challenges arise mostly due to the lack of a comprehensive understanding of all the fundamental mechanisms associated with dopants incorporation and the absence of reliable synthetic procedures where the temperature-dependent dopant impurity atoms diffusion will be minimal [15]. Another challenge involved in doping at the nanoscale is the inherent statistical inhomogeneity of dopants among the nanocrystals. The doped nanomaterials always tend to exhibit a broad range of dopant populations per nanocrystal, which results in effective inhomogeneity in concentration of dopants among nanocrystals. Providing a uniform and instantaneous heating during the reaction process can minimize this problem to a great extent [16]. In this context, microwave heating became the suitable thermal energy source for doping the semiconducting nanocrystals, as it provides rapid and instantaneous heating. Short reaction time, faster reaction rate, uniform volumetric heating, cost-effective and eco-friendly method are the other remarkable features which make microwave heating a prime superior choice over other conventional methods of heating like a hot plate, oil bath, etc. [8]. Moreover, heating by means of conventional methods always results in ‘a self-purification’ mechanism where the dopants are diffused towards the surface of nanocrystals at the time of growth [14]. By adopting microwave-assisted techniques the aforementioned problems encountered while doping at the nanoscale can be eliminated to a great extent and the synthesized products are found to excel both in quality as well as quantity [17].
\nMicrowave is an electromagnetic wave having low energy with a wavelength and a frequency in the range of 1 m to 1 mm and 300 MHz to 300 GHz, respectively as shown in Figure 1. Mainly, the laboratory and household microwave oven operate at a frequency of 2.45 GHz, which corresponds to a wavelength of 11.2 cm. It can travel at the speed of light (~30 cm/nanosecond) like any other electromagnetic wave and consists of electric and magnetic fields oscillating in a direction perpendicular to each other. One can also define it as a Multiphysics phenomenon in which the heating arises due to interaction between matter and electromagnetic radiation. In contrast to other conventional methods of heating, here the medium itself gets self-heated as a result of the alignment of molecular dipoles present in it with respect to the field associated. The electric and magnetic components in microwave interact with matter in different manners as discussed below [1].
\nSchematic representation of the electromagnetic spectrum in terms of wavelengths and frequencies.
The polar molecules are sensitive to an electric field, and thus as a result of force exerted by the field on the charged particles, they start to migrate or rotate in order to align along the field (Figure 2). Since the electric and magnetic components reverse direction rapidly with a frequency of 2.45 GHz, the electric dipoles have no time to orientate to the direction of electric filed. As a result, there occurs the angle between the orientation of the dipoles in space and the direction of the electric field and the energy loss by the dipoles occurs resulting in to rise of dielectric heating. Reflection, absorption, and transmission are the three modes by which the medium reacts to the electromagnetic waves, either in a single or combined fashion [18]. The effective dielectric loss factor for the dielectric heating can be expressed in terms of dipolar polarization, ionic conduction as follows
\nSchematic diagram of the interaction of an electric component of the microwave radiation with matter.
where\n
Like an electric field, a magnetic field interacts too with matter and induces heat through magnetic loss, joule heating, and so on. However, sufficient studies apart from dielectric heating are still very rare. Meanwhile, Cheng et al. reported that magnetic loss contributes significantly to microwave heating compared to dielectric heating [20]. The necessary physical processes generating heat energy as a result of interaction between material medium and the magnetic field component are the eddy current loss, hysteresis loss, and magnetic resonance loss [21, 22]. The overall losses that constitute the effective magnetic permeability (\n
where \n
Microwave heating has been the subject of interest for doping semiconductors at nanoscale owing to its ability to control the synthesis process explicitly. Apart from being cost-effective, the dielectric heating by microwave irradiation minimizes the dopant diffusion problem and provides quick reaction among precursors. The process of nucleation and growth of nanocrystals have been described in theories like LaMer burst nucleation [23], Watzky and Finke’s slow nucleation followed by autocatalytic growth [24], and LSW theory, etc. [25, 26]. Nucleation is the process where nuclei act as a template for nanocrystal growth. Uniform formation of nuclei throughout the growth medium defined as ‘homogeneous nucleation’ can be easily and efficiently achieved by microwave irradiation in contrast to conventional methods of heating. Volumetric heating provided by microwave irradiation raises the internal temperature of the whole medium simultaneously and homogeneously as illustrated in Figure 3. This favors a quick nucleation process which results in solution supersaturation leading to homogeneous nucleation. Microwave-assisted technique aids to measure, manipulate, and thereby optimize the nucleation process and parameters that in turn influences the stability of the synthesized particles along with an added advantage of automatic data recording [12]. Efficient doping is determined by the surface morphology and shape of nanocrystals and the presence of surfactants in the reaction medium. Temperature plays a significant role in molding the aforementioned factors [27]. This demands the necessity for a proper thermal energy source like microwave heating while synthesizing nanocrystals. High penetration depth (d) offered by microwave heating is yet another factor that distinguishes it from the conventional methods of heating. It is defined as the distance at which the microwave power reduces to 1/e of its incident power. It has inverse proportionality with oscillating frequency, dielectric, and magnetic loss factor. The formula for determinate a penetration depth (d) may be written as
\nSchematic illustration of main differences between the microwave heating (a) and traditional heating method (b).
where α is the absorption coefficient of microwaves,\n
The efficient absorption of the EM wave by the solvent is determined by its loss tangent factor. It is defined as the ability of a material to convert electromagnetic energy into heat energy at a given frequency and temperature [1]. A high value is desired for maximum absorption, however, heating aided by microwave radiation is achievable even in the presence of a low tan (δ) solvent provided there exists either a polar reactant or reagent such that the overall dielectric nature of the reaction medium favors the microwave heating. In the case of conventional heating methods, the transfer of heat is slow and inefficient, resulting in a huge temperature gradient owing to the different thermal conductivity of materials. However, in the case of microwave radiation, there is a direct coupling between the microwave energy and the molecules resulting in core volumetric heating. The most commonly used frequency of the microwave is 2.45 GHz, possessing an energy of 0.0016 eV, which is lower than that of Brownian motion and therefore insufficient to break the bonds. This property of microwaves makes them incapable of carrying out any unwanted reactions and thereby solely ensuring effective doping at nanoscale materials.
\nNanocrystals are broadly classified as nanoparticles and quantum dots. Generally, tiny particles of a dimension of 100 nm or below are termed as nanoparticles. However, quantum dots (QDs) are a class of nanomaterials with their charge carriers confined in all three dimensions of the length scale of exciton Bohr radius [28]. While doping the QDs, the dopants have a high tendency to come out of it due to the thermal diffusion because their size is in the nanometer range. This problem can be resolved greatly by having a comprehensive idea about the various mechanisms involved during doping and following a proper synthesis process [29]. However, various properties, including optical, magnetic, and electronic, of semiconducting quantum dots can be tailored in a desired fashion by the incorporation of impurity dopant atoms [30]. Moreover, this can also generate some new physical properties, including spin-polarizable excitonic photoluminescence, exciton storage, excitonic magnetic polaron formation, and magnetic circular dichroism so on. The proper incorporation of impurity atoms into the semiconducting QDs is a tough job but can be identified by observing the following features like red-shifted PL emission and large Zeeman splitting of excitonic excited states that are a result of strong exchange coupling between dopant and the carrier [31, 32]. In the year 2000, Mikulec et al. reported the most significant result on QDs doping; in which they reported manganese (Mn) doped CdSe nanocrystals with the evidential result obtained from electron paramagnetic resonance (EPR) [33]. Later, a variety of doped semiconducting material were reported by tailoring both the host atoms such as ZnS, PbS, MgO, Al2O3, α-Fe2O3, CdS, ZnSe, etc. and dopant atoms such as Mn, Cu, Ag, Fe, Zn, Cr, Er, etc. [34, 35]. However, there is a limitation to select the host system and the respective dopant atoms. Suppose, incorporation of Mn into nanocrystals of CdS and ZnSe easy but not into CdSe even though the bulk solubility almost equal to 50% for all three [27, 36].
\nDepending on dopants’ diffusivity, the dopant precursors are injected at different time intervals, suppose along with the host precursors or at the time of nucleation or growth as shown in Figure 4 [37]. The major problem involved in doping at the nanoscale is that many dopants fail to be incorporated within the host lattice and instead get adsorbed on the surface [38]. High formation energy for defects renders the impurity atoms to be thermodynamically unstable, resulting in the expulsion of dopants from the host lattice, in turn leading to self-purification [14, 27, 39]. Apart from thermodynamics, kinetics also play a significant role in determining the stability of added impurities in solution phase synthesis. Chen et al. have reported a detailed study regarding all the elemental processes involved with doping, such as surface adsorption, lattice incorporation, lattice diffusion, and lattice ejection as represented schematically in Figure 5 [40]. Maintenance of appropriate temperature is a crucial factor even in the phenomena mentioned above.
\nGeneral schematic model of the colloidal synthesis of doped quantum dots [37].
Schematic diagram showing temperature-dependent dopant lattice diffusion [37].
The high cost of commercially doped QDs is one reason that limits its wide range of applications. Therefore, cost-effective synthesis protocols need to be developed to produce high-quality doped QDs. This limitation and the ones mentioned above are lifted off using microwave heating for doping the QDs. It is also found to be an economical and eco-friendly method in line with green chemistry. Now let us discuss some semiconducting QDs systems where doping has been performed with microwave heating technique.
\nCdSe QDs is n-type intrinsically, and a flagship candidate in nanoscale research history shows several novel properties as a member of the II-VI binary semiconductor group. It was attractive to the researchers to demonstrate various optoelectronic applications as its energy band overlaps nicely with the solar energy spectrum [41]. The fundamental properties of CdSe are enhanced via doping, which further increases its demand in the semiconductor industry. However, doping of CdSe by Mn2+ ions is challenging due to the self-purification effect, as reported by Erwin et al. [27, 29, 42]. The doping process is mainly governed by the surface kinetic effect. Microwave heating helps one to have exquisite control over this surface kinetics that eases the doping process.
\nMeladom et al. developed a robust synthesis protocol for efficient doping of Mn2+ into CdSe QDs in an aqueous medium with mild microwave heating as a final step [17]. A household microwave oven was used to heat the CdSe QDs solution for 60 seconds duration with the set point of 450 W (operational frequency 2.45 GHz). This heating step was repeated three times by giving 5 minutes intervals. The motivation was to tune the electrical conductivity of CdSe QDs thin film by varying doping concentration only as the size of QDs kept similar for all the samples. Microwave heating improves the quality of QDs in terms of optical properties, which was confirmed by recording UV–vis absorbance and photoluminescence both excitation and emission spectra, as shown in Figure 6(a) and (b), respectively. In all the cases, peak intensities were enhanced and bandwidth reduced, which indicates the reduction of surface defects of QDs. The chemical composition of the doped CdSe QDs sample was confirmed with X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDS), and inductively coupled plasma - atomic emission spectroscopy (ICP-AES) measurements data. XPS result confirmed the efficient incorporation of Mn atoms as dopants inside the host CdSe QDs (Figure 7).
\nElectronic UV–vis (a) and photoluminescence (b) spectrum of Mn2+ doped CdSe QDs sample with and without microwave irradiation [17].
(a) Survey scan of the X-ray photoelectron spectrum of 2% Mn2+-doped CdSe QDs. (b, c) high-resolution spectrum of Cd 3d electrons depicting doublet splitting with binding energies separated by 6.9 eV and Se 3d, respectively. (d) the high-resolution spectrum of Mn 2p core electrons showing doublet splitting with binding energy separated by 10.9 eV [17].
Microwave-assisted synthesis has also been utilized by many research groups around the world to dope various other binary II-VI semiconductor-based nanocrystals. Molaei et al. reported the synthesis of copper (Cu) doped ZnSe nanocrystals in the aqueous medium to study the doping effect on the optical properties [43]. Synthesis of Mn2+ ion-doped ZnS quantum dots was reported by Joicy et al. using a rapid microwave irradiation step without any surfactants, which showed photocatalytic activity by observing photodegradation of methyl orange dye under UV light irradiation [44]. Here, the zinc blende crystal phase of ZnS was important for the efficient incorporation of Mn atoms. In the same year, Zhu et al reported the synthesis of of Mn-doped ZnS via green and rapid microwave-assisted approach and they also developed indapamide drug detector by recording room-temperature phosphorescence (RTP) with that doped material [45].
\nLater, Zhang et al. reported the aqueous synthesis of Mn and Cu doped ZnSe QDs by microwave radiation with higher quantum yields (QYs) and they have further extended this work to grow the white-light-emitting ZnSe/ZnS core/shell QDs via the co-doping of Mn and Cu [46]. Lead sulphide (PbS) QD are still emerging various applications in optoelectronics and its property was further tuned with a silver (Ag) atom doping. It is also reported by Shkir et al. that the bandgap of PbS QDs was increased with Ag atom incorporation, which was predicted without mentioning the influence of size variation between the samples used [47]. Recently, another work reported on facile microwave synthesis of CdS quantum dots doped with Cr atoms as impurity doping and they have studied various properties like structural, opto-dielectric, electrical, and so on [48].
\nVarious metal oxides nanomaterials play a major role in the development of different novel daily life applications in the fields of display, sensors, medicine, biomedical devices, agriculture, information technology, optical, energy, electronics, and so on. Efforts are ongoing to tune their properties and applications further with incorporating impurity as dopants. For that reason, microwave heating based synthesis protocols is developing as a potential alternative to the conventional heating based growth process. Kar et al. developed a microwave synthesis of rare-earth element Eu3+ doped tin oxide (SnO2) to tune the optical and electrical properties of the host [49]. Jamatia et al. reported the microwave-assisted synthesis of Fe doped ZnO nanoparticles to show their application in polymer light-emitting diodes [50]. The wurtzite hexagonal crystal phase of ZnO nanoparticles and incorporation of the Fe dopant into the host ZnO crystal lattice was confirmed via X-ray diffraction analysis. This report claimed that the bandgap modification of ZnO via Fe doping is estimated from the Tauc plot without considering the influence of size. Similarly, many spinel structured metal oxides were also doped with different transition metal ions via microwave heating based synthesis technique with tunable structural, morphological, optical, vibrational, and magnetic properties and different potential applications like phosphor-based forensic testing and many more [51, 52, 53, 54]. Interestingly, Er3+ doped α-Fe2O3 and Fe doped TiO2 nanoparticles were synthesized successfully with the help of microwave heating to study their crystal structure and optical properties [55, 56]. Recently, Yathisha et al. reported Zn2+ doped MgO nanoparticles utilizing microwave combustion route to study the influence on photovoltaic properties [57]. Therefore, microwave heating could explore further as a low-cost alternative synthesis protocol to design a new variant of nanomaterials.
\nLanthanum trifluoride (LaF3) is an ionic compound that is utilized as core-shell-up conversion nanoparticles (UCNPs) for different filed of applications like sensing, biomedical, and solar cells. Tek et al. reported Yb3+ ion-doped (active) and undoped (inert) LaF3 shell coatings on a 20% Yb, 2% Tm codoped hexagonal phase LaF3 core with the help of microwave -assisted synthesis route [58]. They observed higher optical enhancement of inert shell compared with the active shell at all prominent emission peaks, which is explained with the energy band diagram indicating the energy transfer pathways for the Yb3+ and Tm3+ − co-doping (Figure 8).
\n(a) UCPL data for core, active shell, and inert shell nanoparticles under 980 nm continuous-wave excitation. (b) Energy diagram showing the corresponding transition of UCPL of (a) where the energy transfer pathways for the Yb3+ and Tm3+-codoped up conversion nanoparticles are depicted [58].
Carbon-based materials like graphene can also be doped via microwave (MW) heating. Since the nanocarbon materials are found to be sensitive to microwave radiation [59, 60], the technique of MW heating was employed in the modification of graphene materials. It is also reported that by the use of microwave heating, hollow carbon nanospheres can be synthesized within a short time which can be effectively used as a host material for doping [61, 62]. Figure 9 shows the microwave-assisted approach to prepare metal/graphitic shell nanocrystals and CNT in a very short time using ordinary carbon precursor.
\nMicrowave-induced synthesis of Ni/graphitic-shell nanocrystals and graphitic hollow carbon Nano spheres [61].
The microwave-assisted technique facilitates the growth of heteroatom-doped graphene with better catalytic activity as well. Nitrogen doping up to 8.1% on graphene was achieved by Kwang et al within a minute with the aid of the microwave radiation. The binding configuration of nitrogen over graphitic basal planes can be varied with the irradiation power of microwave. The conductivity enhancement upto 300 Scm−1 was obtained in this case in comparison to nitrogen-doped via arc discharge method, nitrogen plasma process, etc. showing a lesser conductivity [63]. The dielectric heating of MW induces a high energy state that helps the graphitic basal plane to accommodate the dopants in order to convert graphite to N-doped graphene. The selective dielectric heating, which arises due to the difference in the dielectric constants of solvent and reactant can enhance the efficiency of doping without the rise of a thermal gradient [64]. The solid phase microwave-assisted synthetic method is adopted for the large-scale production of N-doped carbon nanodots (CNDs) using different citric acid/urea (C/U) weight ratios, which result in size variation of CNDs as shown in Figure 10 with the transmission electron microscope (TEM) images. The dopant ion concentration can be varied in a precise manner that results in N-doped graphene QDs and graphitic-carbon nitride quantum dots (g-CNQD). The doped material is found to exhibit a 38.7% quantum yield due to the presence of N and O rich edge groups resulting from the interaction of microwave on graphene [65].
\nHR-TEM micrographs of N-doped carbon nanodots (CNDs) samples prepared using the SPMA method for different citric acid /urea (C/U) weight ratios of 3/1 (a), 2/1 (b), 1/1 (c), 1/1.5 (d), 1/2 (e), and 1/3 (f). Inset shows the corresponding selected-area diffraction pattern [65].
Huge enhancement in the conductivity of microwave-assisted doped QDs has been reported in many pieces of literature. Microwave heating enables the tuning of electrical conductivity in a desired manner by proper incorporation of dopants into the desired locations of the host material. This is evidenced by the rise in the electrical conductivity to the order of 104 for 2% Mn2+ doped CdSe over undoped one as shown in Figure 11(a) [17]. Here, the conduction mechanism is controlled by the electric field-assisted thermal ionization of trapped charge carriers in CdSe QDs as described in Poole–Frenkel effect as shown in Figure 11(b) [66]. The bandgap has no role in the conductivity and the observed colossal conductivity enhancement is solely due to the concentration of Mn2+ dopant ions.
\n(a) Current–voltage characteristics of Mn-doped CdSe QDs for the samples with varying dopant concentrations. (b) Poole–Frenkel fitting for all samples with respective straight trend line [17].
The STM study performed on a monolayer device of Mn2+ doped CdSe QDs synthesized via microwave method founds to exhibit excellent memory characteristics as described in Figure 12 [17]. This memristor property is evident from Figure 12(b) where the doped CdSe QDs switched to a high conducting state at the bias of 2.5 V. It is also observed that the device switched back to its low conducting state when the tip swept towards 3 V and the ON/OFF ratio obtained was higher than 102. The reproducible nature of the resistive switching property over many cycles further confirms the reliability of the measurement. The threshold voltage at which the device switches to a high conducting state is found to be decreasing with an increase in the dopant concentration. Thus the notable electric bistability and the low threshold voltage of as synthesized doped CdSe QDs with the aid of simple and domestic microwave method promises its application in vivid area of future technologies which ensures minimum energy consumption per byte of the resistive data storage devices in future.
\n(a, b) The Tunneling current–voltage (I–V) characteristics of a monolayer of undoped and 0.2% Mn2+-doped CdSe QDs. Doped CdSe is showing low conducting state (OFF state, black line) and high conducting state (ON state, red line) for forward and backward voltage sweep direction respectively. (c, d) The differential conductance–voltage characteristics of a monolayer of undoped and 0.2% Mn2+-doped CdSe QDs respectively in their forward (black line) and backward (red line) sweep direction. The topographic images of bare Si(111).and monolayer of undoped CdSe QDs deposited on Si(111) are shown on the insets within (c) and (d) [17].
In this chapter, we mainly discussed the incorporation of impurity dopant atoms into a host semiconducting quantum dots system very efficiently using microwave heating strategy with the help of a large number of examples from the literature. It has also been observed that the zinc blend crystal phase is very efficient for the dopant incorporation than the hexagonal one. This also reflects that microwave heating can be utilized to synthesize various classes of doped zero-dimensional (0D) nanomaterials or quantum dots of many chalcogenides, oxides, carbon dots, and more with the large numbers of dopant atoms easily and more cheaply. Literature shows that the research related to two-dimensional (2D) transition metal dichalcogenides (TMDs) is booming up due to having tunable physical, electronic, and optoelectronic properties. Therefore, it would be intriguing to grow various 2D TMDs, both intrinsic and impurity-doped, via microwave heating, which will definitely reduce cost and different health and environmental hazards.
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