Precursors and solvents used in the synthesis of ZnO by the sol‐gel process.
\r\n\t
",isbn:"978-1-83880-679-8",printIsbn:"978-1-83880-678-1",pdfIsbn:"978-1-83880-680-4",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!0,hash:"dfe986c764d6c82ae820c2df5843a866",bookSignature:"Prof. Petra Surlin",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/9493.jpg",keywords:"Periodontal Morphology, Periodontal Anatomy, Disease Pathogenesis, Periodontal Immunology, Periodontal Examination, Periodontal Instruments, Gingivitis, Periodontal Abscess, Periodontitis, Periodontal Therapy",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 8th 2020",dateEndSecondStepPublish:"December 14th 2020",dateEndThirdStepPublish:"February 12th 2021",dateEndFourthStepPublish:"May 3rd 2021",dateEndFifthStepPublish:"July 2nd 2021",remainingDaysToSecondStep:"a month",secondStepPassed:!0,currentStepOfPublishingProcess:3,editedByType:null,kuFlag:!1,biosketch:"Prof. Petra Surlin, DMD, Ph.D., is a member of the European Federation of Periodontology (EFP) and the International Association of Dental Research (IADR). 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"55075",title:"ZnO Nanostructures Synthesized by Chemical Solutions",doi:"10.5772/intechopen.68278",slug:"zno-nanostructures-synthesized-by-chemical-solutions",body:'\nAn important II–VI semiconductor is ZnO which has been well‐studied and applied in a variety of applications. It has a band gap of 3.6 eV and large exciton binding energy of 60 meV. Nowadays this material is considered as one of the most important large band gap semiconductors due to its easy synthesis, stability at room temperature, eco‐friendly properties, being a direct band gap material and fast mobility. This material exists in three different crystal phases such as zinc blende, cubic or rock salt and wurtzite or hexagonal. The first two phases are obtained only in certain well‐controlled conditions such as certain pressures and on specific substrates. However, the most common phase under ambient conditions is the wurtzite hexagonal crystal structure shown in Figure 1.
\nRepresentation of ZnO wurtzite crystal structure (black and grey balls corresponds to Zn and Oxygen atoms).
Another advantage of this compound is that it can be synthesized and deposited by employing different techniques. Slight variation in process conditions can result in different product morphologies and properties. Since the costs associated with research and industry is always an important consideration, it becomes necessary to use inexpensive and efficient methods to obtain the desired novel nanostructured materials with applications in different fields such as optoelectronics, solar cells, piezoelectric and sometimes in biological materials.
\nSol‐gel, colloidal solution and microwave‐assisted synthesis are techniques that are still important in the synthesis of semiconductor nanomaterials. These techniques share some similar characteristics such as (i) they are relatively inexpensive; (ii) the efficiency of the synthesized materials is high; (iii) process parameters are easily controlled and (iv) these techniques are also well‐studied. For these reasons, in this chapter we have focused on a review of these techniques, especially for the synthesis of ZnO, with emphasis on the recent advances in the synthesis of novel nanomaterials and its applications. A general overview of each process is also presented for ease of readability. The synthesized materials have been structurally characterized using X‐ray diffraction (XRD) and scanning electron microscopy (SEM). Figure 2 shows a representative XRD pattern of ZnO. XRD patterns of synthesized material can be compared to reference patterns to determine phase purity or if there is preferential crystal orientation. Most of the time, ZnO is obtained as a polycrystalline film or powder which can be identified by its numerous diffraction peaks at relative intensities. Depending on the processing conditions, single crystal or preferential growth can occur in thin films that result in different relative peak intensities or missing peaks compared to the reference pattern. The 2‐theta values of the (100), (002) and (101) lines in Figure 2 of the hexagonal crystal planes are located at 31.770, 34.422 and 36.253° for wurtzite ZnO (Ref. JCPDS card # 36‐1451).
\nTypical XRD pattern of ZnO nanoparticles.
Different processing parameters may result in different microscopic product morphologies of ZnO. From SEM, we can observe that this material could be obtained as nanoparticles (Figure 3), polycrystalline (Figure 4) and as a nanostructured thin film (Figure 5). All of these materials were synthesized under non‐extreme conditions using colloidal synthesis to produce the source material. The crystal structure of these materials is the hexagonal wurtzite structure.
\nSEM image of ZnO nanoparticles obtained via colloidal synthesis. The scale bar is 500 nm.
SEM image of polycrystalline ZnO thin film obtained through vacuum evaporation process, colloidal nanoparticles as source were used. The scale bar is 500 nm.
SEM ZnO nanostructures using colloidal nanoparticles as source. The scale bar is 500 nm.
The sol‐gel process encompasses a variety of precursors, solvents and additives. But in general, the basis of the sol‐gel process includes some form of hydrolysis and condensation reactions. In the case of ZnO, usually a zinc salt such as zinc acetate is used with water or an alcohol as the solvent. An example of possible hydrolysis and condensation reactions for ZnO are shown in Eqs. (1) and (2), where Zn(OR)2 is a soluble salt.
\nDuring the hydrolysis reaction, the soluble zinc precursor forms a zinc hydroxide intermediate that is able to condense with other intermediates to grow a zinc oxide inorganic polymer. The final product after drying has an amorphous structure and crystallization of ZnO particles require an annealing step. The morphology of the inorganic network can range from spherical nanoparticles to percolated gels and is highly dependent on the choice of precursors, water content, solute and solvent ratio, aging and additives. The sol‐gel process has proven to be an inexpensive and relatively simple method of ZnO nanoparticle synthesis that is tailorable to produce unique nanostructures for different applications.
\nColloidal synthesis is another well‐known chemical solution method to obtain novel nanomaterials with different morphologies and sizes. All processing conditions involved in the system can be fixed to control nucleation and growth of the materials. The kind of interactions (physical and chemical) between particles include Vander Waals, electrostatic, Ostwald ripening and some other theoretical principles such as Derjaguin, Landau, Venvey and Overbeek theory (DLVO). These interactions can contribute to agglomeration and subsequently precipitation of the particles. Colloidal instability can be prevented through steric stabilization which usually requires a surfactant to maintain the colloidal suspension. Surfactants work in two ways: first, to prevent particulate interactions and second, to prevent the continuous nucleation and growth of particles.
\nMicrowave‐assisted synthesis is a relatively recent technique that has been used for synthesis of nanomaterials. It has been considered as a promising approach to obtain novel nanomaterials in organic and inorganic fields. Additionally, microwave synthesis is considered as a green process and coheres perfectly to the principles formulated by Anastas et al. related to green chemistry [1].
\nOften a domestic microwave is used and the synthesis is carried out in solvent‐free solutions. This technique allows for rapid and homogeneous heating of the system since energy is transmitted directly through molecular vibrations. The short heating ramp time of microwave synthesis allows for better control of particle size distribution compared to conventional heating. On the contrary, the extremely high heating rate of microwave‐assisted synthesis may cause the boiling point of the solution to increase by a few degree Celsius. Additionally, the microwave susceptibility will vary between different materials and temperatures.
\nThe microwave energy is generated by a magnetron that transforms electrical energy into a strong magnetic field. The electromagnetic energy interacts with the solution, vibrating the molecules and giving sufficient activation energy to the system for chemical reactions to take place in seconds or minutes.
\nThe reaction rate during microwave synthesis can be explained through the Arrhenius equation [Eq. (3)] as follows:
\nwhere K is the rate constant, T is the absolute temperature (in Kelvin), A is the pre‐exponential factor, a constant for each chemical reaction that defines the rate due to frequency of collisions in the correct orientation, \n
Bilecka et al. reported that nanoparticle growth can be described using four thermodynamic parameters related to the Arrhenius equation through activation energy [2]. These variables are the activation energies for precursor solvation, monomer formation, nucleation and crystal growth. As with colloidal synthesis, nucleation and growth in microwave synthesis are governed by Ostwald ripening.
\nSol‐gel, colloidal and microwave‐assisted synthesis are effective techniques to efficiently obtain novel ZnO nanostructures. These techniques are relatively inexpensive and do not require sophisticated laboratory equipment. Additionally, slight variations in precursors or process parameters can produce different morphologies that can be applied in different technological fields.
\nThe precursors used in these synthesis routes usually start with a basic salt of Zn, a solvent and a catalyser such as temperature. The Zn precursor must be soluble in the selected solvent such that it can provide the necessary Zn ions to produce ZnO particles. Other reagents may be added in order to substitutionally dope ZnO with metal cations such as Fe, Cu, Co and Ba. Additionally, surfactants may be added to maintain colloidal stability of the product or influence the morphology of the growing particles.
\nDifferent precursors used in sol‐gel and colloidal techniques from recent publications have been summarized in Tables 1 and 2, respectively. The readers are asked to consult the relevant publications for details of these processes.
\nPrecursor | \nSolvent | \nStabilizing agent | \nReference | \nTechnique | \n
---|---|---|---|---|
Zn(CH3OO)2 2H2O | \nCH3OH, C2H5OH, C3H7OH, C3H7OH, C4H9OH | \n(CH2CH2OH)2NH, N(CH2CH2OH)3 | \nPourshaban et al. [3] | \nSol‐gel | \n
Zn(CH3COO)2 2H2O/CuCl | \n2‐methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nJoshi et al. [4] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Ba(NO3)2 | \n2‐methoxyethanol | \n(CH2CH2OH)2NH/DEA | \nKasar et al. [5] | \nSol‐gel | \n
Zn(CH3OO) 2H2O, (NH4)2CO3, Fe(NO3)3 | \nDistilled water/ethylene glycol | \n– | \nBahari et al. [7] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Mn(CH3CO2)2 4H2O | \nIsopropyl alcohol | \nUrea | \nKumar et al. [6] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, C2H3LiO2 | \nC2H5OH | \n(CH2(OH)·CH2·NH2) | \nBoudjouan et al. [8] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, CaCl2 | \nCH3OH, C2H5OH | \n– | \nSlama et al. [9] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, (CH3COO)2·Co 4H2O | \nCH3OH | \nMono ethanolamine (CH2(OH)·CH2·NH2) | \nDhruvash et al. [10] | \nSol‐gel | \n
Zn(CH3COO)2 2H2O | \nC2H5OH | \n– | \nSingh et al. [21] | \nSol‐gel | \n
Zn(CH3COO)2 2H2O/KOH | \nCH3OH | \n– | \nKim et al. [22] | \nSol‐gel | \n
Zn(CH3COO)2·2H2O | \n2‐methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nTabassum et al. [11] | \nSol‐gel | \n
Zn(CH3COO)2·2H2O/Al(NO3)3 9H2O/AgNO3 | \nC2H5OH | \nDiethanolamine (DEA) | \nKhan et al [12] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, NaCl | \nCH3OCH2CH2OH | \n(CH2(OH)·CH2·NH2) | \nZhou et al. [30] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \nIsopropyl alcohol | \n(CH2(OH)·CH2·NH2) | \nChebil et al. [23] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Cu(CH3COO)2 | \n……. | \nDiethanolamine (DEA) | \nAgarwal et al. [14] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \n2‐methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nHaarindraprasad et al. [24] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \nDimethyl formamide | \nDiethanolamine (DEA) | \nBhunia et al. [25] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, C2H7NO2 | \nDistilled water/glacial acetic acid | \n– | \nPara et al. [26] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Ga(NO3)3 xH2O | \n2‐methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nWang et al [27] | \nSol‐gel | \n
[Zn(CH3OO)2 2H2O | \n2‐methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nAlfaro et al. [28] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, LiOH, graphene | \nC2H5OH/EtOH | \n– | \nLi et al. [29] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Mg(CH3COO)2 4H2O, Al(NO3)3 9H2O) | \nIsopropyl alcohol | \nDiethanolamine (DEA) | \nDas et al. [13] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \n1‐butanol | \n(CH2(OH)·CH2·NH2) | \nDemes et al. [31] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, SnCl2.2H2O | \nEthanol and chelating with glycerin | \nAcetic acid | \nKose et al. [32] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Li(CH3‐COO)2.2H2O,Co(CH3COO)2.2H2O | \n(C2H5OH) | \n(C2H6O2) | \nBashir et al. [15] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \nEthanol (C2H5OH) | \n(CH2(OH)·CH2·NH2) | \nAyana et al. [33] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Cu(CO2CH3)2 H2O | \nEthanol (C2H5OH) | \n(CH2(OH)·CH2·NH2) | \nWang et al. [16] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, NaOH | \n2‐Propanol | \n– | \nZimmermann et al. [34] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \nAcetone | \nTEA | \nEfafi et al. [35] | \nSol‐gel | \n
Zinc nitrate hexa hydrate/Na‐CMC | \nDeionized water | \n\n | Muthukrishnan et al [36]. | \nSol‐gel | \n
Zn(NO3)2.6H2O/Bi(NO3)3.5H2O, NaOH | \nDeionized water | \nPEG‐6000 | \nLiu et al. [37] | \nSol‐gel | \n
Ti(OCH(CH3)2)4, Zn(CH3COO)2 2H2O | \nIsopropyl alcohol | \n– | \nBoro et al. [38] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, NH4VO3 | \nCH3OH/MeOH | \n– | \nSlama et al. [17] | \nSol‐gel | \n
ZnCl2, FeCl3, NH4Ac, Zn(CH3OO)2 2H2O | \nC2H6O2 | \n\n | Rabbani et al. [39] | \nSol‐gel | \n
(Zn(CH3COO)2.2H2O)/TiO2 | \nIsopropyl alcohol | \n(CH2(OH)·CH2·NH2) | \nMarimuthu et al. [40] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, Co(NO3)2.6H2O] | \nDouble distilled water | \n[C6H8O7 H2O] | \nBirajdar et al. [18] | \nSol‐gel | \n
Zn(NO3)2, citric acid and tetraethoxysilane | \nEthanol (C2H5OH) | \n– | \nSivakami et al. [41] | \nSol‐gel | \n
Isopropyl orthotitanate (TTIP), zinc nitrate tetra hydrate | \nEthanol (C2H5OH) | \nDiethanolamine (DEA) | \nMoradi et al. [42] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \n2‐Methoxyethanol | \n(CH2(OH)·CH2·NH2) | \nOcaya et al. [43] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O, CoCl2 | \n\n | Polyvinyl alcohol | \nVerma et al. [19] | \nSol‐gel | \n
[Zn(NO3)2 6H2O]/Ga(NO3)3, gelatin | \nDistilled water | \n– | \nKhorsand Zak et al. [20] | \nSol‐gel | \n
Zn(CH3OO)2 2H2O | \nDistilled water/ethanol | \n(CH2(OH)·CH2·NH2) | \nKiani et al. [44] | \nSol‐gel | \n
Precursors and solvents used in the synthesis of ZnO by the sol‐gel process.
Precursor | \nSolvent | \nStabilizing agent | \nReference | \nTechnique | \n
---|---|---|---|---|
Zn(CH3OO)2 2H2O, sulfo propyl methacrylatepotassium | \nEthylene glycol | \n– | \nLiua et al. [45] | \nColloidal | \n
Zn(CH3OO)2 2H2O | \nDistilled water | \nPoly(vinyl alcohol) (PVA) | \nNagvenkar et al. [46] | \nColloidal | \n
Zn(CH3OO)2 2H2O, LiOH·H2O | \nEthanol (C2H5OH) | \n– | \nYuan et al. [47] | \nColloidal | \n
Zn(CH3OO)2 2H2O, tetraalkylammonium hydroxide | \nDMSO | \nNEt4OH | \nPanasiuk et al. [48] | \nColloidal | \n
Zn(CH3OO)2 2H2O | \nEthanol | \nTriethylamine, diethylamine | \nGupta et al. [49] | \nColloidal | \n
(Zn(NO3)2 6H2O), NaOH | \nDistilled water | \n1‐Thioglycerol (TG) and 2 mercaptoethanol (ME) | \nHodlur et al. [50] | \nColloidal | \n
Zn(CH3OO)2 2H2O | \nDeionized water | \nHexamethyl netetramine | \nGuo et al. [56] | \nColloidal | \n
Zn(CH3OO)2 2H2O, KOH | \nMethanol | \n– | \nRahman [51] | \nColloidal | \n
Zn(CH3OO)2 2H2O, KOH | \nMethanol | \nPVP | \nGutul et al. [52] | \nColloidal | \n
Zn(CH3OO)2 2H2O, KOH | \nEthanol | \n3‐aminopropyltriethoxysilane | \nMoghaddam et al. [53] | \nColloidal | \n
Zn(CH3OO)2 2H2O, NaOH | \nEthyl alcohol | \n– | \nLiu et al. [54] | \nColloidal | \n
Zn(CH3OO)2 2H2O | \nDiethylene glycol. | \n– | \nXie et al. [60] | \nColloidal | \n
Zn(CH3OO)2 2H2O | \nEthanol | \nLiOH | \nVerma et al. [61] | \nColloidal | \n
Zn(CH3OO)2 2H2O, NaOH | \n2‐propanol | \n– | \nMoghaddam et al. [64] | \nMicrowave | \n
GO, Zn(NO3)2, NaOH | \nDeionized water | \n– | \nTian et al. [65] | \nMicrowave | \n
Zn(CH3OO)2 2H2O, NaOH | \nDistilled water | \nGuanidinium carbonate, acetyl acetone, | \nHamedani et al. [66] | \nMicrowave | \n
Zinc hydroxide | \nDistilled water | \nCetyltrimethylammonium bromide | \nRai et al. [67] | \nMicrowave | \n
Zn(CH3OO)2 2H2O, NaOH, NH4OH | \nDieonized water | \n– | \nYanga et al. [69] | \nMicrowave | \n
(Zn(NO3)2.6H2O), hydrazine hydrate | \nDistilled water | \n– | \nKrishnakumar et al. [70] | \nMicrowave | \n
ZnSO4·7H2O, GO, NaOH | \nDistilled water | \n– | \nLua et al. [71] | \nMicrowave | \n
Zn(CH3OO)2 2H2O | \nDeionized water | \n– | \nZhu et al. [72] | \nMicrowave | \n
ZnSO4, NaOH | \nDeionized water | \n– | \nLiu et al. [73] | \nMicrowave | \n
Zn(NO3)2 | \nDeionized water | \n– | \nRassaeia et al. [74] | \nMicrowave | \n
Zinc oxide, ammonium hydroxide | \nDeionized water | \n– | \nLu et al. [75] | \nMicrowave | \n
ZnSO4, NaOH | \nDeionized water | \n– | \nLimaye et al. [76] | \nMicrowave | \n
Zinc acetylacetonate monohydrate | \nWater | \nEthoxyethanol, ethoxyethanol, and n‐butoxyethanol | \nSchneider et al. [77] | \nMicrowave | \n
Precursors and solvents used in the synthesis of ZnO by colloidal/microwave synthesis.
Various morphologies of ZnO can be obtained from the sol‐gel process including nanorods [3], inhomogeneous films [4, 5], inhomogeneous nanoparticles [6] and nanocomposites [7].
\nThe structural effects of cation doping on ZnO nanoparticles was investigated in several studies. When doped with lithium, it was found that the concentration of Li+ ion substitution for Zn2+ directly affected the XRD intensity of the (002) plane, but did not affect the grain size or crystallinity of the nanoparticles [8]. When ZnO was doped with Ca2+ ions, the average particle size was increased to 40–90 nm which could be attributed to the larger ionic radius of Ca2+ that substituted for Zn2+ ion sites [9]. Likewise, the average grain size reduced when a small radius ion is substituted for Zn2+ (0.74 Å) in the hexagonal wurtzite structure such as Co2+ (0.58 Å) [10]. Doping with Al3+ ions also showed the same tendency in reducing particle size, however, impurity phases such as Al2O3 and ZnAl2O4 were also observed [11]. Additionally, co‐doping of ZnO with Ag+ and Al3+ ions showed the formation of crystal defects due to the difference in ionic radius between Ag+, Al3+ and Zn2+. Crystallinity improved proportionally with increased Ag+ doping concentration, however, lattice defects and dislocations increased with Al3+ substitution [12]. Further dopant studies also demonstrated that limited dopant precursor solubility provoked a random distribution of dopant throughout the product [13]. Most research about doping ZnO has resulted in improved optical and electrical properties due to improved morphology or intrinsic material properties [14–20].
\nSynthesis of ZnO of different morphologies without doping is also important to consider since product morphology alone can affect device properties. Without any dopant ZnO can be obtained under normal laboratory conditions with well‐aligned nanorods, agglomerated nanoparticles and inhomogeneous thin films composed of nanoparticles, quantum dots, nano‐wires, spheres or nano‐cubes [21–44].
\nColloidal synthesis technique can be utilized to obtain nanocomposites of ZnO and other materials. Nano‐sheets of poly (styrene‐methyl methacrylate‐sulfopropyl methacrylate potassium)/ZnO nanocomposites were obtained by Liua et al. [45]. Dissolving ZnO in other materials can result in a great combination and co‐application of materials such as ZnO/PVA (Polyvinyl alcohol) [46]. The same process was done to produce ZnO/TiO2 multilayer thin films [47]. This technique allows obtaining well size‐controlled nanoparticles such as those reported with use of dimethyl sulfoxide, but the author reports that the solvent and post‐annealing treatment are also important factors in the crystallization process and average particle size [48].
\nSeveral authors have reported that the product morphology can be altered between flakes, hexagons, particles and flower‐like morphologies by adding different surfactant material [49]. Agglomeration of ZnO nanoparticles was reduced by adding capping agents to different thiol molecules during synthesis [50]. It was demonstrated that the colloidal stability of nanoparticles can be maintained after dispersion in monoethanolamine (MEA). Also, hybrid structures can be obtained through this method like ZnO‐Au reported recently [51]. Dispersion of nanomaterials could also be maintained through an additive such as poly (N‐vinylpyrrolidone) which has been shown to maintain colloidal stability for more than a couple of months [52]. In the same way agglomeration of ZnO quantum dots can be prevented through a capping agent such as 3‐aminopropyltriethoxysilane in order to maintain their quantum properties [53]. Stabilization of the colloidal particles ensures that particle size and shape does not change with time allowing for more repetitive results for each batch of material. Stable colloidal solutions have also been used to grow novel nanostructures on several kinds of unique substrates such as wood that can allow for new ecological applications in future [54–63].
\nColloidal and sol‐gel processing are both chemical techniques that can be used to easily obtain different nanomaterials; similarly, microwave‐assisted synthesis can obtain similar products but has been explored very little. In microwave‐assisted synthesis, most reactions take place in a short amount of time and have resulted in the synthesis of good ZnO nanostructures. The technique has obtained spherical nanoparticles that are stable in solution for up to 50 days, and can be deposited several times on a substrate without any change in its morphology. Similarly, it is possible to obtain composites such as ZnO‐nanoparticles on reduced graphene oxide. Also, the morphology is highly dependent on the complexing agent where the reaction takes place or if a dopant is added, such as that reported for obtaining ZnO nanoflowers, nanorods and nanoparticles. Additionally, a research group has confirmed the formation of flower‐like to rod‐like nanostructures by changing the system temperature. Other works have also reported about dumbbell‐shaped nanoparticles, nano‐flowers, graphene‐ZnO nanocomposites, straw‐bundle, chrysanthemum and nanorod‐based microspheres obtained under certain temperature conditions. [2, 64–78].
\nThe techniques listed in the above paragraphs remain as the most important chemical solution‐based routes to synthesize ZnO. Within the same processing method, a variety of material morphologies and properties can be obtained by subtle changes in temperature, additives, dopants or other parameters. There has been a wide range of organic and inorganic particles that have been synthesized and applied in different fields through these techniques. Investigating the effects of processing conditions on ZnO nanoparticles is still a hot topic in current research for their applications in optoelectronic and solar cell devices.
\nMycobacterium leprae (M. leprae) is an acid fast bacilli that is the causative agent of leprosy disease which mainly effects the skin and peripheral nerves. In olden times leprosy was common in temperate climates (e.g. Europe), today it is mainly confined to tropical and subtropical regions. Mode of transmission in leprosy is mainly through inhalation of droplets containing the bacteria. But skin contact is also claimed by many leprologists. The disabilities and deformities associated with leprosy due to neuropathy leads to long-term consequences, including. This in turn is associated with stigma.
The immunity of the host plays an important role in disease progress and control. Thus, fortunately 95% of patients exposed to M. leprae will not develop this disease. The variation in incubation period ranges from 2 to 20 years, or even longer.
Leprosy has been successfully eliminated as a public health problem in 2000 globally and at the national level in 113 countries out of 122 by 2005 [1]. Elimination of leprosy is defined by World Health Organization as a point prevalence below 1 per 10,000 population [2]. However, the number of new patients diagnosed with leprosy is still significant, at more than 200,000 in 2016 globally. The new case detection rate of the disease (NCDR) is only slowly declining (Figure 1) [3].
Trend in case detection and case detection rate, by WHO region, 2006–2016 [3].
The long incubation period, silent symptoms, long duration MDT and unavailability of effective vaccine makes this disease difficult to identify, treat and eradicate. To add to the misery the stigma associated with the disease is another challenge. In such circumstances, prevention and control of disease gains utmost importance.
In 2017, 192,713 patients were on treatment globally which makes the prevalence rate of 0.25 per 10,000 population [4]. Total of 210,671 new cases were reported in same year from 150 countries making NCDR of 2.77 per 100,000 population. Figure 2 below shows the trends over the past decade (2008–2017) in new case detection of leprosy cases globally in the reporting countries of World Health Organization (WHO) [4].
Country-wise trends of detection of new leprosy cases from 2008 to 2017 [4].
The three main goals of control of leprosy are
To detect the pathology early and treat the patient completely.
To prevent the transmission to the others.
To prevent the disabilities and other complications.
Thus the following modalities are adopted to control leprosy:
Medical measures
Social support
Program management
Evaluation
The control of leprosy starts with the estimation of size and magnitude of the problem. Most common epidemiological survey method of collection of data is “Quick random sample survey.” Information about the prevalence of leprosy, age and sex-wise distribution, various forms of leprosy and the health facilities available should be gathered. Roughly the total prevalence of leprosy in an area would be about 4 times that of the cases found among school children [5, 6]. These estimates are essential to plan, implement and to evaluate the results of the control program.
The objective is to detect all the cases as early as possible and to register them. Active case finding is important as the disease is symptomless in the early stages. Cases can be detected by the Contact surveys, Group surveys and Mass surveys. Contact surveys consists of examination of all household contacts with a lepromatous case, particularly children, in areas with prevalence less than 1 per 1000. Contact surveillance of households is recommended for a minimum period of 10 years after case is declared bacteriologically negative, and for 5 years in households with a non-lepromatous case from the time of diagnosis of the index case. Group surveys are done in areas where prevalence of leprosy is more than 1 in 1000 population. This consists of screening certain groups such as school children, slum dwellers, military recruits, industrial workers, etc. through “Skin camps.” Lastly, mass surveys consists of examination of each and every individual by house-to-house visits in hyperendemic areas (prevalence – 10 or more per 1000 population). These are generally carried out by repeated annual examinations of school children which yield better results at relatively low cost [5, 6]. The data of each case is entered in the standardized proforma developed by WHO.
Since an effective vaccine is unavailable for leprosy the secondary prevention (early treatment) becomes more important. Until 1981, Dapsone (Diamino Diphenyl Sulphone—DDS) was used to treat leprosy which resulted in the development of resistance and relapse, making leprosy control difficult.
Multidrug Therapy: In 1982, WHO recommended Multidrug Therapy (MDT) for all leprosy patients. Introduction of MDT has opened a new avenue in the control of leprosy in the world. Aim of MDT is to convert the infectious case into noninfectious as soon as possible, so as to reduce the reservoir of infection in the community.
The main objectives of MDT are:
To ensure early detection of the cases.
To interrupt the transmission of infection.
To prevent drug resistance, relapse and reaction.
The advantages of MDT over dapsone monotherapy are:
Shorter duration of treatment,
Better patient compliance,
High cure rate,
Cost-effectiveness and
Ease in health delivery system.
There are two types of MDT regimens used depending on the symptoms and signs shown by the patients - Paucibacillary (PB) and Multibacillary (MB). Recommended Regimens are discussed below [3, 5, 6, 7]:
i. Multibacillary leprosy:
MDT is recommended for following groups of patients:
All smear positive cases.
Skin lesions more than five in number.
More than one nerve trunk thickening.
All cases of relapse/reactivation and all cases who have been treated with Dapsone monotherapy earlier.
The drugs used in Multibacillary MDT and dosages are:
Rifampicin: 600 mg once monthly, supervised.
Dapsone: 100 mg daily, self administered.
Clofazimine: 300 mg once monthly, supervised and 50 mg daily, self administered.
Duration of treatment for Multibacillary leprosy is 12 months, can be extended to 18 months and continued where possible up to smear negativity. Sometimes LL/BL patients with high bacilli may need 2–3 years or more of MDT for achieving bacteriological negativity.
ii. Paucibacillary leprosy:
The drugs and dose schedule is:
Rifampicin 600 mg once a month for 6 months supervised.
Dapsone 100 mg daily for 6 months self administered.
Paucibacillary leprosy is treated for 6 months.
MDT is not contraindicated in patients with HIV infection.
Each MDT blister pack contains tablets for 4 weeks treatment. For easy identification color coding of the blister pack is done, that is, with different colors for multibacillary and paucibacillary cases both in adults and children.
The treatment in both PB and MB cases varies depending on the age of the patient. The patients between 10 to 14 years are treated as paediatric cases, while >14 years are considered adult. The standard treatment regimen for MB leprosy in adults is given for 12 months. The drugs in each blister pack are (Figure 3):
Two capsules of Rifampicin of 300 mg (600 mg once a month) to be taken as single dose under supervision.
Clofazimine 3 capsules of 100 mg each to be consumed once a month as single dose under supervision and 50 mg daily for next 28 days.
Dapsone 100 mg as single dose and then daily once for 1 month.
MDT for adult MB type of leprosy [2, 7].
The standard adult treatment regimen for PB leprosy is (Figure 4):
Rifampicin: 600 mg once a month.
Dapsone: 100 mg daily.
Duration: 6 months (6 blister packs of 28 days each).
MDT for adult PB type of leprosy [2, 7].
Treatment regimen for MB leprosy in children (ages 10–14 years) is (Figure 5):
Rifampicin: 450 mg once a month.
Clofazimine: 150 mg once a month, and 50 mg every other day.
Dapsone: 50 mg daily.
Duration: 12 months (12 blister packs of 28 days each).
MDT for pediatric MB type of leprosy [2, 7].
Treatment regimen for PB leprosy in children (ages 10–14 years) is (Figure 6):
Rifampicin: 450 mg once a month.
Dapsone: 50 mg daily.
Duration: 6 months (6 blister packs of 28 days each).
MDT for pediatric PB type of leprosy [2, 7].
MDT is provided free-of-charge globally through an agreement between a pharmaceutical company and WHO. WHO manages distribution of MDT to countries in coordination with national leprosy programs.
Clinical surveillance of the patients after completion of treatment is an important part of MDT to ensure complete cure. For paucibacillary cases follow up for at least once a year for 2 years after completion of treatment and for multibacillary cases at least once a year for 5 years [3, 4, 5].
Early diagnosis of cases, aggressive treatment and proactive measures to avoid complications and disabilities is the backbone for the success of any comprehensive program. In addition to accurate reporting and control measures, effective preventions will be needed to achieve elimination. Search for an effective vaccine either to be used alone or in combination with a drug has been going for a long time.
Presently BCG (Bacillus Calmette-Guerin) is the only vaccine that has shown some protection against M. leprae bacillus. A single dose of BCG gives 50 percent or higher protection against the disease. It is the most widely used vaccine in the world, yet the degree of protection it confers is not yet confirmed. The meta-analysis of many experimental studies concludes that the vaccine gives approximately 26% protection against leprosy. But the protection level decreases with time. To overcome this problem more than one dose of vaccine is advised.
Other variants of vaccination are also suggested.
Adding killed M. leprae to BCG: Various modifications have been suggested, such as the addition of killed M. leprae to BCG. This method almost doubles the vaccine efficacy in some populations as concluded by few studies. But the same cannot be said for patients below 15 years.
Vaccination with M. indicus pranii (Mycobacterium W): This strain discovered in India. Testing of the MIP vaccine took place in 2005 and showed that it was effective for seven to 8 years, after which a booster dose would be needed to maintain the immunity. Recently the vaccine was approved by the Drug Controller General of India to be rolled out in a project involving five districts in the states of Bihar and Gujarat, where there are high rates of leprosy. Leprosy patients and their close contacts will benefit from this project, making India the first country in the world to have a large-scale leprosy vaccination initiative [8].
Another milestone in prevention of leprosy is the discovery of the vaccine candidate, called LepVax. Scientists at Infectious Disease Research Institute (IDRI), along with national and international collaborators including the National Hansen’s Disease Program and the National Institute of Allergy and Infectious Diseases (NIAID), part of the National Institutes of Health, with financial support from American Leprosy Missions, have developed this leprosy vaccine. Based on the preclinical studies, the LepVax, has progressed to Phase I clinical testing in the United States, the first stage of safety testing in human volunteers. The clinical trial is focused not only on safety but also evaluates the immune response of the individual to the vaccine.
Indian cancer research center (ICRC) bacilli: Another variant belonging to the M. avium intracellulare group, the ICRC bacilli are thought to induce lepromin conversion in lepromatous leprosy patients and in lepromin-negative leprosy-free individuals. Its efficacy was reported to be 65.5 percent [8].
M. vaccae: The studies with this soil-dwelling mycobacterial species combined with BCG showed to provide greater protection against leprosy, but a Vietnamese trial contradicted the results [8].
M. Habana: This bacilli has been reported to induce lepromin conversion when used as a live vaccine in monkeys, and protected mice against the development of leprosy [8].
Chemoprophylaxis alone provides two-year protective window while effective immunization will provide a much broader protective window. Thus many studies and research is going on to provide both chemoprophylaxis and immunization for immediate and short-term protection and longer-term protection respectively. This strategy could have better impact and distinct appeal in controlling and preventing leprosy. Such trials could also provide a gateway for the assessment and implementation of new emerging vaccines (Figure 7).
Locations of leprosy vaccine testing.
Chemoprohylaxis using effective antibiotics focuses on providing protection to people at risk such as close contacts – family members, neighbors, co-workers, health care providers for lepers etc. Due to the stigma of disease the leprosy cases are found in clusters in all endemic regions, rather than being evenly dispersed over the whole area. Thus these high risk people can be identified and prophylaxis provided along with secondary prevention strategies. The process includes focused surveillance, contact tracing, early diagnosis and treatment. This helps in reducing the incidence and breaking the chain of transmission.
Chemoprophylaxis, as recommended by WHO Guideline Development Group (GDG), is done using single dose rifampicin (SDR) for contacts of leprosy patients both in adults and children of 2 years of age and above. Before starting the drug leprosy and TB disease are to be excluded. There should be no contraindications also for the use of rifampicin.
Other important considerations for the implementation of this chemoprophylaxis by programs are:
Adequate management of contacts.
Consent of the index case to disclose his/her disease.
An RCT found that SDR reduces risk of leprosy over 5–6 years in leprosy contacts. For every 1000 contacts treated with SDR, there were four leprosy cases prevented after 1–2 years and three cases prevented after 5–6 years.
Recommended dosage schedules for SDR are given in Table 1.
Age/weight | Rifampicin single dose |
---|---|
Adults (≥15 years) | 600 mg |
10–14 years | 450 mg |
Children 6–9 years (weight ≥ 20 kg) | 300 mg |
Children <20 kg (≥2 years) | 10–15 mg/kg |
Rifampicin dose for chemoprophylaxis [3].
The limitations of this approach are:
The protection is approximately for only 2 years.
High bacillary load cannot be eliminated using single dose.
Specific screening test needed to distinguish between contacts with high and low bacillary load.
Among communicable diseases, leprosy remains a leading cause of peripheral neuropathy and disability in the world, despite extensive efforts to reduce the disease burden. It is an important aspect of leprosy control. It means the medical, surgical, social, educational, and vocational restoration as far as possible of treated patients to normal activity so that they resume their place in the home, in society and industry [5, 6, 7]. Early treatment helps in disability limitation.
Rehabilitation: WHO has defined rehabilitation as “the combined and coordinated use of medical, social, educational and vocational measures for training and retraining the individual to the highest possible level of functional ability.”
Preventive rehabilitation consists of prevention of development of disabilities in a leprosy patient by early diagnosis and prompt treatment. But once the patient becomes handicapped and suffers from the damage caused, should be trained and retrained to the maximum functional ability so that the patient becomes useful to self, to the family and to community at large by various measures such as medical (physical), surgical, psychological, vocational and social rehabilitation (Flow chart 20.10).
Health education is given to the patient, to the family and to the community at large about leprosy. The education should be directed to ensure general public and patients help them develop their own actions and efforts to change the perception about the disease and seeking professional help whenever required. Early recognition of symptoms, prompt diagnosis, health seeking behavior, personal care, treatment adherence and rehabilitation are important aspects of health education. The key messages included are about the cause of disease and the complete cure available to encourage people for early diagnosis and treatment. It also aims at helping people to change their attitude and behavior by removing the misunderstandings and misconceptions. Mass Health education also helps to eradicate social stigma, social ostracism and social prejudice associated with leprosy which is the biggest hindrance for the eradication of disease.
The complications of the disease cause disfigurement and disabilities which in turn gives way to the stigma and strong discrimination of these patients. This results not only in physical and social isolation also financial dependency, ultimately forcing the leprosy patients to beg on streets for their survival. To address this issue WHO introduced the strategy of community-based rehabilitation (CBR). This intended to enhance the quality of life for lepers with disabilities through community initiatives. Community participation and using local resources to support the rehabilitation of people with disabilities within their own communities is the foundation of this concept [9, 10].
“Enhanced Global Strategy for Further Reducing the Disease Burden due to Leprosy for 2011–2015” was launched in 2009 by the World Health Organization. The target of the program was to reduce Grade 2 Disability rate (G2DR) in leprosy patients by at least 35% by the end of 2015 (G2DR is the number of new cases with grade 2 disability per 100,000 population). Since the elimination of leprosy in 2005, the prevalence is very less and thus G2DR has been proposed as an indicator. The advantage of G2DR as indicator is that, it is less susceptible to operational factors such as detection delay and is a more robust marker for mapping cases of leprosy in any country. This will also help the program implementers to focus on interventions that reduce visible deformities by enhancing early detection and treatment of leprosy patients and ultimately reduce the number of new leprosy cases in the population. However by the end of 2015, only Thailand was able to achieve this target [11].
In 2016, WHO launched the “Global Leprosy Strategy 2016–2020: Accelerating towards a leprosy-free world” [9].
The program aims to reinvigorate efforts to control leprosy and avert disabilities, especially among children still affected by the disease in endemic countries.
The strategy is built around three major pillars:
Strengthen government ownership and partnerships;
Stop leprosy and its complications; and
Stop discrimination and promote inclusion.
The strategy of this program is:
To sustain expertise and increase the number of skilled leprosy staff;
To improve the participation of affected persons in leprosy services;
To reduce visible deformities and stigma associated with the disease;
To call for renewed political commitment and enhanced coordination among partners;
To highlight the importance of research and improved data collection and analysis.
The key interventions needed to achieve these targets include:
Early case detection especially in children before visible disabilities occur thus reduce transmission;
In highly endemic areas or communities detection of disease among higher risk groups through campaigns;
Improving health care coverage and access for marginalized populations such as poor patients, patients in the difficult to reach areas and the areas of conflicts.
Customization of the strategic interventions in endemic countries is permitted to suit the national plans to meet the new targets. E.g. Screening all close contacts of persons affected by leprosy; initiating a shorter and uniform treatment regimen; and incorporating specific interventions against stigmatization and discrimination.
Its ultimate goal of this program is to further reduce the global and local leprosy burden, that is, (a) zero disabilities in children with leprosy-affected, (b) G2DR less than one per million population and (c) repeal of laws that discriminate leprosy patients of their rights.
Author declares no conflict of interest.
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