Examples of reduction reactions that can be used to synthesize borides and carbides [7].
\r\n\t
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Since he graduated he has published several peer-reviewed papers at the national and international levels and he has been a guest researcher and lecturer both at Michigan State University (USA) and at the University of Toronto (Canada) where he has developed part of his Ph.D. research with the Financial support from the Portuguese Foundation for Science and Technology (Ph.D. grant).",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"108118",title:"Dr.",name:"Luis",middleName:null,surname:"Loures",slug:"luis-loures",fullName:"Luis Loures",profilePictureURL:"https://mts.intechopen.com/storage/users/108118/images/system/108118.png",biography:"Luís Loures is a Landscape Architect and Agronomic Engineer, Vice-President of the Polytechnic Institute of Portalegre, who holds a Ph.D. in Planning and a Post-Doc in Agronomy. 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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:"54498",title:"Preparation of Ultra-High Temperature Ceramics–Based Materials by Sol-Gel Routes",doi:"10.5772/67783",slug:"preparation-of-ultra-high-temperature-ceramics-based-materials-by-sol-gel-routes",body:'Temperature at 3000°C is not just hot, but it is extremely hot. It is just a baseline in the world of extreme environment engineering. Very few materials can meet this criterion due to the facts that most of the materials have already melted or decomposed below this temperature. Materials with melting temperatures above 3000°C are very limited, which are shown in Figure 1 [1–4]. The borides, carbides, and nitrides of group IV and V elements have melting temperatures above 3000°C and are considered as ultra‐high temperature ceramics (UHTCs), such as zirconium diboride (ZrB2), hafnium diboride (HfB2), tantalum diboride (TaB2), zirconium carbide (ZrC), hafnium carbide (HfC), tantalum carbide (TaC), and hafnium nitride (HfN) [1].
A comparison of the melting temperatures of the most refractory members of several classes of materials.
Recent interest in UHTCs has been motivated by the search for materials that can withstand extreme environments, such as extreme temperature, chemically aggressive environments, and rapid heating/cooling, etc. [5, 6]. Due to the combination of series of excellent physical and chemical properties, such as high hardness, good high temperature stability, and excellent solid‐phase stability, UHTCs are considered as promising candidates for a variety of high‐temperature structural applications, including engines, hypersonic vehicles, plasma arc electrode, cutting tools, furnace elements, and high temperature shielding. However, owing to the strong covalent bond and relatively low volume diffusion coefficient, UHTCs are difficult to get successfully sintered. Densification of these materials is typically performed by hot pressing and spark plasma sintering with or without sintering aids.
UHTCs can be synthesized by a variety of routes, which can be divided into solid phase protocols and solution based protocols based on the state of the starting materials [7, 8]. Among the solid‐phase protocols, transition metal oxides, carbon black, boron oxide, and boron carbide are commonly used as the starting materials. After ball‐milling and high temperature carbothermal reduction, the mixtures are converted into UHTC powders. Examples of the reactions used to synthesize borides and carbides are listed in Table 1 [7]. These reactions are written for ZrB2 and ZrC, but analogous processes produce other borides and carbides. These solid phase protocols are very straightforward and simple and are used to produce UHTC powders commercially. However, due to the heterogeneity of the reactants, the reactions need to be performed at high temperatures for several hours to complete. Also, those synthesized UHTC powders are micron‐sized particles.
Reactions | Category | Example |
---|---|---|
1 | Carbothermal | ZrO2 + 3C→ZrC + 2CO(1) |
2 | Carbothermal | ZrO2 + B2O3 + 5C→ZrB2 + 5CO(2) |
3 | Borothermal | ZrO2 + 4B →ZrB2 + B2O2(3) |
4 | Boron carbide | 7ZrO2 + 5B4C→7ZrB2 + 3B2O3 + 5CO(4) |
5 | Combined | 2ZrO2 + B4C + 3C→2ZrB2 + 4CO(5) |
Examples of reduction reactions that can be used to synthesize borides and carbides [7].
In solution‐based protocols, soluble transition metal containing precursors, boron precursors, and carbon sources are used as the raw materials to form homogeneous sols/solutions or polymers [8–10]. These sols/solutions or polymers can be converted into UHTC materials after hydrolysis, curing/drying, and pyrolysis at high temperatures. Actually, the formation of UHTCs via solution‐based protocols is still based on the carbothermal or borothermal reactions of metal oxides with carbon. However, due to the homogeneous distribution of all the reactants at the molecular level, the following high temperature reduction reactions can proceed at much lower temperature and fine UHTC powders with particle sizes down to few hundred nanometers can be synthesized. Not only granular UHTC particles but also some other UHTC materials with different morphology can be synthesized through these solution‐based routes.
A sol‐gel technique is one of the solution‐based processes, which enables processing of ceramics at low temperature in various desirable shapes, such as monoliths, films, fibers, or nanosized powders, as shown in Figure 2 [11, 12]. Typically, the sol‐gel technique involves the hydrolysis, condensation of the metal organic and/or metal inorganic compounds, gelation, and the posttreatment of the dried gels to obtain final ceramic products. Small molecular compounds are used as the starting materials in sol‐gel routes. The homogeneity of the starting compounds at molecular level facilitates the preparation of these materials at relatively low temperatures via the sol‐gel technique. The sol‐gel route is an old but an efficient way to produce high quality, fine UHTC powders under moderate conditions compared with other solution‐based protocols [8, 10, 13]. Combined with various shaping techniques, UHTC‐based materials in various desirable shapes, such as nanopowders, nanofibers, and porous ceramics can be prepared from similar starting materials and simple reactive processes via the sol‐gel technique [8, 14–16].
Simplified chart of sol‐gel processes [12].
In this chapter, we will present recent works covering the synthesis of nanopowders, nanofibers, and porous ceramics of UHTC‐based materials via sol‐gel routes. The discussions mainly focus on the synthesis of ZrC‐ and ZrB2‐based materials, but analogous processes produce other borides and carbides. Meanwhile, numbers of publications discussing the utilization of UHTC sols to prepare fiber‐reinforced ceramic composites via polymer infiltration pyrolysis routes will not be discussed here.
It is very straightforward and simple for the researchers to apply a sol‐gel technique to prepare UHTC nanopowders. It seems simple to obtain the sols of the target materials by mixing the precursors of a transition metal with a carbon source and a boron source in liquid state. On drying and after high temperature ceramization, the UHTC nanopowders can be prepared [8, 10]. However, it is not always easy to get homogeneous precursor sols of UHTC materials without considering the chemical compatibility and stability of the precursors.
Generally, transition metal alkoxides, oxychloride, and chloride are used as the starting metal oxide precursors. Bidentate ligands, such as β‐diketones, acetic acid, and cellulose acetate, are used to modify the high reactivity of the metal alkoxide allowing a slow‐down of the system\'s reactivity [17, 18]. The chemically modified metal alkoxide undergoes hydrolysis and condensation in a controlled manner to form preceramics, as illustrated in Eq. (6) [17].
Polyzirconoxane (PZO) can be synthesized by chelation of acetyl acetone to zirconium oxychloride and is widely used as the powdery and soluble zirconia precursor [19, 20]. The synthesis process of PZO is shown in Eq. (7) [20]. It is also possible for the synthesis of powdery preceramic polymers for ZrC through reactions of zirconium oxychloride with acetyl acetone and salicyl alcohol in a one‐pot reaction procedure according to Eq. (8) [21]. The preceramic polymers can be converted into ZrC nanopowders after the high temperature treatment.
While sucrose, phenolic resin, and polyacrylonitrile are used as the carbon source; boron‐containing compounds (e.g., boric acid and triethyl borate) are usually used as the boron source to synthesize metal borides. By mixing the modified metal precursors with carbon and boron sources in controlled molar ratios, the precursor sols for UHTC are prepared.
UHTC nanopowders can be synthesized by directly heating the dried gels in an inert atmosphere. By controlling the composition of the starting sols, unary UHTC nanopowders (e.g., ZrC, HfC, ZrB2, and HfB2) and composite nanopowders (e.g., ZrC‐SiC, ZrB2‐SiC, and ZrB2‐ZrC‐SiC) can be prepared.
Sacks et al. [8] used zirconium and hafnium alkoxides as the metal precursors, acetylacetone as a chemical modifier, and phenolic resin and glycerol as the liquid carbon source. After controlled hydrolysis, condensation and drying of the precursor sol, the dried gel was obtained. The dried gel was heated at temperatures up to 1200–1600°C for carbothermal reduction reaction (Eq. (1)). During heating process, the organic components decompose and leave the fine‐scale mixed metal oxide and amorphous carbon. The carbothermal reduction reaction begins at 1200°C is demonstrated by the appearance of ZrC diffraction peaks in the pyrolyzed products, as shown in Figure 3a. The carbothermal reduction reaction is completed after heat treatment at 1400°C for 2 h. After heated at 1475°C, the average crystallite size of the ZrC nanoparticles is 100 nm. The oxygen content within ZrC nanopowders decreases with the increasing heating temperatures, from 3.3 wt% at 1475°C to 0.1 wt% at 1800°C. The ZrC nanopowders show good sinterability and can reach 98% of relative density after sintering at 1900°C with no pressure, as shown in Figure 3b.
(a) X‐ray diffraction patterns for heat treated samples prepared from a (zirconium n‐propoxide/phenolic resin)‐based sol. (b) Plots of relative density and bulk density versus sintering temperature for dry‐pressed ZrC powder compacts [8].
High pyrolyzing temperatures are effective to synthesize metal carbide nanopowders with low impurity content. However, it causes the increase of the average crystallite size of the products. Dollé et al. [10] developed a two‐step heat treatment approach to realize the purification of ZrC nanopowders with no significant increase in the average crystallite size by using metal alkoxide, sucrose, and acetic acid as the staring materials. Only diffraction peaks of ZrC can be observed when the precursor was heated at 1400°C for 3 h in argon. Only a slight shift of the peaks to the low angles with the increase of heating temperatures indicated an increase in the lattice parameter with temperature. The average crystallite sizes increase from 93 to 150 nm with the temperatures increase from 1400 to 1600°C. During the two‐step heat treatment process, the precursor was first heated at 1400°C for 150 min and then at 1800°C for 6 min maintaining the heating rate at 20°C/min. The average crystallite size came out to be 110 nm, a slight increase as compared to the one heated at 1400°C (Figure 4).
(a) Evolution of the XRD patterns of the different samples as a function of their respective heat treatment under argon flow. (b) SEM image of an agglomerate microstructure of a sample heat treated at 1600°C for 3 h. (c) SEM image of an agglomerate microstructure of a sample heat treated at 1400°C for 150 min then at 1800°C for 6 min [10].
Tao et al. [21] developed a preceramic route to synthesize ZrC nanopowders by using zirconium oxychloride, acetylacetone, and salicyl alcohol as the raw materials (Eq. (8)). ZrC nanopowders can be prepared by directly heating the powdery precursor in argon. Only diffraction peaks of ZrC can be detected when the precursor was pyrolyzed at 1300°C for 2 h (Figure 5a). Such low temperature indicated a fine contact between the metal precursor and the carbon precursor. Disadvantage of the technique is the presence of the residual carbon in the final ZrC products, as can be observed in Figure 5b. ZrC nanoparticles seem embedded in the matrix of amorphous carbon. This might be ascribed to the reason that it is not easy to control the degree of the polymerization during the synthesis process.
(a) XRD patterns of the ceramic products obtained at different temperatures. (b) TEM image of the ZrC powders pyrolyzed at 1300°C for 2 h [21].
Boric acid is the commonly used boron source for the synthesis of metal diboride nanopowders via sol‐gel routes. Li et al. [22, 23] prepared ZrB2 nanopowders by using zirconium n‐propoxide as the zirconia source, sucrose as the carbon source, and boric acid as the boron source. By mixing the acetylacetone‐modified zirconium n‐propoxide with methanol solution of boric acid and sucrose, the precursor sol was obtained. ZrB2 nanopowder was obtained by heating the dried gels at high temperatures in an inert atmosphere (Eq. (2)). The B/Zr molar ratio plays a significant role in the formation of pure ZrB2 during the carbothermal reduction reaction. Boron loss due to the high vapor pressure of boron oxide at high temperature must be compensated during the high temperature carbothermal reduction. Pure ZrB2 nanopowders with particle sizes down to 100 nm can be prepared by tailoring the composition of the starting precursor sols (a B/Zr molar ratio of 2.3) and heat treatment temperature (1550°C) (Figure 6). Rod‐like structure can also be synthesized by controlling the gelation temperature of the precursor sols.
(a) XRD patterns of precursor and precursors pyrolyzed at various temperatures for B/Zr = 2.3. From bottom to top, precursor, 1100, 1300, 1400, 1550°C [22]. (b) XRD patterns of precursors pyrolyzed at 1550°C for 2 h with molar ratios of B/Zr 2.0 (bottom) and 2.3 (top) [22]. (c) SEM image of ZrB2 nanoparticles pyrolyzed at 1550°C for 2 h with B/Zr = 2.3. The scale bar in the SEM is 100 nm [22]. (d) SEM image of ZrB2 nanoparticles pyrolyzed at 1550°C for 2 h with a gelation temperature of 85°C [23].
Walker and Corral [24] applied the metal oxychloride hydrates, triethyl borate, and phenolic resin as the starting materials to synthesize HfB2 and ZrB2, as shown in Figure 7. The starting materials were mixed by high‐energy ultrasonication to form precipitate‐free sols which turn into stable gels without any addition of catalysts. They pointed out that the conversion process to ZrB2 involved the formation of ZrC subsequently reacting with boron oxide to form ZrB2. Both HfB2 and ZrB2 prepared by optimizing the chemistry, processing, and heat treatment conditions can result in the desired final ceramic products.
SEM images of heat‐treated (a) HfB2 and (b) ZrB2 precursor with fine spherical particle morphology and extreme localized particle growth for (c) HfB2 and (d) ZrB2 that forms rod‐like particles within the powder [24].
It is not easy to sinter phase‐pure UHTC materials due to their strong covalent bonds. Sintering aids (e.g., silicon carbide‐SiC) are commonly introduced to the UHTC matrix to improve their sinterability and properties of the corresponding ceramic materials [7]. It is one of the advantages of sol‐gel techniques to obtain homogenous distribution of all reactants at molecular level. Precursors of UHTC‐SiC composite powders can be synthesized by introducing independent precursors of UHTCs and SiC into a solvent (ethanol, toluene, and tetrahydrofuran, etc.) with the liquid precursor itself acting as a mutual solvent. The precursors are dried and cured at relatively low temperatures and then heated at high temperatures to complete the carbothermal reduction reaction to form HTC‐SiC composite powders, such as ZrC‐SiC, ZrB2‐SiC, and HfB2‐SiC, etc. [25–30].
Cai et al. [28] used methylphenyldichlorosilane (MePhSiCl2) as a SiC precursor to react with zirconcene dichloride (Cp2ZrCl2) to form organometallic polymers. ZrC‐SiC composite powders with controlled Zr/Si molar ratios can be synthesized by pyrolyzing the polymers at 1400°C for 2 h. The particles seen in the SEM image are composed of three parts: large grains, the smaller grains, and the black matrix (Figure 8b). It is not easy to precisely control the residue carbon in this reaction system.
(a) XRD patterns of the poly‐yne polymers pyrolyzed at 1400°C and (b) EDS spectra of the ceramic sample from the Zr:Si = 1:1 precursor [28].
Wang et al. [31] prepared ZrC‐SiC hybrid precursors by dissolving acetylacetone‐modified zirconium alkoxide (PZC) into liquid polycarbosilane (LPCS). In their reaction system, LPCS simultaneously played the role of a solvent, carbon source, and silicon source. ZrC‐SiC composite powders with spherical morphology and grain sizes less than 60 nm can be synthesized by heating the hybrid precursors at 1550°C in argon (Figure 9). The constituent of the final ZrC‐SiC composite powders can be controlled by tailoring the mass ratios of LPCS/PZC. The synthesized ZrC‐SiC nanopowders exhibit improved oxidation resistance compare to ZrC nanopowders.
(a) XRD patterns of samples derived from hybrid precursors with various LPCS/PZC mass ratios after pyrolysis at 1550°C in argon and (b) SEM image of the ZrC‐SiC powders derived from a hybrid precursor with LPCS/PZC = 1 in mass ratio [31].
Liang et al. [32] used zirconia sol, tetraethylorthosilicate (TEOS) and sucrose as the independent zirconium‐, silicon‐ and carbon‐containing source. Hybrid sol can be prepared by introducing TEOS and sucrose into zirconia sol. ZrC‐SiC composite powders with controlled constituent are obtained by pyrolyzing the hybrid gels at 1500°C for 1 h in vacuum (Figure 10). It is possible to precisely control both the residue carbon content and SiC content in the final composite powders by using these independent carbon sources and silicon sources as the starting materials. However, no sintering behavior of the as‐synthesized ZrC‐SiC nanopowders is examined.
ZrC‐SiC composite powders with different SiC volume percentage. (a) ZrC‐10 vol% SiC and (b) ZrC‐90 vol% SiC [32].
The sol‐gel technique enables the processing of ceramics in various desirable shapes, such as monoliths, films, fibers, etc. [33]. The viscosity of the liquid precursors of UHTCs can be tuned by condensation polymerization of the sols themselves or by adding viscous polymers into the mixed solution. These viscous precursors can be drawn into fibrous shapes, dried, cured, and heated at high temperatures for the carbothermal reduction reaction to form UHTC ceramic fibers. Combined with different spinning techniques, such as dry spinning and electrospinning, UHTC fibers can be successfully synthesized [16, 17, 34–39].
Hand‐drawing is a simple but effective method to estimate the spinnability of the spinning solution. Fibers are hand‐drawn by extracting a glass rod from the viscous solutions. Spinnability can be estimated by the length of the drawn fibers. Preiss et al. [17] prepared polymeric precursors for carbothermal reactions from the chelate derivatives of zirconium alkoxides in alcohols by reaction with organic compounds having two or more reactive OH groups. These organic groups act as bridging ligands in transesterification and condensation polymerization yielding either spinnable viscous solutions or elastic gels. The spinnability of these polymeric precursors was estimated by hand‐drawing fibers from the solutions. ZrC‐based fibers with a diameter about 20 μm can be obtained by heating the hand‐drawn precursor fibers in an argon atmosphere at 1550°C (Figure 11a and b).
Photograph (a) and SEM, (b) image of ZrC fibers treated at 1550°C [17], (c) XRD patterns of fibrous products obtained by heat treatment at 1500°C in argon and(d) SEM image of ZrC‐SiC fiber with a Si/Zr molar ratio of 0.92 [34].
Hasegawa et al. [34] prepared ZrC‐SiC fibers by using zirconium tetrakis(2,4‐pentanedionate) (ZTP), TEOS, and phenolic resin as raw materials via a hand‐drawing method. The composition of the final ZrC‐SiC fibers can be controlled by tailoring the Si/Zr molar ratios of the starting sols. The preceramic fibers were converted into ZrC or ZrC‐SiC ceramic fibers after pyrolysis at 1500°C for 4 h under argon flow (Figure 11c). The diameter of the as‐prepared ZrC fibers is about 40 μm (Figure 11d).
A continuous dry spinning process was applied to prepare ZrC‐based fibers by Hu et al. [14]. In their works, ZTP and phenolic resin were used as the starting precursors to form a highly viscous mixed sol. Phenolic resin played the role of a carbon source and the spinning aid. ZrC‐based fibers with fine‐diameter (∼20 μm) and relatively smooth surfaces were obtained by dry spinning the mixed sols and heating at 1450°C. The SEM images of the as‐synthesized ZrC fiber show that the fiber has a porous, extremely fine‐grained microstructure (Figure 12).
SEM images of a single ZrC fiber after carbothermal reduction at 1450°C [14].
However, very few studies were reported on the synthesis of UHTC fibers by the dry spinning process due to the brittleness of the ceramic fibers caused by the massive weight loss during carbothermal reduction. The state‐of‐the‐art technique is not mature enough to apply this kind of scalable synthesis process of UHTC‐based fibers.
Electrospinning is a simple and versatile method for generating nanofibers of polymers and ceramics [40, 41]. The typical procedure for the preparation of ceramic nanofibers by electrospinning includes the preparation of precursor solution, the electrospinning of the precursor solution to get inorganic/polymer composite nanofibers, and the postheat treatment to get ceramic nanofibers based on the carbothermal reduction reaction. Generally, high molecular polymers such as polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyacrylonitrile (PAN), and cellulose acetate are used as the spinning aids to facilitate the spinning process. The parameters including applied voltage, flow rate, and working distance influence the microstructure of the final ceramic nanofibers.
Using ZTP as the zirconia source, cellulose acetate as the carbon source and spinning aids, ZrC‐based nanofibers were prepared. ZrC was initially formed at 1400°C and became the major phase at 1600°C. The fibrous structures of the electrospun green nanofibers could be well retained after high temperature ceramization.
Li et al. [39] used PZO as the zirconia source, PAN as the carbon source and spinning aid to synthesize ZrC nanofibers via electrospinning. In their reaction system, a carbon source played significant role in controlling the microstructure of the pyrolyzed ZrC nanofibers. With sucrose used as the extra carbon source in PZO/PAN spinning solution, fine ZrC nanofibers composed of ZrC nanoparticles were obtained after pyrolysis at 1400°C for 2 h (Figure 13b). The as‐synthesized ZrC nanofibers were porous. After sintering, bamboo‐like structures are formed due to Ostwald ripening.
(a) SEM image of ZrC nanofibers heat at 1600°C for 2 h. The spinning solution was prepared from mixing ZTP and phenolic resin with a C/Zr molar ratio of 5.5 [36]. (b) SEM image of ZrC nanofibers after pyrolysis at 1400°C for 2 h under argon flow by using PZO/PAN/sucrose as the spinning solution with a C/Zr molar ratio of 3.3 [39]. (c) and (d) TEM images of ZrC nanofibers after pyrolysis at 1400°C for 2 h electrospun from PZO/PAN spinning solution.
ZrB2 nanofibers can also be prepared by introducing a boron source into the ZrC spinning solutions [16, 37]. Formation of ZrB2 was initiated at 1200°C with complete transformation to pure ZrB2 at 1500°C (Figure 14). The as‐synthesized ZrB2 nanofibers were porous and composed of ZrB2 nanoparticles.
(a) XRD patterns of the nanofibers after pyrolysis. From bottom to top: 2 h at 1100°C, 2 h at 1200°C, 2 h at 1300°C, 2 h at 1400°C, and 1 h at 1500°C in an argon atmosphere; 1 h at 1500°C in vacuum. (b) SEM image of ZrB2 nanofibers after pyrolysis at 1500°C for 1 h in argon. The scale bar in the inset is 500 nm [16].
Materials containing tailored porosity exhibit special properties and features that usually cannot be achieved by their conventional dense counterparts [42, 43]. Nowadays, therefore, porous materials find many applications as end products in several technological processes. Due to the intrinsic properties of porous ceramics, such as lightweight, low thermal conductivity, high specific strength, and excellent thermal insulation, UHTC‐based porous ceramics could be applied as the promising candidate materials in thermal protection systems of hypersonic vehicles.
The processing routes used for the production of porous ceramics can be classified into replica, sacrificial template, and direct‐foaming methods, as schematically shown in Figure 15 [42]. It is important to get a well‐dispersed ceramic slurry or liquid precursor for the fabrication of porous ceramics with tailored microstructure and chemical composition. Sol‐gel techniques have been widely used as ceramic precursors to prepare porous ceramics, such as zirconia, alumina, and silicon carbide–based porous ceramics.
Scheme of possible processing routes used for the production of macroporous ceramics [42]. (a) Replica method; (b) Sacrificial template method; (c) Direct foaming method.
Though sol‐gel routes have been established to synthesize UHTC nanopowders and nanofibers, focus on the preparation of UHTC‐based porous ceramics is rare. The replica process was applied to prepare porous ZrC/C ceramic by Rambo et al. [44] where pine wood was used as the biological template for manufacturing of highly porous, biomorphic ZrC/C ceramics with zirconium n‐propoxide as the zirconia source. Pine wood was first pyrolyzed at 800°C for 1 h under N2 to obtain a biocarbon template. The biocarbon template was then infiltrated with zirconia sol and dried at 110°C for 1 h to obtain the ZrC/C preceramic. ZrC/C‐ceramic was prepared by heating the infiltrated biocarbon template at 1600°C for 1 h under argon flow. The original pine char microstructure was reproduced in the ZrC/C‐ceramic. Island‐like ZrC particles were observed on the cell walls and in the channels, as shown in Figure 16. The porosity of the ZrC/C‐ceramic was ∼78%.
SEM images of the biomorphic ZrC/C‐ceramic at different magnifications [44]. (a) Low magnification SEM image. (b) Higher magnification SEM image of a typical strut from (a).
In direct‐foaming methods, porous materials are produced by incorporating air into a suspension or liquid media, which is subsequently set in order to keep the structure of air bubbles created [42]. The consolidated foams are afterwards heated at high temperatures to obtain porous ceramics. Li et al. [15] prepared ZrC foams by employing a commercial direct‐foaming technique for phenolic resins. Zirconia sol was used as the zirconia precursor, while commercial foamable phenolic resin was used as the carbon source and foaming aid. By thermal‐setting the wet foam and pyrolyzing the foamed green body at 1600°C, highly porous ZrC foam was prepared. The density and porosity of as‐prepared ZrC foam were 0.16–0.19 g/cm3 and 83–90%, respectively. The as‐prepared ZrC foam showed closed cell structures with average cell sizes about 40 μm, as shown in Figure 17. The as‐synthesized ZrC foam displayed excellent thermal stability up to 2400°C. However, it is not possible to precisely control the residue carbon in the ZrC foam in their reaction system. Foamability of the mixtures originated due to phenolic resin decreased as the Zr content increased. About 47 wt% amorphous carbon was observed in the final ZrC foam.
(a) Photographs of the foamed green body and (b) ZrC ceramic foam obtained from pyrolysis at 1600°C for 1 h. SEM images of (c) the preceramic foam and (d) ZrC foam after pyrolysis at 1600°C for 1 h in Ar [15].
Li et al. [45] developed another method for the preparation of stoichiometric ZrC foams by direct foaming of zirconia sols. Sucrose used as a carbon source was dissolved into zirconia sol to get a foamable sol. The stabilization of the wet foam was based on the gelation of the zirconia sol under thermal aging. The microstructure of the ZrC foams can be tailored by controlling the foaming parameters, such as the viscosities of the sols, the concentration of the blowing and curing agents. The ZrC foams prepared with open‐ or closed‐cell structures are shown in Figure 18. The densities of the stoichiometric ZrC foams were in the range of 0.12–0.53 g/cm3.
(a) Photograph of the preceramic foam prepared from direct foaming of zirconia sol. SEM images of the preceramic foams after being pyrolyzed at 1500°C foaming by precursor sol with various viscosities. (b), 1552 cP; (c), 2025 cP; (d), 2699 cP; (e), 2954 cP [45].
Figure 19 shows compressive stress‐strain curves for ZrC foams prepared from direct foaming of zirconia sols [45]. In compression, all show a linear‐elastic regime followed by a plateau of roughly constant stress, leading into a final regime of steeply rising stress. Upon compression, the foam undergoes a progressive collapse of the cells, with the lower part of the foam remains completely undamaged. In the plateau region, the stress is assumed to be independent of the strain as part of the structure collapses, while other parts of the structure remain elastic. Beyond the plateau, densification takes place and the stress rises sharply as complete densification begins.
Typical compressive stress‐strain response of ZrC foams prepared from direct foaming of zirconia sols [45].
A sol‐gel technique has been applied to prepare UHTC‐based materials using metal alkoxide and oxychloride as a metal precursor. First, sols of metal oxide are prepared by hydrolysis of a metal precursor with the modification of bidentate ligands (e.g., β‐diketones, acetic acid, and cellulose acetate) to slow down the system\'s reactivity. Then soluble carbon‐ and boron‐containing compounds, such as sucrose, phenolic resin, PAN, boric acid, and triethyl borate, are introduced to metal oxide sols. The hybrid sols are dried, cured, and heated at high temperatures to complete the conversion of metal oxides to nonoxides. UHTC nanopowders can be synthesized at 1300–1600°C under a protective atmosphere. The average size of the crystallites is controlled in the range of 60–200 nm by controlling the synthesis parameters. UHTC nanofibers can be synthesized by combining a sol‐gel technique with spinning techniques, such as dry spinning and electrospinning. The as‐synthesized UHTC nanofibers are porous and composed of nanoparticles. Porous UHTC materials with controllable cell structures can be prepared by the replica technique and direct‐foaming methods. The as‐prepared porous UHTC materials possess high porosities and can withstand 2400°C high temperature aging.
Although sol‐gel routes provide great possibilities to produce UHTC‐based materials with desired shapes, the high temperature thermal reduction process is still an indispensable procedure during which large mass loss occurs. It is still highly welcomed to synthesize UHTC precursors with high ceramic yield by directly converting into UHTC materials without the reduction process.
The authors express their gratitude for the financial support from the National Natural Science Foundation of China (no. 51602324).
Research methodology is the path through which researchers need to conduct their research. It shows the path through which these researchers formulate their problem and objective and present their result from the data obtained during the study period. This research design and methodology chapter also shows how the research outcome at the end will be obtained in line with meeting the objective of the study. This chapter hence discusses the research methods that were used during the research process. It includes the research methodology of the study from the research strategy to the result dissemination. For emphasis, in this chapter, the author outlines the research strategy, research design, research methodology, the study area, data sources such as primary data sources and secondary data, population consideration and sample size determination such as questionnaires sample size determination and workplace site exposure measurement sample determination, data collection methods like primary data collection methods including workplace site observation data collection and data collection through desk review, data collection through questionnaires, data obtained from experts opinion, workplace site exposure measurement, data collection tools pretest, secondary data collection methods, methods of data analysis used such as quantitative data analysis and qualitative data analysis, data analysis software, the reliability and validity analysis of the quantitative data, reliability of data, reliability analysis, validity, data quality management, inclusion criteria, ethical consideration and dissemination of result and its utilization approaches. In order to satisfy the objectives of the study, a qualitative and quantitative research method is apprehended in general. The study used these mixed strategies because the data were obtained from all aspects of the data source during the study time. Therefore, the purpose of this methodology is to satisfy the research plan and target devised by the researcher.
The research design is intended to provide an appropriate framework for a study. A very significant decision in research design process is the choice to be made regarding research approach since it determines how relevant information for a study will be obtained; however, the research design process involves many interrelated decisions [1].
This study employed a mixed type of methods. The first part of the study consisted of a series of well-structured questionnaires (for management, employee’s representatives, and technician of industries) and semi-structured interviews with key stakeholders (government bodies, ministries, and industries) in participating organizations. The other design used is an interview of employees to know how they feel about safety and health of their workplace, and field observation at the selected industrial sites was undertaken.
Hence, this study employs a descriptive research design to agree on the effects of occupational safety and health management system on employee health, safety, and property damage for selected manufacturing industries. Saunders et al. [2] and Miller [3] say that descriptive research portrays an accurate profile of persons, events, or situations. This design offers to the researchers a profile of described relevant aspects of the phenomena of interest from an individual, organizational, and industry-oriented perspective. Therefore, this research design enabled the researchers to gather data from a wide range of respondents on the impact of safety and health on manufacturing industries in Ethiopia. And this helped in analyzing the response obtained on how it affects the manufacturing industries’ workplace safety and health. The research overall design and flow process are depicted in Figure 1.
Research methods and processes (author design).
To address the key research objectives, this research used both qualitative and quantitative methods and combination of primary and secondary sources. The qualitative data supports the quantitative data analysis and results. The result obtained is triangulated since the researcher utilized the qualitative and quantitative data types in the data analysis. The study area, data sources, and sampling techniques were discussed under this section.
According to Fraenkel and Warren [4] studies, population refers to the complete set of individuals (subjects or events) having common characteristics in which the researcher is interested. The population of the study was determined based on random sampling system. This data collection was conducted from March 07, 2015 to December 10, 2016, from selected manufacturing industries found in Addis Ababa city and around. The manufacturing companies were selected based on their employee number, established year, and the potential accidents prevailing and the manufacturing industry type even though all criterions were difficult to satisfy.
It was obtained from the original source of information. The primary data were more reliable and have more confidence level of decision-making with the trusted analysis having direct intact with occurrence of the events. The primary data sources are industries’ working environment (through observation, pictures, and photograph) and industry employees (management and bottom workers) (interview, questionnaires and discussions).
Desk review has been conducted to collect data from various secondary sources. This includes reports and project documents at each manufacturing sectors (more on medium and large level). Secondary data sources have been obtained from literatures regarding OSH, and the remaining data were from the companies’ manuals, reports, and some management documents which were included under the desk review. Reputable journals, books, different articles, periodicals, proceedings, magazines, newsletters, newspapers, websites, and other sources were considered on the manufacturing industrial sectors. The data also obtained from the existing working documents, manuals, procedures, reports, statistical data, policies, regulations, and standards were taken into account for the review.
In general, for this research study, the desk review has been completed to this end, and it had been polished and modified upon manuals and documents obtained from the selected companies.
The study population consisted of manufacturing industries’ employees in Addis Ababa city and around as there are more representative manufacturing industrial clusters found. To select representative manufacturing industrial sector population, the types of the industries expected were more potential to accidents based on random and purposive sampling considered. The population of data was from textile, leather, metal, chemicals, and food manufacturing industries. A total of 189 sample sizes of industries responded to the questionnaire survey from the priority areas of the government. Random sample sizes and disproportionate methods were used, and 80 from wood, metal, and iron works; 30 from food, beverage, and tobacco products; 50 from leather, textile, and garments; 20 from chemical and chemical products; and 9 from other remaining 9 clusters of manufacturing industries responded.
A simple random sampling and purposive sampling methods were used to select the representative manufacturing industries and respondents for the study. The simple random sampling ensures that each member of the population has an equal chance for the selection or the chance of getting a response which can be more than equal to the chance depending on the data analysis justification. Sample size determination procedure was used to get optimum and reasonable information. In this study, both probability (simple random sampling) and nonprobability (convenience, quota, purposive, and judgmental) sampling methods were used as the nature of the industries are varied. This is because of the characteristics of data sources which permitted the researchers to follow the multi-methods. This helps the analysis to triangulate the data obtained and increase the reliability of the research outcome and its decision. The companies’ establishment time and its engagement in operation, the number of employees and the proportion it has, the owner types (government and private), type of manufacturing industry/production, types of resource used at work, and the location it is found in the city and around were some of the criteria for the selections.
The determination of the sample size was adopted from Daniel [5] and Cochran [6] formula. The formula used was for unknown population size Eq. (1) and is given as
where n = sample size, Z = statistic for a level of confidence, P = expected prevalence or proportion (in proportion of one; if 50%, P = 0.5), and d = precision (in proportion of one; if 6%, d = 0.06). Z statistic (Z): for the level of confidence of 95%, which is conventional, Z value is 1.96. In this study, investigators present their results with 95% confidence intervals (CI).
The expected sample number was 267 at the marginal error of 6% for 95% confidence interval of manufacturing industries. However, the collected data indicated that only 189 populations were used for the analysis after rejecting some data having more missing values in the responses from the industries. Hence, the actual data collection resulted in 71% response rate. The 267 population were assumed to be satisfactory and representative for the data analysis.
The sample size for the experimental exposure measurements of physical work environment has been considered based on the physical data prepared for questionnaires and respondents. The response of positive were considered for exposure measurement factors to be considered for the physical environment health and disease causing such as noise intensity, light intensity, pressure/stress, vibration, temperature/coldness, or hotness and dust particles on 20 workplace sites. The selection method was using random sampling in line with purposive method. The measurement of the exposure factors was done in collaboration with Addis Ababa city Administration and Oromia Bureau of Labour and Social Affair (AACBOLSA). Some measuring instruments were obtained from the Addis Ababa city and Oromia Bureau of Labour and Social Affair.
Data collection methods were focused on the followings basic techniques. These included secondary and primary data collections focusing on both qualitative and quantitative data as defined in the previous section. The data collection mechanisms are devised and prepared with their proper procedures.
Primary data sources are qualitative and quantitative. The qualitative sources are field observation, interview, and informal discussions, while that of quantitative data sources are survey questionnaires and interview questions. The next sections elaborate how the data were obtained from the primary sources.
Observation is an important aspect of science. Observation is tightly connected to data collection, and there are different sources for this: documentation, archival records, interviews, direct observations, and participant observations. Observational research findings are considered strong in validity because the researcher is able to collect a depth of information about a particular behavior. In this dissertation, the researchers used observation method as one tool for collecting information and data before questionnaire design and after the start of research too. The researcher made more than 20 specific observations of manufacturing industries in the study areas. During the observations, it found a deeper understanding of the working environment and the different sections in the production system and OSH practices.
Interview is a loosely structured qualitative in-depth interview with people who are considered to be particularly knowledgeable about the topic of interest. The semi-structured interview is usually conducted in a face-to-face setting which permits the researcher to seek new insights, ask questions, and assess phenomena in different perspectives. It let the researcher to know the in-depth of the present working environment influential factors and consequences. It has provided opportunities for refining data collection efforts and examining specialized systems or processes. It was used when the researcher faces written records or published document limitation or wanted to triangulate the data obtained from other primary and secondary data sources.
This dissertation is also conducted with a qualitative approach and conducting interviews. The advantage of using interviews as a method is that it allows respondents to raise issues that the interviewer may not have expected. All interviews with employees, management, and technicians were conducted by the corresponding researcher, on a face-to-face basis at workplace. All interviews were recorded and transcribed.
The main tool for gaining primary information in practical research is questionnaires, due to the fact that the researcher can decide on the sample and the types of questions to be asked [2].
In this dissertation, each respondent is requested to reply to an identical list of questions mixed so that biasness was prevented. Initially the questionnaire design was coded and mixed up from specific topic based on uniform structures. Consequently, the questionnaire produced valuable data which was required to achieve the dissertation objectives.
The questionnaires developed were based on a five-item Likert scale. Responses were given to each statement using a five-point Likert-type scale, for which 1 = “strongly disagree” to 5 = “strongly agree.” The responses were summed up to produce a score for the measures.
The data was also obtained from the expert’s opinion related to the comparison of the knowledge, management, collaboration, and technology utilization including their sub-factors. The data obtained in this way was used for prioritization and decision-making of OSH, improving factor priority. The prioritization of the factors was using Saaty scales (1–9) and then converting to Fuzzy set values obtained from previous researches using triangular fuzzy set [7].
The researcher has measured the workplace environment for dust, vibration, heat, pressure, light, and noise to know how much is the level of each variable. The primary data sources planned and an actual coverage has been compared as shown in Table 1.
Planned versus actual coverage of the survey.
The response rate for the proposed data source was good, and the pilot test also proved the reliability of questionnaires. Interview/discussion resulted in 87% of responses among the respondents; the survey questionnaire response rate obtained was 71%, and the field observation response rate was 90% for the whole data analysis process. Hence, the data organization quality level has not been compromised.
This response rate is considered to be representative of studies of organizations. As the study agrees on the response rate to be 30%, it is considered acceptable [8]. Saunders et al. [2] argued that the questionnaire with a scale response of 20% response rate is acceptable. Low response rate should not discourage the researchers, because a great deal of published research work also achieves low response rate. Hence, the response rate of this study is acceptable and very good for the purpose of meeting the study objectives.
The pretest for questionnaires, interviews, and tools were conducted to validate that the tool content is valid or not in the sense of the respondents’ understanding. Hence, content validity (in which the questions are answered to the target without excluding important points), internal validity (in which the questions raised answer the outcomes of researchers’ target), and external validity (in which the result can generalize to all the population from the survey sample population) were reflected. It has been proved with this pilot test prior to the start of the basic data collections. Following feedback process, a few minor changes were made to the originally designed data collect tools. The pilot test made for the questionnaire test was on 10 sample sizes selected randomly from the target sectors and experts.
The secondary data refers to data that was collected by someone other than the user. This data source gives insights of the research area of the current state-of-the-art method. It also makes some sort of research gap that needs to be filled by the researcher. This secondary data sources could be internal and external data sources of information that may cover a wide range of areas.
Literature/desk review and industry documents and reports: To achieve the dissertation’s objectives, the researcher has conducted excessive document review and reports of the companies in both online and offline modes. From a methodological point of view, literature reviews can be comprehended as content analysis, where quantitative and qualitative aspects are mixed to assess structural (descriptive) as well as content criteria.
A literature search was conducted using the database sources like MEDLINE; Emerald; Taylor and Francis publications; EMBASE (medical literature); PsycINFO (psychological literature); Sociological Abstracts (sociological literature); accident prevention journals; US Statistics of Labor, European Safety and Health database; ABI Inform; Business Source Premier (business/management literature); EconLit (economic literature); Social Service Abstracts (social work and social service literature); and other related materials. The search strategy was focused on articles or reports that measure one or more of the dimensions within the research OSH model framework. This search strategy was based on a framework and measurement filter strategy developed by the Consensus-Based Standards for the Selection of Health Measurement Instruments (COSMIN) group. Based on screening, unrelated articles to the research model and objectives were excluded. Prior to screening, researcher (principal investigator) reviewed a sample of more than 2000 articles, websites, reports, and guidelines to determine whether they should be included for further review or reject. Discrepancies were thoroughly identified and resolved before the review of the main group of more than 300 articles commenced. After excluding the articles based on the title, keywords, and abstract, the remaining articles were reviewed in detail, and the information was extracted on the instrument that was used to assess the dimension of research interest. A complete list of items was then collated within each research targets or objectives and reviewed to identify any missing elements.
Data analysis method follows the procedures listed under the following sections. The data analysis part answered the basic questions raised in the problem statement. The detailed analysis of the developed and developing countries’ experiences on OSH regarding manufacturing industries was analyzed, discussed, compared and contrasted, and synthesized.
Quantitative data were obtained from primary and secondary data discussed above in this chapter. This data analysis was based on their data type using Excel, SPSS 20.0, Office Word format, and other tools. This data analysis focuses on numerical/quantitative data analysis.
Before analysis, data coding of responses and analysis were made. In order to analyze the data obtained easily, the data were coded to SPSS 20.0 software as the data obtained from questionnaires. This task involved identifying, classifying, and assigning a numeric or character symbol to data, which was done in only one way pre-coded [9, 10]. In this study, all of the responses were pre-coded. They were taken from the list of responses, a number of corresponding to a particular selection was given. This process was applied to every earlier question that needed this treatment. Upon completion, the data were then entered to a statistical analysis software package, SPSS version 20.0 on Windows 10 for the next steps.
Under the data analysis, exploration of data has been made with descriptive statistics and graphical analysis. The analysis included exploring the relationship between variables and comparing groups how they affect each other. This has been done using cross tabulation/chi square, correlation, and factor analysis and using nonparametric statistic.
Qualitative data analysis used for triangulation of the quantitative data analysis. The interview, observation, and report records were used to support the findings. The analysis has been incorporated with the quantitative discussion results in the data analysis parts.
The data were entered using SPSS 20.0 on Windows 10 and analyzed. The analysis supported with SPSS software much contributed to the finding. It had contributed to the data validation and correctness of the SPSS results. The software analyzed and compared the results of different variables used in the research questionnaires. Excel is also used to draw the pictures and calculate some analytical solutions.
The reliability of measurements specifies the amount to which it is without bias (error free) and hence ensures consistent measurement across time and across the various items in the instrument [8]. In reliability analysis, it has been checked for the stability and consistency of the data. In the case of reliability analysis, the researcher checked the accuracy and precision of the procedure of measurement. Reliability has numerous definitions and approaches, but in several environments, the concept comes to be consistent [8]. The measurement fulfills the requirements of reliability when it produces consistent results during data analysis procedure. The reliability is determined through Cranach’s alpha as shown in Table 2.
Internal consistency and reliability test of questionnaires items.
K stands for knowledge; M, management; T, technology; C, collaboration; P, policy, standards, and regulation; H, hazards and accident conditions; PPE, personal protective equipment.
Cronbach’s alpha is a measure of internal consistency, i.e., how closely related a set of items are as a group [11]. It is considered to be a measure of scale reliability. The reliability of internal consistency most of the time is measured based on the Cronbach’s alpha value. Reliability coefficient of 0.70 and above is considered “acceptable” in most research situations [12]. In this study, reliability analysis for internal consistency of Likert-scale measurement after deleting 13 items was found similar; the reliability coefficients were found for 76 items were 0.964 and for the individual groupings made shown in Table 2. It was also found internally consistent using the Cronbach’s alpha test. Table 2 shows the internal consistency of the seven major instruments in which their reliability falls in the acceptable range for this research.
Face validity used as defined by Babbie [13] is an indicator that makes it seem a reasonable measure of some variables, and it is the subjective judgment that the instrument measures what it intends to measure in terms of relevance [14]. Thus, the researcher ensured, in this study, when developing the instruments that uncertainties were eliminated by using appropriate words and concepts in order to enhance clarity and general suitability [14]. Furthermore, the researcher submitted the instruments to the research supervisor and the joint supervisor who are both occupational health experts, to ensure validity of the measuring instruments and determine whether the instruments could be considered valid on face value.
In this study, the researcher was guided by reviewed literature related to compliance with the occupational health and safety conditions and data collection methods before he could develop the measuring instruments. In addition, the pretest study that was conducted prior to the main study assisted the researcher to avoid uncertainties of the contents in the data collection measuring instruments. A thorough inspection of the measuring instruments by the statistician and the researcher’s supervisor and joint experts, to ensure that all concepts pertaining to the study were included, ensured that the instruments were enriched.
Insight has been given to the data collectors on how to approach companies, and many of the questionnaires were distributed through MSc students at Addis Ababa Institute of Technology (AAiT) and manufacturing industries’ experience experts. This made the data quality reliable as it has been continually discussed with them. Pretesting for questionnaire was done on 10 workers to assure the quality of the data and for improvement of data collection tools. Supervision during data collection was done to understand how the data collectors are handling the questionnaire, and each filled questionnaires was checked for its completeness, accuracy, clarity, and consistency on a daily basis either face-to-face or by phone/email. The data expected in poor quality were rejected out of the acting during the screening time. Among planned 267 questionnaires, 189 were responded back. Finally, it was analyzed by the principal investigator.
The data were collected from the company representative with the knowledge of OSH. Articles written in English and Amharic were included in this study. Database information obtained in relation to articles and those who have OSH area such as interventions method, method of accident identification, impact of occupational accidents, types of occupational injuries/disease, and impact of occupational accidents, and disease on productivity and costs of company and have used at least one form of feedback mechanism. No specific time period was chosen in order to access all available published papers. The questionnaire statements which are similar in the questionnaire have been rejected from the data analysis.
Ethical clearance was obtained from the School of Mechanical and Industrial Engineering, Institute of Technology, Addis Ababa University. Official letters were written from the School of Mechanical and Industrial Engineering to the respective manufacturing industries. The purpose of the study was explained to the study subjects. The study subjects were told that the information they provided was kept confidential and that their identities would not be revealed in association with the information they provided. Informed consent was secured from each participant. For bad working environment assessment findings, feedback will be given to all manufacturing industries involved in the study. There is a plan to give a copy of the result to the respective study manufacturing industries’ and ministries’ offices. The respondents’ privacy and their responses were not individually analyzed and included in the report.
The result of this study will be presented to the Addis Ababa University, AAiT, School of Mechanical and Industrial Engineering. It will also be communicated to the Ethiopian manufacturing industries, Ministry of Labor and Social Affair, Ministry of Industry, and Ministry of Health from where the data was collected. The result will also be availed by publication and online presentation in Google Scholars. To this end, about five articles were published and disseminated to the whole world.
The research methodology and design indicated overall process of the flow of the research for the given study. The data sources and data collection methods were used. The overall research strategies and framework are indicated in this research process from problem formulation to problem validation including all the parameters. It has laid some foundation and how research methodology is devised and framed for researchers. This means, it helps researchers to consider it as one of the samples and models for the research data collection and process from the beginning of the problem statement to the research finding. Especially, this research flow helps new researchers to the research environment and methodology in particular.
There is no “conflict of interest.”
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\\n\\nIntechOpen will help you complete your payment safely and securely, keeping your personal, professional and financial information safe.
\\n\\n7. ONLINE PUBLICATION, PRINT AND DELIVERY OF THE BOOK
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