Details characteristic of nanomaterial classification.
\r\n\tThis book intends to cover major mineral deficiency problems such as calcium, iron, magnesium, sodium, potassium and zinc. These minerals have very important task either on intracellular or extracellular level as well as regulatory functions in maintaining body homeostasis.
\r\n\r\n\t
\r\n\tBoth macrominerals and trace minerals (microminerals) are equally important, but trace minerals are needed in smaller amounts than major minerals. The measurements of these minerals quite differ. Mineral levels depend on their uptake, metabolism, consumption, absorption, lifestyle, medical drug therapies, physical activities etc.
\r\n\tAs a self-contained collection of scholarly papers, the book will target an audience of practicing researchers, academics, PhD students and other scientists. Since it will be published as an Open Access publication, it will allow unrestricted online access to chapters with no reading or subscription fees.
",isbn:"978-1-83881-085-6",printIsbn:"978-1-83881-081-8",pdfIsbn:"978-1-83881-086-3",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"8bc7bd085801296d26c5ea58a7154de3",bookSignature:"Dr. Gyula Mozsik and Dr. Gonzalo Díaz-Soto",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/8935.jpg",keywords:"Calcium, Iron, Magnesium, Potassium, Sodium, Zinc, Diagnostic tools, Treatments, Food Fortification, Malnutrition, Metabolic Disorders, Lifestyle",numberOfDownloads:741,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"May 26th 2020",dateEndSecondStepPublish:"June 16th 2020",dateEndThirdStepPublish:"August 15th 2020",dateEndFourthStepPublish:"November 3rd 2020",dateEndFifthStepPublish:"January 2nd 2021",remainingDaysToSecondStep:"9 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"Professor Emeritus of Medicine at Univesity of Pecs, Hungary, and recipient of Andre Roberts award from the International Union of Pharmacology in 2014. He published 360 peer-reviewed papers, 196 book chapters, 692 abstracts, 19 monographs, and edited 32 books.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"58390",title:"Dr.",name:"Gyula",middleName:null,surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik",profilePictureURL:"https://mts.intechopen.com/storage/users/58390/images/system/58390.jpg",biography:"Gyula Mózsik, MD,PhD, ScD(med) is a professor emeritus of medicine at First Department of Medicine, Univesity of Pécs, Hungary. He was head of the Department from 1993 to 2003. His specializations are medicine, gastroenterology, clinical pharmacology, clinical nutrition. His research fields are biochemical and molecular pharmacological studies in gastrointestinal tract, clinical pharmacological and clinical nutritional studies, clinical genetic studies, and innovative pharmacological and nutritional (dietetical) research in new drug production and food production. He published around 360 peer-reviewed papers, 196 book chapters, 692 abstracts, 19 monographs, 32 edited books. He organized 38 national and international (in Croatia ,France, Romania, Italy, U.S.A., Japan) congresses /Symposia. He received the Andre Robert’s award from the International Union of Pharmacology, Gastrointestinal Section (2014). 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He finished his specialisation on Endocrinology and Nutrition Hospital Clinic of Barcelona. He currently works at the Clinical University Hospital of Valladolid in the Endocrinology, Diabetes and Nutrition Department.",institutionString:"University of Valladolid",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"2",institution:{name:"Hospital Clínico Universitario de Valladolid",institutionURL:null,country:{name:"Spain"}}},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"6",title:"Biochemistry, Genetics and Molecular Biology",slug:"biochemistry-genetics-and-molecular-biology"}],chapters:[{id:"72450",title:"Parathyroid Glands and Hyperparathyroidism: A General Overview",slug:"parathyroid-glands-and-hyperparathyroidism-a-general-overview",totalDownloads:109,totalCrossrefCites:0,authors:[null]},{id:"73735",title:"Mineral Deficiencies a Root Cause for Reduced Longevity in Mammals",slug:"mineral-deficiencies-a-root-cause-for-reduced-longevity-in-mammals",totalDownloads:86,totalCrossrefCites:0,authors:[null]},{id:"73026",title:"Calcium and Metabolic Bone Disorders",slug:"calcium-and-metabolic-bone-disorders",totalDownloads:115,totalCrossrefCites:0,authors:[null]},{id:"72852",title:"Severe Hypocalcemia after Total Parathyroidectomy Plus Autotransplantation for Secondary Hyperthyroidism-Risk Factors and a Clinical Algorithm",slug:"severe-hypocalcemia-after-total-parathyroidectomy-plus-autotransplantation-for-secondary-hyperthyroi",totalDownloads:83,totalCrossrefCites:0,authors:[null]},{id:"72573",title:"Familial Syndromes of Primary Hyperparathyroidism",slug:"familial-syndromes-of-primary-hyperparathyroidism",totalDownloads:85,totalCrossrefCites:0,authors:[null]},{id:"73976",title:"Nutrigenomics: An Interface of Gene-Diet-Disease Interaction",slug:"nutrigenomics-an-interface-of-gene-diet-disease-interaction",totalDownloads:222,totalCrossrefCites:0,authors:[null]},{id:"74772",title:"Organoleptic, Sensory and Biochemical Traits of Arabica Coffee and their Arabusta Hybrids",slug:"organoleptic-sensory-and-biochemical-traits-of-arabica-coffee-and-their-arabusta-hybrids",totalDownloads:42,totalCrossrefCites:0,authors:[null]}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"184402",firstName:"Romina",lastName:"Rovan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/184402/images/4747_n.jpg",email:"romina.r@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. 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The development of nanomaterial has been attracted great interest in the worldwide in the past few years. The turning point for nanomaterials research was the discovery of carbon nanotubes in 1991 [1]. Nanomaterials are usually defined as having a particle size between 1 and 100 nanometers (nm). They are bigger than individual atoms (measured in angstroms, 1 Å = 10−10 m. One nanometer is millionth of millimeter. It is equal to 100,000 times smaller than the diameter of human hair. After this discovery, there was an explosive increase in the number of research teams working in the field. The properties of nanomaterials deviate from those of “bulk” materials with the same composition, thus allowing for many interesting applications. At nanodimensions, quantum effects, like quantum confinement, permit multiple applications [2, 3, 4]. Some of nanotechnology applications include alternative energy [3], electronics [5, 6], catalysis [5], biomedicine [2], batteries [7], water treatment [8], and materials reinforcement [9] (Figure 1).
(a) Evolution of science and technology and the future [10]; (b) an example of nanomaterial comparison; and (c) an example of the nanorod image [11].
Classification is based on the number of dimensions, which are not confined to the nanoscale range (<100 nm) (Figure 2 and Table 1):
zero-dimensional (0-D);
one-dimensional (1-D);
two-dimensional (2-D); and
three-dimensional (3-D).
0-D, 1-D, 2-D and 3-D nanomaterial [12].
Details characteristic of nanomaterial classification.
1-D nanostructures as a series of the most important materials owed by it fascinating physical properties. Due distinct structure-dependent properties had lead it application widely especially in solar energy conversion, thermoelectric devices, energy storage technology. 1-D nanostructures mainly show three different morphologies (Table 2):
nanorod;
nanowires; and
nanotube.
Nanorods, nanowires and nanotube.
Among those 1-D nanostructures, nanorods have the advantage as it can be made from most elements (metals and nonmetals) and compounds, and the synthetic requirements for their production are more flexible than for nanotubes and nanowires. Nanorods have typical lengths of 10–120 nm. For example, metallic nanorods, semiconductor nanorods, carbon nanorods, and oxides nanorods, are essential for the development of electronic, optical, magnetic, and micromechanical devices [5, 6].
Due to their shape anisotropy (physical properties), nanorods are attractive component to be studied and ideal candidates for many application. It was discovered that ability of the nanorods was enhanced as compared spherical particles. This is due to the increase of aspect ratio of the particle lead to the increased of excitation of surface plasmons in the nanoparticles. Particularly, the strength of the dipole moment is within a nanoparticle due to incrementing of surface plasmons. Therefore, an increase of surface plasmons lead to the enhancement of electrical field in nanorods as compared spherical particles. One example of benefit of a rod-like shape demonstrated by Alivisatos and co-workers [14] who observed partially aligned CdSe nanorods provided an effective, directed path for charge carriers to move throughout the photovoltaic device and be collected. Similarly, the incorporation of nanorods within P3HT film could improve the external quantum efficiency by a factor of 3 as the aspect ratio increased from 1 to 10. The accumulation of electrons was improved as the aspect ratio of nanoparticles increased. Furthermore, alignment of nanorods also plays a key role in improving it properties. Work by Winey group [15] studying Ag nanorods for polystyrene composites and discovered that the aspect ratio of anisotropic nanoparticle play role in the electrical conductivity of polymer composites. Particularly, due to the minimal percolation threshold of rod-shape particles as compared to spherical particles. Percolation has been found to be depended on both size and shape of nanoparticles. Larger in both length and diameter of rod-shape particles are expected to share many advantages in the oriental properties of nanorods. Last but not least, nanorods offer more advantages over isotropic (homogeneous and uniform) particles. It can be summarized that the efficiency of nanorods depends strongly on nanorods aspect ratio, volume fraction, polydispersity and orientation.
Various nanorods have been extensively studied such as carbon nanorods, ZnO nanorods, gold nanorods and magnetic nanorods. Recently, various techniques have been proposed for synthesizing the nanorods. It can be classified into either via physical or chemical methods or known as bottom-up or top-down techniques. The method such as thermal hydrolysis, hydrothermal route, sol-gel, vapor condensation, spray pyrolysis, pulse laser decomposition, laser ablation, thermal evaporation, pulse combustion-spray pyrolysis, electro-mechanical, flame spray plasma, microwave plasma, low energy beam deposition, ball-milling, chemical vapor deposition, laser ablation, chemical reduction, co-precipitation, hybrid wet chemical route, physical evaporation, electrophoretic deposition, radio frequency (RF) magnetron sputtering, vapor deposition, metal assisted growth, template assisted routes, metal-assisted growth and seed-based growth, simple chemical etching, etc. Typically, nanorods prepared by controlling the nucleation growth than transverse one.
Carbon nanorods have attracted great interest from past few decades owing to their physical (particle size, shape, large surface area and greater pore size distribution) and chemical properties [16, 17, 18]. Nanorods made of carbon also known as “carbon nanorods” and “diamond nanorods.” Diamond nanorods have a crystalline structure like diamond with sp3 carbon hybridization. The yield and purity of synthesizing the carbon nanorods are strongly dependent on the composition of the inert atmosphere and its pressure. Generally, the carbon nanorods had better physicochemical properties after introducing different functionalities in the carbon nanorods pore surfaces. It will permit many applications, like in catalysis, water treatment, supercapacitors, and others. Carbon nanorods large applied as anodic material in batteries apart from their application like fillers [19] and high performance electrode materials in batteries [20, 21, 22, 23]. Till now, various synthesis methods have been proposed and it can be classified as “bottom up” (like synthesis from small molecules or colloidal solutions) or “top down” (like starting with bigger structures). The top-down method for synthesizing carbon nanorods including, simple chemical etching and electrochemical etching. Meanwhile, bottom-up approach including template assisted, metal assisted, hydrothermal route, vapor deposition (CVD), seed based and other synthesis in solution.
A recent finding was discussed on the recent advanced efforts in the preparation of carbon nanorods from metal-organic frameworks (MOFs) [24]. MOFs-a class of porous and crystalline material have attracted a great deal attention due to their fascinating architectures as well as their useful properties [25]. MOFs could be synthesized using both organic and inorganic components. Eventhough MOFs is well-established excellent porous material, yet the thermal transformation of MOFs into carbon materials accompanied by partial or complete collapse of their original morphology. Due to this reasons, the synthesis of nonhollow (solid) 1-D of carbon nanorods with moderate aspect ratio, high surface area and good performance capacitor electrodes is achieved by self-scarified and morphology-preserved thermal transformation of MOF-74 [24] (Figure 3).
(a) The secondary building unit and 3-D crystal structure of MOF-74 and (b) scheme of synthesis of MOF-74-rod, carbon nanorods. (b) The secondary building unit and 3-D crystal structure of MOF-74.
The reaction of zinc nitrate and 2,5-dihydroxyterephthalic acid in N, N-dimethylformaide (DMF) by traditional hydrothermal method resulted in formation of microcrystalline MOF-74. The room-temperature reaction of those components in the presence of salicylic acid as a modulator led to the formation of rod-shaped MOF-74 (MOF-74-Rod, 30–60 nm wide, 200–500 long) as observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The addition of salicylic acid directed MOF growth in a rod-shape morphology by stabilizing the active metal sites on the MOF crystal surface [26]. The thermal transformation of MOF-74-Rod at 1000°C results in the formation of carbon nanorods. In comparison of MOF-74-Rod (377 m2 g−1), higher surface area of MOF-74 (411 m2 g−1) might be attributed to the perfect arrangement of MOF crystallites in the domain structure. The pore size distribution for MOF-74-Rid confirms the formation of micro (∼1.5 nm) and mesopores (∼6.5 nm), whereas MOF-74 shows the presence of microspores (∼1.2 nm) exclusively. The great different in pore size distribution attributed to the formation of voids resulted from lateral attachment of MOF nanorods. The MOF-74-Rod showed excellent capacitor performance with specific capacitance value of 164 F g-1 at sweep rate of 10 mVs−1. Overall from this study, open up new avenues for efficient product of 1-D carbon material with promising applications in electrochemical devices.
ZnO has a wide band-gap (3.37 eV at room temperature). ZnO is known to have wurtzite structure with lattice constant (a) 3.249 Å, (c) 5.207 Å. It has a large excitonic binding energy of 60 MeV, which is greater than the thermal energy at room temperature, makes it a promising candidate for applications in blue-UV light emission and room-temperature UV lasing. ZnO posed an excellent chemical and thermal stability and the electrical properties. Since Zno has lack of center symmetry, make it results in a piezoelectric effect, whereby a mechanical stress/strain could be transformed into electrical voltage and vice versa, due to the relative displacement of the cations and anions in the crystal [27]. Single crystal of ZnO exhibit significantly faster electron transport and greater mobility. The faster electron transport is a result of the high electron diffusion coefficients, which will provide significant advantages to device performance [28]. Since ZnO could emits at the near ultraviolet, has transparent conductivity and piezoelectric properties, thus, ZnO is an interesting material for semiconductor and laser devices, piezoelectric transducers, transparent electronics, surface acoustic wave devices, spin functional devices, and gas sensing. Overall, ZnO is an excellent material for sensor application attributed by its large surface to volume ratio that leads to the enhancement of it sensitivity, bio-safety and bio-compatibility. A recent research has demonstrated that creation of highly oriented and ordered array of ZnO nanostructures has greatly stimulate interest in development of novel devices [29]. The large surface area of nanorods makes ZnO attractive for gas and chemical sensing. High oriented array of ZnO nanorods (and nanowires) can be produced via various chemical, electrochemical and physical deposition techniques such as chemical vapor deposition (CVD) or metal organic CVD (MOCVD), vapor-liquid-solid (VLS) growth, electrochemical deposition (ED) and hydrothermal approaches.
Recently, a great deal of attention has been focused on the study of synthesizing the ZnO nanorods via VLS method. In this case, gold (Au) nanoparticles are used as catalyst in order to promoting the ZnO nanorods formation. Unfortunately, the are some apparent drawbacks in VLS growth technique. Generally, it required high growth temperature > 900°C in order to dissolving the Zn vapor into the Au catalyst simultaneously forming an alloy droplet. After saturated, Zn precipitates out from the droplet and further oxidized as ZnO nanorods grow. The other drawback from VLS growth method is that at the tips of ZnO nanorods there are always impurity particles that might be undesirable for fabrication. Due to this reason, the synthesizing ZnO nanorods via CVD and MOCVD were highlighted. The synthesis temperature used generally mild reaction temperature and high purity of ZnO nanorods could formed.
Apparently, the CVD process took place in a horizontal quartz tube placed in a rapid thermal furnace. Figure 4(a) shows a schematic illustration of the CVD furnace including a horizontal quartz tube of 1-in. A high-purity metallic granulated zinc (99.99%) was placed in an alumina boat which was then inserted at the end of quartz ampoule sealed at one end. Au nanoparticles are used as catalyst deposited on Chip B and C. Once the temperature went above the melting point of zinc metal (420°C), zinc would gradually vaporize to fill the quartz vial and then diffuse to Chip B and then to Chip C. The Au catalyst further formed liquid droplet and super saturated with Zn vapor. The nucleation growth of ZnO started with the arrival of oxygen gas. The ZnO will precipitate when the droplet reached a critical radius and continuously growth. Typically, ZnO synthesis was synthesized follow several steps. Initially, the quartz tube evacuated to 10–2 Torr, follow by purged using Ag gas to maintain a 1 atm ambient. The furnace temperature rapidly increased to 700°C under constant Ag flow and maintain within a period of time. Finally, the oxygen gas (O2 mixed Ag) was then flown through quartz tube forcing a precipitate to form. As shown in Figure 4(c), shows prismatic hexagonal rods of ZnO grown area. The ZnO crystal continuously growth perpendicular from the surface on one single nanowires forming comb structure (Figure 4(d)). Thick ZnO needle can be found at the outer edge (Figure 4(e)). With sufficient oxygen concentration, wires with larger diameter are grown.
Schematic illustration of the (a) CVD system with a horizontal quartz tube placed in a furnace. A small quartz vial inside the quartz tube is used to trap zinc vapor during the synthesis process, (b) MOCVD system, (ce) SEM image for ZnO nanorods from CVD system, (f) SEM image for ZnO nanorods from MOCVD system and (g) SEM image of a ZnO nanorod, indicating a diameter of 110 nm.
In the case of MOCVD techniques, in MOCVD generally, the use of organic precursor, such as Zn(C2H5)2 and O2 system, are involved. The ZnO films or nanorods were deposited on p-type silicon with (100) orientation. Figure 4(b) shows a schematic diagram of the MOCVD system. Mass flow controllers separately controlled the flow of Ar and O2 gases and the gas flow ratio of Ar to O2 was in the range of 1–2. The substrate temperature was varied as a process variable ranging from 250 to 500°C [30]. The deposition time was set to 10 min [30]. In this study the SEM image reveals that ZnO nanorods are directly grown on Si substrates (Figure 4(f)) and the diameter of ZnO nanorod ranges from 40 to 120 nm (Figure 4(g)). In summary, the uniform ZnO nanorods have successfully synthesized in bulk quantities directly on the Si substrate using the MOCVD technique.
Recently, several studies have demonstrates the growth of ZnO nanorods could be achieved molecular beam epitaxy (MBE). In MBE, the growth is performed under clean, low pressure condition and the reactants are very pure Zn metal and atomic O from a plasma generator [31]. In MBE system, the potential contamination is minimized [31] . The ZnO layers typically were grown on p-type silicon wafer Si(100) under conditions: substrate temperature 300–430°C, temperature of the Zn-Knudsen cell 300°C (Zn beads of purity 99.9999 were filled), pressure of the chamber during the growth was ∼(1–4) × 10–4 mbar and oxygen plasma was generated [32]. The ZnO nanorods of reasonable quality could be deposited forming cored nanorod (Figure 5(a and b)). This cored nanorods could be produced using Mg-doping during MBE growth. Similarly, Heo et al. [33] report on catalyst-driven MBE of ZnO nanorods. The single ZnO nanorod growth is realized via nucleation on Ag films that are deposited on SiO2-terminated Si substrate surface (Figure 5(c)). Growth occurs at substrate temperatures within range of 300–500°C. The nanorods are uniform cylinders exhibiting diameter of 15–40 nm (Figure 5(d)) and lengths in excess of 1 μm. Eventhough CVD, MOCVD and MBE such an attractive technique in developing ZnO nanorods but these growth techniques are complicated and growth temperatures used are high (435°C).
(a) Schematic of coaxial nanorods having a lateral heterostructure (top), (b) transmission electron micrographs showing cored (Zn1 − x Mgx)O nanorods a having Zn-rich phase surrounded by another (Zn1 − x Mgx)O phase (bottom), (c) SEM image of ZnO nanorods nucleated on Ag-coated Si/SiO2 substrate and (d) TEM and selected area diffraction image of a single crystal ZnO nanorod.
The hydrothermal method [34, 35] has attracted considerable attention due to its unique advantages-it is simple, low temperature (60–100°C), high yield, low cost, uncomplicated process, excellent morphology-well-defined structure and controllable process [36]. Particularly, chemical precursor solution involves in formation of ZnO nanorods via hydrothermal route is Zn salt and hexamethylenetetramine on Si substrates with a seed layer prepared from zinc acetate solution. Polyethyleneimine was added to the solution to increase the nanorod aspect ratio [37]. The growth temperature and the growth time were constantly kept at lower temperature < 100°C and under certain period of time. Recently, ZnO nanorods with hexagonal structure were synthesized via hydrothermal route by Polsongkram and co-workers using zinc nitrate [Zn(NO3)2 6H2O] that was mixed with hexamethylenetetramine (HMT) (C6H12N4) solution and treated under temperature 60–95°C. It is evident that the at 95°C, the sample mainly consists of ZnO nanorods and most of them assembly into branched and urchin-like morphologies (Figure 6(a)). It was discovered that the hexagonal ZnO nanorods formed about 2 mm in length 100–150 nm in diameter. The nanorods grown larger (thick branched rods) when the temperature reduce to 75 and 60°C [35] (Figure 6(c and d)). This study also found that controlled growth of nanorods ranging from a thinner to a larger diameter can be realized by appropriate choice of the initial precursor concentration and deposition time. The hexagonal ZnO nanorods formation via hydrothermal method also in agreement with Phromyothin findings (Figure 6(d and e)) [38]. Similarly, this study also discovered that as the precursor concentration increased, the average diameter of ZnO nanorods will enlarge. It can be suggested that the precursor concentration provides the crucial role on the physical morphology and crystal growth direction of ZnO nanorods.
Scanning electron microscopy (SEM) images of the ZnO nanorods grown from ZnNO3-0.040 M: HMT-0.025 M aqueous solution in 30 min at different temperatures: (a) 95°C, (b) 75°C and (c) 60°C [35], (d and e) FESEM images of ZnO nanorods synthesized via hydrothermal method [38] and (f and g) SEM images of ZnO nanorods via ED method.
Last but not least, the ZnO nanorods also could be synthesized via ED method. ED method has many advantages including a low growth temperature, simple and low cost process without the need for vacuum systems for preparing ZnO nanorods with high crystallinity, being suited for scale-up and good electrical contact between the structures and the substrate [39]. However, in ED method when the ZnO nanorods were growth using electrochemical on transparent conducting oxides (TCOs, i.e. ITO and FTO), electrodes and a previously deposited ZnO seed layer are necessary to precisely control the morphology and aspect ratio of the as-grown ZnO nanostructures. In ED method the ZnO nanorods were electrodeposited from the zinc nitride aqueous solution in an electrode system. Typically, electrodepositions were conducted in a water bath at 80°C. Figure 6(f) presents the electrodeposited ZnO results, the result showed the SEM images of ZnO nanorods on predeposited PAN film [40]. The ZnO nanorods exhibited good vertical alignment, and with significant hexagonal cross section and a relatively uniform size with an average diameter of 180 nm.
Much attention has been given recently to gold nanorods (Au nanorods), mainly due to their applications in biomedicine. Gold nanorods show two absorption bands, known as surface plasmon resonance (SPR) bands, called the TSPR (transverse) in the visible and LSPR (longitudinal) in the near infrared (NIR) region [41]. This last one is useful for medical applications because NIR radiation is the one that penetrates the most in living tissues. The absorbed radiation is converted into heat, thus showing promise for cancer treatment. Also, these nanorods have localized surface plasmon resonances (LSPRs) that allow for unique scientific and technical applications [42]. In particular, the synthesis of well-defined size and shapes of Au nanorods has attracted much attention due to its importance in electronic and optical properties of these nanomaterials. The longitudinal bands of Au nanorods can be tuned by changing their aspect ratio, simultaneously make it possible to gain absorption bands at the desired wavelength in the NIR. Small change in aspect ratio will result in drastic change in the NIR absorption wavelength. The Au nanorods could be synthesized via two general growth approaches, which are bottom-up and top-down methods. For bottom-up methods, Au nanorods are generated through nucleation in aqueous solutions and subsequent overgrowth, where Au salts are usually used to provide the Au source through reduction. Particularly, bottom-up method including wet-chemical, electrochemical, sonochemical, solvothermal, microwave-assisted and photochemical reduction technique. All of these method involving the use of reduced aqueous solvated Au salts by various reducing agents, such as sodium borohydride, ascorbic acid, and small Au clusters, under different external stimuli (triggering the reduction of Au salt). The length of Au nanorods could be elongated with the use of template, it serves to confine the growth along one direction during the reduction.
The electrochemical method was the first technique for developing the Au nanorods. Briefly, the Au and Pt were used as the anode and cathode, respectively. These electrodes will be immersed in an electrolytic solution containing the cationic surfactant such as hexadecyltrimethylammonium bromide (CTAB) and co-surfactant. The CTAB works as supporting electrolyte and stabilizer (preventing aggregation of the nanorods), and CTAB induces the formation of rods. The length of the nanorods is determined by the presence of a silver plate in the solution. The silver metals react with the Au ions generated by the dissolution of the anode. The researchers found that the amount of dissolved silver and the concentration of Ag+ ions determined the length of the nanorods [25]. The larger the area of silver plate, the higher the amount of Ag+ ion species formed and the higher the speed of silver will be released and thus, the longer the Au nanorods formed [43].
Based on previous literature for Au nanorods formation via bottom-up method, seed mediated growth has been by far the most efficient and popular approach [44]. This method utilizes “soft templates” for growing Au (Figure 7), which was developed by Murphy and El-Sayed studies [42]. Highly yield monodisperse Au nanorods with greater uniformity could be developed via this method. Typically, small Au nanoparticles seed of ∼1.5 nm is initially prepared by reducing chloroauric acid with borohydride in an aqueous CTAB solution [42]. The seed solution will be mixed with growth solution containing metal salt (weak reducing agent) such as ascorbic acid and a surfactant-directing agent CTAB. The CTAB will absorbed onto Au nanorods forming a bilayer. It is suggested that aspect ratio of Au nanorods can be controlled by ratio metal see/metal salt in growth solution. According to former study, the CTAB will bind to the crystallographic faces of Au existing along the sides of pentahedrally twinned rods, as compared to the faces at the tip. The seed-mediated growth technique is the presence of CTAB is one of the most widely used and the yields of the nanorods from the seed-mediated growth method can be as high as 99%. It have been reported that the size and shape of Au nanorods could be tailored by adjusting the growth condition such as the pH of growth solution, composition of surfactant, amount of the reagent, growth temperature and structure of the seed in the seed-mediated growth process. Interestingly, recent study demonstrated high yield and greater uniformity of Au nanorods could be obtained via seed-mediated growth through the use of aromatic additive to CTAB [45]. Figure 7(a and c) showed TEM images of Au nanorods synthesized with 0.0126 M sodium 3-methylsalicylate (additive) present in the growth solution. The nanorods obtained have an average diameter of 14.0 (1.0 nm and a length of 33.0 ± 2.5 nm. On the other hand, slightly longer nanorods are made when 0.010 M sodium salicylate is used as the additive (Figure 7(b and d)).
(a–d) TEM images for Au nanorods synthesized via seed-mediated growth with the addition of aromatic additive [45].
Eventhough the bottom-up method results in excellent monodisperse Au nanorods with small diameter and high uniformity, yet them suffer some drawback where typically, selective placement of Au nanorods at desired locations on substrates by the bottom-up methods has been very difficult owing to the random nature of the reduction of Au ions and the deposition of Au atoms in reaction solutions. Moreover, the shape and size of Au nanorods also varied from different synthesis batches. This will affect their optical and catalytic properties and applications. Last but not least, bottom-up method suffers in placing Au nanorods into large-area, ordered arrays. Due to these reasons, top-down approaches gained interest.
It is well-established that top-down method could promote high production homogeneous Au nanorods with controlled particle geometries and regular inter-particle arrangements, which is valuable for quantitative characterization as well as device applications. In top-down methods, Au nanorods are obtained through a combination of different physical lithography processes and Au deposition [42]. Particularly, there are two technique used for top-down method in synthesizing the Au nanorods. First method is through the removal of Au from predeposited Au films using ion beam or etching techniques. Second method is by employing the lithography techniques to create mask. Au layer then deposited on the substrate which is covered by the mask via physical method: thermal, electron-beam evaporation or sputtering. The synthesized Au nanorods further obtained from lift-off process. Generally, the size of Au nanorods obtained via top-down method is limited by the resolution of lithography method. Interestingly, recent study by Koh and co-worker reported that state-of-the-art electron beam lithography system able to produce the size of Au nanorods within diameter ranging from ∼10 to >100 nm [46]. The Au nanorods were fabricated on 30-nm-thick silicon-nitride (SiN) membranes (Figure 8(a)). High-resolution TEM images of individual nanostructures of Au nanorods in Figure 8(b) reveal that the Au nanostructures were polycrystalline in nature. The polycrystallinity of the metal structures could potentially be a drawback of lithographically defined metal structures, as chemically synthesized metal nanoparticles can be a single crystal when synthesized in certain conditions. Eventhough, Au nanorods successfully synthesized via top-down method yet this method is time consuming and costly makes them impractical for fabrication of Au nanorods in bigger scales. Furthermore, Au nanorods obtained from vacuum deposition techniques also can degrade their plasmonic properties due to the electron scattering at the grain boundaries. Due to these reason had limit their usage in device application and simultaneously make the top-down method to be unattractive in fundamental research.
(a) SEM images of an array of Au nanostructures with elongated and (b) TEM image of individual Au nanorods [46].
Nanostructured iron oxide magnetite (Fe3O4) behaves supermagnetic and widely used in the biomedical field as well as device application. Generally, the magnetic nanoparticle could be utilized as nanoadsorbents, cancer diagnostic and treatment, contrast agent in magnetic resonance imaging (MRI), etc. Meanwhile for 1-D magnetite extremely important in building block for nanodevices. It has been found that size and shape of magnetite nanoparticles play key role in controlling the corresponding properties [47]. The magnetite nanoparticles could be synthesis via aqueous co-precipitation, magnetic field induction, CVD, template mediated, etc. [48, 49, 50]. The aqueous co-precipitation of Fe2+ and Fe3+ by a base, usually sodium hydroxide or aqueous ammonia, is the well-known method which is usually carried out for synthesizing the magnetite nanoparticle [51]. This method is the most scalable chemical synthesis routes which results in iron oxide nanospherical crystal. However, there is a study also found that innovative modification in co-precipitation technique through incorporation of special aqueous solution will lead to the formation of nanocubes or nanorods iron oxide particle’s. This was in agreement with Khalil finding’s [52].
Recently, considerable attention has been drawn to production of 1-D magnetite nanorods due to their high surface to volume ration and superior properties. Due to the high aspect ratio, magnetic nanorods have the high values of coercivity and produce a lot of heat in high frequency magnetic field, which offer longer blood circulation times, stronger interaction with tumors, enhanced retention at tumor sites and improved targeting efficiency [47, 53]. All of these reasons stimulate their making in excellent candidates as targeting pharmaceutical carrier or MRI contrast agents. For instance, iron oxide nanocubes including nanorods structure with a length larger than 100 nm could be achieved via thermal decomposition, wet chemical, hydrothermal, template mediated, solvothermal, hydrolysis and sol-gel.
Thermal decomposition method involved chemical decomposition at high temperature, lead to the breaking of the chemical bonds. The thermal decomposition method for synthesis iron oxide nanorods involve metal-organic compound. The obtained nanorods generally with diameter and length within range of 50–100 nm. This method typically led large nanorods structure due to the annealing by high reaction temperature. It is in agreement with Chen et al. finding reported that with the increasing reaction temperature, the aspect ratio of the products decreases to some extent, thus no any rod-like particles produced when high temperatures synthesis method is used [54]. Meanwhile, eventhough the co-precipitation method is a conventional method for synthesizing iron oxide nanorods, yet this method often uses trioctylphosphine (TOP), tributylphosphine (TBP), trioctylphosphine oxide (TOPO) or oleylamine (OA) and other long chain amines as solvents and capping agents in order to prevent the uncontrolled precipitation. Since this nanoparticle used for biomedical application, hence the nanoparticles of iron oxides should be a nontoxic. The usage of nontoxic capping agent and stabilizer eliminates the use of toxic and expensive chemical such as TOP, TBP or amines.
In the past years, the wet chemical synthesis of iron oxide nanorods via one step wet chemical method have been reported by several groups [54, 55]. Chen’s group reported in the one-step synthesis method and a surfactant, polyethylene glycol (PEG) was used as template and ferrous ammonia sulfate was use as precursor [54]. This study agreed that a formation of iron oxide nanorods can be achieved at longer retention synthesis time and adjusting the diffusion of ammonia by implementation a suitable ratio between the rates of deposition and oxidation of ferrous ions. These were in agreement with TEM image the iron oxide synthesize at from 2 to 10 h and it is reveals that the iron oxide nanorods could be obtained upon extended reaction time. By adjusting pressure of ammonia, i.e., adjusting the concentration of aqueous ammonia in the right flask also results in formation of pure magnetite phase. Further study on synthesizing iron oxide nanorods via wet chemical method were also reported by Ahmed and co-worker [56]. The obtained nanoparticles were rod shaped and consisted mainly of maghemite (ϒ-Fe2O3) phase. The nanoparticles also appear superparamagnetic behavior under room temperature.
Solvothermal method is an effective method for producing iron oxide nanorods. Si et al. present a method for obtaining the iron oxide nanorods via solvothermal method, and product showed formation of iron oxide nanorods with diameter size within range of 58–250 nm and width from 8 to 64 nm (Figure 9(a and b)) [57]. The iron oxide nanorods obtained exhibit uniform size and greater dispersion in nonpolar solvent (cyclohexane). It also revealed the single crystalline nature of nanorods is successfully produced upon synthesis process. The effectiveness of solvothermal method in producing iron oxide nanorods was in agreement Sun and co-worker finding, which reported that Fe3O4 single crystal nanorods with a uniform length between 64 and 140 nm can be prepared using Fe(CO)5 in the presence of oleic acid through a solvothermal process [58].
TEM image of iron oxide nanorods in (a) cyclohexane and (b) water prepared via solvothermal method [57], (c) iron oxide nanorods mechanism via template mediated approach, (d) TEM image of the iron oxide nanorods, and (e) high resolution TEM image of iron oxide nanorods synthesized via template mediated approach [59].
Recent by Kloust et al. also discovered that the iron oxide nanorods can be produced directly from template mediated approach [59]. The iron oxide nanorods synthesis directly from iron oleate in one-step procedure. The iron oleate is used as a precursor. In this method, the iron oxide nanodot string together in a row to form rods-structure (Figure 9(c)). Based on the TEM image the formed iron nanorods exhibit a mean length of approximately 24 nm and mean diameter 2.5 nm with an associated aspect ratio of 10 (Figure 9(d)). The iron oxide nanorods produced particularly small and thin nanorods. The nanodot string combination mechanism have been confirmed in TEM micrograph, which shows the alignment of single dot characteristic. The high resolution TEM image of iron oxide nanorods (Figure 9(e)) confirms this characteristic and show twisted crystal-orientations of single nanocrystal. Further magnetic characterization reveals that the iron oxide nanorods synthesized via template mediated approach posed super-paramagnetic behavior. In the blocked state the nanorods exhibit a magnetic easy axis parallel to the long axis of nanorods due to the enhancement shape anisotropy. Kloust et al. [59] also presented a method for preparation of iron oxide nanorods with a template approach, where iron oxide nanodots string together. The procedure uses iron oleate as a precursor and is a one-step synthesis. A precise tuning of the width of the nanorods between 1 and 6 nm was realized.
Hydrothermal method might flexible method for synthesizing iron oxide nanorods. Thus, several procedures have been developed [48, 49, 50]. Hydrothermal methods rely on the ability of water at elevated pressures and temperatures to hydrolyze and dehydrate metal salts, and the very low solubility of the resulting iron oxide in water at these conditions to generate supersaturation [60]. Extremely high supersaturation could be achieved in the reaction process attributed by the lower solubility of metal hydroxides and oxides, thus very fine crystals will form. Similar case with thermal decomposition methods, the hydrothermal system also involves high temperature synthesis condition. Thus, the size of the nanoparticles had a larger particle (if the hydrothermal method proceed under supercritical temperature (<350°C)). This was due to the promotion of crystal growth that results from the dissolution and precipitation process in sub-critical water. The particle size also increased with the increase in reaction pressure in supercritical water [61]. Liang and co-workers report the variation of crystallite and particles size of iron oxide at temperature 250 and 350°C; the crystallite size of iron oxide increased significantly as the temperature was raised from 250 to 350°C. This phenomenon is due to the nucleation process which occurred as the monomer concentration reached the saturation point [62]. Interestingly, the size of particles will reduce and become smaller if the hydrothermal method proceeded under temperature > 380°C (above critical temperature). This is probably due to a rather low solvent power of supercritical water and an extremely high hydrolysis rate of iron salt in supercritical water. Therefore, very high super-saturation is achieved in which results in fine iron oxide crystals nucleating in situ immediately. It is in agreement with Arai et al. study [61]. Eventhough hydrothermal method considered effective in synthesizing iron oxide nanoparticles, yet the particles shape difficult to control in order to form pure rod-like structure.
Other method that effective in synthesizing the iron oxide nanorods is sol-gel method. Piao et al. reported on wrap-bake-peel process for nanostructural transformation from β-FeOOH nanorods to biocompatible iron oxide nanocapsules [63]. This process involves silica coating, heat treatment and lastly the removal of silica layer, in order to transform the phases and structures of nanostructured materials while preserving their nanostructural characteristic. Water dispersible hollow iron oxide nanocapsules were obtained by applying the wrap-bake-peel process to β-FeOOH nanoparticles. The synthesized magnetite nanocapsules could be successfully used not only as a drug-delivery vehicle, but also as a T2 MRI contrast agent.
Although the process of synthesis of metallic nanoparticles provides a number of benefits, it is still difficult to achieve formation of nanoparticles of various shapes and sizes, which is significant as shape and size dictate possible nanoparticle activity. Therefore, regulation of nanoparticle shape and size has received a great deal of attention. When marine microbes were employed to synthesize metallic nanoparticles, consideration was given to a range of factors related to metallic nanoparticle nucleation and formation. More specifically, to achieve metallic nanoparticles of uniform size and shape, the factors of pH, reaction temperature, time and reactant concentrations were taken into account.
The development of metallic nanoparticles depends significantly on the pH of the reaction medium [64]. Gold nanoparticles mediated by Rhodopseudomonas capsulate occurred at pH ranging between 4 and 7, while extracellular formation of gold nanoparticles of round shape and 10–20 nm in size occurred at pH 7 and a number of nanoplates occurred at a pH value of 4. Comparable results were obtained when Shewanella algae were used to synthesize gold nanoparticles intracellularly under conditions without oxygen and with H2 gas serving as electron donor at a temperature of 25°C [65]. Thus, gold nanoparticles of 10–20 and 15–200 nm in size respectively occurred in periplasmic space with pH 7 and on bacterial surface with pH 2.8. Hence, it can be concluded that pH has great significance for morphological modulation and detection of nanoparticle development site.
The dependence of microorganism-based synthesis of metallic nanoparticles as well as nanoparticle morphology and yield on the temperature of reaction is well established. In a recently conducted study, silver nanoparticles were synthesized extracellularly by Phoma glomerate supernatant under conditions of bright sunlight [66]. The maximum yield of silver nanoparticles was achieved at 25°C, while the temperatures of 90, 65, 37 and 4°C were associated with gradually diminishing yield. Furthermore, alkaline pH enabled synthesis optimization. A different study introduced silver nitrate solution in cell-free filtrate of fungus Trichoderma viride and silver nanoparticles were synthesized under conditions without light and at different temperatures for a period of 1 day. Thus, round-shaped silver nanoparticles of 2–4 nm in size formed at 40°C, round- and rod-shaped nanoparticles of 10–40 nm in size were observed at 27°C, and nanoplates of 80–100 nm in size formed at 10°C [67].
Metallic nanoparticle size and shape also depend on the synthesis reaction time. One study employed Vibrio alginolyticus supernatant to synthesize silver nanoparticles extracellularly and observed that the greater the reaction time the higher the yield was, while the UV-vis peak was maintained more or less unchanged; on the other hand, the UV-vis peak shifted toward higher wavelength in the context of intracellular synthesis [68]. The conclusion derived was that extracellular synthesis of silver nanoparticles had time-dependent yield but size was unaffected. However, intracellular synthesis was associated with size enlargement as the reaction time was increased. Comparable results were obtained by a different study that undertook extracellular synthesis of silver and gold nanoparticles by employing single-cell protein (Spirulina platensis) [69]. Nanoparticles expanded in size as the reaction time was increased, whilst also showing greater aggregation and greater instability [70]. Another study synthesized various metallic nanoparticles with a range of microorganism species and observed that yield increased in direct proportion with reaction time increase [71].
The development of metallic nanoparticles is subject to the influence of reactant concentration as well. One study reported that the size and shape of gold nanoparticles were considerably impacted by the use of different gold salt concentration alongside Penicillium brevicompactum supernatant in reaction medium [72]. Gold salt concentrations of 1 and 2 mM respectively resulted in round gold nanoparticles of 10–50 and 10–70 nm nanoparticles. Furthermore, hexagonal and triangular particles developed when round nanoparticles were added. Nanoparticles of 50–120 nm with particles of different shapes (round, triangular, diamond-like) developed at gold salt concentration of 3 mM. A different study also found that lower and higher metal salt concentrations respectively led to the development of round nanoparticles and triangular and hexagonal nanoplates [73]. Moreover, there is evidentiary support that increase in yeast extract concentration leads to the development of nanoparticles of reduced size [74], while increase in fungal filtrate concentration intensifies development of nanoparticles [66]. In addition, a study highlighted that manipulation of parameters of environment and nutrition enabled synthesizing nanoparticles with control of size and shape [71]. Thus, the above evidence confirms that regulation of metallic nanoparticle size and shape is significantly dependent on reactant concentration.
In summary, uniform 1-D magnetite nanorods showed fascinating physical properties this due to the distinct structure-dependent properties of nanorods structures. Larger in both length and diameter of rod-shape particles are expected to share many advantages in the oriental properties of nanorods. Last but not least, nanorods offer more advantages over isotropic (homogeneous and uniform) particles. It can be summarized that the efficiency of nanorods depends strongly on nanorods aspect ratio, volume fraction, polydispersity and orientation. There are many methods for synthesizing carbon nanorods, ZnO nanorods, Au nanorods and iron oxide nanorods. Overall, bottom-up was very effective method for synthesizing nanorods particles. Yet, bottom-up method still suffer with some drawbacks; placing metal into large area, ordered array and purity problem. Due to these reasons, top-down approaches gained interest, but top-down method is time consuming and costly for industrial practical.
The authors acknowledge the financial support from the PUTRA grant-UPM (Vot No: 9344200), MOSTI-e Science (Vot No: 5450746), Geran Putra Berimpak (GPB) UPM/800-3/3/1/GPB/2018/9658700 and University of Malaya’s RU grant (Project No:RU007C-2017D).
Water is most essential for sustaining life and enhancing the quality of life, but it can transmit diseases. When adequate access to clean, safe water is lacking, incidences of waterborne diseases become rampant [1, 2]. Unsafe drinking water is one of the major causes of diarrhoeal diseases, which are known to be a leading cause of mortality globally especially in children aged five and below [3]. The 2015 WHO/UNICEF Joint Monitoring Programme (JMP) update reports that 69% of Nigeria’s population use improved drinking water sources, which are presumed to be safe [4]. However, due to non-functionality, unsustainability, and lack of proper maintenance of most improved water sources, they are often of non-satisfactory quality [1, 5]. Therefore, the reality is that a lesser percentage of Nigerians than presented actually have access to safe drinking water. Furthermore, even where there is access to safe water, because most of these water sources are not located on premises or piped directly into the houses, there is the risk of contamination in the process of collection, transportation, and storage, thereby leaving the initially safe water unsafe at the point of consumption [2, 6]. It is therefore essential to ensure water is safe for drinking at the point of consumption. Point-of-use water treatment implies any water treatment system that purifies water at the point of consumption and it involves effective treatment and safe storage. It has been identified as an important public health intervention which serves to reduce the faecal-oral transmission of diarrhoeal diseases [7].
Recent studies on point-of-use household water treatment systems, suggest that ceramic water filters are the most sustainable and lowest cost options for water purification in developing countries [8]. The essential raw materials, basically clay and combustible bio-wastes, required to make this technology available and accessible in Nigeria are locally available in large quantities. However, there is a wide knowledge gap in the exploration and development of the technology of manufacturing ceramic water filters in the country. As much as there exists a need for household water treatment method such as the ceramic water filters, not many manufacturers engage in the production of ceramic filters. The springing forth of many peri-urban settlements in many Nigerian cities like Akure leaves the nation fraught with an urgent need to explore innovative solutions to put an end in sight to the prevalent water-related health challenges.
While household water treatment and safe storage systems have been considered as effective, low-cost alternatives and a reliable means of achieving safe water at point of use, having shown to significantly reduce diarrhoeal prevalence [6, 7, 9]; very few potters engage in the making of the ceramic water filters. In Nigeria, there are two factories that currently produce ceramic water filters, although production is fraught with many challenges such as understanding the technology behind the working of the filtration system. The major challenge however, to the establishment of a ceramic water filter production facility is the acquisition of the filter press machine.
The ceramic filter press machine is the priority piece of equipment required in the production process of ceramic water filters [10, 11]. The filter press machine, which is mostly hydraulic operated, is used to form the filters into its shape by the application of pressure to the clay mixture in-between a set of moulds. This method of forming is most suitable for making ceramic water filters because a non-plastic material mix is desired and therefore can be only formed successfully by semi-dry pressing techniques. This all-important equipment for the production of ceramic water filters is quite expensive to purchase, with very high shipping and importation costs and tariffs.
Personal communications in a pilot study with operators of ceramic water filter factories in Nigeria reveals that the cost of acquisition of a piece of filter press machine with its corresponding aluminium moulds ranged from $3000 to $3500 (USD). This is also confirmed by other researchers [10], stating that the cost of this press is estimated at over $3000 and therefore is considered a fundamental limiting factor to production of ceramic water filters to meet demands in areas where it is needed. While the Resource Development International - Cambodia (RDIC) approximated the cost at $2300, excluding shipping and handling costs [12]. This is too high an investment cost for a start-up ceramic/pottery business to bear considering the economic conditions in the country. Therefore the only feasible option to the making of ceramic water filters in Nigeria, to improve access to safe drinking water at the point-of-use, is to resort to the design and fabrication of a filter press machine using locally available materials.
The Potters Without borders (PWB) is one of the organizations that have carried out research on ceramic water filters and design of hydraulic filter press machine [10]. The PWB filter press machine design was adopted for this study, whose objective was to design and fabricate a hydraulic filter press unit using locally sourced materials with a view to promote the affordability and availability of this technology for the manufacture of ceramic water filters, consequently increasing access to safe drinking water in Nigeria.
At its inception by Fernando Mazariegos, the ceramic pot water filter was shaped by hand on the potters’ wheel. But in the 1980s, the Central American Institute of Industrial Research and Technology (ICAITI) introduced the use of hydraulic presses in the shaping of ceramic water filters resulting in more efficient ceramic water filter production and performance [10]. However, other literature [13] reports that the first press and the first set of moulds were developed to standardize the shape of the ceramic water filter (see Figure 1).
Ron Rivera working on the first ceramic filter press [13].
While the Potters Without Borders (PWB) press design is the most commonly used, other attempts have been made to explore different press designs to improve the workings and efficiency of the presses in the production of ceramic water filters and to meet the specific socio-economic needs of varying localities. The PWB filter press design operates with a 20-ton hydraulic jack and a hand lever for lifting and lowering the H-slide to which the male mould is attached. It produces the flat-bottomed ceramic water filters, using a set of aluminium moulds.
A recent study [14] on a multi-component water treatment, reported that they created a simple plastic press mould to shape the ceramic component of their water filtration system with the aim to improve efficiency and allow for easy replication. (see Figure 2).
Modelled diagram of the press mould and product [14].
Another study [10] designed a low-cost filter press with the goal of less than $200 in cost, less manpower requirement and shorter manufacture time. Their work concentrated on designing and prototyping a low-cost, filter press using locally-sourced materials. They attempted to achieve a lower filter formation pressure as a key requirement to reducing the cost, considering that using a 2-ton car jack instead of the 20-ton hydraulic jack used by PWB would greatly reduce cost. The press was designed for the round-bottom filters and adopted an inverted design in which the car jack was mounted to the frame headstock and the female mould was suspended on the underside of the jack elevator while the male mould sat on the base [10]. For the moulds, they improvised with the use of inexpensive aluminium bowls (see Figure 3).
A low-cost filter press prototype [10].
A group of researchers [11] in their study described the use of a 30-ton manually operated hydraulic press developed and manufactured by MEC Ltd., India. The press makes use of a screw system to lower and lift the male mould which is attached to the die screw connector plate, while the female mould sits on a base plate which is attached to the hydraulic jack (see Figure 4). This press produces the flat-bottomed, frustum shaped filters of 23 cm height with 25.5 cm base diameter.
Filter press operated with screw and hydraulic system [11].
The Ceramic Filter Manufacturing Manual [15] developed by Pure Home Water, reported two types of press designs for shaping ceramic water filters; the Potters for Peace (PfP) press and the Mani press. The PfP press design as described in the text is a portable press that uses a 20-ton hydraulic jack with a removable female mould while the male mould is attached to a moveable shaft on the frame. It operates a crankshaft system which allows for the lifting and lowering of the shaft that holds the male mould. The hydraulic jack is positioned above the male mould after it has been lowered into the female mould which contains the clay (see Figure 5).
Operating the portable PfP press with crank system [15].
The Mani press has both its male and female moulds attached; while the male mould is attached to an extendable table, the female mould is attached to the press frame. It uses an 8-ton hydraulic jack and works with a pulley system that operates with a hand crank for lifting and lowering the female mould (see Figure 6).
The Mani press [15].
The mould in the PfP press described in the Ceramic Filter Manufacturing Manual [15] is made of nylon while the material used to make the Mani press moulds was not stated in their report but can be made of concrete or metal. It, however, concluded that the Mani press delivered greater advantage and ease in use than the portable PfP press. The RDIC manual [12] describes a fully automated hydraulic system-operated ceramic water filter press. It uses a set of metal moulds, most likely aluminium. The male mould is attached to the frame headstock while the female mould is attached to a moveable shaft which is controlled by the hydraulic system which works with the use of an electric motor (see Figure 7). This action controls the press and the release of the clay filter mix in between the moulds.
An electric motor driven hydraulic press [12].
The features of the various designs of ceramic water filter presses reviewed in the course of this study are presented in Table 1.
Ref. no | Description | Type of filters | Position of moulds | Mould material | Mould moving mechanism | Mode of operation |
---|---|---|---|---|---|---|
14 | Hand press mould | Ceramic filter component | — | Plastic | — | Hand/manual |
10 | Low-cost filter press | Round bottom | Inverted; female above | Aluminium bowls | — | 2-ton hydraulic car jack |
11 | MEC India manufactured press | Flat bottom | Upright; male above | — | Hand-operated screw system | 30-ton hydraulic jack |
15 | PfP portable press | Flat bottom | Upright; removable female mould positioned below | Nylon | Hand-operated crank system | 20-ton hydraulic jack |
15 | Mani press | Round bottom | Inverted; male attached to extendable surface | — | Crank-operated pulley system | 8-ton hydraulic jack |
12 | RDI-C | Flat bottom | Upright; male above | Metal | — | Automated hydraulic system |
10 | PWB | Flat bottom | Upright; male above | Aluminium | Hand-operated lever | 20-ton hydraulic jack |
Features of the various types of ceramic water filter presses reviewed in this study.
After a review of the designs of ceramic water filter presses as discussed hitherto, the PWB ceramic water filter press design was adopted based on the following considerations:
A non-electrically operated press was desired to overcome the challenge of poor electricity supply within the country;
The use of a fully manual system was also not desirable because it will increase the time taken to press one filter; therefore a hydraulic press mechanism was desired;
A lever was preferred for the lowering and lifting of the moulds, to the crank (as in the portable PfP press [15]) and the screw (as in [11]) because it makes the filter pressing more cumbersome and time consuming;
The moulds were preferred fitted to the press frame to overcome the challenge of misalignment of moulds, possible in removable moulds, and as well, the inconvenience and health hazard of lifting heavy moulds in each process of filter pressing (as in the portable PfP press [15]).
Based on these specific requirements, the Potters Without Borders (PWB) ceramic water filter press design was adapted for manufacture in Akure, Nigeria. The PWB ceramic water filter press is said to have several benefits with respect to design and operation. Its high-strength (20-ton) design allows the pressing of flat-bottom filters [10] while creating stability and preventing deformation in the shaped filters. The flat-bottom filters are said to provide more surface area and therefore higher flow rates [10]. Some of the adjustments made to the PWB filter press design, included the replacement of the hydraulic car jack with a locally fabricated industrial hydraulic jack, as well as the design and manufacture of the press mould to fit locally available wide-rimmed plastic containers to meet the water needs in larger households.
Flow chart of steps taken in fabricating the ceramic water filter press.
It became expedient to fabricate a hydraulic press machine to facilitate the shaping of the ceramic water filters by the press cast method. This is the most suitable method of forming the ceramic filters because the mix is highly non-plastic and hence cannot withstand other ceramic forming techniques besides slip casting which is not very feasible at the desired dimensions of ceramic water filters.
For this study to ensure the economic feasibility, sustainability and hence the scalability of the manufacture of the ceramic water filter press in Nigeria, it was important to set a cost limit for fabricating the press; and this was set at 350000 naira (approximately $1000). This was done considering the issue of low access to capital for start-ups, which is common in the country. This study, however, intends to encourage local potters to venture into the production of ceramic water filters by alleviating some of the cost-related challenges of setting up a filter production unit.
All the materials and manpower used in fabricating this press were sourced from within the country. The hydraulic press machine typically consists of two parts; the moulds and the frame which holds the moulds and the hydraulic component. The procedures engaged in the making of both parts are discussed further.
The mould for the filter press machine was designed and made using aluminium as material, which was shaped using the sand casting method. The processes involved in the making of the filter mould include; generating a CAD drawing (see Figure 8), detailing the dimensions of the moulds; and the making of a wooden mould patterns (see Figures 9 and 10) from which sand moulds were derived.
CAD drawing for moulds (material: Aluminium).
Wooden patterns for the mould.
Top view of wooden patterns for the mould.
The mould design was generated during the course of the study using dimensions which were estimated by the researcher to produce a ceramic water filter that would fit into commonly available wide-rimmed large plastic containers. The size of the container was used as mark up for the determination of the dimensions of the moulds. The core and drag mould components were designed to give a pressed ceramic filter product of 30 mm thickness all round; this is to accommodate the high shrinkage possible in most plastic ball clays available for use in South West Nigeria; as well as to allow for longer contact time with silver for the inactivation of pathogens in water and greater possibility of trapping the pathogens as they travel through the filter walls. With this design sketch, a wooden pattern made of cut out pieces of 2-inch plywood held together with resin bond, was derived. The pattern is highly essential to the process because the sand moulds which was used for casting the metal form is taken from it. So it is important to ensure correctness of dimensions and form in the wooden pattern.
The process of making of the sand moulds included filling up firmly, a square-shaped wooden frame in which the wooden pattern has been placed with fine sand (see Figure 11); after which the pattern is taken out and the sand is smoothened out using a metal spoon (see Figures 12–14). The metal cast was then taken from the prepared sand mould.
Filling the frame with sand.
Pattern taken out.
Smoothening the sand mould.
Finished sand mould.
Pieces of waste aluminium collected from the local scrap market were charged into the rotary furnace and melted (see Figure 15) at temperatures between 600 and 700°C. The crucible bearing the molten aluminium was removed from the furnace using a pair of furnace tongs (see Figure 16) and the crucible holding the molten metal was set in a 2-man carrier rod (see Figure 17).
Process of melting the scrap aluminium in a rotary furnace.
Removing molten aluminium from the furnace using a pair of tongs.
Crucible set in the carrier rod in readiness for casting.
It is important to remove dross and check for unmolten particles of other metals before casting (see Figure 18). The molten metal is then poured into the sand moulds by means of crucible tongs and carrier rod (see Figures 19 and 20).
Stoking the molten metal to remove dross and other particles.
Pouring in the molten metal into the sand mould using furnace tongs.
Casting process using the crucible carrier.
In the process of pouring in the molten material, it is important to poke at it using a metal rod to aid the removal of any air bubbles that may have been trapped in while pouring (see Figure 21). The metal cast is afterwards left to cool for about 24 hours before it is removed from the mould (see Figure 22). The surface finish of the cast aluminium mould is mostly dull, lacks lustre and sometimes presents tiny holes as seen in Figure 23. Polishing the metal is therefore important to give a more usable finish to the cast aluminium moulds (see Figure 24).
Poking the poured-in metal to remove trapped air.
Cooling.
Cast aluminium moulds.
Polished aluminium mould.
The last phase in the making of the mould was the machining and polishing of the cast. Aluminium was the material used to make the moulds in this study. This is because aluminium is a non-rust metal and it is more affordable than stainless steel and can easily be machined because it is a relatively soft metal. Aluminium is also a very available material in most scrap markets across the country, and hence easy to access for this purpose. The machining or polishing of the moulds was carried out using a horizontal lathe machine in a privately-owned engineering workshop.
The frame of the hydraulic press machine was made from cast iron and steel parts. The design for the frame was adapted from the Potters Without borders (PWB) ceramic water filter press design (see Figure 25). The PWB filter press design incorporates the use of a removable car jack as its hydraulic mechanism. The design for this study has incorporated a hydraulic controller system which is comprised of a box, an industrial jack to drive the pressing mechanism which is expected to be more durable than the car jack over time and continued use; and a pressure gauge to measure the pressure applied in the pressing of each filter to enhance consistency in production.
PWB design of press machine [10].
The metal parts for the frame were sourced from Akure and Ibadan in South-west Nigeria. Cast iron was the major material from which the parts of the frame were made. Some parts were also of made of steel. The long metal parts were cut into dimensions (see Figures 26 and 27) and holes were drilled through them to enable assembly of the frame using nuts and bolts. Bolting was preferred to welding in the assembly of the machine parts, to allow room for adjustments and for easy movement and transportation of the machine. The cutting and welding of the frame was followed by the mounting of the moulds. The male component of the mould was bolted onto a metal plate which is welded to the headstock of the frame, and the female component was fitted via bolting onto the moveable H-slide (see Figure 28). The lever system which is used to control the lifting of the H-slide bearing the female mould during pressing and release of the moulds, was subsequently fixed in place (see Figure 29) and test run to assess the mould alignment (see Figure 30). The hydraulic jack was thereafter installed and tested in operation with the lever as shown in Figure 31. Finally, the hydraulic control box was installed and connected to the jack and the entire frame was sprayed with paint to improve its aesthetic and prevent rusting (see Figure 32). The making of the frame and the hydraulic control box, as well as the assembly of the moulds was done at Danzaki Engineering Services, a privately-owned mechanical engineering workshop in Akure, Nigeria.
Cut out metal parts for the frame.
Metal parts of frame in mock assembly.
Press frame with moulds mounted.
Installation of the lever mechanism.
Testing the installed lever and jack.
Press with hydraulic system installed.
Finished ceramic water filter press.
The outcome of the study showed the local availability of the required skills and material resources to locally manufacture a ceramic water filter hydraulic press machine in Nigeria. The total cost of the local production of the press though slightly above the set target, is approximated at $1000 USD and is about one-thirds of the cost of acquiring a press of similar specifications of foreign origin without the attending shipping and clearing costs.
The manufactured ceramic water filter press was effective in the shaping of ceramic water filters as indicated in the evenness in form and thickness of the filters pressed during a test run of the filter press (see Figure 33).
Freshly pressed ceramic water filter using the fabricated press.
The technical specifications of the ceramic water filters produced from the manufactured filter press are outlined as having an inner height of 15 cm and inner diameter of 28.5 cm; with an estimated volume capacity of 12 L. This is specified to fit into a 30-L capacity bucket with a rim diameter of 30 cm. Shrinkage allowance of 10% was estimated and factored into the design to ensure the resulting filters fit onto the desired bucket.
However, there were a few limitations to the study as outlined thus: At the size required for the set of moulds, it was difficult to find a lathe machine of a size that could hold the cast moulds for machining. Therefore, alternative materials may be explored besides aluminium, especially such materials as would not require machining/polishing. Also, there were issues surrounding the dimensions presented in the CAD sketch as generated by a draughtsman, this resulted in error in the moulds cast. This was, however, corrected by altering the dimensions of the mould during the process of machining in order to achieve even thickness around the product; and this action reduced the size of the mould and hence the resulting filter is shorter than other filters available.
This book chapter documents the procedure and results obtained in a study carried out to explore the local manufacturing of a ceramic filter press in order to prove the viability and cost efficiency of producing it locally as compared with the cost of acquiring the imported presses. This is in a view to encourage the set-up of more ceramic water filter producing factories in Nigeria, thereby bringing closer home the technology that would make clean, safe water more accessible and available to communities and households across the country.
The study indicates that ceramic water filter presses with hydraulic components as well as its corresponding set of moulds can be successfully and inexpensively manufactured in Nigeria, using all materials and skills sourced locally from within the country.
The authors would like to acknowledge the Management of the Federal University of Technology, Akure and TETFund for providing funding for this work under the IBR grant with reference number, VCPU/TETFund/155.
We appreciate Engr. A. Smart and Engr. Idowu of EMDI, Akure, for analyzing the possible designs for the hydraulic press system with us at the commencement of this study; Mr. Yekin Obe and staff of Foundry Department, FIIRO, Lagos, for their assistance with the casting of the filter moulds; and Mr. J. O. Oke and Mr. M. Familusi of the Industrial Design Department, FUTA for their assistance in the entire course of the study and specifically for test running the equipment after its manufacture. Our appreciation also goes to Robert Pillers for reviewing the filter press in progress and making useful inputs that led to some adjustments.
We would like to declare that there is no conflict of interest.
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