Advanced Powder Technology 19 (2008) 443457

www.brill.nl/apt

Review paper Review of Recent Research on Nanoparticle Production in Thailand

Tawatchai Charinpanitkul a , Kajornsak Faungnawakij b and Wiwut Tanthapanichakoon b,
a

Center of Excellence in Particle Technology, Chulalongkorn University, Bangkok 10330, Thailand b National Nanotechnology Center, National Science and Technology Development Agency, Pathumthani 12120, Thailand Received 10 April 2008; accepted 2 May 2008

Abstract Powder technology has already extended its scope of interest to nanoparticles with novel properties and functionalities. Since the establishment of the National Nanotechnology Center (NANOTEC) in 2003, research activities in nanotechnology have shot up remarkably, including the production of nanoparticles via physical, chemical and biological methods. This article reviews and introduces recent works on nanoparticle production in Thailand, especially NANOTEC and her nation-wide network of Centers of Excellence. The categories of nanoparticles of interest extend from metal and zinc oxide nanoparticles to carbon nanoparticles and titanate nanostructures. However, thin lms and nanolms lie beyond the scope of this review. Koninklijke Brill NV, Leiden and Society of Powder Technology, Japan, 2008 Keywords Nanoparticle technology, vapor-phase production, liquid-phase production, solid-phase production, Thailand, carbon nanotubes

1. Introduction Nanotechnology is recognized as a revolutionary manufacturing technology of the 21st century involving multidisciplinary research issues that rely on the understanding and control of substances at the nanoscale length of around 1100 nm. Nanotechnology is not limited to working with matter at the nanoscale, but also encompasses research and development of materials, devices and systems that exhibit novel properties and functions due to their nanoscale dimensions or components. Similarly, nanoparticles refer to ultrane particles whose sizes are in the range of
*

To whom correspondence should be addressed. E-mail: wiwut@nanotec.or.th

DOI:10.1163/156855208X336693

Koninklijke Brill NV, Leiden and Society of Powder Technology, Japan, 2008

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1 nm to several hundred nanometers, depending on the materials, elds and applications concerned [1, 2]. They include particles smaller than the so-called submicron particles and the longest wavelength of visible light of about 400 nm. In some applications, they are limited to particles smaller than 1020 nm where their physical properties would drastically change [1]. Since the establishment of the National Nanotechnology Center (NANOTEC) in 2003, research activities in nanotechnology in Thailand have shot up remarkably. As in many countries, nanotechnology has opened new doors to innovations in science and technology, thereby enabling academic and technological platforms and capabilities to improve the life quality of the Thais and enhance the competitiveness of Thai industries in the global arena. NANOTEC has set up a nation-wide network of Centers of Excellence (COE) in nanoscience and technology strategically located in eight universities across the nation. In addition, independent and joint research works with academic institutions and the industrial sector have been implemented in various aspects of nanoparticle synthesis, production, processing, handling, applications, utilizations and safety. Meanwhile, powder/particle technology has gradually become well established in Thailand since the setup of the Thai Powder Technology Center in 1993 and the Center of Excellence in Particle Technology (CEPT) in Chulalongkorn University in 2002. This article reviews and introduces the recent works on nanoparticle production in Thailand with the focus on recent works in NANOTEC, her network of COEs and CEPT. The types of nanoparticles of interest extend from metal and metal oxide nanoparticles to carbon nanoparticles (CNPs) and titanate nanotubules. However, it should be noted that thin lms and nanolms lie beyond the scope of this review. 2. Nanoparticle Production Technology Production of nanoparticles requires understanding of the fundamentals of nanoscale chemistry and physics, and know-how to commercialize them. Broadly speaking, there are two approaches to nanoparticle production: top-down and bottom-up. The former makes a material decrease its size from large to nanoscale, whereas the latter produces nanomaterials by starting from the atomic level [2]. In a narrower sense, the production methods can be classied in several ways, e.g. by the type of growth media and the form of products. Based on the phase in which nanoparticles were formed and regardless of the original phases of the precursors, this review groups the production methods in three categories: production in the vapor phase, liquid phase and solid phase, respectively. Figure 1 illustrates the corresponding simplied concepts of nanoparticle formation. Table 1 summarizes the characteristics of nanoparticles produced via various methods. Nanoparticle production in the vapor phase is often carried out at elevated reaction temperatures and under vacuum, e.g. arc discharge in gas [3, 4] or, under atmospheric pressure, e.g. arc discharge in liquid [5], pyrolysis [6] and chemical vapor deposition [7]. It is worth noting that athough arc discharge can be performed either in gas or liquid, particle

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Figure 1. Schematic diagram of simplied concepts of nanoparticle production in gas, liquid and solid phases.

formation proceeds only in the vapor phase. Generally the particle formation mechanism can be described as follows: (i) vaporization of precursors along with some catalyst, (ii) nucleation and (iii) growth stage. The ow eld pattern of the vapor-

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Table 1. Characteristics of nanoparticles produced via various methods References Particle size (nm) Aspect ratio () BET surface area (m2 /g) [19]

Production method

Characteristics of nanoparticles

Materials

Morphology

Arc discharge arc-in-liquid 1030 2050 2100 NR NR

carbon

MWCNTs multi-shelled nanoparticle

Pyrolysis copyrolysis 2040 1030 1020 1 4 25170 25170 45133 1.75.6 6176 520 (rod) 25005000

[23] [24] [25] [26] [27] [28] NR 179258 NR 87112 203 [34] [29] [30] [33] [31] NR NR NR NR NR NR

ame pyrolysis 7196 100400 130 (pod size) 60180 60180 2270 67110 10 9901880 815 712

Fe-encapsulated carbon Pd-doped ZnO

MWCNTs nanocapsule sphere/rod-like/hexagonal

NR NR 63.780.1

Other gas-phase reaction oxidation

ZnO

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Au-doped ZnO TiO2

nanosphere tetrapod tetrapod/multipod nanowire nanowire nanowire

Solvothermal solvothermal sonication-assisted hydrothermal hydrothermal

ZnO titanate PbTiO3 TiO2

nanorod nanotubule nanopowder sphere nanorod/nanoparticle composite

Table 1. (Continued.) References Particle size (nm) Aspect ratio () BET surface area (m2 /g) [38]

Production method Morphology

Characteristics of nanoparticles

Materials

Solgel conventional 510

V-doped ZnO

surfactant-assisted

TiO2 NiO Pt-loaded TiO2

nanorod sphere sphere sphere sphere

200 100 <1000 1525 12 (Pt), 525 (TiO2 )

NR NR 125 38 89

[37] [39] [40]

Other liquid-phase reaction reduction

electrospinning

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templating emulsion liquid membrane microemulsion

Au Au Ag Ba0.6 Sr0.4 TiO3 NaCo2 O4 TiO2 Au hydroxyapatite ZnS

disordered (aggregates) sphere/polygonal sphere nanober nanober nanober nanowire (step-cone) sphere nanorods ellipsoid sphere nanotube

3060 1550 5 160200 20200 80100 200 <20 200750 70120 5100 2040

NR NR NR NR 80 35 50100

NR NR NR NR NR NR NR 58227 NR NR NR NR

[42] [41] [43] [45] [46] [47] [44] [49] [48]

NR not reported.

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ized species and type of catalyst play key roles in the formation mechanism [810]. Various nanoparticle products could be obtained from these techniques, e.g. singlewalled/multi-walled carbon nanotubes (SWCNTs/MWCNTs) and metal/metal oxide nanoparticles. Nanoparticle production in the liquid phase follows a wet chemical route. A number of methods have been proposed for controlling the type, shape and size of nanoparticles, ranging from the solvothermal method, including the hydrothermal method operating at high temperature and pressure, to the solgel method, templatebased method and micelle/microemulsion method operating at low temperature. In some cases, combined methods, such as the surfactant-assisted templating solgel method and hydrothermal microemulsion method, have been employed. Generally, the liquid-phase method is conducted in a batch or semibatch system. The particle formation mechanism in liquid phase is similar to that of the gas phase. The nanoparticles can be formed in amorphous and crystalline phases, while their size and shape can be controlled by controlling the nucleation and growth rates of particles. The products range from metal/metal oxide nanoparticles/nanobers to semiconductive compounds. Production of nanoparticles in the solid phase has recently been developed. Often referred to as the mechanochemical method [11, 12], the most commonly used method generally employs a grinding method and can produce nanoparticles of metals, metal oxides, complex oxides, etc. [1]. The resultant nanoparticles have unique characteristics such as narrow size distribution and good dispersibility. Since few research works on nanoparticle production by solidsolid reactions, such as grinding and vibro-milling, have been carried out in Thailand [1317], they will not be discussed in this review. 3. Gas-Phase Production 3.1. Arc Discharge There are many methods to produce CNPs, e.g. laser ablation, vacuum arc discharge, thermal pyrolysis of organic compounds and plasma-enhanced vapor deposition [5, 6, 10, 18]. Meanwhile, novel economical processes for synthesizing CNPs have been developed and the arc in water method is one of the promising techniques [10]. Arc plasma is generated by gradually reducing the gap between the anode and cathode, which are generally made of graphitic carbon. As the carbon electrodes are vaporized, molecular carbon clusters are formed, which in turn undergo a self-assembly process to form carbon nanostructures. Simultaneous heat and mass transfer during arc discharge and formation of CNPs are recognized as the key controlling parameters for CNP synthesis. Sano et al. imposed a convective ow onto the arc plasma and discovered an optimal condition in which convective cooling could provide the highest yield of CNPs [10]. Recently, electrodes made of carbon and its composites as well as alternative carbon sources, such as liquid hydrocarbons, have been employed to produce carbon

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Figure 2. Typical TEM images of nanoparticles produced via arc discharge and pyrolysis methods: (a) MWCNTs and multi-shelled CNPs synthesized by arc discharge in ethanolwater, (b) highly magnied image of a MWCNT tip which reveals a clear graphene layer and (c) CNTs synthesized by pyrolysis at 800 C with an inset magnied image [19, 23].

nanoparticles and their derivatives. Muthakarn et al. conrmed that arc discharge in alcohols, alkanes and aromatics provided higher CNP yield than the conventional arc in water [19]. Figure 2 reveals a typical example of transmission electron microscopy (TEM) images of the synthesized CNPs in the case of pure ethanol. The main product was MWCNTs, while some multi-shelled carbon nanoparticles were also obtained. The magnied image in Fig. 2(b) reveals that the synthesized MWCNT is made of multi-layers of seamlessly rolled graphene sheets. 3.2. Pyrolysis Thermal pyrolysis in the absence, or with a trace, of O2 is known to be efcient for large-scale production of CNPs at low operating costs [6, 20]. The pyrolysis of organometallic compounds, such as ferrocene and nickel phthalocyanine, was employed for synthesizing CNTs and carbon nanocapsules (CNCs) containing metallic nanoparticles. The encapsulated metallic particles could act as a catalyst for CNP synthesis. However, using additional hydrocarbon sources, e.g. benzene [21] or acetylene [22], mixed with the organometallic compounds can either provide more CNPs or reduce the required amount of organometallic compounds.

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Charinpanitkul et al. successfully employed copyrolysis of ferrocenenaphthalene mixtures in nitrogen to synthesize CNPs [23]. The resultant CNTs and CNCs contained Fe particles in their carbon shells. Figure 2(c) shows examples of TEM image of the nanoparticle products. It was found that the nanostructure, particle size distribution and yield of the synthesized products strongly depended on the pyrolysis temperature. The hydrodynamic diameter of the synthesized CNPs was around 4080 nm. Using zinc naphthenate and Pd (II) acetylacetonate dissolved in toluene/acetonitrile as precursors, Liewhiran et al. employed ame spray pyrolysis to produce ZnO doped with 05 mol% Pd in a single step [24]. 3.3. Other Alternative Approaches Having high potential for fabrication of short-band semiconductor laser and visible photoelectronic devices, ZnO is one of the most promising oxide semiconductors. Charinpanitkul et al. [25, 26] employed the gas-phase reaction to control the synthesis of ZnO nanospheres, nanotetrapods and nanomultipods. Scanning electron microscopy (SEM) and TEM images of typical ZnO nanoparticles formed either in a single-heated-zone reactor or in a double-heated-zone reactor equipped with/without an orice are shown in Fig. 3. The orice is employed to enhance

Figure 3. Typical SEM images of ZnO nanoparticles: (a) tetrapods with long-length pods, (b) tetrapods with short-length pods and (c) nanopowders. Insets in (a) show magnied TEM images [25, 26].

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the mixing between Zn vapor and air. The synthesized ZnO particles were collected on a silicon wafer while being quenched with cooling water in order to enhance deposition ux by thermophoresis and to avoid the growth of the collected particles on the substrate. Combining the experimental results with computational uid dynamics simulations, the formation mechanisms of ZnO nanotetrapods and nanospheres have been modeled. Meanwhile, Hongsith et al. prepared ZnO nanowires and Au-doped ZnO nanowires via oxidation reaction at 600 for 24 h. An ethanol sensor based on these ZnO nanowires was successfully fabricated by applying Ag electrodes at each end of the detector tube and inserting a coil heater into the tube [27]. Titanium dioxide (TiO2 ) and TiO2 -derived nanoparticles are widely used in various applications, such as dye-sensitized solar cells, photocatalytic wastewater treatment, gas sensors, etc. Although TiO2 nanoparticles are commonly produced via wet chemical routes, e.g. solgel, microemulsion and hydrothermal methods, gas-phase methods have been reported, such as the metalloorganic chemical vapor deposition process and thermal evaporation method. However, none of these dry methods could grow the TiO2 nanostructures as a size-controlled process. Daothong et al. reported the size-controlled growth of TiO2 nanowires by oxidation of Ti substrates in the presence of ethanol vapor at low pressure and high temperature [28]. 4. Liquid-Phase Production 4.1. Solvothermal Synthesis Solvothermal synthesis is one of the most powerful strategies employed for the crystallization of various unique nanoparticles. A solvothermal reaction is the reaction of a hot solution within or on the surface of a substance. When the solvent is water, it is called hydrothermal synthesis. The reactions proceed in a sealed pressure vessel (autoclave) at temperatures above the boiling point of the solvent and internal autogeneous pressure. Viriya-empikul et al. discovered a step towards the length control of titanate nanotubules (TNTs) using hydrothermal reaction with sonication pretreatment [29]. Without sonication, the average length of the TNTs synthesized by the hydrothermal process was as short as around 60 nm due to constricted diffusion of the hydroxyl (OH ) and sodium ions (Na+ ) through the narrow interparticle space of the agglomerated titania precursors, thereby retarding the TNT formation. When the sonication pretreatment was applied, much longer TNTs with an average hydrodynamic size of 4901760 nm were produced. A mechanism contributing to the length control was proposed based on microscopic observations. Rujiwatra et al. showed that nanoparticles of perovskite lead titanate (PbTiO3 ) were successfully prepared from a stoichiometric proportion at low temperature and short reaction time of only 130 C and 3.5 h, respectively. The employment of ultrasonic treatment prior to hydrothermal reaction was examined in detail. Ultrasonic waves simultaneously acted

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both as a catalyst to lower the hydrothermal reaction temperature to a level suitable for the single-phase PbTiO3 and as an external inuence to provide a high degree of size homogeneity [30]. Pavasupree et al. synthesized high surface area TiO2 nanoparticles with mesoporous structures by the hydrothermal method. Various forms of nanoparticles, i.e. nanopowders, nanosheets, nanorods and nanowires, could successfully be synthesized with different features of particle size, BET surface area, pore structure and photocatalytic activity [31, 32]. Supphasrirongjaroen et al. synthesized pure anatase TiO2 nanopowders by the solvothermal method. The TiO2 spheroidal powder was subjected to rapid quenching in various media such as H2 O, air and liquid N2 . The quenching process represented a simple novel route for modifying the surface defects of nano-TiO2 and its photocatalytic activity for ethylene decomposition [33]. Tonto et al. showed that ZnO nanorods could be prepared by a one-step solvothermal reaction of zinc acetate in various alcohols. The as-synthesized ZnO was found to be an aggregation of nanorods. The linear relation between the boiling point of the solvent and the aspect ratio of the nanorod can be used to select the appropriate solvent for the preparation of ZnO nanorods with the desired aspect ratio [34]. 4.2. SolGel The solgel process is a simple wet chemical route for the synthesis of colloidal dispersions of inorganic and organicinorganic hybrid materials, particularly oxides and oxide-based hybrids in various forms of powders, bers, thin lms and monoliths [35, 36]. Since the precipitated powder obtained is amorphous in nature, further heat treatment is generally required for crystallization. Phonthammachai et al. prepared mesoporous nanocrystalline titanium dioxide via the solgel technique using titanium glycolate as precursor in HCl solution at various HCl:H2 O ratios [37]. The kinetics of formation was thoroughly discussed. The material calcined at 800 C was found to consist primarily of spherical particles with diameters smaller than 1 m. The fractal dimension of the critical gel cluster decreased with the acid ratio, whereas the gel strength increased. Apparently an increase in the acidity led to a less-dense but somewhat stronger network structure. Maensiri et al. reported the optical properties of nanocrystalline powders of the wurtzite V-doped ZnO synthesized by a simple solgel method using metal acetylacetonates of Zn and V, and poly(vinyl alcohol) as precursors [38]. The morphology of the powder as revealed by SEM and TEM was affected by the amount of V, causing the formation of either nanorods, nanoparticles or both forms. The photoluminescence spectra of all the samples showed four distinct bands: a strong ultraviolet emission, a weak blue, a weak bluegreen and a weak green, which indicated their high structural and optical quality. Sreethawong et al. synthesized a series of metal-based mesoporous oxide nanoparticles under mild conditions through a facile route of modied solgel process with surfactant-assisted templating technique. Nanocrystalline mesoporous structures of NiO, Pt-loaded TiO2 , In2 O3 and

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Nd2 O3 were successfully synthesized by properly manipulating the hydrolysis and condensation steps of precursors and solvents, respectively [39, 40]. 4.3. Other Alternative Approaches One of the popular alternative methods is the reduction process [4143]. Patungwasa and Hodak controlled the size distribution and, to a minor extent, the shape of Au nanoparticles prepared by adjusting the pH of the reacting mixture in the citrate reduction of AuCl4 [42]. The resulting nanoparticles ranged from polyhedron types obtained at low pH, elliptical particles at intermediate pH and spheroids at pH higher than 7.0. The charge of the citrate stabilizing agent modulates the aggregation process after reduction of the AuCl4 ion. Dubas and Pimpan synthesized Ag nanoparticles having average size of 5 nm by reduction of silver nitrate in the presence of humic acids, which acted as capping agents [43]. When exposed to an increasing concentration of sulfurazon-ethyl, the solution with suspended nanoparticles was found to change from yellow to orange red and purple as the herbicide concentration increased. Recently, Laocharoensuk et al. developed a method to synthesize step-like porous Au nanowires of different shapes and diameters by sequentially depositing alloy segments with different Au:Ag ratios and dealloying the Ag component. For example, step-cone and nano-barbell porous Au nanowires were generated by a membrane-templated sequential deposition of AuAg alloy segments from plating solutions of monotonically decreasing or alternating Au:Ag composition ratios [44]. Electrospinning was originally developed for making ultrane polymer bers. Recently electrospinning has been applied to the synthesis of organicinorganic hybrid bers. The morphology of the nanobers depends on the process parameters such as applied electric eld strength and type of precursor solution. Maensiri et al. focused on the production of metal oxide nanobers by the electrospinning technique [46, 47]. Nanobers of sodium cobalt oxide, barium strontium titanate and TiO2 with a diameter range of 20200 nm were successfully produced. Charinpanitkul et al. synthesized ZnS nanoparticles with distinguishable morphology in quaternary water-in-oil microemulsion systems using various types of cosurfactants [48]. It could clearly be shown that the size and the morphology of the ZnS nanoparticles are dependent upon the types of cosurfactant and the reactant concentration as well as the molar ratio of water to the surfactant. Employing various synthesis conditions, nanorods, nanotubes, hollow tubes, spherical quantum dots and ellipsoidal nanoparticles could be synthesized. Further investigations on the accurate control of ZnS size and morphology were conducted with collaboration among Thai and Indian researchers. Jarudilokkul et al. prepared hydroxyapatites (HAp) nanoparticles by means of an emulsion liquid membrane system (ELM) or water-in-oil-in-water system [49]. The aim of the work was to evaluate the preparation of HAp nanoparticles using ELM consisting of a mixture of biodegradable surfactant and an extractant caproic acid. The ELM system yielded nanoparticles with spherical morphology and narrow particle size range (smaller than 70 nm),

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which are signicantly different from those prepared by the precipitation method. An increase in the reaction and calcination temperatures resulted in a reduction of the specic surface area. 5. Conclusions This article reviews and introduces recent works on nanoparticle production in Thailand, especially NANOTEC and its COE network. The review introduced a number of production methods, such as arc discharge in gas or liquid, pyrolysis and gas-phase oxidation, as well as solvothermal, including hydrothermal, solgel, electrospinning, emulsion/microemulsion and liquid-phase reduction. A variety of nanoparticle products, such as CNTs, Fe-encapsulated CNCs, metaldoped/undoped ZnO and TiO2 , and metallic Au and Ag, can be successfully formed as tubes, spheres, rods, tetrapods, multipods, sheets, wires and bers. Acknowledgments Technical support from researchers at NANOTEC is acknowledged. T. C. acknowledges nancial support from the Centennial fund of Chulalongkorn University to the CEPT. References
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