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The CLOU and conversion performances were studied by a micropacked bed reactor, and crystalline phase structure and homogeneity and bulk density identified as the most important parameters affecting the performance of the OCM. Bulk density is correlated with the sintering temperature, atmosphere and time at sintering temperature, while phase homogeneity is a function of the raw materials chosen, agglomeration method and sintering procedure.

Specific challenges are identified in the control of slurry homogeneity and sintering conditions in upscaled production. The fabrication parameters of the otherwise same ingredients result in quite different morphology and quality of performance in large scale.

The development of power generation technologies using conventional hydrocarbon fuels with carbon capture and storage CCS is a necessary solution to link the contemporary power technologies with environmental demands while all-renewable power technologies emerge. In this context, chemical looping combustion CLC is an interesting technology, as CLC allows higher efficiency and lower cost compared to other oxy-combustion technologies.

In CLC, oxygen from the air is utilized indirectly in the combustion reactor fuel reactor via a solid oxygen carrier material OCM that cycles between an air reactor where OCM takes up oxygen from air and a fuel reactor where OCM combusts the fuel.

As it intrinsically purifies the used oxygen, it removes the necessity for a stand-alone cryogenic air separation unit. The OCM is generally a binary, ternary or quaternary transition metal oxide, which utilizes the transition metal redox activity to uptake and release oxygen [ 1 , 2 , 3 ]. In the context of fast circulating fluidized bed CLC configuration, the OCM is subject to substantial chemo-mechanical stresses during the redox cycling, through which it must retain a high oxygen capacity, fast redox kinetics and good mechanical properties [ 4 , 5 , 6 ].

Furthermore, for industrial application the cost of materials must be low, the component elements abundant, and the active materials and their by-products must be environmentally benign and non-toxic. Considering this long list of demanding requirements, only a handful of materials are proven to pass these criteria. This family of perovskites is especially of interest for large CLC applications, due to low cost and wide abundance of Ca and Mn ores as well as their relatively small environmental impact [ 7 , 8 , 9 ].

Although undoped CaMnO 3 perovskite oxide is still considered, it is more common to see doped calcium manganite in publications focusing on perovskite OCMs. On A-site doping, partial substitution of the calcium by strontium, barium and lanthanum [ 12 , 13 ] is reported, as well as A-site-deficient compounds [ 14 , 15 ]. More relevant and interesting is the doping of the transition metal on the B-site, with partial substitution of manganese by magnesium, iron, titanium, or a combination of two or more of them [ 14 , 15 , 16 , 17 , 18 , 19 , 20 , 21 , 22 , 23 , 24 , 25 ].

Although it has limited miscibility in the perovskite structure, magnesium has positive catalytic effect on the methane reforming.

The most important dopant is titanium, as stability of the perovskite structure is shown to be enhanced by substitution of Ti on the B-site [ 15 , 25 , 26 ]. This is due to the higher enthalpy of formation of CaTiO 3 compared to CaMnO 3 [ 27 ], which stabilizes the perovskite structure at reducing conditions of the fuel reactor. Furthermore, it has been shown that it has good chemical stability and shows small dimensional changes upon redox cycling [ 30 ].

It is also observed that the re-oxidation is faster for Ti-substituted CaMnO 3 at high temperatures [ 22 ], and additional Fe doping positively influences the reduction reaction rate and broadened the operation window of the OCM to lower temperatures as well as improve microstructural stability during redox cycling [ 16 ].

Although Ti-doping does not assist with the known sulfur intolerance of CaMnO 3 [ 14 , 20 , 21 ], remedial technologies for reactivation of the poisoned OCM in situ in the fuel reactor are already developed [ 31 ]. In this study, we analyze the mechanical and thermochemical performance of the laboratory-scale and ton-scale OCMs with the nominal composition CaMn 0.

CaMn 0. Two OCM samples with the same nominal composition were manufactured and studied. The first sample was manufactured at laboratory scale by VITO using a semi-industrial spray-drying method.

The second sample was manufactured at the ton scale by Euro Support using an industrial spray-drying technology. The description of manufacturing of both samples is as follows:. This suspension was then homogenized using a Netzsch horizontal attrition mill prior to spray drying. During spray drying, the water-based suspension was continuously stirred with a propeller blade mixer while being pumped to the 2-fluid spray-dry nozzle, positioned in the lower cone part of the spray drier type 6.

The suspension was atomized into a large number of small droplets in the chamber of the spray drier, which was filled with hot air from the top, thus creating a mixed flow regime. As such, the droplets quickly achieve a spherical shape due to surface tension effects.

In addition, the large surface-to-volume ratio of the droplets allows rapid water evaporation, resulting in dry particles which are subsequently separated from the hot air. In order to develop a stable industrial process, the stability of the raw mix slurry needed to be extended.

In order to obtain the desired final particles size with a high yield ratio, a single fluid high-pressure system was used in place of a 2 fluid spray-dry nozzle. This is known to give a sharper particle size distribution especially for bigger spheres as needed for the OCM production. In the high-pressure nozzle, the droplet formation is achieved by a combination of a nozzle plate through which the suspension is pressed via a swirl chamber that creates an additional circular movement in the suspension.

The formation of the spheres is a function of the pressure, the nozzle size and the rheological properties of the suspension. Therefore, the change in atomization technology also required changes in the rheological behavior of the suspension in order to get a similar shape for the spheres.

The rest of the spray-drying process was identical to the process of VITO. The full sample was calcined in a stacked saggar configuration. Samples were characterized before and after the redox cycling. The sieved materials were deposited on conductive adhesive tape and excess material gently blown off. Images were acquired based on secondary electron SE detectors which show topographic contrast and back-scattered electron BSE which reflect the local density of the samples high density induces high brightness.

Nitrogen was used as the carrier gas in a single-point BET surface area measurement. The sample was then cooled down to room temperature in nitrogen. XRD patterns were recorded at room temperature both before and after the experiment.

The composition of the outlet gas was followed by mass spectrometry in order to study the CLOU effect and conversion. Microstructure and morpho-chemical mapping of laboratory-scale up and ton-scale bottom CMTM samples. The EDS morpho-chemical mapping of constituent elements in average magnification is shown to the right.

High-magnification back-scattered electron images confirm that the microstructure and present phases are, however, different. The fresh laboratory-scale CMTM material is highly spherical and contains minimal doughnut or necking.

X-ray diffraction measurements support the SEM—EDS results and suggest that the predominant phase in the sample is a perovskite of approximate stoichiometry of CaTi 0. The element analysis also reveals separate Ti-rich and Mn-rich areas, supporting the coexistence of calcium manganate phases with the calcium manganese titanate observed by XRD.

Rietveld fit to the room temperature data for laboratory-scale CMTM sample. The microstructure and morpho-chemical mapping of fresh ton-scale CMTM samples are also presented in Fig. Although similar in nominal composition, this material differs from laboratory-scale synthesized sample in microstructure and grain sizes.

The microstructure is also quite different, and the grain sizes are much smaller. The sample is also inhomogeneous with respect to composition, with Ca-, Mn- and Ti-rich areas evident in the elemental mapping.

Despite the relatively higher density, a lower level of reaction is indicated by the microstructure. It is noted that the mechanical strength is equivalent to that of laboratory-scale batch. The minor perovskite phase exhibits unit cell dimensions close to those reported for CaTiO 3 [ 36 ] and so is presumed to be a Ti-rich member of the same solid solution.

Though solution of Ti into CaMnO 3 would be expected to raise these transition temperatures [ 36 ], our observation is in good qualitative accord with the results of Leonidova et al.

The most important parameters affecting sintering are temperature, time and atmosphere. These parameters were investigated in depth for this system Jing et al. It was also shown that for upscaled calcination, an air atmosphere should be used. In Fig. As the firing temperature is closely correlated with crystalline phases formed and their homogeneity, as well as the sample density, it primarily defines most of the performance characteristics of the CMTM OCM: Selectivity and activity toward chemical reactions such as methane conversion are a function of the crystalline phases present and their available surface area, and mechanical properties such as attrition index through changing the crushing strength are a function of sample density Fig.

A difficult balance is then sought, which trades density and thus strength for increased surface area and thus increased activity , while ensuring the presence of the correct crystalline phases.

To achieve the optimum balance, samples must be processed within a relatively narrow sintering temperature window. The significantly higher density obtained for the ton-scale sample here, despite successful pre-sintering studies to determine the optimum firing temperature, highlights the difficulties with maintaining a homogenous and controlled thermal regime when upscaling.

The attrition and conversion values are extracted from [ 23 ]. In order to study CLOU, redox performance and differences in the reaction rates of the two CMTM samples, pulsed and continuous analyses are performed in a micropacked bed reactor. The results for both samples are summarized in Fig. The left part of this figure shows the CLOU effect oxygen release under He inert condition, while the right part shows the re-oxidation oxygen uptake.

Considering the equal amounts of O 2 and N 2 in the oxidizing gas prior to and after the inert step, the difference between the O 2 and N 2 graphs corresponds to the oxygen CLOU capacity of the sample. It is clear from Fig. Therefore, at any time, the N 2 concentration can be used as a reference. By applying this reference, via subtraction of N 2 Fig. From Fig. Oxygen release in He CLOU left and oxygen uptake during oxidation right for laboratory-scale top and ton-scale bottom samples.

As the nominal composition of both samples is equal, it is clear that the better homogeneity and lower density of the laboratory-scale sample result in better CLOU performance than for the ton-scale sample. The CLOU capacity decreases with decreasing temperature, and the laboratory-scale material has the highest CLOU capacity at all the temperatures of study. This is due to an increased fraction of CMT perovskite structure in this sample.

The ton-scale sample exhibits much lower CLOU capacity compared to its nominal value, due to its lack of complete intermixing and unreactive CaO left over in the structure.

Very small reforming activities are observed. Experiments using CH 4 as reductant were also performed on both samples. The results for this are shown for both samples in Fig. This figure focuses only on the reduction part and shows the concentration of CO 2 in outlet gases during reduction with methane.

This confirms the lower CLOU capacity for the ton-scale sample, as the CH 4 conversion is also lower compared to the laboratory-scale one.

This difference is particularly pronounced at lower temperatures where the bulk oxygen diffusion is significantly lower, and cannot balance for the smaller specific surface area of this sample.

Concentration of CO 2 in outlet gases. The formed crystalline phases, their homogeneity and achieved bulk density are identified as the most important parameter affecting the performance of the OCM. Bulk density is directly and significantly correlated with the sintering temperature, under the applied conditions.

In other words, most of the important parameters defining the performance of the perovskite OCM are decided by the sintering temperature if time and atmosphere are kept constant. These parameters include crushing strength, attrition index, specific surface area, CLOU capacity and gas conversion.

Production of granulates with high ratios of crystalline perovskite phases in large scale needs further optimization in order to better homogenize formed crystalline phases, most importantly through optimization of large-scale calcination procedure.

J Therm Anal Calorim. Fe 2 O 3 —Al 2 O 3 oxygen carrier materials for chemical looping combustion, a redox thermodynamic and thermogravimetric evaluation in the presence of H2S.

Applied Nanotechnology takes an integrated approach to the scientific, commercial and social aspects of nanotechnology, exploring:. In this 2e, new chapters have been added on energy applications and the role of nanotechnology in sustainability. The section on the safety of nanoproducts has also been updated, and material on funding and commercialization has been updated and expanded, with new case studies illustrating the experience of new startups in a challenging economic environment.

Nanostructured semiconductor metal oxides, such as TiO2, WO3, Fe2O3 or ZnO, are being widely investigated for their use as photoanodes, due to their higher surface areas in contact with the electrolyte, which increases the efficiency of photoelectrochemical processes. Metal oxide nanostructures have been synthesized by a number of different techniques. Anodization is one of the simpler methods used to synthesize nanostructured photoanodes, and the morphology and size of nanostructures can be designed by adequately controlling anodization parameters. Besides, these nanostructures are directly bound to the metallic back contact, improving significantly the efficiency of electron collection. It has been observed that hydrodynamic conditions during anodization using a rotating disk electrode, RDE greatly influenced the morphology of nanostructures and, therefore, their photoelectrochemical performance. The objective of this chapter is to review the innovative nanostructures with high-aspect ratios that can be fabricated by anodization under different hydrodynamic conditions.


Nanostructured lipid carriers NLC represent the novel and widely explored generation of lipid nanoparticles. These are the second-generation solid lipid nanoparticles SLN developed with the aim to overcome limitations of SLN mainly with respect to limited drug loading and drug leakage during its storage. NLC are fabricated by mixing solid lipids with spatially incompatible liquid lipids leading to nanoparticulate structures with improved drug loading and controllable release properties. Out of the numerous methods reported to prepare NLC, microemulsion template ME technique is the most simple and preferred method. This methodology of preparation of lipid nanoparticles obviates the need for specialized equipment and energy to generate NLC, enables achieving desirable particle size of nanoparticles by modulating the size of the emulsion droplet, and is also feasible for easy scale-up. This chapter describes microemulsion template technique for fabrication of NLC based gel for topical delivery, particularly with respect to its method of preparation and product analysis.

Magnetic Information-Storage Materials

The purpose of this chapter is to review the current status of magnetic materials used in data storage. The emphasis is on magnetic materials used in disk drives and in the magnetic random-access memory MRAM technology. For magnetic recording media, the advances are in high-magnetization metal alloys with large values of switching coercivity. The status of MRAM cell technology and some closely related key problems are reviewed. Historical variation of areal density from an IBM perspective. However, this paper discusses only the fundamental technology associated with digital magnetic recording, including the devices used to record and read back the recorded data and the media on which the data is recorded. The discussion is also restricted to the materials and not to any of the mechanical structures associated with the recording heads or disks.

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The CLOU and conversion performances were studied by a micropacked bed reactor, and crystalline phase structure and homogeneity and bulk density identified as the most important parameters affecting the performance of the OCM. Bulk density is correlated with the sintering temperature, atmosphere and time at sintering temperature, while phase homogeneity is a function of the raw materials chosen, agglomeration method and sintering procedure. Specific challenges are identified in the control of slurry homogeneity and sintering conditions in upscaled production. The fabrication parameters of the otherwise same ingredients result in quite different morphology and quality of performance in large scale.

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Every tank we build is a custom project, designed and fabricated to perform a specific function. With a combined fabrication area of over , square feet, we have extensive capabilities and efficient, state-of-the-art equipment, including:. From these facilities, we ship materials down the street or around the world.

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