Development of supported catalysts on porous structures for hydrogen generation and catalytic combustion applications in the framework of renewable energies 

Period: 01-01-2016 / 31-12-2018
Financial source: Ministerio de Economía y Competitividad
Code: CTQ2015-65918-R

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The depletion of fossil fuels (in a short and long term) and the global warming derived from greenhouse effect are consequences of the extensive use of these fuels. In this context, hydrogen appears as an attractive, clean and abundant energy carrier in the context of a wider use of clean and removable energies. For the implementation of the “hydrogen economy” many technological challenges regarding hydrogen production (free from CO2), transport, storage (in a safe manner) and combustion (to produce heat or electricity) should be met first. New research will be conducted in this project on the basis of our previous results regarding the study of complex hydrides for hydrogen storage and the development of catalysts and processes for hydrogen generation and use in portable applications. In particular, new catalysts will be developed on porous structures such as polymeric, metallic and ceramic membranes and/or foams with high actual interest. Catalysts will we developed and studied for hydrogen generation and combustion reactions according to the following research lines:
1) Development of new materials (catalysts and supports) with a high added value of the complete system catalyst + support. Porous Ni and SiC foams together with PTFE membranes will be selected as supports for the studies. The main objective is to design new catalysts on technologically interesting supports such as separating membranes, electrolytes, electrodes and/or hydrogen combustors. These new catalysts will be developed following the objective of reducing the amount of noble metals by combining or replacing with another non-noble metals (e.g. Pt-Cu and Ni-Fe) and/or with metalloids (e.g carbides, borides, etc). Wet impregnation methods will be used and special emphasis will be put on the use of the PVD methodology (magnetron sputtering) recently employed in our laboratory for the fabrication of Co thin films with very good results. The latter methodology opens a highly interesting research field because permits to tune microstructure and composition (i.e. Co, Co-B, Co-C) on demand.
2) Characterization of the prepared materials from a microstructural and chemical point of view. Modern nanoscopies will play a key role in the characterization, comprehension and further improvement of these highly nanostructured catalysts.
3) Catalytic studies on the prepared materials will be carried out in three catalytic tests: i) the hydrogen generation through hydrolysis reactions, ii) the photocatalytic water splitting, and iii) the catalytic hydrogen combustion. These reactions are of high interest in the context of the hydrogen economy.
--The interaction of these three research lines as proposed in this project will permit to achieve basic knowledge on the rational design of nanocatalysts supported on porous materials. Structure-composition-activity relationships will be established through catalytic and photo-catalytic studies in combination with characterization techniques based on high resolution analytical TEM and additional spectroscopic techniques.


Period: 2016 / 2020
Financial source: Ministerio de Economía y Competitividad
Code: MAT2015-69035-REDC

Application of advanced electron microscopy techniques to the characterization of nanostructures coatings for clean energy applications 

Period: 01-03-2015 / 28-02-2017
Financial source: Junta de Andalucía
Code: TAHUB-050 (Talent Hub – Marie Curie)

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The Transmission Electron Microscopy (TEM) technique is a widely used and very powerful tool to understand the behavior of materials giving microstructural information with a high spatial resolution. The continuous advances in electron microscopy provide nowadays a complete set of techniques available in modern TEM microscopes leading to an exhaustive microstructural and chemical characterization in the Nano-scale. Recently, a FEI TECNAI F30 microscope with GIF Quantum filter has been installed at the host Institution (Institute of Materials Science of Seville, ICMS, Instituto de Ciencia de Materiales de Sevilla). It includes: conventional and scanning transmission electron microscopy (TEM) and scanning-transmission electron microscopy (STEM) modes with a high structural resolution. a high-angle annular dark field (HAADF) detector for enhanced atomic number contrast. An X-Ray emission detector (EDX) for chemical and elemental mapping information. An energy filter analyzer for Electron Energy Loss analysis (EFTEM and EELS, respectively) for structural, chemical bonds and elemental mapping information. A tomography holder and software for 3D visualization of nanostructures is also available.
The high specialization required to take profit of all the information available with the modern TEM facilities makes relevant to propose the present project which will be devoted to the application and development of the TEM techniques applied to investigate, up to the nanoscale, the microstructure and chemical behavior of nanostructured thin films and coatings. These catalytic coatings have been developed in the PVD (Physical Vapor Deposition) laboratory of the NanoMatMicro group at the ICMS. The coatings will be applied for clean and sustainable energy applications. In particular Co-based catalytic coatings have been investigated for the catalyzed sodium borohydride and ammonia borane hydrolysis reactions for hydrogen generation in portable applications. The evolution of catalysts surface after use will be an area of high interest to understand deactivation mechanisms and durability. The comparison of pure Co with CoB and CoC catalysts and the novel capabilities of magnetron sputtering for developing these supported catalysts will be also studied thanks to the advanced TEM techniques.

Development of novel materials and processes for the generation and use of hydrogen mainly in portable applications 

Period: 01-01-2013 / 31-12-2015
Financial source: Ministerio de Economía y Competitividad
Code: CTQ2012-32519

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Hydrogen as a vector of transport and storage of energy is a very attractive candidate in the context of increased use of renewable and clean energies. This project will address the study of the different processes that lead to the final configuration of an integrated systems for hydrogen generation and use mainly in portable applications (and potentially scalable for stationary applications). In particular, work will be carried out in this project in the following lines:
a) Research on new lightweight compounds for use in hydrogen generation processes on a small scale by chemical routes (hydrolysis). Typically hydrolysis reactions of borohydrides (i.e. NaBH4) and compounds like ammonia borane, hydrazine borane or hydrazine. This line includes the development of catalysts at the nanoscale using wet chemical methods for their synthesis: Metal-metalloid nanostructures (i.e. Co-B, Co-B-P and similar ones) and bimetallic catalysts (including or not metalloid) of low cost which potentiate synergistic effects (i.e. CoRu, NiPt or Co-Ru-B). The topic also includes the development of portable reactors for these processes and the development of new substrates and monoliths, studies of adherence and durability of the catalyst.
b) Research on new host-guest systems containing hydrogen for reversible storage (loading / unloading). Mainly porous supports (host) like the so called "nanoscaffolds" (based on C or BN) infiltrated with borohydrides materials (guest) (i.e. titanium borohydride) typically used for reversible hydrogen storage. These new materials must present improved charging and de-charging kinetics.
c) Studies of coupling a hydrogen generator system with a low cost fuel cell. Typically a continuous reactor for the hydrolysis of NaBH4 with Co-B catalyst for providing H2 at constant flow rate conditions to directly feed a PEM fuel cell of 60 W.
d) Fundamental studies for the development of catalysts and supports for the controlled combustion of hydrogen. It's a new line in the research group based on wet chemical preparation of noble metal nanoparticle catalysts on commercial porous ceramic supports (i.e. SiC). The line also includes the design of a reactor for laboratory-scale study of heat production by controlled combustion of hydrogen.
e) Development of sputtering technology ("magnetron sputtering") for the preparation of catalysts and nano-structures on various substrates for use in the processes developed in the previous sections. The group has extensive experience in this technology to be applied in novel ways in this project leading to a great versatility regarding nanostructure, composition and addition of additives to improve catalytic activity, durability and selectivity of catalysts.
f) Microstructural and chemical characterization of new materials and catalysts developed in the project. We are dealing typically with materials of controlled nanostructure where modern nanoscopic techniques will play a key role in the custom manufacturing of these materials

Development of processes for the catalytic combustion of hydrogen and study of the integration in devices for portable applications 

Period: 16-05-2014 / 15-05-2016
Financial source: Junta de Andalucía
Code: P12-TEP-862

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Hydrogen is an attractive candidate as a vector for storage and transport of energy in the context of an increased use of renewable and clean energies. The production and use of energy based on hydrogen technology is particularly important for small-scale portable (and potentially scalable for stationary) applications. In this project the process of catalytic (controlled) combustion of hydrogen will be investigated in the various aspects that could lead to a final integrated configuration with a H2 generation system for portable applications. For that the project will take advantage of the synergy of integrating two researcher groups from the PAI: i) The TEP217 group, specialists in storage and generation of hydrogen based on metal hydrides, complex hydrides and hydride composites reactive systems; and in the use of catalysts and additives to control and improve the kinetics of these processes. ii) The FQM342, specialist group for the fabrication of porous ceramics of high interest as catalyst supports for harsh combustion environments. Further collaboration is completed with the participation of the company Abengoa Hidrógeno SA that will be involved as sub-contractor as specialist in systems for the production and storage of hydrogen.
In particular we will work on this project in the following lines:
1.- Development of catalysts and supports for catalytic combustion. Typically porous biomorphic silicon carbide ceramics and classic noble metal catalysts, as well as new low cost catalysts to be developed in the project.
2.- Development of reactors needed for the study of the catalytic combustion. Typically hydrogen flows from a few ml/min to the scale of a H2 generator already available in the range 0.5 to 1.5 L/min.
3.- Coupling the catalytic combustion system with a portable hydrogen generation systems that we have developed in previous projects.
4.- Application of the sputtering technology in an exploratory manner in this project to deposit the catalyst materials for the H2 catalytic combustion on porous substrates.
5.- Microstructural and chemical characterization of the supports and catalysts in the nanoscale to follow the procedures of synthesis and evolution in operation.

Nanostructure control in coatings prepared by magnetron sputtering with functional applications.  

Period: 1-11-2011 / 31-10-2015
Financial source: Agencia Estatal Consejo Superior de Investigaciones Científicas
Code: PIE-201160E091

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This PIE intramural project comes to cover the completion of a doctoral thesis in the JAE -Predoc-CP program of the CSIC.
Due to the relative simplicity and robustness of the PVD processes (physical deposition from the vapor phase) and in particular of the sputtering technique (MS, magnetron sputtering), this method has become one of the most effective and versatile process for deposition of thin films and coatings. The microstructural control of coatings in the nano-scale allows modifying and designing the properties depending on the final application. Nowadays different types of coatings (nanocrystalline, multilayers or "nanocoposites") can be made by MS varying the process parameters such as: distance between target and substrate, gas and pressure in the gas phase, use of reactive gases, substrate temperature, bias potential, sputtering power (DC, DC-pulsed or RF), or composition and number of targets.

Therefore the overall objective of the project is to modify the nanostructure of coatings by introducing nano-particles and nano-bubbles in a controlled manner to obtain optical, mechanical or functional properties of interest.

Sustainability of the Advanced Laboratory for Nanoscopies and Spectroscopies.  

Period: 01-01-2014 / 31-12-2016
Financial source: Agencia Estatal Consejo Superior de Investigaciones Científicas
Code: PIE-201460E018

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The LAboratory for Nanoscopies and SpEctroscopies (LANE), recently installed at the Materials Science Institute of Seville, is equipped with a FEI TECNAI F30 microscope with GIF Quantum filter. It includes: conventional (TEM) and scanning transmission electron microscopy (STEM) modes with a high structural resolution; a high-angle annular dark field (HAADF) detector for enhanced atomic number contrast; an X-Ray emission detector (EDX) for chemical and elemental mapping information; an energy filter analyzer for Electron Energy Loss analysis (EFTEM and EELS, respectively) for structural, chemical bonds, and elemental mapping information. A tomography holder and software for 3D visualization of nanostructures is also available.  The LANE laboratory is also equipped with a SEM microscope Hitachi S4800 with a field emission gun, an EDX analyzer, and a dedicated detector and sample holder to work in transmission mode.

The main objective of the proposal is to ensure the long-term sustainability of the laboratory promoting research and development of nanostructured materials with special emphasis on the chemical and microstructural characterization at the nanoscale in order to understand the behavior and the final properties. Specific scientific objectives are:

  1. Development of new manufacturing strategies of nanostructured coatings, thin films and nanoparticles mainly based on the technology of "magnetron sputtering".
  2. Study of materials and catalysts for hydrogen storage, production, and use mainly in portable applications.
  3. Microstructural and chemical characterization: Nanoscopies and spectroscopies. Mainly using advanced electron microscopy techniques as mentioned above along with other techniques such as XPS spectroscopy or the X-ray diffraction applied to the study of nanomaterials.

It is also an objective of the intramural project to enhance the achievement of European projects facilitating the availability of international cooperation sessions promoting visits and international collaborations which support the priorities of the advanced laboratory.

COST MP1103. Nanostructured materials for solid-state hydrogen storage. 

Period: 25-10-2011 / 24-10-2015
Financial source: European Science Foundation
Code: COST-MP1103

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This COST Action deals with the future of energy storage and aims to set up a competitive and coordinated network capable to define new and unexplored ways for Solid State Hydrogen Storage (SSHS) by innovative and interdisciplinary research within the European Research Area (ERA). This Action focuses on SSHS in light-weight nanostructured materials to discover novel guidelines and phenomena for the design of advanced SSHS systems. This Action will exploit the potential of state-of-the-art synthesis techniques, structure analysis and computer simulations to achieve truly atomic-level control in the design of materials’ structure, microstructure and chemical bonding which are crucial for the assessment of structure-properties relationships.

Through the control of the hydrogen binding energy and the optimization of hydrogen transport and surface catalysis, the final goal is the development of SSHS materials with tailored properties that find practical implementation in transportation and energy sectors to sustain in medium-long terms the economies of European countries.

This Action contributes to form a critical mass of researchers, increasing cooperation and interaction to coordinate outstanding R&D and innovation-based growth in the field of SSHS materials, in order to overcome the present bottlenecks for their widespread industrial application.

Advanced laboratory for the nano-analysis of novel functional materials   (AL-NANOFUNC)

Period: 01-10-2011 / 30-03-2015
Financial source: Unión Europea
Code: REGPOT-CT-2011-285895

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The AL-NANOFUNC project has been designed to install and fully develop at the Materials Science Institute of Seville (ICMS, CSIC-Univ.Seville, Spain) an advanced laboratory for the Nano-analysis of novel functional materials. Advanced Nanoscopy facilities, based on latest generation electron microscopy equipments, will be devoted to breakthrough research in specific topics of high interest:

i) Nanomaterials for sustainable energy applications;
ii) protective and multifunctional thin film and nanostructured coatings;
iii) nanostructured photonic materials and sensors.

To take the ICMS laboratories to a leading position that is competitive in a world-wide scenario, the AL-NANOFUNC project is contemplated to up-grade the actual research potential in several directions:

i) improve equipment capabilities regarding the Analytical High Resolution Electron Microscopy facilities;
ii) improve the impact and excellence of basic research through hiring of experienced researchers and transnational exchange with the reference centers in Europe;
iii) develop and improve the innovation potential of the ICMS’s research by opening the new facilities to companies and stakeholders;
iv) organize workshops and conferences, dissemination and take-up activities to improve research visibility.

Close collaborations with reference centers and companies in Liège (Belgium), Graz (Austria), Jülich (Germany), Oxford (England), Cambridge (England), Dübendorf (Switzerland) and Rabat (Morocco), as well as with laboratories at Andalucian Universities, are foreseen in this project.
Five companies in Andalusia will also collaborate in close synergies to promote the long-term strategic lines of interest for the region in the natural and artificial stone products and solar and renowable energy sectors.