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Elaboración, caracterización e hidruración de materiales para electrodos negativos de baterías

Cuscueta, Diego J. (2010) Elaboración, caracterización e hidruración de materiales para electrodos negativos de baterías. Tesis Doctoral en Ciencias de la Ingeniería, Universidad Nacional de Cuyo, Instituto Balseiro.

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Resumen en español

Las baterías de Ni‐MH permiten acumular y liberar energía eléctrica mediante una re‐acción electroquímica donde los materiales activos que intervienen son el hidróxido de Níquel en el electrodo positivo, el cual está ampliamente estudiado, y una aleación metálica capaz de almacenar hidrógeno en forma de hidruro en el electrodo negativo. En esta tesis doctoral se planteó como objetivos generales estudiar nuevas aleaciones absorbedoras de hidrógeno y construir los dispositivos (prototipos de batería de Ni‐MH) y equipos (galvanostato) que permitan llevar a cabo los estudios necesarios, tanto en la inves‐tigación sobre los electrodos como en el desarrollo industrial de baterías. Para eso, primero se propuso aprender diversas técnicas que permitan fabricar y carac‐terizar un material y correlacionar sus resultados. Se estudió un compuesto obtenido luego de sinterizar la mezcla de polvos de la aleación LaNi_4,7Al_0,3 y Cu, utilizados como material activo y ligante mecánico respectivamente. Los resultados mostraron que el desempeño electroquímico fue afectado debido al prolongado tratamiento térmico, el cual provocó cam‐bios en la composición de la aleación debido a la interdifusión de Ni y Cu. Los resultados obtenidos por la técnica de espectroscopía mecánica permitieron comprobar la fragmenta‐ción de las partículas que se produce durante la hidruración electroquímica. Además se pudo apreciar el arrastre de dislocaciones con hidruros segregados en sus núcleos y la preci‐pitación y disolución de hidruros. Posteriormente se fabricó en forma satisfactoria y se estudió la aleación LmNi_4Co_0,31Mn_0,31Al_0,42 (Lm = Mischmetal rico en La). Esta aleación es interesante por su reducido contenido de Co, elemento que ha demostrado mejorar notablemente el desempeño electroquímico, pero que presenta una notable incidencia en el costo de la batería. Durante el estudio de la aleación también se optimizó el tamaño inicial de partícula para la preparación de los electrodos. Los resultados de la caracterización electroquímica mostraron que la alea‐ción estudiada presenta una capacidad de descarga superior a una típica aleación comercial, con la ventaja de su reducido contenido de Co, por lo que presenta atractivas perspectivas para ser utilizada en electrodos comerciales. También se estudió la influencia del Mg en la aleación La_1‐xMg_xNi_3,8Co_0,3Mn_0,3Al_0,4 (0<x<0,2), la cual también presenta reducido contenido de Co. El objetivo fue analizar si la sustitución de La por Mg mejoraba el desempeño electroquímico de la aleación. El agregado de Mg, a aleaciones madre previamente fabricadas, se realizó mediante la técnica de aleado por molienda mecánica. Este proceso originó un reducido tamaño inicial de partícula que determinó un buen comportamiento electroquímico en estabilidad cíclica y en “rate capabili‐ty”, pero con una reducida capacidad de descarga. Además, con el objetivo de probar diferentes materiales como almacenadores electro‐químicos de energía, se analizaron electrodos fabricados con carbón activado, el cual se destaca por su elevada área superficial, conocido proceso de fabricación y reducido costo. Se determinaron las características superficiales mediante la obtención del área superficial y la distribución del tamaño de los poros. Se realizó la caracterización electroquímica de diversos electrodos y se determinaron posibles aplicaciones y usos del carbón activado como almace‐nador de energía. Con el objetivo de analizar en forma controlada algunas variables propias de un desa‐rrollo comercial, se fabricaron prototipos de batería de Ni‐MH. Se estudiaron y caracterizaron 3 diseños, explicando las dificultades y errores que surgieron y la forma en que se resolvieron. Se presenta un dispositivo final que tiene la posibilidad de extender el estudio a variables que no se pueden considerar en una celda de laboratorio. Posteriormente se muestran resultados de pruebas realizadas en los prototipos desarrollados. Con la finalidad de determinar el desempeño como separador eléctrico de una batería de Ni‐MH, se estudiaron materiales de fibra de vidrio, construidos con distintas estructuras y tipos de vidrios. También se presentan los resultados de como afecta al desem‐peño electroquímico de una batería, la presión con que es compactado el sistema electrodos y separador. Se utilizan masas de diferente peso para regular con precisión la compactación entre electrodos. Además se caracterizó la presión interna de gases producidos en el prototi‐po durante sobrecargas, y se determinan condiciones de uso que optimizan el desempeño, manteniendo la seguridad del usuario. Por último y como parte de una necesidad en el laboratorio, pero también con posibles aplicaciones comerciales o didácticas, se desarrolla el diseño completo y la construcción de un galvanostato, equipo utilizado para estudiar el desempeño de baterías. El mismo es to‐talmente configurable mediante un software de PC, presenta 4 canales independientes de trabajo, 4 rangos de corriente (0,3 – 3A) y un amplio rango de lectura de potencial (‐10 a 10 V). Se describen en forma detallada las especificaciones técnicas.

Resumen en inglés

The Ni‐MH batteries are capable of storing and releasing energy by means of an elec‐trochemical reaction taking place between a positive Nickel hydroxide electrode, which has been already widely studied, and a hydrogen storage alloy in the negative electrode. The general aim of this doctoral thesis work was the search and study of new hydro‐gen storage alloys and the construction of devices (Ni‐MH battery prototypes) and equipments (galvanostat) that allows carry out the necessary studies, both in research of electrodes as in the industrial development of batteries. For this, it was first proposed to learn various techniques to fabricate and characterize a material and the correlation of their results. A compound obtained from the powder mixture sintering of the LaNi_4.7Al_0.3 alloy and Cu, as active material and mechanical binder respec‐tively, was studied. The results showed that the electrochemical performance was affected due to prolonged heating, which caused changes in the composition of the alloy due to in‐terdiffusion of Ni and Cu. The results of mechanical spectroscopy technique let show the fragmentation of the particles produced during the electrochemical hydriding. Results also show the dragging of dislocations with hydrides segregated in their nuclei, and precipitation and dissolution of hydrides. The LmNi_4Co_0.31Mn_0.31Al_0.42 alloy (Lm = La rich Mischmetal) was satisfactorily fabricated and studied. The attraction of this alloy is the low‐Co content, an element that had demostrated the significantly improvement of the electrochemical performance but has a significant impact on the cost of the battery. During the study of the alloy, the initial particle size for the preparation of the electrodes was also optimized. The electrochemical characteri‐zation showed that the studied alloy has a higher discharge capacity than a typical commercial one, with the advantage of low‐Co content, thus offering attractive prospects for its use in commercial electrodes. The Mg influence in the La_1‐xMg_xNi_3.8Co_0.3Mn_0.3Al_0.4 (0 <x <0.2) alloy, which has also low‐Co content, was studied. The aim was to analyze whether the substitution of La by Mg improves electrochemical performance of the alloy. The Mg addition over master alloys previously prepared was made by the mechanical alloying technique. This process produced a reduced initial particle size of the alloy, resulting in a good behavior in cyclic stability and high‐rate capability, but a reduced discharge capacity. Furthermore, with the aim of testing different materials for electrochemical storage of energy, the use of negative electrodes prepared with activated carbon was examined, which is notable for its high surface area, known manufacturing process and reduced cost. Surface characteristics of carbon were determined by means of surface area and pore size distribu‐tion measurements. The electrochemical characterization of different electrodes was performed, and the possible applications and uses of activated carbon as energy storage were determined. Ni‐MH battery prototypes were fabricated in order to analyze, in a controlled way, some variables of a commercial development. Three designs were studied and characterized, explaining the difficulties and errors found and how they were resolved. A final prototype with the possibility of extending the study to variables that cannot be considered in a labora‐tory cell is presented. Abstract Then, tests results obtained from the developed battery prototype are shown. Some fi‐ber glass materials, with different structures and glass types were studied in order to determine its performance acting as electrical separator of electrodes in a Ni‐MH battery. The prototype was also used to analyze how is affected the electrochemical performance of a battery due to the mechanical pressure used to assemble the system formed by the electrodes and the separator. The pressure was regulated in a precise way by means of masses of differ‐ent weight attached to the device. Moreover, the inner pressure of gases produced during overcharge was characterized and use rules were determined for optimize performance while maintaining user safety. Finally, the complete design and construction of a galvanostat was developed as a part of the laboratory requirements, but also with potential commercial and educational applica‐tions. The galvanostat is one of the main equipments used to study the performance of batteries. It is fully configurable by a PC software, presents 4 independent work channels, 4 current ranges (0.3 – 3 A) and a wide potential range (‐10 to 10 V). The technical specifica‐tions are described in detail.

Tipo de objeto:	Tesis (Tesis Doctoral en Ciencias de la Ingeniería)
Palabras Clave:	Activated carbon; Carbón activado; Negative electrode alloy; Aleaciones de electrodo negativo; Battery prototype; Prototipo de batería; Galvanostat; Galvanostato
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Materias:	Ingeniería > Ensayo de materiales Metalurgia > Aleaciones
Divisiones:	Investigación y aplicaciones no nucleares > Física > Física de metales
Código ID:	167
Depositado Por:	Marisa G. Velazco Aldao
Depositado En:	12 Aug 2010 13:54
Última Modificación:	09 May 2011 11:24

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