Notas de Metalurgia Fisica - UNIDAD 1 - 2012

UNIVERSIDAD AUTNOMA DE ZACATECAS
Programa de Ingeniera Mecnica
Av. Lpez Velarde No. 801 Col. Centro Zacatecas, Zacatecas, C.P. 98000 Tel. 01 (492) 923 94 07 ext. 1615
Notas del Programa Metalurgia Fsica
Material Preparado por: Dr. Vctor Hugo Baltazar Hernndez
Notas de la materia Metalurgia Fsica
CONTENIDO
1 LAS HERRAMIENTAS DEL METALURGISTA .............................................................................. 3 1.1 MTODOS PARA LA CARACTERIZACIN DE LOS METALES Y SUS ALEACIONES ................................. 3 1.1.1 La metalografa .................................................................................................... 3
1.2 MICROSCOPA PTICA, ELECTRNICA (SEM) Y DE TRANSMISIN (TEM) ....................................... 8 1.2.1 1.2.2 1.2.3 Microscopa ptica (light microscopy) .............................................................. 8 Microscopa Electrnica de Barrido (Scanning Electron Microscopy) ....... 14 Microscopa Electrnica de Transmisin (Transmission Electron Microscopy) ............................................................................................................................ 24 1.3 ANALISIS DE XRD (X-RAY DIFFRACTION) ...................................................................................... 29 1.3.1 1.3.2 1.3.3 1.3.4 1.3.5 Electromagnetic radiation ................................................................................. 29 Production of X-Rays ........................................................................................ 30 X-Ray Diffraction ................................................................................................ 32 Diffractometers ................................................................................................... 34 Applications of X-Ray Diffraction ..................................................................... 35
1.4 ENSAYOS O PRUEBAS NO DESTRUCTIVAS (NON-DESTRUCTIVE TESTING) ...................................... 35 1.4.1 Lquidos Penetrantes ........................................................................................ 35
1.5 ENSAYOS MECNICOS ..................................................................................................................... 44 1.6 REFERENCIAS .................................................................................................................................. 45
Dr. Vctor Hugo Baltazar Hernndez
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1 Tcnicas de Caracterizacin del Metalurgista

1.1
1.1.1
Mtodos para la caracterizacin de los metales y sus aleaciones

La metalografa La metalografa o microscopa estudia microscpicamente las caractersticas estructurales
de un metal o de una aleacin. Sin duda, el microscopio es la herramienta ms importante del metalurgista tanto desde el punto de vista cientfica como desde el tcnico. Es posible determinar el tamao de grano, y el tamao, forma y distribucin de varias fases e inclusiones que tienen gran efecto sobre las propiedades mecnicas del metal. La microestructura revelara el tratamiento mecnico y trmico del metal y, bajo un conjunto de condiciones dadas, podr predecirse su comportamiento esperado. La experiencia ha demostrado que el xito en el estudio microscopico depende en mucho del cuidado que se tenga para preparar la muestra. El microscopio mas costoso no revelara la estructura de una muestra que haya sido preparada en forma deficiente. El procedimiento que se sigue en la preparacin de una muestra es comparativamente sencillo y requiere de una tcnica desarrollada solo despus de prctica constante. El ltimo objetivo es obtener una superficie plana, sin ralladuras, semejante a un espejo. Las etapas necesarias para preparar adecuadamente una muestra metalogrfica se explican en lo siguientes subndices [1]. 1.1.1.1 Muestreo La seleccin de una muestra para estudio micrasc6pico puede ser muy importante. Si lo que se va a investigar es una falla, se debe escoger la muestra ms prxima al rea de la falla y comparrsele con una tomada de la seccin normal o sana. Si el material es suave, como metales o aleaciones no ferrosas y aceros no tratados trmicamente, la seccin puede obtenerse por corte manual con una segueta. Si el material es duro, la seccin puede obtenerse mediante un disco cortador abrasivo, el cual es un plato delgado fabricado de un abrasivo de tipo adecuado, que gira a alta velocidad. La muestra debe mantenerse fra durante la operacin de corte [1]. 1.1.1.2 Esmerilado burdo o tosco Siempre que sea posible, la muestra debe ser de un tamao fcil de manipular. Una muestra blanda se puede aplanar si se mueve lentamente hacia arriba y hacia abajo a travs de la superficie
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de una lima plana poco spera. La muestra blanda o dura puede esmerilarse burdamente sobre una lija de banda (rotatoria), manteniendo la muestra fra sumergindola frecuentemente en agua durante la operacin de esmerilado. En todas las operaciones de esmerilado y pulido, la muestra debe moverse en sentido perpendicular a las ralladuras existentes. Esto facilitara darse cuenta del momento en que las ralladuras mas profundas hayan sido sustituidas por las menos profundas, caractersticas del abrasivo ms fino. El esmerilado contina hasta que la superficie quede plana y libre de mellas, rebabas, etc., y todas las ralladuras debidas al corte manual o al disco cortador no son visibles. La Figura 1.1 muestra la superficie despus del esmerilado [1].
a)
b)
c)
Figura 1.1 a) Superficie de la muestra despus del esmerilado burdo, amplificacin 100x. b) Superficie de la muestra despus del pulido intermedio en papel 400, amplificaci6n 100x. c) Superficie de la muestra sin ralladuras despus del pulido final, amplificacin 50x. Los puntos negros son impurezas de xido.
1.1.1.3
Montaje Las muestras pequeas o de forma incomoda deben montarse de alguna manera para
facilitar el pulido intermedio y final. Alambres, varillas pequeas, muestras de hoja metlica, secciones delgadas, etc., deben montarse en un material adecuado o sujetarse rgidamente en una monta mecnica.
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Los materiales plsticos sintticos que se acoplan a la muestra en una prensa para montar especial proporcionan las bases de un tamao uniforme conveniente (generalmente de 2,5, 3, 4 cm. de dimetro) para manipular las muestras en ulteriores operaciones de pulido. Estas bases, cuando se han hecho en forma adecuada, son muy resistentes a la accin de los reactivos de ataque que se emplean comnmente. La resina termofijadora que mas se emplea para montar muestras es la baquelita. Los polvos para moldear baquelita se fabrican en colores de este material, lo cual simplifica la identificaci6n de las muestras montadas. La muestra y la cantidad correcta de polvo de baquelita, o una preforma de baquelita, se colocan en el cilindro de la prensa de montar. La temperatura aumenta gradualmente hasta 150C y se aplica una presin de moldeo de unas 4 000 lbs/pulg2 simultneamente. Una vez que la baquelita esta adherida y curada cuando se alcanza esta temperatura, la base con la muestra puede extraerse del dado de moldeo mientras esta caliente. La lucita es la resina termoplstica mas comn; es completamente transparente cuando se moldea en forma adecuada, como se ve en la Figura 1.2. Esta transparencia resulta til cuando es necesario observar la seccin exacta que se pule o cuando por cualquier otra razn se desea ver por completo la muestra en la base. Al contrario de los plsticos termofijados, las resinas termoplsticas no sufren cura a la temperatura de moldeo, sino que adquieren estabilidad al enfriarse. La muestra y la cantidad de polvo de lucita adecuadas se colocan en la prensa para montar y se someten a la misma temperatura y presin que para la baquelita (150C y 4 000 Ibs,/pulg2 ) . Una vez alcanzada esta temperatura, se quita la bobina de calentamiento y las aletas de enfriamiento se colocan alrededor del cilindro para enfriar la base hasta 75 C en unos 7 min. al tiempo que se mantiene la presin de moldeo. Si se saca la base todava caliente o si se deja enfriar lentamente en el cilindro de moldeo a la temperatura ambiente sin sacarla, se opacara.
Figura 1.2 a) Muestra montada en baquelita, aumentada 2x, b) muestra montada en lucita, aumentada 2x, c) muestra sostenida en un dispositivo de sujecin de metal, aumentada 2x
Las muestras pequeas pueden montarse en forma conveniente para prepararlas mtalogrficamente en un dispositivo de sujecin hecho en el laboratorio, como el de la Figura 1.2c. Las muestras laminares delgadas, cuando se montan en tal dispositivo de sujecin, suelen alternarse
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con hojas metlicas "rellenadoras" de metal que tienen aproximadamente la misma dureza que las muestras. Si se usan hojas rellenadoras, se conservara la superficie libre de las irregularidades de la muestra y se evitara, de alguna manera, que los bordes de la muestra se redondeen durante el pulido [1]. 1.1.1.4 Pulido intermedio Despus de montada, la muestra se pule sobre una serie de hojas de esmeril o lija con abrasivos ms finos, sucesivamente. El primer papel es generalmente No. 300, luego 400, 600, 800, y finalmente 1200. La Figura 1.1b muestra la superficie despus del pulido intermedio con lija de 400. Por lo general, las operaciones de pulido intermedio con lijas de esmeril se hacen en seco; sin embargo, en ciertos casos, como el de preparacin de materiales suaves, se puede usar un abrasivo de carburo de silicio. Comparado con el papel esmeril, el carburo de silicio tiene mayor rapidez de remocin y, como su acabado es a base de resina, se puede utilizar con un lubricante, el cual impide el sobrecalentamiento de la muestra, minimiza el dao cuando los metales son blandos y tambin proporciona una accin de enjuague para limpiar los productos removidos de la superficie de la muestra, de modo que el papel no se ensucie [1]. 1.1.1.5 Pulido fino El tiempo utilizado y el xito del pulido fino dependen en mucho del cuidado puesto durante los pasos de pulido previo. La ltima aproximacin a una superficie plana libre de ralladuras se obtiene mediante una rueda giratoria hmeda cubierta con un pao especial cargado con partculas abrasivas cuidadosamente seleccionadas en su tamao. Existe gran disponibilidad de abrasivos para efectuar el ltimo pulido. En tanto que muchos harn un trabajo satisfactorio, parece haber preferencia por la forma gamma del oxido de aluminio para pulir materiales ferrosos y de los basados en cobre, y oxido de cerio para pulir aluminio, magnesio y sus aleaciones. Otros abrasivos para pulido final que se emplean a menudo son la pasta de diamante, oxido de cromo y oxido de magnesio. La seleccin de un pao para pulir depende del material que vaya a pulirse y el propsito del estudio metalogrfico. Se pueden encontrar paos de lanilla o pelillo variable, desde aquellos que no tienen pelillo (como la seda) hasta aquellos de pelillo intermedio (como pao ancho, pao de billar y lonilla) adems de aquellos de pelillo profundo (como el terciopelo). Tambin se pueden encontrar paos sintticos para pulir con fines de pulido general, de los cuales el Gamal y el Micropao son los que se utilizan ms ampliamente. Una muestra pulida en forma adecuada
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mostrara nicamente las inclusiones no metlicas; adems, estar libre de ralladuras (Figura 1.1c) [1]. 1.1.1.6 Ataque El propsito del ataque qumico es hacer visibles las caractersticas estructurales del metal o aleacin. El proceso debe ser tal que queden claramente diferenciadas las partes de la microestructura. Esto se logra mediante un reactivo apropiado que somete a la superficie pulida a una accin qumica.
a)
b)
c)
Figura 1.3 a) Fotomicrografa de la diferencia en composicin qumica de las fases. B) Fotomicrografa de hierro puro, c) Ilustracin del aspecto microscpico de las fronteras de grano que aparecen como lneas obscuras.
En las aleaciones compuestas de dos o ms fases, las componentes se revelan durante la accin qumica, al atacar preferencialmente, el reactivo, a una o ms de estas constituyentes debido a la diferencia en composicin qumica de las fases (Figura 1.3a). En las aleaciones uniformes de una sola fase o metales puros, se obtiene contraste y las fronteras de grano se hacen visibles debido a las diferencias en la rapidez a que los diversos granos son atacados por el reactivo (Figura 1.3b). Esta diferencia en la rapidez de ataque esta asociada principalmente con el ngulo que guardan las diferentes secciones de grano con el plano de la superficie pulida. Debido al ataque qumico por el
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reactivo de ataque, las fronteras de grano apareceran como valles en la superficie pulida. Al chocar con la orilla de estos valles, la luz del microscopio se reflejara fuera del microscopio, haciendo que las fronteras de grano aparezcan como lneas oscuras. Esto se muestra en la Figura 1.3c. La seleccin del reactivo de ataque esta determinada por el metal o aleacin y la estructura especifica que se desea ver. Ver tabla 1.3 en [] en el cual se enumeran algunos de los reactivos de ataque comunes [1].
1.2
1.2.1
Microscopa ptica, electrnica (SEM) y de transmisin (TEM)

Microscopa ptica (light microscopy) Basic Principles The light microscope provides two-dimensional representation of structure over a total
1.2.1.1
magnification range of roughly 40 to 1250. Interpretation of such images is a matter of skill and experience and needs to allow for the three-dimensional nature of features observed. The main components of a benchtype microscope are (1) an illumination system comprising a light source and variable apertures, (2) an objective lens and an ocular lens (eyepiece) mounted at the ends of a cylindrical body tube, and (3) a specimen stage (fixed or rotatable). Metallic specimens that are to be examined at high magnifications are successively polished with 6, 1 and sometimes 0.25 m diamond grit. Examination in the as-polished condition, which is generally advisable, will reveal structural features such as shrinkage or gas porosity, cracks and inclusions of foreign matter. Etching with an appropriate chemical reagent is used to reveal the arrangement and size of grains, phase morphology, compositional gradients (coring), orientation-related etch pits and the effects of plastic deformation. Although actually only a few atomic diameters wide, grain boundaries are preferentially and grossly attacked by many etchants. In bright-field illumination, light is reflected back towards the objective from reflective surfaces, causing them to appear bright. Dark-field illumination reverses this effect, causing grain boundaries to appear bright. The degree of chemical attack is sensitive to crystal orientation and an etched polycrystalline aggregate will often display its grain structure clearly (Figura 1.4a). Preparation techniques for ceramics are essentially similar to those for metals and alloys. However, their porosity can cause two problems. First, there is a risk of entrapping diamond particles during polishing, making ultrasonic cleaning advisable. Second, it may be necessary to strengthen the structure by impregnating with liquid resin in vacuo, provided that pores are interconnected. The objective, the most important and critical component in the
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optical train of the light microscope, is made up of a number of glass lenses and, sometimes, fluorite (CaF2) lenses also. Lenses are subject to spherical and chromatic aberrations. Minimization and correction of these undesirable physical effects, greatly aided by modern computational techniques, is possible and objectives are classified according to the degree of correction, i.e. achromats, fluorites (semi-apochromats), apochromats. Lenses are usually coated in order to increase light transmission. As magnification is increased, the depth of field of the objective becomes smaller, typically falling from 250m at 15 to 0.08m at 1200, so that specimen flatness becomes more critical. The focal length and the working distance (separating its front lens from the specimen) of an objective differ. For instance, an f 2mm objective may have a working distance of 0.15 mm. [2]
Figura 1.4 (a) Reflection of light from etched specimen. (b) Use of oil to improve numerical aperture of objective.
Resolution, rather than magnification, is usually the prime concern of the skilled microscopist. It is the smallest separating distance () that can be discerned between two lines in the image. The unaided eye, at the least distance of comfortable vision (about 250 mm), can resolve 0.1 mm. Confusingly, the resolution value for a lens with a so-called high resolving power is small. Resolution is determined by (1) the wavelength () of the radiation and (2) the numerical aperture (NA) of the objective, and is expressed by the Abbe formula =/2NA. The numerical aperture value, which is engraved upon the side of the objective, indicates the light-gathering power of the compound lens system and is obtained from the relation NA=n sin , where n is the refractive index of the medium between the front lens face of the objective and the specimen and is the semi-apex angle of the light cone defined by the most oblique rays collected by the lens. Numerical apertures range in typical value from 0.08 to 1.25. Despite focusing difficulties and the need for costly lenses, efforts have been made to use short-wavelength
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ultraviolet radiation: developments in electron microscopy have undermined the feasibility of this approach. Oil-immersion objectives enable the refractive index termto be increased (Figura 1.4b). Thus, by replacing air (n=1) with a layer of cedar wood oil (n=1.5) or monobromonaphthalene (n=1.66), the number of rays of reflected light accepted by the front lens of the objective is increased, and resolution and contrast are improved. The range of wavelengths for visible light is approximately 400700 nm; consequently, using the Abbe formula, it can readily be shown that the resolution limit of the light microscope is of the order of 200 nm. The useful range of magnification is approximately 5001000NA. The lower end of the range can be tiring to the eyes; at the top end, oil-immersion objectives are useful [2].
Magnification is a subjective term; for instance, it varies with the distance of an image or object from the eye. Hence, microscopists sometimes indicate this difficulty by using the more readily defined term scale of reproduction, which is the lineal size ratio of an image (on a viewing screen or photomicrograph) to the original object. Thus, strictly speaking, a statement such as 500 beneath a photomicrograph gives the scale of reproduction, not the magnification [2]. The ocular magnifies the image formed by the objective: the finally observed image is virtual. It can also correct for certain objective faults and, in photomicrography, be used to project a real image. The ocular cannot improve the resolution of the system but, if inferior in quality, can worsen it. The most widely used magnifications for oculars are 8 and 12.5 [2]. Two-dimensional features of a standard bench microscope, the mechanical tube length tm and optical tube length to, are of special significance. The former is the fixed distance between the top of the body tube, on which the ocular rests, and the shoulder of the rotatable nosepiece into which several objectives are screwed. Objectives are designed for a certain tm value. A value of 160 mm is commonly used. (In Victorian times, it was 250 mm, giving a rather unwieldy instrument.) The optical tube length to is the distance between the front focal point of the ocular and the rear focal plane of the objective. Parfocalization, using matched parfocal objectives and oculars, enables the specimen to remain in focus when objectives are step-changed by rotating the nosepiece. With each change, to changes but the image produced by the objective always forms in the fixed focal phase of the ocular. Thus, the distance between the specimen and the aerial image is kept constant. Some manufacturers base their sequences of objective and ocular magnifications upon preferred numbers1 rather than upon a decimal series. This device facilitates the selection of a basic set of lenses that is comprehensive and useful (exempt from empty magnification). For example, the Michel series of 6.3, 8, 10, 12.5, 16, 20, 25, etc., a geometrical progression with a common ratio of approximately 1.25, provides a basis for magnification values for objectives and
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oculars. This rational approach is illustrated in Figura 1.5. Dashed lines represent oculars and thin solid lines represent objectives. The bold lines outline a box within which objective/ocular combinations give useful magnifications. Thus, pairing of a 12.5 ocular with a 40 objective (NA=0.65) gives a useful magnification of 500 [2].
Figura 1.5 Range of useful magnification in light microscope (from Optical Systems for the Microscope, 1967, p. 15; by courtesy of Carl Zeiss, Germany).
1.2.1.2
Selected microscopical techniques Phase-contrast microscopy Phase-contrast microscopy is a technique that enables special surface features to be studied
even when there is no color or reflectivity contrast. The light reflected from a small depression in a metallographic specimen will be retarded in phase by a fraction of a light wavelength relative to that reflected from the surrounding matrix and, whereas in ordinary microscopy a phase difference in the light collected by the objective will not contribute to contrast in the final image, in phase-contrast microscopy small differences in phases are transformed into differences in brightness which the eye can detect [2]. General uses of the technique include the examination of multi-phased alloys after light etching, the detection of the early stages of precipitation, and the study of cleavage faces, twins and other deformation characteristics. The optimum range of differences in surface level is about 2050 nm, although under favorable conditions these limits may be extended. A schematic diagram of the basic arrangement for phase contrast in the metallurgical microscope is shown in Figura 1.6a. A hollow cone of light produced by an annulus A is reflected by the specimen and brought to an image in the back focal plane of the objective. A phase plate of suitable size should, strictly, be
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positioned in this plane but, for the ease of interchangeability of phase plates, the position Q in front of the eyepiece E is often preferred. This phase plate has an annulus, formed either by etching or deposition, such that the light it transmits is either advanced or retarded by a quarter of a wavelength relative to the light transmitted by the rest of the plate and, because the light reflected from a surface feature is also advanced or retarded by approximately /4, the beam is either in phase or approximately /2 or out of phase with that diffracted by the surface features of the specimen. Consequently, reinforcement or cancellation occurs, and the image intensity at any point depends on the phase difference produced at the corresponding point on the specimen surface, and this in turn depends upon the height of this point relative to the adjacent parts of the surface. When the light passing through the annulus is advanced in phase, positive phase contrast results and areas of the specimen which are proud of the matrix appear bright and depressions dark; when the phase is retarded, negative contrast is produced and pits appear bright and hills dark [2].
Figura 1.6 Schematic arrangement of microscope system for phase-contrast (a) and polarized light (b) microscopy.
Polarized-light microscopy The basic arrangement for the use of polarized light is shown in Figura 1.6b. The only requirements of this technique are that the incident light on the specimen be plane polarized and that the reflected light be analyzed by a polarizing unit in a crossed relation with respect to the polarizer, i.e. the plane of polarization of the analyzer is perpendicular to that of the polarizer [2]. The application of the technique depends upon the fact that plane-polarized light striking the surface of an optically isotropic metal is reflected unchanged if it strikes at normal incidence. If the light is not at normal incidence the reflected beam may still be unchanged, but only if the angle
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of incidence is in, or at right angles to, the plane of polarization, otherwise it will be elliptically polarized. It follows that the unchanged reflected beam will be extinguished by an analyzer in the crossed position, whereas an elliptically polarized one cannot be fully extinguished by an analyzer in any position. When the specimen being examined is optically anisotropic, the light incident normally is reflected with a rotation of the plane of polarization and as elliptically polarized light; the amount of rotation and of elliptical polarization is a property of the metal and of the crystal orientation. If correctly prepared, as-polished specimens of anisotropic metals will respond to polarized light and a grain-contrast effect is observed under crossed polars as a variation of brightness with crystal orientation. Metals which have cubic structure, on the other hand, will appear uniformly dark under crossed polars, unless etched to invoke artificial anisotropy, by producing anisotropic surface films or well-defined pits. An etch pit will reflect the light at oblique incidence and elliptically polarized light will be produced. However, because such a beam cannot be fully extinguished by the analyzer in any position, it will produce a background illumination in the image which tends to mask the grain-contrast effect [2]. Clearly, one of the main uses of polarized light is to distinguish between areas of varying orientation, since these are revealed as differences of intensity under crossed polars. The technique is therefore very useful for studying the effects of deformation, particularly the production of preferred orientation, but information on cleavage faces, twin bands and sub-grain boundaries can also be obtained. If a sensitive tint plate is inserted between the vertical illuminator and the analyzer, each grain of a sample may be identified by a characteristic color which changes as the specimen is rotated on the stage. This application is useful in the assessment of the degree of preferred orientation and in recrystallization studies. Other uses of polarized light include distinguishing and identifying phases in multi-phase alloys [2]. Near-perfect extinction occurs when the polars of a transmission microscope are crossed. If a thin section or slice of ceramic, mineral or rock is introduced and the stage slowly rotated, optically anisotropic crystals will produce polarization colors, developing maximum brilliance at 45 to any of the four symmetrical positions of extinction. The color of a crystal depends upon its birefringence, or capacity for double-refraction, and thickness. By standardizing the thickness of the section at 3050m and using a MichelLvy color chart, it is possible to identify crystalline species. In refractory materials, it is relatively easy to identify periclase (MgO), chromite (FeCrO4), tridymite (SiO2) and zircon (ZrSiO4) by their characteristic form and color [2]. As birefringence occurs within the crystal, each incident ray forms ordinary and extraordinary rays which are polarized in different planes and travel through the crystal at different velocities. On leaving the analyzer, these out-of-phase fast and slow rays combine to produce the
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polarization color. This color is complementary to color cancelled by interference and follows Newtons sequence: yellow, orange, red, violet, blue, green. More delicate, higher-order colors are produced as the phase difference between the emergent rays increases. Anisotropic crystals are either uniaxial or biaxial, having one or two optic axes, respectively, along which birefringence does not occur. (Optic axes do not necessarily correspond with crystallographic axes.) It is therefore possible for quartz (uniaxial) and mica (biaxial) crystals to appear black because of their orientation in the slice. Uniaxial (tetragonal and hexagonal systems) can be distinguished from biaxial crystals (orthorhombic, triclinic and monoclinic systems) by introducing a Bertrand lens into the light train of the microscope to give a convergent beam, rotating the stage and comparing their interference figures: uniaxial crystals give a moving ring and brush pattern, biaxial crystals give two static eyes. Cubic crystals are isotropic, being highly symmetrical. Glassy phases are isotropic and also appear black between crossed polars; however, glass containing residual stresses from rapid cooling produces fringe patterns and polarization colors. The stress-anisotropic properties of plastics are utilized in photoelastic analyses of transparent models of engineering structures or components made from standard sheets of constant thickness and stressoptic coefficient (e.g. clear Bakelite, epoxy resin). The fringe patterns produced by monochromatic light and crossed polars in a polariscope reveal the magnitude and direction of the principal stresses that are developed when typical working loads are applied [2]. 1.2.2 1.2.2.1 Microscopa Electrnica de Barrido (Scanning Electron Microscopy) Introduction In 1993, Charles Smithart was convicted of the murder of an 11-year-old girl in the town of Glennallen, Alaska. Prosecutors suspected Smithart after he was spotted at the scene of the crime, but they had no evidence directly linking him to the murder. That's where a scanning electron microscope (SEM) came in. Using the X-ray spectroscopy detector of an SEM, a forensic scientist analyzed bits of iron found at the scene of the crime. He found that they had a globular shape that only welding or grinding produces. As it turned out, Smithart had a welding rig in his shop and would sometimes repair bicycles for the local children. Thanks to the tremendous capabilities of scanning electron microscopes, prosecutors had the evidence they needed to link Smithart to the crime. Why was an SEM, rather than a regular light, or optical, microscope from the local high school, necessary to examine the evidence for Smithart's trial? For one thing, SEMs can magnify objects at upward of 300,000 times the size of the object studied. Scientists refer to this number as the magnification power and denote it, for example, as 300,000x. In contrast, run-of-the-mill
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optical microscopes tend to have a magnification power of a few hundred times. SEMs also have tremendous depth of field compared to traditional microscopes, providing an almost 3-D image for researchers to analyze, as compared to the flatter image an optical microscope produces. Lastly, these advanced microscopes can look past the surface of an object, telling researchers information about its composition. All of these attributes proved essential in examining evidence from the Smithart case. Of course, SEMs have their share of drawbacks as well, like cost. Even the cheapest among them cost tens of thousands of dollars. They're also bulky and complex instruments, requiring considerable expertise to operate. As a result, their use is typically limited to research and industrial applications, though recent breakthroughs have made SEMS more accessible in other applications. In this article, we'll learn how SEMs are able to produce such detailed and striking images. In the process, we'll explore what goes into operating one, as well as some of the most recent breakthroughs in SEM technology. But before we learn about where the technology is headed, let's look at where it all began [3]. 1.2.2.2 How scanning electron microscope works
Figura 1.7 How scanning electron microscopes work
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We've begun to get an idea of what SEMs are capable of. Now we're ready to take a look at the various components of one and how they work together to form an image. While the variations from one model to the next are seemingly endless, all SEMs share the same basic parts. Electron gun: Electron guns aren't some futuristic weapon used in the newest Vin Diesel movie. Instead, they produce the steady stream of electrons necessary for SEMs to operate. Electron guns are typically one of two types. Thermionic guns, which are the most common type, apply thermal energy to a filament (usually made of tungsten, which has a high melting point) to coax electrons away from the gun and toward the specimen under examination. Field emission guns, on the other hand, create a strong electrical field to pull electrons away from the atoms they're associated with. Electron guns are located either at the very top or at the very bottom of an SEM and fire a beam of electrons at the object under examination. These electrons don't naturally go where they need to, however, which gets us to the next component of SEMs. Lenses: Just like optical microscopes, SEMs use lenses to produce clear and detailed images. The lenses in these devices, however, work differently. For one thing, they aren't made of glass. Instead, the lenses are made of magnets capable of bending the path of electrons. By doing so, the lenses focus and control the electron beam, ensuring that the electrons end up precisely where they need to go. Sample chamber: The sample chamber of an SEM is where researchers place the specimen that they are examining. Because the specimen must be kept extremely still for the microscope to produce clear images, the sample chamber must be very sturdy and insulated from vibration. In fact, SEMs are so sensitive to vibrations that they're often installed on the ground floor of a building. The sample chambers of an SEM do more than keep a specimen still. They also manipulate the specimen, placing it at different angles and moving it so that researchers don't have to constantly remount the object to take different images. Detectors: You might think of an SEM's various types of detectors as the eyes of the microscope. These devices detect the various ways that the electron beam interacts with the sample object. For instance, Everhart-Thornley detectors register secondary electrons, which are electrons dislodged from the outer surface of a specimen. These detectors are capable of producing the most detailed images of an object's surface. Other detectors, such as backscattered electron detectors and X-ray detectors, can tell researchers about the composition of a substance. Vacuum chamber: SEMs require a vacuum to operate. Without a vacuum, the electron beam generated by the electron gun would encounter constant interference from air particles in the atmosphere. Not only would these particles block the path of the electron beam, they would also be knocked out of the air and onto the specimen, which would distort the surface of the specimen.
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As with many things, an SEM is more than the sum of its parts. Read on to see how all of these components work together to create astounding images of very, very tiny things [4]. 1.2.2.3 Effects of Electron Bombardment Electron bombardment of a sample is unique to microprobe analysis and produces a large number of effects from the target material (Figura 1.8). The incident electrons interact with specimen atoms and are significantly scattered by them (rather than penetrating the sample in a linear fashion). Most of the energy of an electron beam will eventually end up heating the sample (phonon excitation of the atomic lattice); however, before the electrons come to rest, they undergo two types of scattering: elastic and inelastic. In elastic scattering, the electron trajectory changes, but its kinetic energy and velocity remain essentially constant (due to large differences between the mass of the electron and nucleus). This process is known as electron backscattering (although later we will confine the term "backscattered electrons" to those scatter out of the sample).
Figura 1.8 Effects produced by electron bombardment of a material.
In inelastic scattering, the trajectory of the incident electron is only slightly perturbed, but energy is lost through interactions with the orbital electrons of the atoms in the specimen. Inelastic interactions produce diverse effect including: phonon excitation (heating) cathodoluminescence (visible light fluorescence) continuum radiation (bremsstrahlung or braking radiation)
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characteristic x-ray radiation plasmon production (secondary electrons) Auger electron production (ejection of outer shell electrons)
Two major factors control which effects can be detected from the interaction volume. First, some effects are not produced from certain parts of the interaction volume (Figura 1.9). Beam electrons lose energy as they traverse the sample due to interactions with it and if too much energy is required to produce an effect, it will not be possible to produce it from deeper portions of the volume. Second, the degree to which an effect, once produced, can be observed is controlled by how strongly it is diminished by absorption and scattering in the sample. For example, although secondary and Auger electrons are produced throughout the interaction volume, they have very low energies and can only escape from a thin layer near the sample's surface. Similarly, soft X-rays, which are absorbed more easily than hard X-rays, will escape more readily from the upper portions of the interaction volume. Absorption is an important phenomenon and is discussed in more detail below.
Figura 1.9 Generalized illustration of interaction volumes for various electron-specimen interactions. Auger electrons (not shown) emerge from a very thin region of the sample surface (maximum depth about 50 ) than do secondary electrons (50-500 ).
1.2.2.4
SEM imaging Secondary Electrons Figure 1.10 shows the microstructure of the specimen by means of secondary electrons
(SE) signal at a voltage level of 20kV and a spot size of 40 m. Some features can be identified from this SE signal based on the surface topography (due to prior etching). These features have been labelled as a and b that possibly correspond to different phases (Figure 1.10), however the
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information obtained from this SE signal is merely qualitatively and cannot provide further information other than imaging. As secondary electrons are generated through inelastic interactions and their interaction volume is in the order of a few hundreds of nanometers (50 to 500 ) into the surface; only basic information of the topography is to be collected from this type of signal. The interaction or excitation volume of electrons is hemispherical jug-shaped with neck of jug at the specimens surface and is directly proportional on the accelerating voltage and inversely proportional to materials density. Electron penetration generally ranges from 1-5 m with the beam incident perpendicular to the sample. Thus for phases having high density the interaction volume is lower. As the accelerating voltage increases, then the interaction volume (given by x and y) increases according to the relations given by equations 1 and 2 [5].
x( m) =
1.5 0.1Eo
Equation 1
y ( m) =
1.5 0.077 Eo
Equation 2
Where E o is the accelerating voltage (keV) and is the materials density. Of course, the interaction volume for SE signal has to be extracted from the total volume of interaction. For example, bombarding a material with density of 2.7 g/cm3 (assuming an aluminium alloy) and accelerating voltage of 20 kV (this experiment) the total penetration of electrons (in other words volume of interaction) gives:
x = 3.3125 m and y = 2.55 m
The depth of electron penetration of an electron beam is also a function of its angle of incidence, the magnitude of its current and the average atomic number. Moreover, the main reason for coating a non-conductive specimen (such a conductive sample mounted in bakelite) with a conductive material (such as gold) is to increase the number of secondary electrons that will be emitted from the sample.
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Figure 1.10 Secondary electrons (SE) image sampling
Backscattered Electrons Figura 1.11 shows a SEM micrograph obtained by means of backscattered electrons (BS) signal. Careful observations on this image clearly revealed three distinct regions (well contrasted) identified as: dark, grey and white colored. Therefore, this metal resulted in three distinct phases as identified by the difference on image contrast. The identified phases were labeled as a, b and c as indicated in Figura 1.11. Black areas (indicated by the arrows) correspond apparently to gaps within the material possibly due to the etching, in this work EDS analysis was not conducted in those areas. Backscattered electrons are produced by elastic interactions of beam electrons with nuclei of atoms in the specimen. Many incident electrons undergo a series of such elastic event that cause them to scattered back out the specimen. The fraction of the beam electrons backscattered in this way varies strongly with the atomic number Z of the scattering atoms, but does not change much
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with changes in E o . The backscattered coefficient, which is the number of produced backscattered electrons, is given by equation 3 [6]:
bs pe
Equation 3
where pe is the number of incident electrons and bs is the number of backscattered electrons. For a pure element, the backscattered coefficient, depend on Z, can be calculated by:
= 0.0254 + 0.016Z 1.86 x10 4 Z 2 + 8.3x10 7 Z 3
Equation 4
For homogeneous mixtures mix is calculated from the weight fractions of elemental components by:
mix = Ci i
i
In summary, dark phase correspond to the lowest atomic number (Z) phase in this alloy. Grey and lighter regions correspond to higher Z numbers. Basically as all phases (elements) have different size nuclei, as the size of the atom nuclei increases, the number of BSE increases.
Figura 1.11 Backscattered electrons (BS) image sampling
1.2.2.5
Volume of Excitation Two factors limit the size and shape of the interaction volume: (1) energy loss through
inelastic interactions and (2) electron loss or backscattering through elastic interactions. The resulting excitation volume is a hemispherical to jug-shaped region with the neck of jug at the
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specimen surface. The analyst must remember that the interaction volume penetrates a significant depth into the sample and avoid edges where it may penetrate overlapping materials. The depth of electron penetration of an electron beam and the volume of sample with which it interacts are a function of its angle of incidence, the magnitude of its current, the accelerating voltage, and the average atomic number (Z) of the sample. Of these, accelerating voltage and density play the largest roles in determining the depth of electron interaction (Figura 1.12).
Figura 1.12 Schematic depiction of the variation of interaction volume shape with average sample atomic number (Z) and electron beam accelerating voltage (E o ). The actual shape of the interaction volume is not as long-necked since the electron beam in microprobe analysis has a diameter of about 1 m (see Figure 2.1b).
Electron penetration generally ranges from 1-5 m with the beam incident perpendicular to the sample. The depth of electron penetration is approximately (Potts, 1987, p. 336):
For example, bombarding a material with a density of 2.5 g/cm3, about the minimum density for silicate minerals, with E o = 15 keV, gives x = 2.3 m. The width of the excited volume can be approximated by (Potts, 1987, p. 337):
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Both of these are empirical expressions. A theoretical expression for the "range" of an electron, the straight line distance between where an electron enters and its final resting place, for a given E o is (Kanaya & Okayama, 1972):
The volume of interaction can be modeled by Monte Carlo simulation. In such models, the likelihood of incident electrons interacting with the sample and scattering and the angle of deflection are determined probabilistically. X-ray generation depths depend strongly on density and accelerating voltage (Figure 2.2b.). The results derived from Monte Carlo modeling yield a volume of interaction that is very similar to that determined by etching experiments. The excited volume is roughly spherical and truncated by the specimen surface. The depth of the center of the sphere decreases with increasing atomic number of the target [7].
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Figura 1.13 Comparison of electron paths (top) and sites of X-ray excitation (bottom) in targets of aluminum, copper, and gold at 20 keV, simulated in a Monte Carlo procedure.
1.2.3 1.2.3.1
Microscopa Electrnica de Transmisin (Transmission Electron Microscopy) Introduction A typical commercial transmission electron microscope (TEM) costs about $2 for each
electron volt of energy in the beam, and if you add on all the options, it can cost about $4-5 per eV. As you'll see, we use beam energies in the range from 100,000-400,000 eV, so a TEM becomes an extremely expensive piece of equipment. Consequently, there have to be very sound scientific reasons for investing such a large amount of money in one microscope [8]. Transmission electron microscopy (TEM) is the pre-eminent method for determining dislocations and other crystallographic defects character and for performing chemical and crystallographic analysis of micrometer and smaller precipitates and other microstructures. Use of TEM in materials science/engineering can be introduced here in only a few additional pages and is well worth the small increment of effort. Since most defect characterization requires an understanding of diffraction contrast, this is an important constituent of this chapter. A TEM equipment is shown in Figura 1.14.
Figura 1.14 A transmission electron microscope Philips CM-12
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1.2.3.2
Depth of field The depth of field of a microscope is a measure of how much of the object we are looking at
remains "in focus" at the same time. Like the resolution, this property is governed by the lenses in the microscope. The best electron lens is not a very good one, as we've already mentioned, and has been compared to using the bottom of a Coca-Cola bottle as a lens for light microscopy. To minimize this problem we have to use very small limiting apertures in the lenses, narrowing the beam down to a thin "pencil" of electrons which at most is a few micrometers across. These apertures cut down the intensity of the electron beam, but also act to increase the depth of focus of the images that we produce. Remember that "depth of field" refers to the specimen while "depth of focus" refers to the image. While this large depth of field is chiefly used in the SEM to produce 3D-like images of the surfaces of specimens with large changes in topography, it is also critical in the TEM. It turns out that in the TEM, all of the specimen is usually in focus at the same time, independent of the specimen topography, as long as it's electron transparent! Figura 1.15 shows a TEM image of some dislocations in a crystal. The dislocations appear to start and finish in the specimen, but in fact they are threading their way through the specimen from the top to the bottom, and they remain in sharp focus at all times. Furthermore, we can record the final image at different positions below the final lens of the instrument and it will still be in focus.
Figura 1.15 TEM image of dislocations in GaAs (Gallium arsenide). A band of dislocations threads through the thin specimen from the top to the bottom but remains in focus through the foil thickness.
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1.2.3.3
Diffraction Thompson and Reid showed that electrons could be diffracted when passing through thin
crystals of nickel, and the possibility of combining electron diffraction into TEMs was realized by Kossel and Mllenstedt (1939). Today, electron diffraction is an indispensable part of TEM and is arguably the most useful aspect of TEM for materials scientists. Figura 1.16 shows a TEM diffraction pattern which contains information on the crystal structure, lattice repeat distance, and specimen shape, as well as being a most striking pattern. We'll see that the pattern can always be related to the image of the area of the specimen from which it came, in this case shown in the inset. You will also see in Part II that, in addition to the things we just listed, you can conduct a complete crystallographic symmetry analysis of minuscule crystals, including such esoteric aspects as pointgroup and space-group determination, and at all times the crystallography can be related to the image of your specimen. There is no similar capability on a light microscope because of the relatively large wavelength of visible light. So an electron microscope can produce atomic level images, can generate a variety of signals telling you about your sample chemistry and crystallography, and you can always produce images that are in focus. There are many other good reasons why you should use electron microscopes. We hope they will become evident as you read through this book. At the same time there are many reasons why you should not always seek to solve your problems with the TEM, and it is most important that you realize what the instrument cannot do, as well as knowing its capabilities [8].
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Figura 1.16 TEM diffraction pattern from a thin foil of Al-Li-Cu containing various precipitate phases, shown in the inset image. The central spot (X) contains electrons that come directly through the foil and the other spots and lines are diffracted electrons which are scattered from different crystal planes.
1.2.3.4
Interpreting TEM images Another problem is that the TEM presents us with 2D images of 3D specimens, viewed in
transmission. Our eyes and brain routinely understand reflected light images but are ill-equipped to interpret TEM images, and so we must be cautious. Hayes (1980) illustrates this problem well by showing a picture of two rhinos, side by side such that the head of one appears attached to the rear of the other (see Figure 1.17). As Hayes puts it: "when we see this image we laugh" (because we understand its true nature in 3D) "but when we see equivalent (but more misleading) images in the TEM, we publish!" So beware of artifacts, which abound in TEM images.
Figure 1.17 Photograph of two rhinos taken so that, in projection, they appear as one two-headed beast. Such projection artifacts in reflected light images are easily discernible to the human eye but similar artifacts in TEM images are easily mistaken for "real" features.
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One aspect of this particular drawback is that, generally, all the TEM information that we talk about in this book (images, diffraction patterns, spectra) is averaged through the thickness of the specimen. In other words, a single TEM image has no depth sensitivity, as is apparent. 1.2.3.5 Specimen Preparation All the above advantages of the TEM bring accompanying drawbacks. First of all, the price to pay for any high-resolution imaging technique is that you only look at a small part of your specimen at any one time. The higher the resolution, therefore, the worse the sampling abilities of the instrument. We have an instrument that is a terrible sampling tool! This only serves to emphasize that before you put your specimen in the TEM you must have examined it with techniques that offer poorer resolution but better sampling, such as your eyes, the visible-light microscope, and the scanning electron microscope. In other words, know the forest before you start looking at the leaves on the trees. Your specimens have to be thin if you're going to get any information using transmitted electrons in the TEM. "Thin" is a relative term, but in this context it means "electron transparent." For a specimen to be transparent to electrons it must be thin enough to transmit sufficient electrons such that enough intensity falls on the screen or photographic film to give us an interpretable image in a reasonable time. Generally this requirement is a function of the electron energy and the average atomic number of the specimen. Typically for 100-keV electrons, specimens of aluminum alloys almost up to 1 pm would be thin, while steel would be thin up to about several hundred nm. However, it is an axiom in TEM that thinner is better, and specimens below 100 nm should be used wherever possible, and in extreme cases, such as when doing HRTEM or electron spectrometry, specimen thicknesses <50 nm are essential. These demands become less strict as the beam voltage increases, but this is offset by the danger of beam damage. So it should be obvious to you by now that while TEM and associated techniques are tremendously powerful characterization tools when used properly, they should never be used in isolation to solve a materials problem. You must understand your material at low magnification with your eyes and with visible-light microscopy and scanning electron microscopy (SEM) before venturing into TEM studies. Otherwise you may fall foul of some of the limitations we have just listed [8].
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1.3
1.3.1
Anlisis de XRD (X-Ray Diffraction)

Electromagnetic radiation Discovered in 1885, these rays are invisible and travel in straight lines and more penetrating
than visible light.
What are x-rays? X-rays are electromagnetic radiation which is exactly the same nature of visible light but of very much shorter wavelength. Wavelengths: X-rays 0.5 to 2.5 , visible light (V.L.) - 6000 X-rays are associated with and electric field E in the y direction and a magnetic field H in the z direction.
Figure 1.18 Electric and magnetic fields associated with a wave moving in the x-direction
A amplitude, frequency The variation of E is not sinusoidal but it matters little, the important issue is its periodicity.
Figura 1.19 shows the variation of E graphically
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Figura 1.19 The variation of E, (a) with t at a fixed value of x and (b) with x at a fixed value of t
the wavelength and the frequency are connected by the relation
where c is the velocity of light of 3x108 m/s
What is the intensity? Intensity is a flow of energy through unit area perpendicular to the direction of motion of the wave. The average value of the intensity is proportional to the square of the amplitude on the wave. In absolute units intensity is measured in joules/m2/sec but this measurement is difficult one. Most x-rays intensity measurements are made by counting the number of photons incident on a detector.
Classical theory: electromagnetic radiation has been considered wave motion. Quantum theory: electromagnetic radiation is considered can also been considered as a stream of particles called quanta or photons. Each photon is associated with it an amount of energy of h where h is Planks constant (6.63x10-34 joule*sec)
Radiation has thus a dual wave-particle character. 1.3.2 Production of X-Rays How are x-rays produced?
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X-rays are produced when an electrical charged particle (electron) of sufficient kinetic energy decelerates. Electrons are being produced in an x-rays tube by maintaining a high voltage across the electrodes drawing the electrons to the anode or target.
The kinetic energy of electrons on impact is given by
where e is the charge on the electron (1.6x10-19 coulombs) and V is the voltage across the electrodes; m (9.11x10-31 kg) is the mass of the electron and 2 is the velocity in m/sec just before impact.
X-rays coming from the target are found to consist of a mixture of different wavelengths and the variation of intensity with wavelength depends on the tube voltage (i.e.30,000V).
Since x-rays are produced whenever high-speed electrons collide with a metal target. Any x-ray tube must contain (a) a source of electrons, (b) a high accelerating voltage, and (c) a metal target. Furthermore, since most of the kinetic energy of the electrons is converted into heat in the target, the latter is almost alwavs watercooled to prevent its melting. A1l x-ray tubes contain two electrodes, an anode (the metal target) maintained, with few exceptions, at ground potential, and a cathode, maintained at a high negative potential, normally of the order of 30,000 to 50,000 volts for diffraction work. X-ray tubes may be divided into two basic types, according to the way in which electrons are provided: gas tubes (obsolete), in which electrons are produced by the ionization of a small quantity of gas (residual air in a partly evacuated tube), and filament tubes, in which the source of electrons is a hot filament. Filament tubes were invented by Coolidge in 1913. They consist of an evacuated glass envelope which insulates the anode at one end from the cathode at the other, the cathode being a tungsten filament and the anode a water-cooled block of copper containing the desired target metal as a small insert at one end. Figure 1.20 is a photograph of such a tube, and Figure 1.21 shows its internal construction.
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Figure 1.20 Sealed x-ray tube.
Figure 1.21 Cross section of sealed x-ray tube (schematic)
1.3.3
X-Ray Diffraction Differences in the path length of various rays arise quite naturally when considering how a
crystal diffracts x-rays. Figura 1.22 shows a section of a crystal, its atoms arranged on a set of parallel planes A, B, C, D, ... , normal to the plane of the drawing and spaced a distance d' apart. Assume that a beam of perfectly parallel, perfectly monochromatic x-rays of wavelength is incident on this crystal at an angle , called the Bragg angle, where is measured between the incident beam and the particular crystal planes under consideration.
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Figura 1.22 Diffraction of x-rays by a crystal.
Whether this incident beam of x-rays will be diffracted by the crystal and, if so, under what conditions, are the questions central to this chapter. A diffracted beam may be defined as a beam composed of a large number of scattered rays mutually reinforcing one another. Diffraction is, therefore, essentially a scattering phenomenon. Atoms scatter incident x-rays in all directions and the following paragraphs demonstrate that in some of these directions the scattered beams will be completely in phase and so reinforce each other to form diffracted beams. For the particular conditions described by Figura 1.22, the only diffracted beam formed is that shown, namely one making an exit angle with respect to the diffraction planes equal to the angle of incidence. This will be shown, first, for one plane of atoms and, second, for all the atoms making up the crystal. Consider rays 1 and la in the incident beam; they strike atoms K and P in the first plane of atoms and are scattered in all directions. Only in the directions 1 and 1a, however, are these scattered beams completely in phase and so capable of reinforcing one another; they do so because the difference in their length of path between the wave fronts XX' and YY' is equal to:
Similarly, the rays scattered by all the atoms in the first plane in a direction parallel to 1' are in phase and add their contributions to the diffracted beam. This will be true of al1 the planes separately, and it remains to find the condition for reinforcement of rays scattered by atoms in different planes. Rays 1 and 2, for example, are scattered by atoms K and L, and the path difference for rays 1K1' and 2L2' is:
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This is also the path difference for the overlapping rays scattered by S and P in the direction shown, since in this direction there is no path difference between rays scattered by S and L or P and K. Scattered rays 1' and 2' will be completely in phase if this path difference is equal to a whole number n of wavelengths, or if:
This relation was first formulated by W. L. Bragg and is known as Bragg's law. It states the essential condition which must be met if diffraction is to occur, n is called the order of diffraction; it may take on any integral value consistent with sin not exceeding unity and is equal to the number of wavelengths in the path difference between rays scattered by adjacent planes. The rays scattered by all the atoms in all the planes are therefore completely in phase and reinforce one another (constructive interference) to form a diffracted beam in the direction shown. In all other directions of space the scattered beams are out of phase and annul one another (destructive interference). The diffracted beam is rather strong compared to the sum of all the rays scattered in the same direction, simply because of the reinforcement which occurs, but is extremely weak compared to the incident beam since the atoms of a crystal scatter only a small fraction of the energy incident on them [9]. 1.3.4 Diffractometers Depending solely on the way it is used, the basic x-ray diffractometer/spectrometer is really two instruments: 1. An instrument for measuring x-ray spectra by means of a crystal of known structure. 2. An instrument for studying crystalline (and noncrystalline) materials by measurements of the way in which they diffract (scatter) x-rays of known wavelength. The term spectrometer was originally used to describe both instruments, but, properly, it should be applied only to the first. The second instrument is aptly called a diffractometer: this name serves well to emphasize the particular use to which the instrument is being put, namely, diffraction analysis rather than spectrometry. An example of a diffractometer is shown in Figure 1.23.
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Figure 1.23 Diffractometer
1.3.5
Applications of X-Ray Diffraction In general the following applications can be found in a diffraction technique: Phase identification Determination of crystal structure Phase diagram determination Quantitative phase analysis Precise parameter measurements Structure of polycrystalline aggregates Stress measurement Orientation of single crystals Crystal quality Polymers Small Angle scattering
1.4
1.4.1
Ensayos o pruebas no destructivas (non-destructive testing)

Lquidos Penetrantes Introduccin a los Lquidos Penetrantes Discontinuidades que detecta, defectos superficiales como: poros, grietas, rechupes,
1.4.1.1
traslapes, costuras, laminaciones, etc. Materiales: Slidos metlicos y no metlicos
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VENTAJAS Muy econmico Inspeccin a simple vista No se destruye la pieza Se obtiene resultados inmediatos.
DESVENTAJAS Solo detecta fallas superficiales Difcil establecimiento de patrones La superficie a inspeccionar debe estar limpia y sin recubrimientos No se puede inspeccionar materiales demasiado porosos
PRINCIPIOS FSICOS Capilaridad: Es la accin que origina que un liquido ascienda o descienda a travs de los llamados tubos capilares. Cohesin: Es la fuerza que mantiene a las molculas de un cuerpo a distancias cercanas unas de las otras. Adherencia: Es la fuerza de atraccin entre molculas de sustancias diferentes. Viscosidad: Es la resistencia al deslizamiento de una capa de un fluido sobre otra capa. Tensin superficial: Es la fuerza no compensada que ejerce la superficie del lquido debido a la tensin no compensada de las molculas subsuperficiales sobre la membrana superior.
1.4.1.2
Caractersticas de los lquidos penetrantes El lquido penetrante tiene la propiedad de penetrar en cualquier abertura u orificio en la
superficie del material. El penetrante ideal debe reunir lo siguiente:
Habilidad para penetrar orificios y aberturas muy pequeas y estrechas. Habilidad de permanecer en aberturas amplias. Habilidad de mantener color o la fluorescencia. Habilidad de extenderse en capas muy finas. Resistencia a la evaporacin. De fcil remocin de la superficie.
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De difcil eliminacin una vez dentro de la discontinuidad. De fcil absorcin de la discontinuidad. Atoxico. Inoloro. No corrosivo. Antiinflamable. Estable bajo condiciones de almacenamiento. Costo razonable.
Propiedad fsica Capilarida d Tensin superficial Adherenci a Cohesin Viscosidad Partculas
Penetrante
Revelador
Alta
Baja
Baja
Alta
Baja
Alta
Baja Baja Pequeas
Alta Alta Grandes
Tensin superficial: Es una de las propiedades ms importantes. Se requiere una tensin superficial baja para obtener buenas propiedades de penetracin y mojado Poder humectante: El penetrador debe ser capaz de mojar completamente la superficie del material y es una de las propiedades ms importantes. Esto se refiere al ngulo de contacto del lquido con la superficie, el cual debe ser lo mas bajo posible. Viscosidad: Esta propiedad no produce efecto alguno en la habilidad del lquido para penetrar, aunque afecta la velocidad de penetracin. Los penetrantes de alta viscosidad penetran lentamente, en tanto que los de baja viscosidades escurren muy rpido y tiene la tendencia a no ser retenidos en los defectos de poca profundidad; por lo tanto se recomienda una viscosidad media.
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Volatilidad: Los lquidos penetrantes no deben ser voltiles. Si existe una evaporacin excesiva se los productos del penetrante, se ver afectada la sensibilidad de todo el proceso, debido tanto al desequilibrio de la formula, como a la perdida del poder humectante. Gravedad especifica o densidad relativa: No juega un papel directo sobre
el comportamiento de un penetrante dado; sin embargo, con densidades bajas se facilita el transporte de materiales extraos que tendern a sedimentar en el fondo cuando se usan tanques abiertos. La mayora de los lquidos penetrantes tienen densidades relativas que varan entre 0.86 y 1.06 a 16C, por lo general la densidad es menor a 1. Punto de inflamacin: Como medida de seguridad practica los lquidos penetrantes debern poseer un punto de inflamacin elevado con el fin de reducir los peligros de incendio. Generalmente el punto de inflamacin es mayor de 95 C y en recipientes abiertos no debe ser menor de 65 C. Inactividad qumica: Los productos usados en la formulacin de los lquidos penetrantes deben se inertes y no corrosivos con respecto a los materiales a ser ensayados y a los recipientes que los contienen. Capacidad de disolucin: El penetrante debe tener una elevada capacidad para contener grandes concentraciones de pigmentos coloreados o fluorescentes usados y mantenerlos en solucin. 1.4.1.3 Mtodo de aplicacin de los lquidos penetrantes en Pruebas No Destructivas Se aplica el lquido penetrante a la superficie de la pieza a ser examinada, permitiendo que penetre en las aberturas del material, despus de lo cual el exceso del lquido es removido. Se aplica entonces el revelador, el cual es humedecido o afectado por el penetrante atrapado en las discontinuidades de esta manera se incrementa la evidencia de las discontinuidades, tal que puedan ser vistas ya sea directamente o por medio de una lmpara o luz negra.
Tipo I = Penetrante fluorescente Tipo II = Tintas permanentes o visibles Proceso A = Penetrante lavable en agua Proceso B = Penetrante postemulsificado Proceso C = Penetrante removido con solvente Revelador seco: Grano fino se aplica por espolvoreado, rociado o sumergido. Revelador no acuoso: Es una suspensin absorbente, aplicado por roco Revelador hmedo: Es una suspensin absorbente de polvo en agua, se aplica por inmersin. Porttil ( atomizador ) Estacionario ( inmersin )
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Simple vista Spoteheck (porttil) Luz negra Syglo (estacionario) Porttil Liquido penetrante Removedor Revelador Incoloro Blanco Rojo Estacionario Verde (fluorescente) Incoloro Blanco
PREPARACIN Y LIMPIEZA DE LA PIEZA: Limpiar cuidadosamente la superficie a inspeccionar de pintura, aceite, grasa y otros contaminantes. Ser necesario eliminar los restos de xidos, pinturas, grasas, aceites, taladrillas, carbonillas, etc. Y esto se hace por mtodos qumicos, ya que los mecnicos, estn prohibidos por la posibilidad que tiene su aplicacin de tapar defectos existentes. Se pueden usar todos aquellos procesos que dejen a la superficie limpia y seca; que no daen al espcimen y que no empleen productos que sean incompatibles con los componentes. Soluciones detergentes en caliente por inmersin, desengrase en fase de vapor o desengrase mediante disolvente, son los principales mtodos para eliminar grasas y aceites. Los xidos y las carbonillas trmicas se eliminaran con desoxidantes alcalinos o cidos y a veces, principalmente en superficies rectificadas se hace un ataque cido a fondo que abre las grietas durante la operacin. Las pinturas se eliminan con productos custicos en caliente o basados en ellos. APLICACIN DEL PENETRANTE. Los penetrantes se aplican por inmersin, rociado con un cepillo o brocha, vertiendo el liquido sobre la pieza o cualquier otro mtodo, vertiendo el liquido sobre la pieza o cualquier otro mtodo que cubra la zona que se inspecciona. Ser necesario obtener una pelcula fina uniforme en toda la superficie y se deber esperar un tiempo llamado tiempo de penetracin para que el liquido penetre en grietas. Este tiempo oscila entre los 5 y 15 minutos dependiendo del material y la clase de grietas.
ELIMINACIN DEL EXCESO DE PENETRANTE. Se debe retirar la capa superficial del penetrante de forma que lo nico que permanezca sea el que se hubiera alojado en las discontinuidades. Se entiende por exceso de penetrante todo liquido que no se ha introducido en los defectos y que permanece sobrante sobre la superficie de la pieza a inspeccionar.
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Esta etapa es critica y de su correcta realizacin depender el resultado final de la inspeccin, ya que es necesario eliminar y limpiar el exceso de penetrante de tal modo que no extraigamos el penetrante introducido en los defectos. Si no se ha eliminado perfectamente el liquido penetrante, en la inspeccin final aparecern manchas de penetrante produciendo indicaciones falsas e incluso, el enmascaramiento de las grietas. Para saber si hemos eliminado bien el exceso de penetrante es necesario hacer una inspeccin visual. Es aconsejable quitar en primer lugar la mayor parte del penetrante con trapos o papel absorbente y despus eliminar el resto utilizando trapos o papel ligeramente impregnados en disolvente.
APLICACIN DEL REVELADOR. Aplicar el revelador y dejarlo actuar. El revelado es la operacin que hace visible al ojo humano la posicin del defecto. El revelador es bsicamente un producto en polvo de compuestos qumicos blancos, inertes y con una granulometra tal que dispone de un gran poder de absorcin. Una vez aplicado el revelador, hay que esperar un tiempo para que absorba el penetrante, este tiempo oscila entre 5 y 15 minutos. Durante la preparacin de las piezas para la inspeccin es necesario secarlas despus de la aplicacin del revelador hmedo o eliminar el remanente antes del uso del polvo revelador seco.
INSPECCIN FINAL DE LA PIEZA. Una vez transcurrido el tiempo de revelado, se procede a la inspeccin de los posibles defectos de las piezas procesadas. El tiempo de revelado depende del tipo de penetracin, del revelador y del defecto, pero deber permitirse tiempo suficiente para que se formen las indicaciones. La inspeccin se realiza antes de que el penetrante comience a exudar sobre el revelador hasta el punto de ocasionar la perdida de definicin. El proceso de inspeccin se compone de tres etapas. Inspeccin. Interpretacin. Una regla prctica es que el tiempo de revelado nunca debe ser menor a siete minutos. Indicaciones relevantes. Son las causadas por discontinuidades que estn generalmente presentes en el diseo. Indicaciones falsas. Son el resultado de alguna forma de contaminacin con penetrantes, estas indicaciones no pueden referirse a ningn tipo de discontinuidad.
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LIMPIEZA FINAL. Se debe llevar a cabo en razn de los productos usados en el ensayo. Tiempo de Penetracin
Material Proceso Tipo de discontinuidad Fundicin Extrusin y forja Aluminio Soldadura Todos Todos Porosidades Traslapes Falta de fusin Porosidades Grietas Grietas de fatiga Fundicin Extrusin y forja Magnesio Soldadura Todos Porosidades Traslapes Falta de fusin Porosidades Grietas Grietas de fatiga Fundicin Extrusin y forja Acero Soldadura Todos Todos Porosidades Traslapes Falta de fusin Porosidades Grietas Grietas de fatiga Fundicin Latn y bronce Extrusin y forja Recubrimientos Porosidades Traslapes Falta de fusin Tipo I Y II Proceso A 5 a 10 min NR 30 30 30 NR 15 NR 30 30 30 NR 30 NR 60 60 30 NR 10 NR 15 Tipo I Y II Proceso B 5 min 10 5 5 10 30 5 10 10 10 10 30 10 10 10 10 10 30 5 10 10 Tipo I Y II Proceso C 3 min 7 3 3 5 5 3 7 5 5 5 7 5 7 7 7 7 10 3 7 3
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Todos
Porosidades Grietas
15 30 5 a 30 5 a 30 30 30 30 NR
10 10 5 5 5 5 20 20 a 30
3 3 5 5 3 3 5 15
Plsticos Vidrio Herramienta con punta de carburo
Todos Todos
Grietas Grietas Falta de fusin Porosidades Grietas
Titanio y aleacionesa altas temperaturas Todos metales
Todos
Todos
Esfuerzos o Granulacin Interna
NR
240
240
NR = no recomendable
Gua de Seleccin del proceso
PROBLEMA
PROCESO OBSERVACIONES TIPO I Y II
Alta produccin de artculos pequeos Alta produccin de artculos grandes Alta sensibilidad para discontinuidades finas Discontinuidades superficiales, rayones, etc. Deben detectarse Artculos con rugosidad superficial
Pequeas cantidades mojadas en canastas
Grandes forjas, extrusiones, etc.
Indicaciones mas claras y mas brillantes
Puede controlarse la profundidad de emulsificacin.
Artculos con cuerdas y cueros. A
El penetrante podra fijarse en las esquinas.
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Artculos con rugosidad superficial media
AB
La eleccin depende de los requerimientos de produccin y sensibilidad.
Prueba por puntos. Se necesita equipo porttil. No se dispone de agua y electricidad
C C C
Artculos anodizados, agrietados C B A despus del anodizado Repetir el proceso C
De preferencia el orden indicado
Cinco a seis repeticiones podran ser el limite.
Deteccin de fugas
AB
CARACTERSTICAS DEL PENETRANTE FLUORESENTE
TIPO
VENTAJAS La fluorescencia asegura visibilidad Fcilmente lavable con agua. Grandes cantidades de especimenes pequeos. Superficies rugosas.
DESVENTAJAS Requiere luz negra y reas obscuras. No es seguro en la deteccin de rayones y fallas superficiales. No es seguro volver a probar. No es seguro en superficies anodizadas. cidos y cromatos afectan la sensibilidad. Fcilmente sobre lavado. El penetrante esta expuesto a la contaminacin del agua.
LAVADO CON AGUA
Cueros y cuerdas. Amplio rango de discontinuidades. Rpido. Proceso sencillo.
La fluorescencia asegura visibilidad.
Requiere luz negra y reas obscuras.
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Alta sensibilidad para POST discontinuidades muy finas.
Requiere mas paso. Requiere equipo para la aplicacin de emulsivo. Difcil remocin del penetrante en cuerdas, cueros, agujeros ciegos y superficies rugosas
EMULSIFICADO Bueno para discontinuidades superficiales. Fcilmente lavable con agua despus de la emulsificacin. Tiempo de penetracin corto. No puede ser fcilmente sobre lavado La fluorescencia asegura visibilidad REMOVIDO CON SOLVENTE Porttil. No requiere agua.
Requiere luz negra y reas obscuras. Material inflamable. No puede usarse en tanques
Bueno sobre piezas anodizadas. abiertos. Para verificacin por puntos. Las piezas pueden ser re probadas Difcil su empleo sobre superficies rugosas tales como fundicin de magnesio.
1.5
Ensayos mecnicos
Se propone asignar los siguientes porcentajes a los diferentes rubros para la
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1.6
Referencias
[1] Avner, Sydney H., Introduccin a la Metalurgia Fsica, McGraw Hill. (1988). [2] R. E. Smallman, A.H.W. Ngan, Physical Metallurgy and Advanced Materials, seventh edition, Ed. Butterworth-Heinemann (2007). [3] http://science.howstuffworks.com/scanning-electron-microscope.htm [4] http://science.howstuffworks.com/scanning-electron-microscope2.htm [5] http://www4.nau.edu/microanalysis/microprobe/interact-volume.html [6] http://www.concrete.cv.ic.ac.uk/durability/research%20techniques%20sem.htm [7] http://www4.nau.edu/microanalysis/Microprobe/Interact-Volume.html [8] David B. Williams, C. Barry Carter, Transmission Electron Microscopy Basics I, Springer Science+Business Media Inc., 1996 [9] B.D. Cullity, S.R. Stock, Elements of X-Ray Diffraction, Third Edition, Prentice Hall, 2001
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UNIVERSIDAD AUTNOMA DE ZACATECAS

Programa de Ingeniera Mecnica

Notas del Programa Metalurgia Fsica

Material Preparado por: Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

1.5 ENSAYOS MECNICOS ..................................................................................................................... 44 1.6 REFERENCIAS .................................................................................................................................. 45

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

1 Tcnicas de Caracterizacin del Metalurgista

Mtodos para la caracterizacin de los metales y sus aleaciones

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Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

Microscopa ptica, electrnica (SEM) y de transmisin (TEM)

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Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

Figura 1.7 How scanning electron microscopes work

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Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

Figura 1.8 Effects produced by electron bombardment of a material.

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Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

x = 3.3125 m and y = 2.55 m

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Notas de la materia Metalurgia Fsica

Figure 1.10 Secondary electrons (SE) image sampling

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

= 0.0254 + 0.016Z 1.86 x10 4 Z 2 + 8.3x10 7 Z 3

Figura 1.11 Backscattered electrons (BS) image sampling

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

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Notas de la materia Metalurgia Fsica

Figura 1.14 A transmission electron microscope Philips CM-12

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Notas de la materia Metalurgia Fsica

Dr. Vctor Hugo Baltazar Hernndez

Notas de la materia Metalurgia Fsica