UNIVERSIDAD AUTÓNOMA DE ZACATECAS

Programa de Ingeniería Mecánica

Av. López Velarde No. 801 Col. Centro Zacatecas, Zacatecas, C.P. 98000 Tel. 01 (492) 923 94 07 ext. 1615

Notas del Programa Metalurgia Física

Material Preparado por: Dr. Víctor Hugo Baltazar Hernández

Notas de la materia Metalurgia Física

CONTENIDO

1 LAS HERRAMIENTAS DEL METALURGISTA .............................................................................. 3 1.1 MÉTODOS PARA LA CARACTERIZACIÓN DE LOS METALES Y SUS ALEACIONES ................................. 3 1.1.1 La metalografía .................................................................................................... 3

1.2 MICROSCOPÍA ÓPTICA, ELECTRÓNICA (SEM) Y DE TRANSMISIÓN (TEM) ....................................... 8 1.2.1 1.2.2 1.2.3 Microscopía óptica (light microscopy) .............................................................. 8 Microscopía Electrónica de Barrido (Scanning Electron Microscopy) ....... 14 Microscopía Electrónica de Transmisión (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 Líquidos Penetrantes ........................................................................................ 35

1.5 ENSAYOS MECÁNICOS ..................................................................................................................... 44 1.6 REFERENCIAS .................................................................................................................................. 45

Dr. Víctor Hugo Baltazar Hernández

2012

2

Notas de la materia Metalurgia Física

1 Técnicas de Caracterización del Metalurgista
1.1
1.1.1

Métodos para la caracterización de los metales y sus aleaciones
La metalografía La metalografía o microscopía estudia microscópicamente las características estructurales

de un metal o de una aleación. Sin duda, el microscopio es la herramienta más importante del metalurgista tanto desde el punto de vista científica como desde el técnico. Es posible determinar el tamaño de grano, y el tamaño, forma y distribución de varias fases e inclusiones que tienen gran efecto sobre las propiedades mecánicas del metal. La microestructura revelara el tratamiento mecánico y térmico del metal y, bajo un conjunto de condiciones dadas, podrá predecirse su comportamiento esperado. La experiencia ha demostrado que el éxito 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 preparación de una muestra es comparativamente sencillo y requiere de una técnica desarrollada solo después de práctica constante. El último objetivo es obtener una superficie plana, sin ralladuras, semejante a un espejo. Las etapas necesarias para preparar adecuadamente una muestra metalográfica se explican en lo siguientes subíndices [1]. 1.1.1.1 Muestreo La selección 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 más próxima al área de la falla y comparársele con una tomada de la sección normal o sana. Si el material es suave, como metales o aleaciones no ferrosas y aceros no tratados térmicamente, la sección puede obtenerse por corte manual con una segueta. Si el material es duro, la sección 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 fría durante la operación de corte [1]. 1.1.1.2 Esmerilado burdo o tosco Siempre que sea posible, la muestra debe ser de un tamaño fácil de manipular. Una muestra blanda se puede aplanar si se mueve lentamente hacia arriba y hacia abajo a través de la superficie

Dr. Víctor Hugo Baltazar Hernández

2012

3

Notas de la materia Metalurgia Física

de una lima plana poco áspera. La muestra blanda o dura puede esmerilarse burdamente sobre una lija de banda (rotatoria), manteniendo la muestra fría sumergiéndola frecuentemente en agua durante la operación 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, características del abrasivo más fino. El esmerilado continúa 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 después del esmerilado [1].

a)

b)

c)
Figura 1.1 a) Superficie de la muestra después del esmerilado burdo, amplificación 100x. b) Superficie de la muestra después del pulido intermedio en papel 400, amplificaci6n 100x. c) Superficie de la muestra sin ralladuras después del pulido final, amplificación 50x. Los puntos negros son impurezas de óxido.

1.1.1.3

Montaje Las muestras pequeñas o de forma incomoda deben montarse de alguna manera para

facilitar el pulido intermedio y final. Alambres, varillas pequeñas, muestras de hoja metálica, secciones delgadas, etc., deben montarse en un material adecuado o sujetarse rígidamente en una monta mecánica.

Dr. Víctor Hugo Baltazar Hernández

2012

4

la base con la muestra puede extraerse del dado de moldeo mientras esta caliente. Víctor Hugo Baltazar Hernández 2012 5 . las resinas termoplásticas no sufren cura a la temperatura de moldeo. son muy resistentes a la acción de los reactivos de ataque que se emplean comúnmente. como se ve en la Figura 1. sino que adquieren estabilidad al enfriarse.2 a) Muestra montada en baquelita. lo cual simplifica la identificaci6n de las muestras montadas. Las muestras laminares delgadas. al tiempo que se mantiene la presión de moldeo. Los polvos para moldear baquelita se fabrican en colores de este material.5. se colocan en el cilindro de la prensa de montar. La muestra y la cantidad correcta de polvo de baquelita. Esta transparencia resulta útil cuando es necesario observar la sección exacta que se pule o cuando por cualquier otra razón se desea ver por completo la muestra en la base. La temperatura aumenta gradualmente hasta 150°C y se aplica una presión de moldeo de unas 4 000 lbs/pulg2 simultáneamente. b) muestra montada en lucita. Si se saca la base todavía caliente o si se deja enfriar lentamente en el cilindro de moldeo a la temperatura ambiente sin sacarla.Notas de la materia Metalurgia Física Los materiales plásticos sintéticos que se acoplan a la muestra en una prensa para montar especial proporcionan las bases de un tamaño uniforme conveniente (generalmente de 2. como el de la Figura 1. 3. de diámetro) para manipular las muestras en ulteriores operaciones de pulido./pulg2 ) . Estas bases. Una vez que la baquelita esta adherida y curada cuando se alcanza esta temperatura. La lucita es la resina termoplástica mas común. c) muestra sostenida en un dispositivo de sujeción de metal. es completamente transparente cuando se moldea en forma adecuada. Al contrario de los plásticos termofijados. ó 4 cm. suelen alternarse Dr. 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.2. 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 presión que para la baquelita (150°C y 4 000 Ibs. se opacara. o una preforma de baquelita. La resina termofijadora que mas se emplea para montar muestras es la baquelita.2c. Una vez alcanzada esta temperatura. cuando se montan en tal dispositivo de sujeción. aumentada 2x. aumentada 2x Las muestras pequeñas pueden montarse en forma conveniente para prepararlas métalográficamente en un dispositivo de sujeción hecho en el laboratorio. Figura 1. cuando se han hecho en forma adecuada. aumentada 2x.

en ciertos casos. La última aproximación a una superficie plana libre de ralladuras se obtiene mediante una rueda giratoria húmeda cubierta con un paño especial cargado con partículas abrasivas cuidadosamente seleccionadas en su tamaño. Víctor Hugo Baltazar Hernández 2012 6 . Comparado con el papel esmeril.Notas de la materia Metalurgia Física con hojas metálicas "rellenadoras" de metal que tienen aproximadamente la misma dureza que las muestras. desde aquellos que no tienen pelillo (como la seda) hasta aquellos de pelillo intermedio (como paño ancho. se conservara la superficie libre de las irregularidades de la muestra y se evitara. También se pueden encontrar paños sintéticos para pulir con fines de pulido general. luego 400. de los cuales el Gamal y el Micropaño son los que se utilizan más ampliamente. 300.5 Pulido fino El tiempo utilizado y el éxito del pulido fino dependen en mucho del cuidado puesto durante los pasos de pulido previo. como el de preparación de materiales suaves. oxido de cromo y oxido de magnesio. 800.4 Pulido intermedio Después de montada. sin embargo. 1. Existe gran disponibilidad de abrasivos para efectuar el último pulido. que los bordes de la muestra se redondeen durante el pulido [1]. Si se usan hojas rellenadoras.1. parece haber preferencia por la forma gamma del oxido de aluminio para pulir materiales ferrosos y de los basados en cobre. El primer papel es generalmente No. minimiza el daño cuando los metales son blandos y también proporciona una acción de enjuague para limpiar los productos removidos de la superficie de la muestra. Se pueden encontrar paños de lanilla o pelillo variable. 600. 1. el carburo de silicio tiene mayor rapidez de remoción y. Otros abrasivos para pulido final que se emplean a menudo son la pasta de diamante.1. sucesivamente. las operaciones de pulido intermedio con lijas de esmeril se hacen en seco. Por lo general. de modo que el papel no se ensucie [1]. En tanto que muchos harán un trabajo satisfactorio.1. como su acabado es a base de resina. la muestra se pule sobre una serie de hojas de esmeril o lija con abrasivos más finos. La selección de un paño para pulir depende del material que vaya a pulirse y el propósito del estudio metalográfico. paño de billar y lonilla) además de aquellos de pelillo profundo (como el terciopelo). se puede usar un abrasivo de carburo de silicio. el cual impide el sobrecalentamiento de la muestra.1b muestra la superficie después del pulido intermedio con lija de 400. se puede utilizar con un lubricante. de alguna manera. y finalmente 1200.1. La Figura 1. Una muestra pulida en forma adecuada Dr. magnesio y sus aleaciones. y oxido de cerio para pulir aluminio.

Esto se logra mediante un reactivo apropiado que somete a la superficie pulida a una acción química. 1. 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. El proceso debe ser tal que queden claramente diferenciadas las partes de la microestructura.3 a) Fotomicrografía de la diferencia en composición química de las fases.1c) [1]. a) b) c) Figura 1. además.1. el reactivo. B) Fotomicrografía de hierro puro. Esta diferencia en la rapidez de ataque esta asociada principalmente con el ángulo que guardan las diferentes secciones de grano con el plano de la superficie pulida.3b).3a).Notas de la materia Metalurgia Física mostrara únicamente las inclusiones no metálicas. Debido al ataque químico por el Dr. estará libre de ralladuras (Figura 1. En las aleaciones compuestas de dos o más fases. Víctor Hugo Baltazar Hernández 2012 7 .6 Ataque El propósito del ataque químico es hacer visibles las características estructurales del metal o aleación. las componentes se revelan durante la acción química. a una o más de estas constituyentes debido a la diferencia en composición química de las fases (Figura 1.1. c) Ilustración del aspecto microscópico de las fronteras de grano que aparecen como líneas obscuras. al atacar preferencialmente. En las aleaciones uniformes de una sola fase o metales puros.

1 magnification range of roughly ×40 to ×1250. In bright-field illumination. Although actually only a few atomic diameters wide. causing grain boundaries to appear bright. Al chocar con la orilla de estos valles. and (3) a specimen stage (fixed or rotatable). the most important and critical component in the Dr. 1.4a). The main components of a benchtype microscope are (1) an illumination system comprising a light source and variable apertures. their porosity can cause two problems.2. light is reflected back towards the objective from reflective surfaces. Metallic specimens that are to be examined at high magnifications are successively polished with 6. la luz del microscopio se reflejara fuera del microscopio. The objective.2. orientation-related etch pits and the effects of plastic deformation.Notas de la materia Metalurgia Física reactivo de ataque. las fronteras de grano aparecerían como valles en la superficie pulida. Second. it may be necessary to strengthen the structure by impregnating with liquid resin in vacuo. which is generally advisable.1 Microscopía óptica. 1 and sometimes 0.25 μm diamond grit. However. Ver tabla 1. phase morphology.1. provided that pores are interconnected. First. Víctor Hugo Baltazar Hernández 2012 8 . cracks and inclusions of foreign matter. (2) an objective lens and an ocular lens (eyepiece) mounted at the ends of a cylindrical body tube. there is a risk of entrapping diamond particles during polishing. La selección del reactivo de ataque esta determinada por el metal o aleación y la estructura especifica que se desea ver. Examination in the as-polished condition. The degree of chemical attack is sensitive to crystal orientation and an etched polycrystalline aggregate will often display its grain structure clearly (Figura 1.3 en [] en el cual se enumeran algunos de los reactivos de ataque comunes [1]. will reveal structural features such as shrinkage or gas porosity. grain boundaries are preferentially and grossly attacked by many etchants. haciendo que las fronteras de grano aparezcan como líneas oscuras. Interpretation of such images is a matter of skill and experience and needs to allow for the three-dimensional nature of features observed. compositional gradients (coring). electrónica (SEM) y de transmisión (TEM) Microscopía óptica (light microscopy) Basic Principles The light microscope provides two-dimensional representation of structure over a total 1. making ultrasonic cleaning advisable. Esto se muestra en la Figura 1. Preparation techniques for ceramics are essentially similar to those for metals and alloys.2 1. Dark-field illumination reverses this effect. Etching with an appropriate chemical reagent is used to reveal the arrangement and size of grains.3c. causing them to appear bright.

Notas de la materia Metalurgia Física optical train of the light microscope. an f 2mm objective may have a working distance of 0. achromats. and is expressed by the Abbe formula δ=λ/2NA.4 (a) Reflection of light from etched specimen. fluorites (semi-apochromats). is possible and objectives are classified according to the degree of correction. the resolution value for a lens with a so-called high resolving power is small. The unaided eye. (b) Use of oil to improve numerical aperture of objective. can resolve 0. apochromats. is made up of a number of glass lenses and. the depth of field of the objective becomes smaller. Lenses are subject to spherical and chromatic aberrations. greatly aided by modern computational techniques. As magnification is increased. Resolution. Confusingly. sometimes. rather than magnification. so that specimen flatness becomes more critical.e. typically falling from 250μm at ×15 to 0. Lenses are usually coated in order to increase light transmission.15 mm. It is the smallest separating distance (δ) that can be discerned between two lines in the image. at the least distance of comfortable vision (about 250 mm).25. Numerical apertures range in typical value from 0. Resolution is determined by (1) the wavelength (λ) of the radiation and (2) the numerical aperture (NA) of the objective. [2] Figura 1.08μm at ×1200. fluorite (CaF2) lenses also. i. The numerical aperture value. is usually the prime concern of the skilled microscopist. which is engraved upon the side of the objective. The focal length and the working distance (separating its front lens from the specimen) of an objective differ. Despite focusing difficulties and the need for costly lenses. For instance. where n is the refractive index of the medium between the front lens face of the objective and the specimen and α is the semi-apex angle of the light cone defined by the most oblique rays collected by the lens. Víctor Hugo Baltazar Hernández 2012 9 . Minimization and correction of these undesirable physical effects. efforts have been made to use short-wavelength Dr.1 mm.08 to 1. indicates the light-gathering power of the compound lens system and is obtained from the relation NA=n sin α.

The most widely used magnifications for oculars are ×8 and ×12. by replacing air (n=1) with a layer of cedar wood oil (n=1. Objectives are designed for a certain tm value. be used to project a real image. a geometrical progression with a common ratio of approximately 1. it can readily be shown that the resolution limit of the light microscope is of the order of 200 nm. not the magnification [2]. it was 250 mm. oil-immersion objectives are useful [2].. the number of rays of reflected light accepted by the front lens of the objective is increased. It can also correct for certain objective faults and. ×12. using the Abbe formula. microscopists sometimes indicate this difficulty by using the more readily defined term ‘scale of reproduction’. With each change. The former is the fixed distance between the top of the body tube. The ocular magnifies the image formed by the objective: the finally observed image is virtual. for instance. the distance between the specimen and the aerial image is kept constant. This device facilitates the selection of a basic set of lenses that is comprehensive and ‘useful’ (exempt from ‘empty’ magnification).5 [2]. ×16. Magnification is a subjective term. if inferior in quality. ×8. can worsen it. at the top end. it varies with the distance of an image or object from the eye. which is the lineal size ratio of an image (on a viewing screen or photomicrograph) to the original object. the Michel series of ×6. 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. on which the ocular rests. using matched parfocal objectives and oculars. etc. The ocular cannot improve the resolution of the system but. Thus. a statement such as ×500 beneath a photomicrograph gives the scale of reproduction.4b). and the shoulder of the rotatable nosepiece into which several objectives are screwed.3. are of special significance.5. For example. in photomicrography. A value of 160 mm is commonly used.5) or monobromonaphthalene (n=1. the mechanical tube length tm and optical tube length to. (In Victorian times. Two-dimensional features of a standard bench microscope. Víctor Hugo Baltazar Hernández 2012 10 . ×20. Oil-immersion objectives enable the refractive index termto be increased (Figura 1. strictly speaking. consequently.25. and resolution and contrast are improved. The range of wavelengths for visible light is approximately 400–700 nm. ×25. ×10. Hence. enables the specimen to remain in focus when objectives are step-changed by rotating the nosepiece. The ‘useful’ range of magnification is approximately 500–1000NA.66). provides a basis for magnification values for objectives and Dr. to changes but the image produced by the objective always forms in the fixed focal phase of the ocular. The lower end of the range can be tiring to the eyes. Thus.Notas de la materia Metalurgia Física ultraviolet radiation: developments in electron microscopy have undermined the feasibility of this approach. Thus. Some manufacturers base their sequences of objective and ocular magnifications upon preferred numbers1 rather than upon a decimal series.

1967. 1. p.6a. General uses of the technique include the examination of multi-phased alloys after light etching. The bold lines outline a box within which objective/ocular combinations give ‘useful’ magnifications. 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. by courtesy of Carl Zeiss. A schematic diagram of the basic arrangement for phase contrast in the metallurgical microscope is shown in Figura 1. The optimum range of differences in surface level is about 20–50 nm.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. 15.65) gives a ‘useful’ magnification of ×500 [2]. twins and other deformation characteristics. Figura 1. although under favorable conditions these limits may be extended. Thus. strictly.5 Range of ‘useful’ magnification in light microscope (from Optical Systems for the Microscope. the detection of the early stages of precipitation. 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. whereas in ordinary microscopy a phase difference in the light collected by the objective will not contribute to contrast in the final image.2. in phase-contrast microscopy small differences in phases are transformed into differences in brightness which the eye can detect [2]. be Dr. Germany). This rational approach is illustrated in Figura 1. A phase plate of suitable size should.Notas de la materia Metalurgia Física oculars.5. Víctor Hugo Baltazar Hernández 2012 11 . pairing of a ×12.5 ocular with a ×40 objective (NA=0. and the study of cleavage faces. Dashed lines represent oculars and thin solid lines represent objectives.1.

Notas de la materia Metalurgia Física positioned in this plane but. positive phase contrast results and areas of the specimen which are proud of the matrix appear bright and depressions dark. 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. the position Q in front of the eyepiece E is often preferred. Figura 1. Polarized-light microscopy The basic arrangement for the use of polarized light is shown in Figura 1. 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.e. for the ease of interchangeability of phase plates. the plane of polarization of the analyzer is perpendicular to that of the polarizer [2]. Consequently. This phase plate has an annulus. and this in turn depends upon the height of this point relative to the adjacent parts of the surface. Víctor Hugo Baltazar Hernández 2012 12 .6b. negative contrast is produced and ‘pits’ appear bright and ‘hills’ dark [2]. formed either by etching or deposition. the beam is either in phase or approximately λ/2 or π out of phase with that diffracted by the surface features of the specimen. but only if the angle Dr. If the light is not at normal incidence the reflected beam may still be unchanged. i. reinforcement or cancellation occurs. when the phase is retarded. When the light passing through the annulus is advanced in phase. 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. and the image intensity at any point depends on the phase difference produced at the corresponding point on the specimen surface.6 Schematic arrangement of microscope system for phase-contrast (a) and polarized light (b) microscopy. because the light reflected from a surface feature is also advanced or retarded by approximately λ/4.

In refractory materials. the amount of rotation and of elliptical polarization is a property of the metal and of the crystal orientation. developing maximum brilliance at 45◦ to any of the four symmetrical positions of extinction. otherwise it will be elliptically polarized. If correctly prepared. because such a beam cannot be fully extinguished by the analyzer in any position. Near-perfect extinction occurs when the polars of a transmission microscope are crossed. An etch pit will reflect the light at oblique incidence and elliptically polarized light will be produced. tridymite (SiO2) and zircon (ZrSiO4) by their characteristic form and color [2]. Metals which have cubic structure. mineral or rock is introduced and the stage slowly rotated. but information on cleavage faces. these out-of-phase ‘fast’ and ‘slow’ rays combine to produce the Dr. will appear uniformly dark under crossed polars. The technique is therefore very useful for studying the effects of deformation. on the other hand. When the specimen being examined is optically anisotropic. 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. unless etched to invoke artificial anisotropy. the light incident normally is reflected with a rotation of the plane of polarization and as elliptically polarized light. the plane of polarization. particularly the production of preferred orientation. This application is useful in the assessment of the degree of preferred orientation and in recrystallization studies. Víctor Hugo Baltazar Hernández 2012 13 . it will produce a background illumination in the image which tends to mask the grain-contrast effect [2]. If a ‘sensitive tint’ plate is inserted between the vertical illuminator and the analyzer. one of the main uses of polarized light is to distinguish between areas of varying orientation. optically anisotropic crystals will produce polarization colors. chromite (FeCrO4). whereas an elliptically polarized one cannot be fully extinguished by an analyzer in any position.Notas de la materia Metalurgia Física of incidence is in. and thickness. Other uses of polarized light include distinguishing and identifying phases in multi-phase alloys [2]. However. It follows that the unchanged reflected beam will be extinguished by an analyzer in the crossed position. The color of a crystal depends upon its birefringence. On leaving the analyzer. or capacity for double-refraction. or at right angles to. If a thin section or slice of ceramic. Clearly. twin bands and sub-grain boundaries can also be obtained. since these are revealed as differences of intensity under crossed polars. it is possible to identify crystalline species. by producing anisotropic surface films or well-defined pits. each grain of a sample may be identified by a characteristic color which changes as the specimen is rotated on the stage. it is relatively easy to identify periclase (MgO). By standardizing the thickness of the section at 30–50μm and using a Michel–Lévy color chart. each incident ray forms ordinary and extraordinary rays which are polarized in different planes and travel through the crystal at different velocities. As birefringence occurs within the crystal.

Using the X-ray spectroscopy detector of an SEM. prosecutors had the evidence they needed to link Smithart to the crime.000x. microscope from the local high school. Anisotropic crystals are either uniaxial or biaxial. 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.2. In contrast. This color is complementary to color cancelled by interference and follows Newton’s sequence: yellow.Notas de la materia Metalurgia Física polarization color.2. As it turned out. Cubic crystals are isotropic. That's where a scanning electron microscope (SEM) came in. (Optic axes do not necessarily correspond with crystallographic axes. 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]. Why was an SEM. red. 1. necessary to examine the evidence for Smithart's trial? For one thing. green. or optical. as 300. but they had no evidence directly linking him to the murder.) It is therefore possible for quartz (uniaxial) and mica (biaxial) crystals to appear black because of their orientation in the slice. run-of-the-mill Dr. for example. clear Bakelite. Glassy phases are isotropic and also appear black between crossed polars. respectively.000 times the size of the object studied. along which birefringence does not occur. being highly symmetrical. Scientists refer to this number as the magnification power and denote it. rotating the stage and comparing their interference figures: uniaxial crystals give a moving ‘ring and brush’ pattern. violet.2. Prosecutors suspected Smithart after he was spotted at the scene of the crime. rather than a regular light. SEMs can magnify objects at upward of 300. blue. triclinic and monoclinic systems) by introducing a Bertrand lens into the light train of the microscope to give a convergent beam. having one or two optic axes. Víctor Hugo Baltazar Hernández 2012 14 .1 Microscopía Electrónica 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.g. a forensic scientist analyzed bits of iron found at the scene of the crime. higher-order colors are produced as the phase difference between the emergent rays increases. Uniaxial (tetragonal and hexagonal systems) can be distinguished from biaxial crystals (orthorhombic. epoxy resin). He found that they had a globular shape that only welding or grinding produces. Thanks to the tremendous capabilities of scanning electron microscopes. however. More delicate. orange. biaxial crystals give two static ‘eyes’.2 1. glass containing residual stresses from rapid cooling produces fringe patterns and polarization colors. Smithart had a welding rig in his shop and would sometimes repair bicycles for the local children. Alaska.

2. SEMs have their share of drawbacks as well. though recent breakthroughs have made SEMS more accessible in other applications.Notas de la materia Metalurgia Física optical microscopes tend to have a magnification power of a few hundred times. providing an almost 3-D image for researchers to analyze.2 How scanning electron microscope works Figura 1. let's look at where it all began [3]. their use is typically limited to research and industrial applications. In the process. as compared to the flatter image an optical microscope produces. these advanced microscopes can look past the surface of an object. But before we learn about where the technology is headed. They're also bulky and complex instruments.7 How scanning electron microscopes work Dr. In this article. we'll explore what goes into operating one. we'll learn how SEMs are able to produce such detailed and striking images. as well as some of the most recent breakthroughs in SEM technology. like cost. telling researchers information about its composition. SEMs also have tremendous depth of field compared to traditional microscopes.2. As a result. 1. Of course. Víctor Hugo Baltazar Hernández 2012 15 . All of these attributes proved essential in examining evidence from the Smithart case. Lastly. requiring considerable expertise to operate. Even the cheapest among them cost tens of thousands of dollars.

which has a high melting point) to coax electrons away from the gun and toward the specimen under examination. however. These detectors are capable of producing the most detailed images of an object's surface. Thermionic guns. ensuring that the electrons end up precisely where they need to go. they would also be knocked out of the air and onto the specimen. The lenses in these devices. Víctor Hugo Baltazar Hernández 2012 16 . the lenses are made of magnets capable of bending the path of electrons. Instead. they produce the steady stream of electrons necessary for SEMs to operate. Lenses: Just like optical microscopes. Everhart-Thornley detectors register secondary electrons. These electrons don't naturally go where they need to. Detectors: You might think of an SEM's various types of detectors as the eyes of the microscope. SEMs are so sensitive to vibrations that they're often installed on the ground floor of a building. the lenses focus and control the electron beam. Not only would these particles block the path of the electron beam. Electron guns are typically one of two types. which are electrons dislodged from the outer surface of a specimen.Notas de la materia Metalurgia Física We've begun to get an idea of what SEMs are capable of. Sample chamber: The sample chamber of an SEM is where researchers place the specimen that they are examining. which are the most common type. These devices detect the various ways that the electron beam interacts with the sample object. Other detectors. While the variations from one model to the next are seemingly endless. Without a vacuum. In fact. They also manipulate the specimen. 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. can tell researchers about the composition of a substance. Because the specimen must be kept extremely still for the microscope to produce clear images. Instead. all SEMs share the same basic parts. on the other hand. work differently. placing it at different angles and moving it so that researchers don't have to constantly remount the object to take different images. Vacuum chamber: SEMs require a vacuum to operate. Field emission guns. Now we're ready to take a look at the various components of one and how they work together to form an image. they aren't made of glass. which would distort the surface of the specimen. the sample chamber must be very sturdy and insulated from vibration. however. which gets us to the next component of SEMs. create a strong electrical field to pull electrons away from the atoms they're associated with. SEMs use lenses to produce clear and detailed images. The sample chambers of an SEM do more than keep a specimen still. By doing so. Dr. the electron beam generated by the electron gun would encounter constant interference from air particles in the atmosphere. apply thermal energy to a filament (usually made of tungsten. For instance. Electron gun: Electron guns aren't some futuristic weapon used in the newest Vin Diesel movie. For one thing. such as backscattered electron detectors and X-ray detectors.

the trajectory of the incident electron is only slightly perturbed. Víctor Hugo Baltazar Hernández 2012 17 . Most of the energy of an electron beam will eventually end up heating the sample (phonon excitation of the atomic lattice). 1. The incident electrons interact with specimen atoms and are significantly scattered by them (rather than penetrating the sample in a linear fashion). This process is known as electron backscattering (although later we will confine the term "backscattered electrons" to those scatter out of the sample). very tiny things [4].Notas de la materia Metalurgia Física As with many things. Read on to see how all of these components work together to create astounding images of very. but its kinetic energy and velocity remain essentially constant (due to large differences between the mass of the electron and nucleus). the electron trajectory changes. they undergo two types of scattering: elastic and inelastic. In elastic scattering.2. but energy is lost through interactions with the orbital electrons of the atoms in the specimen.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 Effects produced by electron bombardment of a material.8). Figura 1. In inelastic scattering. before the electrons come to rest. Inelastic interactions produce diverse effect including: phonon excitation (heating) cathodoluminescence (visible light fluorescence) continuum radiation (bremsstrahlung or “braking” radiation) Dr. an SEM is more than the sum of its parts. however.

once produced. they have very low energies and can only escape from a thin layer near the sample's surface. 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. however the Dr.2. Second. First. For example. some effects are not produced from certain parts of the interaction volume (Figura 1. can be observed is controlled by how strongly it is diminished by absorption and scattering in the sample. will escape more readily from the upper portions of the interaction volume.9 Generalized illustration of interaction volumes for various electron-specimen interactions.4 SEM imaging Secondary Electrons Figure 1. Auger electrons (not shown) emerge from a very thin region of the sample surface (maximum depth about 50 Å) than do secondary electrons (50-500 Å). the degree to which an effect. Absorption is an important phenomenon and is discussed in more detail below. although secondary and Auger electrons are produced throughout the interaction volume. Figura 1. soft X-rays. Similarly. Some features can be identified from this SE signal based on the surface topography (due to prior etching).9).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 µm.10). Víctor Hugo Baltazar Hernández 2012 18 .Notas de la materia Metalurgia Física 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. it will not be possible to produce it from deeper portions of the volume.2. These features have been labelled as “a” and “b” that possibly correspond to different phases (Figure 1. 1. which are absorbed more easily than hard X-rays.

Moreover. then the interaction volume (given by x and y) increases according to the relations given by equations 1 and 2 [5]. 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.Notas de la materia Metalurgia Física information obtained from this SE signal is merely qualitatively and cannot provide further information other than imaging. Of course. Electron penetration generally ranges from 1-5 µm with the beam incident perpendicular to the sample.077 Eo ρ Equation 2 Where E o is the accelerating voltage (keV) and ρ is the material’s density. Dr. Thus for phases having high density the interaction volume is lower.5 0. Víctor Hugo Baltazar Hernández 2012 19 . 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. As the accelerating voltage increases.5 0. 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 Ǻ) into the surface.1Eo ρ Equation 1 y ( µm) = 1. the magnitude of its current and the average atomic number.3125 µm and y = 2. 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 material’s density. only basic information of the topography is to be collected from this type of signal. x( µm) = 1. For example. the interaction volume for SE signal has to be extracted from the total volume of interaction.55 µm The depth of electron penetration of an electron beam is also a function of its angle of incidence.

Therefore. Víctor Hugo Baltazar Hernández 2012 20 . grey and white colored. but does not change much Dr.10 Secondary electrons (SE) image sampling Backscattered Electrons Figura 1.Notas de la materia Metalurgia Física Figure 1. The identified phases were labeled as “a”.11 shows a SEM micrograph obtained by means of backscattered electrons (BS) signal. Many incident electrons undergo a series of such elastic event that cause them to scattered back out the specimen. Black areas (indicated by the arrows) correspond apparently to gaps within the material possibly due to the etching. Backscattered electrons are produced by elastic interactions of beam electrons with nuclei of atoms in the specimen. “b” and “c” as indicated in Figura 1.11. this metal resulted in three distinct phases as identified by the difference on image contrast. in this work EDS analysis was not conducted in those areas. The fraction of the beam electrons backscattered in this way varies strongly with the atomic number Z of the scattering atoms. Careful observations on this image clearly revealed three distinct regions (well contrasted) identified as: dark.

3x10 −7 Z 3 Equation 4 For homogeneous mixtures η mix is calculated from the weight fractions of elemental components by: η mix = ∑ Ciη i i In summary. Grey and lighter regions correspond to higher Z numbers. The backscattered coefficient.016Z − 1.11 Backscattered electrons (BS) image sampling 1. the backscattered coefficient.Notas de la materia Metalurgia Física with changes in E o .0254 + 0.2. the number of BSE increases. depend on Z. is given by equation 3 [6]: η= η bs η pe Equation 3 where η pe is the number of incident electrons and η bs is the number of backscattered electrons. Basically as all phases (elements) have different size nuclei. Figura 1. dark phase correspond to the lowest atomic number (Z) phase in this alloy. as the size of the atom nuclei increases. which is the number of produced backscattered electrons. For a pure element.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.2. Víctor Hugo Baltazar Hernández 2012 21 . The resulting excitation volume is a hemispherical to jug-shaped region with the neck of jug at the Dr. can be calculated by: η = −0.86 x10 −4 Z 2 + 8.

and the average atomic number (Z) of the sample. 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 µm (see Figure 2. 337): Dr. The depth of electron penetration is approximately (Potts.5 g/cm3. about the minimum density for silicate minerals. 1987. with E o = 15 keV. 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. Of these. Víctor Hugo Baltazar Hernández 2012 22 . the accelerating voltage. accelerating voltage and density play the largest roles in determining the depth of electron interaction (Figura 1.3 µm. 336): For example. p. bombarding a material with a density of 2. the magnitude of its current. 1987. 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 width of the excited volume can be approximated by (Potts.12). Figura 1. p.Notas de la materia Metalurgia Física specimen surface. gives x = 2.12 Schematic depiction of the variation of interaction volume shape with average sample atomic number (Z) and electron beam accelerating voltage (E o ).1b). Electron penetration generally ranges from 1-5 µm with the beam incident perpendicular to the sample.

the likelihood of incident electrons interacting with the sample and scattering and the angle of deflection are determined probabilistically.2b. In such models. for a given E o is (Kanaya & Okayama. 1972): The volume of interaction can be modeled by Monte Carlo simulation. A theoretical expression for the "range" of an electron. Víctor Hugo Baltazar Hernández 2012 23 . Dr. X-ray generation depths depend strongly on density and accelerating voltage (Figure 2. the straight line distance between where an electron enters and its final resting place.). 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]. The results derived from Monte Carlo modeling yield a volume of interaction that is very similar to that determined by etching experiments.Notas de la materia Metalurgia Física Both of these are empirical expressions.

A TEM equipment is shown in Figura 1. copper.2. Consequently.000-400. Since most defect characterization requires an understanding of diffraction contrast. we use beam energies in the range from 100. simulated in a Monte Carlo procedure. Víctor Hugo Baltazar Hernández 2012 24 .13 Comparison of electron paths (top) and sites of X-ray excitation (bottom) in targets of aluminum.3 1.000 eV.1 Microscopía Electrónica de Transmisión (Transmission Electron Microscopy) Introduction A typical commercial transmission electron microscope (TEM) costs about $2 for each electron volt of energy in the beam. As you'll see. 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.2.14 A transmission electron microscope Philips CM-12 Dr.Notas de la materia Metalurgia Física Figura 1. this is an important constituent of this chapter. and gold at 20 keV. and if you add on all the options. 1. Figura 1. it can cost about $4-5 per eV.14. so a TEM becomes an extremely expensive piece of equipment.3. 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. there have to be very sound scientific reasons for investing such a large amount of money in one microscope [8].

3. Dr. Furthermore. These apertures cut down the intensity of the electron beam. Figura 1. Like the resolution. narrowing the beam down to a thin "pencil" of electrons which at most is a few micrometers across. The best electron lens is not a very good one. 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. To minimize this problem we have to use very small limiting apertures in the lenses. as long as it's electron transparent! Figura 1. 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. but also act to increase the depth of focus of the images that we produce. as we've already mentioned.2. It turns out that in the TEM.Notas de la materia Metalurgia Física 1. all of the specimen is usually in focus at the same time. independent of the specimen topography. A band of dislocations threads through the thin specimen from the top to the bottom but remains in focus through the foil thickness.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.15 shows a TEM image of some dislocations in a crystal. and has been compared to using the bottom of a Coca-Cola bottle as a lens for light microscopy. we can record the final image at different positions below the final lens of the instrument and it will still be in focus. Víctor Hugo Baltazar Hernández 2012 25 . this property is governed by the lenses in the microscope. it is also critical in the TEM. and they remain in sharp focus at all times.15 TEM image of dislocations in GaAs (Gallium arsenide).

Dr. and specimen shape. in this case shown in the inset. including such esoteric aspects as pointgroup and space-group determination.Notas de la materia Metalurgia Física 1. We hope they will become evident as you read through this book.2. There are many other good reasons why you should use electron microscopes. At the same time there are many reasons why you should not always seek to solve your problems with the TEM. you can conduct a complete crystallographic symmetry analysis of minuscule crystals. and you can always produce images that are in focus. electron diffraction is an indispensable part of TEM and is arguably the most useful aspect of TEM for materials scientists. as well as being a most striking pattern. can generate a variety of signals telling you about your sample chemistry and crystallography. Figura 1. Víctor Hugo Baltazar Hernández 2012 26 . and the possibility of combining electron diffraction into TEMs was realized by Kossel and Móllenstedt (1939). and it is most important that you realize what the instrument cannot do. You will also see in Part II that. lattice repeat distance.3. as well as knowing its capabilities [8].3 Diffraction Thompson and Reid showed that electrons could be diffracted when passing through thin crystals of nickel.16 shows a TEM diffraction pattern which contains information on the crystal structure. So an electron microscope can produce atomic level images. in addition to the things we just listed. We'll see that the pattern can always be related to the image of the area of the specimen from which it came. There is no similar capability on a light microscope because of the relatively large wavelength of visible light. Today. and at all times the crystallography can be related to the image of your specimen.

shown in the inset image. Figure 1. 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. Dr. Our eyes and brain routinely understand reflected light images but are ill-equipped to interpret TEM images. Víctor Hugo Baltazar Hernández 2012 27 .2.Notas de la materia Metalurgia Física Figura 1. which abound in TEM images.16 TEM diffraction pattern from a thin foil of Al-Li-Cu containing various precipitate phases. 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. in projection. 1. and so we must be cautious. Hayes (1980) illustrates this problem well by showing a picture of two rhinos. we publish!" So beware of artifacts.3.17 Photograph of two rhinos taken so that. viewed in transmission. side by side such that the head of one appears attached to the rear of the other (see Figure 1. they appear as one two-headed beast. 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.17).4 Interpreting TEM images Another problem is that the TEM presents us with 2D images of 3D specimens.

specimens of aluminum alloys almost up to 1 pm would be thin. Víctor Hugo Baltazar Hernández 2012 28 ." 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. 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. such as your eyes. know the forest before you start looking at the leaves on the trees. as is apparent. Typically for 100-keV electrons. Otherwise you may fall foul of some of the limitations we have just listed [8]. the worse the sampling abilities of the instrument. diffraction patterns. and the scanning electron microscope. 1. but this is offset by the danger of beam damage. they should never be used in isolation to solve a materials problem. and specimens below 100 nm should be used wherever possible. Your specimens have to be thin if you're going to get any information using transmitted electrons in the TEM. spectra) is averaged through the thickness of the specimen. specimen thicknesses <50 nm are essential. all the TEM information that we talk about in this book (images. but in this context it means "electron transparent. and in extreme cases. In other words. "Thin" is a relative term. However.3. The higher the resolution. First of all. it is an axiom in TEM that thinner is better. therefore. a single TEM image has no depth sensitivity. generally. In other words. the visible-light microscope. Generally this requirement is a function of the electron energy and the average atomic number of the specimen. These demands become less strict as the beam voltage increases. 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. So it should be obvious to you by now that while TEM and associated techniques are tremendously powerful characterization tools when used properly. 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.Notas de la materia Metalurgia Física One aspect of this particular drawback is that.5 Specimen Preparation All the above advantages of the TEM bring accompanying drawbacks. Dr. while steel would be thin up to about several hundred nm. such as when doing HRTEM or electron spectrometry.2.

5 to 2.3. ν – frequency The variation of E is not sinusoidal but it matters little. Figure 1.6000 Ǻ X-rays are associated with and electric field E in the “y” direction and a magnetic field H in the “z” direction. these rays are invisible and travel in straight lines and more penetrating than visible light.1 Análisis de XRD (X-Ray Diffraction) Electromagnetic radiation Discovered in 1885. Wavelengths: X-rays – 0.19 shows the variation of E graphically Dr. What are x-rays? X-rays are electromagnetic radiation which is exactly the same nature of visible light but of very much shorter wavelength. Figura 1.L. the important issue is its periodicity.) .3 1. visible light (V.5 Ǻ.Notas de la materia Metalurgia Física 1.18 Electric and magnetic fields associated with a wave moving in the x-direction A – amplitude. Víctor Hugo Baltazar Hernández 2012 29 .

(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.19 The variation of E. Most x-rays intensity measurements are made by counting the number of photons incident on a detector. Each photon is associated with it an amount of energy of hν where h is Planks constant (6.2 Production of X-Rays How are x-rays produced? Dr.63x10-34 joule*sec) Radiation has thus a dual wave-particle character.Notas de la materia Metalurgia Física Figura 1. Víctor Hugo Baltazar Hernández 2012 30 . Quantum theory: electromagnetic radiation is considered can also been considered as a stream of particles called quanta or photons. 1. In absolute units intensity is measured in joules/m2/sec but this measurement is difficult one. The average value of the intensity is proportional to the square of the amplitude on the wave. Classical theory: electromagnetic radiation has been considered wave motion.3.

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. according to the way in which electrons are provided: gas tubes (obsolete).Notas de la materia Metalurgia Física X-rays are produced when an electrical charged particle (electron) of sufficient kinetic energy decelerates.6x10-19 coulombs) and V is the voltage across the electrodes.21 shows its internal construction. since most of the kinetic energy of the electrons is converted into heat in the target. at ground potential. Filament tubes were invented by Coolidge in 1913. Dr. 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. X-ray tubes may be divided into two basic types. an anode (the metal target) maintained.000V).20 is a photograph of such a tube. and filament tubes. and a cathode. and Figure 1. Furthermore.000 volts for diffraction work. Since x-rays are produced whenever high-speed electrons collide with a metal target. in which the source of electrons is a hot filament.e. 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. maintained at a high negative potential. the latter is almost alwavs watercooled to prevent its melting. The kinetic energy of electrons on impact is given by where e is the charge on the electron (1. in which electrons are produced by the ionization of a small quantity of gas (residual air in a partly evacuated tube). Figure 1. m (9.11x10-31 kg) is the mass of the electron and υ2 is the velocity in m/sec just before impact.000 to 50. They consist of an evacuated glass envelope which insulates the anode at one end from the cathode at the other. A1l x-ray tubes contain two electrodes.30. and (c) a metal target. Víctor Hugo Baltazar Hernández 2012 31 . with few exceptions. normally of the order of 30. (b) a high accelerating voltage. Any x-ray tube must contain (a) a source of electrons.

3. Assume that a beam of perfectly parallel. C. perfectly monochromatic x-rays of wavelength λ is incident on this crystal at an angle θ. where θ is measured between the incident beam and the particular crystal planes under consideration. . normal to the plane of the drawing and spaced a distance d' apart. .3 X-Ray Diffraction Differences in the path length of various rays arise quite naturally when considering how a crystal diffracts x-rays. D.. called the Bragg angle.21 Cross section of sealed x-ray tube (schematic) 1.22 shows a section of a crystal. its atoms arranged on a set of parallel planes A. Víctor Hugo Baltazar Hernández 2012 32 .20 Sealed x-ray tube. Dr. B.Notas de la materia Metalurgia Física Figure 1. Figure 1.. Figura 1.

second.22. essentially a scattering phenomenon. for one plane of atoms and.22 Diffraction of x-rays by a crystal. Rays 1 and 2. Whether this incident beam of x-rays will be diffracted by the crystal and. This will be true of al1 the planes separately. under what conditions. Only in the directions 1 and 1a. they do so because the difference in their length of path between the wave fronts XX' and YY' is equal to: Similarly. if so. Consider rays 1 and la in the incident beam. are these scattered beams completely in phase and so capable of reinforcing one another. for example. the only diffracted beam formed is that shown. for all the atoms making up the crystal. Víctor Hugo Baltazar Hernández 2012 33 . and the path difference for rays 1K1' and 2L2' is: Dr. For the particular conditions described by Figura 1. Diffraction is. therefore. and it remains to find the condition for reinforcement of rays scattered by atoms in different planes. A diffracted beam may be defined as a beam composed of a large number of scattered rays mutually reinforcing one another. 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. first. namely one making an exit angle θ with respect to the diffraction planes equal to the angle θ of incidence. are scattered by atoms K and L. 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 shown. however. they strike atoms K and P in the first plane of atoms and are scattered in all directions. are the questions central to this chapter.Notas de la materia Metalurgia Física Figura 1.

namely. The diffracted beam is rather strong compared to the sum of all the rays scattered in the same direction. or if: This relation was first formulated by W. properly. An instrument for measuring x-ray spectra by means of a crystal of known structure. The second instrument is aptly called a diffractometer: this name serves well to emphasize the particular use to which the instrument is being put. An example of a diffractometer is shown in Figure 1. diffraction analysis rather than spectrometry.4 Diffractometers Depending solely on the way it is used. 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. n is called the order of diffraction.Notas de la materia Metalurgia Física This is also the path difference for the overlapping rays scattered by S and P in the direction shown.3. since in this direction there is no path difference between rays scattered by S and L or P and K. 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. It states the essential condition which must be met if diffraction is to occur. the basic x-ray diffractometer/spectrometer is really two instruments: 1. it may take on any integral value consistent with sinθ not exceeding unity and is equal to the number of wavelengths in the path difference between rays scattered by adjacent planes. The term spectrometer was originally used to describe both instruments.23. An instrument for studying crystalline (and noncrystalline) materials by measurements of the way in which they diffract (scatter) x-rays of known wavelength. Bragg and is known as Bragg's law. Scattered rays 1' and 2' will be completely in phase if this path difference is equal to a whole number n of wavelengths. it should be applied only to the first. simply because of the reinforcement which occurs. 2. Víctor Hugo Baltazar Hernández 2012 34 . L. In all other directions of space the scattered beams are out of phase and annul one another (destructive interference). Dr. but.

23 Diffractometer 1.1 traslapes.4. etc. rechupes. laminaciones. grietas.4.Notas de la materia Metalurgia Física Figure 1. costuras. 1.4 1. defectos superficiales como: poros.3. Víctor Hugo Baltazar Hernández 2012 35 .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 1.1 Ensayos o pruebas no destructivas (non-destructive testing) Líquidos Penetrantes Introducción a los Líquidos Penetrantes Discontinuidades que detecta.1. Materiales: Sólidos metálicos y no metálicos Dr.

4.1. DESVENTAJAS Solo detecta fallas superficiales Difícil establecimiento de patrones La superficie a inspeccionar debe estar limpia y sin recubrimientos No se puede inspeccionar materiales demasiado porosos PRINCIPIOS FÍSICOS Capilaridad: Es la acción que origina que un liquido ascienda o descienda a través de los llamados tubos capilares. Resistencia a la evaporación. El penetrante ideal debe reunir lo siguiente: Habilidad para penetrar orificios y aberturas muy pequeñas y estrechas. Tensión superficial: Es la fuerza no compensada que ejerce la superficie del líquido debido a la tensión no compensada de las moléculas subsuperficiales sobre la membrana superior. Habilidad de extenderse en capas muy finas.2 Características de los líquidos penetrantes El líquido penetrante tiene la propiedad de penetrar en cualquier abertura u orificio en la superficie del material. Dr. Viscosidad: Es la resistencia al deslizamiento de una capa de un fluido sobre otra capa. 1. Cohesión: Es la fuerza que mantiene a las moléculas de un cuerpo a distancias cercanas unas de las otras. Habilidad de mantener color o la fluorescencia. De fácil remoción de la superficie. Habilidad de permanecer en aberturas amplias. Adherencia: Es la fuerza de atracción entre moléculas de sustancias diferentes.Notas de la materia Metalurgia Física VENTAJAS Muy económico Inspección a simple vista No se destruye la pieza Se obtiene resultados inmediatos. Víctor Hugo Baltazar Hernández 2012 36 .

en tanto que los de baja viscosidades escurren muy rápido y tiene la tendencia a no ser retenidos en los defectos de poca profundidad. por lo tanto se recomienda una viscosidad media. el cual debe ser lo mas bajo posible. Propiedad física Capilarida d Tensión superficial Adherenci a Cohesión Viscosidad Partículas Penetrante Revelador Alta Baja Baja Alta Baja Alta Baja Baja Pequeñas Alta Alta Grandes Tensión superficial: Es una de las propiedades más importantes. Víctor Hugo Baltazar Hernández 2012 37 . Inoloro. Antiinflamable. Estable bajo condiciones de almacenamiento. Costo razonable. No corrosivo. Esto se refiere al ángulo de contacto del líquido con la superficie.Notas de la materia Metalurgia Física De difícil eliminación una vez dentro de la discontinuidad. Los penetrantes de alta viscosidad penetran lentamente. Dr. Viscosidad: Esta propiedad no produce efecto alguno en la habilidad del líquido para penetrar. De fácil absorción de la discontinuidad. aunque afecta la velocidad de penetración. Se requiere una tensión superficial baja para obtener buenas propiedades de penetración y mojado Poder humectante: El penetrador debe ser capaz de mojar completamente la superficie del material y es una de las propiedades más importantes. Atoxico.

Gravedad especifica o densidad relativa: No juega un papel directo sobre el comportamiento de un penetrante dado. 1. Inactividad química: Los productos usados en la formulación de los líquidos penetrantes deben se inertes y no corrosivos con respecto a los materiales a ser ensayados y a los recipientes que los contienen. 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. sin embargo. aplicado por rocío Revelador húmedo: Es una suspensión absorbente de polvo en agua. 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.1.86 y 1. Si existe una evaporación excesiva se los productos del penetrante. Víctor Hugo Baltazar Hernández 2012 38 . con densidades bajas se facilita el transporte de materiales extraños que tenderán a sedimentar en el fondo cuando se usan tanques abiertos. Portátil ( atomizador ) Estacionario ( inmersión ) Dr. después de lo cual el exceso del líquido es removido. se aplica por inmersión. Revelador no acuoso: Es una suspensión absorbente.Notas de la materia Metalurgia Física Volatilidad: Los líquidos penetrantes no deben ser volátiles. se verá afectada la sensibilidad de todo el proceso. como a la perdida del poder humectante. debido tanto al desequilibrio de la formula. rociado o sumergido.4. tal que puedan ser vistas ya sea directamente o por medio de una lámpara o luz negra. permitiendo que penetre en las aberturas del material. Generalmente el punto de inflamación es mayor de 95 °C y en recipientes abiertos no debe ser menor de 65 °C.3 Método de aplicación de los líquidos penetrantes en Pruebas No Destructivas Se aplica el líquido penetrante a la superficie de la pieza a ser examinada.06 a 16°C. Punto de inflamación: Como medida de seguridad practica los líquidos penetrantes deberán poseer un punto de inflamación elevado con el fin de reducir los peligros de incendio. Capacidad de disolución: El penetrante debe tener una elevada capacidad para contener grandes concentraciones de pigmentos coloreados o fluorescentes usados y mantenerlos en solución. por lo general la densidad es menor a 1. La mayoría de los líquidos penetrantes tienen densidades relativas que varían entre 0.

Se pueden usar todos aquellos procesos que dejen a la superficie limpia y seca. Soluciones detergentes en caliente por inmersión. etc. grasa y otros contaminantes. principalmente en superficies rectificadas se hace un ataque ácido a fondo que abre las grietas durante la operación. Los penetrantes se aplican por inmersión. están prohibidos por la posibilidad que tiene su aplicación de tapar defectos existentes. desengrase en fase de vapor o desengrase mediante disolvente. aceites. vertiendo el liquido sobre la pieza o cualquier otro método. ya que los mecánicos. aceite. Será necesario obtener una película fina uniforme en toda la superficie y se deberá esperar un tiempo llamado tiempo de penetración para que el liquido penetre en grietas. Será necesario eliminar los restos de óxidos. Se debe retirar la capa superficial del penetrante de forma que lo único 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. carbonillas. Las pinturas se eliminan con productos cáusticos en caliente o basados en ellos. ELIMINACIÓN DEL EXCESO DE PENETRANTE. APLICACIÓN DEL PENETRANTE. son los principales métodos para eliminar grasas y aceites. vertiendo el liquido sobre la pieza o cualquier otro método que cubra la zona que se inspecciona. Dr. Este tiempo oscila entre los 5 y 15 minutos dependiendo del material y la clase de grietas. grasas. que no dañen al espécimen y que no empleen productos que sean incompatibles con los componentes. pinturas.Notas de la materia Metalurgia Física Simple vista Spoteheck (portátil) Luz negra Syglo (estacionario) Portátil Liquido penetrante Removedor Revelador Incoloro Blanco Rojo Estacionario Verde (fluorescente) Incoloro Blanco PREPARACIÓN Y LIMPIEZA DE LA PIEZA: Limpiar cuidadosamente la superficie a inspeccionar de pintura. Y esto se hace por métodos químicos. rociado con un cepillo o brocha. Los óxidos y las carbonillas térmicas se eliminaran con desoxidantes alcalinos o ácidos y a veces. Víctor Hugo Baltazar Hernández 2012 39 . taladrillas.

Notas de la materia Metalurgia Física Esta etapa es critica y de su correcta realización dependerá el resultado final de la inspección. Para saber si hemos eliminado bien el exceso de penetrante es necesario hacer una inspección visual. Una vez aplicado el revelador. estas indicaciones no pueden referirse a ningún tipo de discontinuidad. este tiempo oscila entre 5 y 15 minutos. El tiempo de revelado depende del tipo de penetración. Una regla práctica es que el tiempo de revelado nunca debe ser menor a siete minutos. El revelado es la operación que hace visible al ojo humano la posición del defecto. Son el resultado de alguna forma de contaminación con penetrantes. Si no se ha eliminado perfectamente el liquido penetrante. inertes y con una granulometría tal que dispone de un gran poder de absorción. en la inspección final aparecerán manchas de penetrante produciendo indicaciones falsas e incluso. hay que esperar un tiempo para que absorba el penetrante. Es aconsejable quitar en primer lugar la mayor parte del penetrante con trapos o papel absorbente y después eliminar el resto utilizando trapos o papel ligeramente impregnados en disolvente. Durante la preparación de las piezas para la inspección es necesario secarlas después de la aplicación del revelador húmedo o eliminar el remanente antes del uso del polvo revelador seco. Interpretación. Aplicar el revelador y dejarlo actuar. el enmascaramiento de las grietas. Víctor Hugo Baltazar Hernández 2012 40 . APLICACIÓN DEL REVELADOR. Una vez transcurrido el tiempo de revelado. INSPECCIÓN FINAL DE LA PIEZA. Indicaciones relevantes. ya que es necesario eliminar y limpiar el exceso de penetrante de tal modo que no extraigamos el penetrante introducido en los defectos. se procede a la inspección de los posibles defectos de las piezas procesadas. Indicaciones falsas. Inspección. El proceso de inspección se compone de tres etapas. Dr. Son las causadas por discontinuidades que están generalmente presentes en el diseño. La inspección se realiza antes de que el penetrante comience a exudar sobre el revelador hasta el punto de ocasionar la perdida de definición. del revelador y del defecto. pero deberá permitirse tiempo suficiente para que se formen las indicaciones. El revelador es básicamente un producto en polvo de compuestos químicos blancos.

Notas de la materia Metalurgia Física LIMPIEZA FINAL. Víctor Hugo Baltazar Hernández 2012 41 . Tiempo de Penetración Material Proceso Tipo de discontinuidad Fundición Extrusión y forja Aluminio Soldadura Todos Todos Porosidades Traslapes Falta de fusión Porosidades Grietas Grietas de fatiga Fundición Extrusión y forja Magnesio Soldadura Todos Porosidades Traslapes Falta de fusión Porosidades Grietas Grietas de fatiga Fundición Extrusión y forja Acero Soldadura Todos Todos Porosidades Traslapes Falta de fusión Porosidades Grietas Grietas de fatiga Fundición Latón y bronce Extrusión y forja Recubrimientos Porosidades Traslapes Falta de fusión 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 Dr. Se debe llevar a cabo en razón de los productos usados en el ensayo.

Dr.Notas de la materia Metalurgia Física 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 Plásticos Vidrio Herramienta con punta de carburo Todos Todos Grietas Grietas Falta de fusión Porosidades Grietas Titanio y aleacionesa altas temperaturas Todos metales Todos Todos Esfuerzos o Granulación Interna NR 240 240 NR = no recomendable Guía de Selección del proceso PROBLEMA PROCESO OBSERVACIONES TIPO I Y II Alta producción de artículos pequeños Alta producción de artículos grandes Alta sensibilidad para discontinuidades finas Discontinuidades superficiales. etc. rayones. extrusiones. A El penetrante podría fijarse en las esquinas. etc. A Artículos con cuerdas y cuñeros. B Indicaciones mas claras y mas brillantes B Puede controlarse la profundidad de emulsificación. Deben detectarse Artículos con rugosidad superficial A Pequeñas cantidades mojadas en canastas B Grandes forjas. Víctor Hugo Baltazar Hernández 2012 42 .

DESVENTAJAS Requiere luz negra y áreas obscuras. Víctor Hugo Baltazar Hernández 2012 43 . No es seguro en superficies anodizadas. Se necesita equipo portátil. Detección de fugas A–B CARACTERÍSTICAS DEL PENETRANTE FLUORESENTE TIPO VENTAJAS La fluorescencia asegura visibilidad Fácilmente lavable con agua. Dr. Ácidos y cromatos afectan la sensibilidad. Fácilmente sobre lavado. No se dispone de agua y electricidad C C C Artículos anodizados. Grandes cantidades de especimenes pequeños. La fluorescencia asegura visibilidad. agrietados C – B – A después del anodizado Repetir el proceso C De preferencia el orden indicado Cinco a seis repeticiones podrían ser el limite. LAVADO CON AGUA Cuñeros y cuerdas. El penetrante esta expuesto a la contaminación del agua. Proceso sencillo. No es seguro en la detección de rayones y fallas superficiales. Prueba por puntos.Notas de la materia Metalurgia Física Artículos con rugosidad superficial media A–B La elección depende de los requerimientos de producción y sensibilidad. Requiere luz negra y áreas obscuras. No es seguro volver a probar. Rápido. Superficies rugosas. Amplio rango de discontinuidades.

Notas de la materia Metalurgia Física Alta sensibilidad para POST discontinuidades muy finas. Víctor Hugo Baltazar Hernández 2012 44 . abiertos. Fácilmente lavable con agua después de la emulsificación. 1.5 Ensayos mecánicos Se propone asignar los siguientes porcentajes a los diferentes rubros para la Dr. agujeros ciegos y superficies rugosas EMULSIFICADO Bueno para discontinuidades superficiales. Requiere mas paso. cuñeros. Requiere equipo para la aplicación de emulsivo. No puede usarse en tanques Bueno sobre piezas anodizadas. Requiere luz negra y áreas obscuras. Las piezas pueden ser re probadas Difícil su empleo sobre superficies rugosas tales como fundición de magnesio. Para verificación por puntos. Difícil remoción del penetrante en cuerdas. Tiempo de penetración corto. No puede ser fácilmente sobre lavado La fluorescencia asegura visibilidad REMOVIDO CON SOLVENTE Portátil. Material inflamable. No requiere agua.

Prentice Hall. [3] http://science.. Barry Carter. Víctor Hugo Baltazar Hernández 2012 45 .html [6] http://www.R.htm [5] http://www4. Williams.howstuffworks.htm [7] http://www4. A. S. Ngan. Springer Science+Business Media Inc.Notas de la materia Metalurgia Física 1. Stock. Physical Metallurgy and Advanced Materials. Elements of X-Ray Diffraction.html [8] David B.com/scanning-electron-microscope.com/scanning-electron-microscope2. Cullity.ac.H.edu/microanalysis/Microprobe/Interact-Volume. Butterworth-Heinemann (2007).uk/durability/research%20techniques%20sem. Ed. 2001 Dr. Third Edition.howstuffworks. Smallman. Transmission Electron Microscopy – Basics I. C.. 1996 [9] B. Sydney H.nau.6 Referencias [1] Avner. [2] R.W. E.cv.D.edu/microanalysis/microprobe/interact-volume. (1988). Introducción a la Metalurgia Física.nau.concrete.ic.htm [4] http://science. seventh edition. McGraw Hill.

Sign up to vote on this title
UsefulNot useful