UNIVERSIDAD NACIONAL DE SAN AGUSTN DE AREQUIPA FACULTAD DE INGENIERA DE PROCESOS ESCUELA PROFESIONAL DE INGENIERA METALRGICA

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Cap. 2 2.1. 2.2. 2.3. 2.4. 2.5. 2.6. 2.7. 2.8.

Tcnicas de Preparacin de Muestras Introduccin Objetivos y Parmetros de Preparacin de Muestras Extraccin de Muestras Seccionamiento de Muestras Montaje de Muestras Desbaste y Pulido Mecnico Pulido Qumico y Electroltico Tcnicas de contraste y Ataque
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Etapas de preparacin: muestreo, seccionamiento, y preparacin de la superficie Criterios de preparacin de una muestra Preparacin Sistemtica: reglas para muestras similares Reproducibilidad del mtodo de preparacin y el control de los parmetros (rpp, fuerza, aditivos, tiempo) Estructura real: caractersticas de la superficie preparada Resultados aceptables de la preparacin
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 Remover la deformacin inducida por el seccionamiento, desbaste y pulido. Eliminar las rayas del desbaste inicial. Evitar la formacin de huecos, erosin, agrietamiento de partculas duras, manchas y otros defectos de preparacin. Minimizar el relieve La superficie debe ser plana, particularmente en los bordes. Se deber mantener planas las superficies revestidas
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 Para revelar la estructura real de la muestra se deber

Eliminar la deformacin inducida por corte, esmerilado y pulido o debe ser poca profunda para que sea eliminada por el reactivo de ataque (rayas, extracciones, picaduras, grietas, manchas, relieves, etc.) limpiar las muestras entre las etapas de preparacin, despus de la preparacin y despus del ataque. El atacante seleccionado debe ser o general o selectivo en su accin para producir fases o lmites de grano limpios, precisos y un contraste alto.
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 La preparacin de muestras materialogrficas requiere de cinco operaciones: corte, montaje (opcional), esmerilado, pulido y Ataque (opcional)
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 Superficie del disco o paos

Usar el recomendado por el mtodo a aplicarse

Abrasivo
debe tener una dureza de 2.5 a 3 veces la dureza del material a ser preparado

Tamao de grano del abrasivo

al inicio ms pequeo y entre etapas, el intervalo ms grande posible.

Lubricante
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alta cantidad con poca cantidad de abrasivo para materiales blandos, menos cantidad con alto contenido de abrasivo para materiales duros, el pao debe estar hmedo pero no mojado
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 Velocidad rotacional
usar la recomendada de acuerdo al material a prepararse

Fuerza
El rea de la muestra montada deber ser 50% del soporte

Tiempo
Debe ser lo mas corto posible, examinar cada minuto

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La muestra debe ser representativa del material a caracterizar Todos los procesos de seccionamiento producen dao; algunos mtodos (como el oxicorte o corte abrasivo seco) producen cantidades extremas de daos. Las normas ASTM E 45, E 1122 y 1245 E aconsejan que se bene tomar varias muestras para estudiar las inclusiones en aceros. Para estudiar el tamao de grano, es comn usar una muestra de un lote. Para estudiar el efecto de la deformacin en la forma del grano de los metales forjados, se requiere tomar un mnimo de dos secciones - una perpendicular a, y otro paralelo a, la direccin de deformacin
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Mtodos de seccionamiento muestras metalogrficas

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Mtodos dependiente de la profundidad deformacin de corte del metal

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La seleccin del disco abrasivo es importante evitar la introduccin de niveles innecesarios de dao al cortar las muestras
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Materiales Acero, materiales ferrosos, aceros endurecidos Aceros de alta aleacin Metales no ferrosos, metales duros Materiales duros y tenaces, cermets, cermicos Materiales duros y frgiles, ceramicos, minerales
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Disco de corte: abrasivo/ligante Al2O3 (corundum)/bakelita Nitruro de boro cbico (CBN)/bakelita Carburo de silicio (SiC)/bakelita Diamante/bakelita Diamante/metal

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Alambre de corte recubierto con pasta de diamante, carburo de boro, carburo de silicio, corindn o de granate.

Para el seccionamiento de monocristales, soportes de catalizadores, dispositivos electrnicos, materiales reforzados con fibras (vidrios cermicos y polmeros)
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nodo

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Limitado a materiales o compuestos conductres que tienen una cantidad menor de materiales no conductores. Se utiliza para seccionar metales duros, metales con cristales simples y para cortar tambin cermicos.
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En el caso de materiales con baja conductividad trmica y baja resistencia a la fractura (por ejemplo, vidrios y cermicos) el proceso est acompaado por un choque trmico considerable.
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metales duros, fundicin gris o vidrios y cermicos

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Probablemente, el mtodo ms cuidadoso para el corte de metales no metales con enlace inico con casi ningn dao en la superficie El corte y fresado se realiza con hilos o cuerdas infiltrados con cido o con chorros de cido de 150 m de ancho. El procedimiento es asistido con electricidad con el uso de un hilo o boquilla como ctodo y la muestra como nodo. Estos tratamientos toman bastante tiempo y as se limitan a los cristales individuales de corte o de secciones Estos tratamientos toman bastante tiempo y por lo tanto estn limitados al corte de monocristales o de secciones delgadas.
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Materiales biolgicos, polmeros

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Montaje de muestras en un dispositivo de sujecin es necesario cuando se preparan muestras irregulares, pequeas, muy blandas, frgiles, y en los casos en que se requiere una retencin de borde.
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(a) Tube section

(b) Sheet
(c) Rods
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(d) Irregular pieces

(e) Wires
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(a) molde flexible. (b) molde de plstico

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Have the lowest shrinkage of all cold mounting resins. The curing time is relatively long, but the adhesion to most materials is excellent. They are also used for vacuum impregnation
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Easy-to-use resins with short curing times Negligible shrinkage

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Curing times are relatively short and the hardened sample is duroplastic
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The sample is placed in the mounting press, the resin is added, and the sample is processed under heat and high pressure

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Two mounts can be produced at one time using the duplexing spacer. Cycle times range from 8-12 minutes.
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 Requirements of hot and cold mounting materials

Specimens thoroughly cleaned either with an ultrasonic cleaner or lightly brushed with water containing a detergent Inert to the specimen, mold, and etchant Moderate viscosity during the actual embedding process; no generation of air bubbles after solidification Low linear shrinkage and good adhesion to the specimen Grinding and polishing behavior similar to those of the specimen, as well as similar chemical resistance to all reagents used during the specimen preparation
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Comparison of hot and cold mounting materials Hot compression mounting materials Powder, granulates, or preforms are densified by pressure and heat in a mounting press. Starting material has a durable shelf life. Time required per mount is ~15 min.
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Cold/room-temperature-curing
Liquid and/or powder are mixed together with a hardener and cast into suitable mold. Starting material should be stored cool and has a limited shelf life. Curing time per sample ranges from 10 min to 12 h; many samples can be mounted simultaneously.

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Comparison of hot and cold mounting materials Hot compression mounting materials Thermosetting plastics Phenol resins (Bakelite) Epoxy resins Diallyl phthalate Polymerization is irreversible; material cannot resoften. Heat to ~150 C under pressure. Samples can be removed hot from the mounting press, but cooling under pressure is recommended. Cold/room-temperature-curing

Epoxy resins Polyester resins Polymerization is irreversible; material will not resoften. Hardening reaction may increase the temperatures! This is directly related to the mixing ratio, the ambient temperatures, the volume of the mixed components, and the heat transfer by the molds.
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Comparison of hot and cold mounting materials Hot compression mounting materials Thermoplastics Acrylics Material can be resoftened with heat. Heat without pressure and cool under pressure. Cold/room-temperature-curing

Acrylics Material can be resoftened. Temperature may increase from 50120 C. Curing times are short.

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Properties of some important mounting materials Material Property Hot mounting materials Phenol Low hardness, poor adhesion (may be improved during cooling resins under pressure). Poor chemical resistance to aggressive (bakelite) chemicals and hot etchants. Easy to use, low cost Epoxy Only little shrinkage during curing, good edge retention. resins Resistant to etchants Diallyl Suitable for hard materials. No shrinkage during curing. phthalate Resistant to aggressive chemicals and hot etchants. Mounting conditions must be strictly followed. Acrylics Care must be taken during grinding; material may crack due to imposed stresses. Poor adhesion. Not resistant to aggressive chemicals. Transparent. Sample should be well cooled during curing. Suitable for pressure-sensitive specimens; pressure is only to be applied during the cooling cycle.
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Properties of some important mounting materials Material Property Cold mounting materials Epoxy Good adhesion. High viscosity, fills cracks, gaps, and pores easily resins and is therefore well suited for infiltration. Resistant to etchants and solvents. Nearly transparent. Mold material should be made of silicon rubber, polyethylene, or Bakelite. Curing time at least 8 h. Work under a fumehood because poisonous fumes are being generated. Skin irritant Polyester Good abrasion resistance, therefore well suited for hard materials. resins Shrinkage. Chemical resistance varies with the product. Acrylics Shrinkage. Short curing times. Poor resistance to alcohol and chlorohydrocarbon
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When the thickness of the coated sample is known (Fig. 3.19a), then the following equation applies: L = S L/S, or if the angle (Fig. 3.19b) of the supporting wedge is known, then L = L sin
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When analyzing thin layers and surface defects, it is important to have a sample with good edge retention Rinsing the sample with a wetting agent and using a material generating low shrinkage during the curing cycle is beneficial the sample surface is reinforced with an additional layer. By addition of ceramic particles, such as alumina powder, the hardness of the mounting material can be increased and adjusted to the hardness of the sample

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 the sample must have an electric contact. This can either be a hole drilled through the mounting material or a wire attached to the sample before mounting They are plastic materials, to which metal powders such as iron, silver, copper, or graphite have been added. Another excellent technique is to embed the sample in lowmelting bismuth alloys
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Specimens with voids, pores, and small cracks, and sample material that are fragile or brittle are prone to breakouts Only Epoxy resins can be used for vacuum impregnation due to their low viscosity and their low vapour pressure
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 Metal powders with a particle size above 2 m should be cold mounted in epoxy resin with pressurizing equipment. Powders that tend to agglomerate with a particle size less than 2 m (e.g., ceramic powders) can be embedded as follows:
the powder is placed in a test tube and put under vacuum with a threeway tap using running water; it is then infiltrated with a mixture of methacrylic acid methyl ester and 1% (wt%) of benzole peroxide. This mixture cures in 12 h at 50C, with the test tube kept closed. The test tube is then broken and the powder sample is processed as usual.
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Mechanisms of material removal

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Surface roughness and deformation depth of steel as a function of grit size of grinding medium
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Proper grinding removes damaged or deformed surface material, while introducing only limited amounts of new deformation.. The lapping process is an alternative to grinding, in which the abrasive particles are not firmly fixed to paper. Instead a paste and lubricant is applied to the surface of a disc.. Grinding can be divided into two individual processes: plane grinding and fine Grinding
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Copper specimen ground with 180 grit paper

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Copper specimen ground with 400 grit paper

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Copper specimen ground with 800 grit paper

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Copper specimen ground with 1200 grit paper

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Manual grinder/polisher machine

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conducted with particles of 6- or 3-m

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With particles of 1-m

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Copper specimen polished to 6 micron level

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Copper specimen polished to 1 micron level

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 Specimen Movement:
rotate in a direction counter to the rotation of the polishing wheel. the specimen is continually moved back and forth between the center and the edge of the wheel, After each step, the specimen is rotated 45 to 90 so that the abrasion is not unidirectional

Polishing Pressure
The correct amount of applied pressure must be determined by experience

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 Washing and Drying

The specimen is washed by swabbing with a liquid detergent solution, rinsed in warm running water, then with ethanol, and dried in a stream of warm air. Ultrasonic cleaning may be needed if the specimens are porous or cracked

Cleanness
The precautions for cleanness of the specimen, the metallographers hands, and the equipment

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Ginder/polisher machine with power head

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Fully automatic specimen preparation system

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Vibratory polisher
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 Electrolytic polishing
to grind the surface to a 600-grit finish and then electropolish for about 1- o 2-minutes soft single-phase metals and alloys Suitable electrolytes: diluted phosphoric, sulfuric or perchloric acid, acetic acid or alcohol

Chemical polishing
The agents are usually strongly oxidizing
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Circuitos elctricos y arreglos de los equipos usados para el pulido electroltico

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Detalles de una conexin elctrica indirecta de una probeta montada

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Combined techniques, such as alternating mechanical and electrolytic polishing or etch-polishing, give improved results in the case of soft or tough metals since deformation and reaction layers at the surface of the sample are easily removed. Moreover, refractory metals, multiphase alloys and coated materials can be satisfactorily treated. Etch-polishing is also applicable to some ceramics, e.g. grain boundary phases in AlN or Al2O3 become visible if NaOH is added to the abrasive suspension
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"revelar" la microestructura: fases, lmites de grano, impurezas, zonas deformadas, etc. de materiales metlicos. Puede realizarse por frotamiento o mediante inmersin de la muestra en el reactivo. Inmediatamente despus del ataque la probeta debe ser lavada con agua y secada con un chorro de alcohol y aire caliente El nital (solucin diluida de cido ntrico en alcohol) y el picrato sdico hirviendo se recomienda para el ataque del acero
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Etched copper specimen

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Over etched copper specimen

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Specimen levelling press

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Heat Tinting: Grain structure of annealed CP titanium revealed by heat tinting on a hot plate
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Characteristic curve for an electrolytic cell

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Diagram of the etching and polishing electrolytic

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Microstructure of plasma-etched sialon ceramic (currently limited to silicon nitride ceramics)

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Microstructure of thermally etched Al2O3-15 vol.% ZrO2 ceramic. The white particles are zirconia
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Effect of ion milling on titanium. Mechanically prepared surface on left and ion milled surface on right
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 Instead of an epoxy resin, Canadian Balsam is often used, especially if the index of refraction of the resin has to be known In geosciences, the thickness of the thin section is normalized to 20-30 m according to the interference colors of quartz.
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For the characterization of ceramics the thickness may be chosen according to the particle size
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Preparation of thin sections

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