Metallographic Techniques for Copper Beryllium and Nickel
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Metallographic Techniques For Beryllium Copper and Beryllium Nickel Alloys by John Harkness and Dr. Amitava Guha Beryllium copper and beryllium nickel alloys can be article "Toxicity of Metal Powders" in Volume 7 of easily examined metallographically by following the 9th Edition of the ASM Metals Handbook. standard procedures. These procedures are outlined Conventional, commercially available in detail in this paper and provide the information metallographic preparation facilities normally can necessary for examining the structure of these be used safely to prepare these alloys. alloys. This paper describes procedures for selecting a metallographic specimen; mounting, grinding and Specimen Preparation polishing the specimen; and etching it to reveal the Metallographic equipment and procedures for metallurgical structure. The included beryllium-containing alloys are much the same as photomicrographs serve as examples of the those recommended for general metallurgical structure of commonly used tempers of these laboratory use. commercial alloys. Sectioning of specimens is carried out by sawing, Health and Safety abrasive cutting, or shearing, depending on section thickness and strength. Abrasive wheels formulated Despite low concentrations of beryllium in for nonferrous or medium-hardness materials and commercial beryllium copper and beryllium nickel general purpose use are satisfactory for beryllium alloys (nominally 2 wt% or less), these materials copper. Wheels formulated for hard materials and can be hazardous to health if excessive quantities of heavy sections are better for beryllium nickel. dusts, mists, or fumes containing particles of alloy Abrasive cutting should be performed wet to avoid small enough (10/um or less) to enter the lungs are thermal damage to the specimen and to minimize inhaled. Special precautions are not required for metallic dust. Sufficient surface metal is then metallographic sectioning, grinding, or polishing removed from the sectioned faces of the specimen performed wet with water or cutting oil or for dry by wet rough grinding to eliminate any deformed shearing of clean, thin-section strip or wire. material introduced during sectioning. Adequate ventilation should be provided for dry Mounting is usually required for specimens too sectioning, grinding or polishing operations which small to be hand-held while polishing or for those produce dust or fumes. Metallographic preparation requiring edge preservation. Flat strip or transverse equipment and laboratory work surfaces should be sections of small diameter rod and wire may be damp wiped periodically to remove accumulation of stacked and gripped in reusable metal screw clamps dry alloy particles. Beryllium-containing alloys are for unembedded preparation. Alternatively, samples not harmful in contact with skin or wounds, or if may be embedded with cold-mounting or swallowed. For additional information, see the compression-molding resins. Commercial metal or https://materion.com/products/high-performance-alloys plastic sample clips are used to stand the sample cylindrical metallographic mounts or various upright in the mold. Transparent mounting resins numbers and sizes of unembedded samples. The are preferred for delicate fabricated parts, such as holders are rotated by the sample mover head of the electrical contacts, to help locate features of machine at approximately 150 rpm and are interest in the final plane of polish. When distortion mechanically pressed against the rotating work of the sample under pressure is to be avoided, wheel, which can be a coarse grinding stone, a cold-mounting is favored over compression wheel accepting successively finer grades of molding. abrasive paper, or a cloth covered polishing wheel. Edge retention may be enhanced by nickel plating Some systems also employ lapping techniques. prior to mounting or by using hard compression- Work wheels must be manually changed between molding resins formulated for edge preservation. preparation steps, but the specimens are never Glass beads or alumina (Al203) granules added to removed from the holder until they are ready to be cold-mounting resins for the same purpose will etched. This preserves a common plane of polish likely contaminate the polishing wheel and cause and maintains flatness of the prepared surfaces. undesirable specimen scratching, particularly in the Due to the high pressures and short cycle times softer forms of beryllium copper. typically used, these automatic machines increase Grinding. Coarse grinding is performed wet on a metallographic laboratory productivity and improve belt or disk grinder using 120 or 180 grit abrasive edge preservation and phase retention. paper to remove any deformed metal layer. Fine Automatic metallographic preparation techniques grinding is also performed wet, either by hand on vary according to the machine used and materials strips of abrasive paper or mechanically on 300 rpm being prepared, but the following procedures have or faster disks using, successively, 240, 320, 400 been successfully used for beryllium-containing and 600 grit abrasives. The sample is rotated 90° alloys and can be adapted to any automatic system. between each grinding. Silicon carbide or Al203 Holders containing mounted specimens or abrasives may be used. relatively square cut, unembedded specimens are Mechanical polishing is usually accomplished in rough ground on 120 or 240 grit paper and fine rough and final stages. Rough polishing is ground on, successively, 240, 320,400 and 600 grit performed using a 6/zm diamond on a wheel papers. Very uneven, unembedded specimens may covered with a hard, napless chemotextile cloth. require coarse 60 or 80 grit stone or paper grinding Extender oil is applied sparingly, and the wheel is to bring all the samples in a holder to a single plane rotated at approximately 300 rpm or less. The of polish. A copious flow of recirculated specimen is initially positioned so that the direction water-base coolant is applied to the work wheel of polishing is perpendicular to the 600 grit grinding during each grinding step. It is not necessary to scratches. Maintaining this orientation, it is briefly wash the samples in the holder between grindings. rotated counter to the rotation of the wheel to Wheel speeds of 150 rpm, pressures of 150 N distribute the rough polishing scratches randomly. (35 Ibf), and times of approximately 30 seconds per Final polishing is performed using 0.05/im Al203 grinding are usually sufficient. Zirconia (Zr02) in distilled water suspension and a wheel covered abrasive papers will last longer than silicon carbide with low-nap rayon cloth. Speeds are the same as or Al203 under these grinding conditions. The those used for coarse polishing. The wheel is kept loaded sample holder is then ultrasonically cleaned moderately saturated with polishing suspension, in alcohol, dried in an air blast and returned to the and the specimen is counter-rotated to vary the machine for polishing. direction of final polishing. An exception to this Two or three polishings may be employed. One procedure is the case of the softer annealed or approach, which applies primarily to holders lightly cold worked tempers of beryllium copper, in containing up to six 30 mm (1.25 inch) diameter which unidirectional final polishing parallel to the mounts, begins with 6/um diamond on a hard, specimen long axis helps to minimize scratching. napless chemotextile, proceeds to 3/zm diamond on The specimen is washed under running water after a low-nap cloth and finishes with 1/um diamond on each polishing step with mild soap and a cotton a soft, high-nap cloth. Wheel speed in each case is swab, then rinsed with alcohol and dried under a 150 rpm. The first and second polishings use a warm air blast. pressure of 150 N (35 Ibf) for 2 min per step; the Automatic Grinding and Polishing. Several final polishing, 100 N (25 Ibf) pressure for 35 automatic metallographic preparation machines are seconds. Polishing extender is dripped sparingly on available that provide rapid and reproducible the wheels during each step, and the sample holder grinding and polishing of multiple specimens and work wheels should rotate in the same through the use of preset pressure control and a direction in each step. cycle timer. These machines use metal sample Another approach, useful for high volume holder disks that accommodate 4 to 12 or more production of embedded and unembedded samples. - 2- is to use a 9//m diamond slurry on a lapping disk, concentrated HN03 presoak is omitted to avoid followed by a 0.3yum Al20 3 suspension on a low-nap pitting. rayon cloth, with an optional intermediate step of In addition to grain structure and flow patterns, 3yum Al203 suspension on a hard chemotextile. macroetched samples of beryllium coppers with Times and pressures are varied to suit the size and 1.6 wt% or more Be reveal locally heat-affected number of samples. zones as light etched areas if reannealed or unaged The sample holder is ultrasonically cleaned and and as dark etched areas if aged. Light etched or dried after each polishing, and the samples are then reddish colored areas adjacent to exterior or crack removed from the holder for etching and final surfaces in uniformly aged materials usually signal examination. Specimens of different alloys and environmental attack leading to local depletion of hardnesses usually may be mixed in a single holder beryllium and lack of aging response. Matrix without harming the prepared surfaces of the softer darkening on etching is not as pronounced in aged samples. beryllium nickel and is absent in beryllium coppers ElectropoSishing. Clean, as-rolled strip surfaces containing less than 0.6 wt% Be, limiting the or sectioned sample faces of beryllium copper alloys information revealed by macroetching of these prepared through 400 to 600 grit grinding paper alloys essentially to matters of grain morphology. may be electropolished. A satisfactory all-purpose Castings and cast billet exhibit columnar dendritic electrolyte for beryllium copper alloys is a mixture and/or equiaxed grain growth depending upon of 1 part nitric acid (HN03) and 2 parts methanol solidification conditions.