A Universal Method for the Mechanical Preparation of Aluminium Alloy Specimens with High Edge Retention and their

Subsequent Colour Etching

Thomas Zwieg Danish Institute of Technology, Aarhus, Denmark 1. Introduction Numerous methods and recipes have been published on the metallographic preparation and etching of aluminium alloys. Nevertheless, new preparation equipment and consumables and the introduction of novel etching recipes, particularly those for colour etching, continue to provide metallographers with new opportunities to improve or optimise existing methods. This article presents a fast and universally applicable method of mechanical preparation based on Struers' MD (Magnetic Disc) System and its MD-Largo disc, which was developed for the fine grinding of soft materials in the HV 40150 hardness range. The technique discussed here enables specimens of aluminium alloys to be prepared with excellent edge retention. The method can be applied to almost all types of cast and wrought aluminium alloys by making minor adjustments to the force and duration of the preparation process, and has proved to be particularly beneficial when preparing specimens of aluminium materials with significantly harder surface coatings. A large number of etchants for use on aluminium materials have been described in the literature (see e.g. Refs. 1-3). Unfortunately, information contained in these references, such as "suitable for use with most types of aluminium ..." (1), have driven some metallographers and students to despair as they have attempted, unsuccessfully, to etch aluminium alloys with these so-called "universal" etchants. Metallographers who have worked with aluminium alloys have almost certainly learned by experience that most of these etchants are only suitable for use on specific alloys or narrowly defined groups of alloys. The investigation of a new material, which may well belong to the same group of alloys as the alloy usually prepared, differing only, perhaps, in the content of one of the alloying elements, can lead to a result wholly different to that normally to be expected. In the worst case, etching may cause severe pitting rather than revealing the desired grain boundaries or surfaces. A good case in point is Bohner's etchant, which produces excellent results when used to etch the grain boundaries of the alloy EN AW 6060 (approx. 0.5 % Si). However, when this etchant is used on the alloy EN AW 6005 (approx. 0.7 % Si), the grain boundaries are barely revealed, whilst attempts to etch the alloy EN AW 6082 (approx. 1 % Si) with Bohner's etchant causes significant pitting. The only really universal etchant for aluminium materials is Barker's
DIN EN 573 [EN AW] 2024 2219 3103 5019 5052 5083 5754 6005 6060 6061 6063 6082 7005 7020 7075 7175 Chemical symbol AlCu4Mg1 AlCu6Mn AlMn1 AlMg5 AlMg2,5 AlMg4,5Mn0,7 AlMg3 AlSiMg AlMgSi AlMg1SiCu AlMg0,7Si AlSi1MgMn AlZn4,5Mg1,5Mn AlZn4,5Mg1 AlZn5,5MgCu AlZn5,5MgCu

method of electrolytic etching with subsequent optical microstructural contrasting in polarized light. However, this method of etching requires electrical contact with the specimen, which is not always easy to achieve. The aluminium colour etchant developed by Weck (4) has proved to be very useful particularly for etching casting alloys. This etchant has the advantages of being chemically relatively innocuous and of not attacking intermetallic phases and precipitates, which are often etched away by many well-known etchants. One disadvantage of this etchant is its extremely sensitive reaction to remnant deformation layers on the surface of the prepared specimen. Frequently, poor results are achieved when this etchant is used on mechanically prepared specimens of many aluminium materials. This article describes a simple double etching technique that enables the required level of microstructural contrast to be achieved using Weck's etchant on mechanically prepared specimens. 2. Materials The methods of specimen preparation and etching were tested and successfully applied to a large number of different cast and wrought aluminium alloys over a period of about two years. Tables 1 to 3 present a selection of the aluminium materials tested. 3. Preparation 3.1. Mounting The specimens of the various aluminium materials can be cold or hot mounted. When selecting a
Table 1: List of the wrought aluminium alloys investigated

DIN 1725 GK-AlSi12 GK-AlSi10Mg GF-AlSi7Mgwa GD-AlSi9Cu3 GD-AlSi12 GD-AlSi10Mg GD-AlMg9

Casting process Gravity die casting Investment casting Pressure die casting

Alloy Casting alloy

Surface coating 1. Al 2O3/TiO-plasma or flame-sprayed coating, lacquered 2. CrN coatings 1. Anodic coatings (anodised) 2. Hard anodic coatings with PTFE 3. Lacquer coatings 4. Electroless plated nickel coatings

Wrought alloys

Table 2: List of the aluminium cast alloys investigated

Table 3: List of the surface coatings investigated

mounting resin, it is important to ensure that the hardness of the resin is comparable to or slightly greater than that of the hardest constituent in the surface of the specimen (e.g. intermetallic phases, edge layers). When investigating surface coatings, it proves expedient to hot-mount the specimen after tightly wrapping it in thin metal foil (e.g. household aluminium foil or nickel foil) as this allows the coating to be well separated from the mounting resin. Similarly, the foil chosen should have a hardness comparable to that of the coating. 3.2. Grinding Grinding was performed on a semi-automatic preparation system (RotoSystem, Struers) with a disc diameter of 250 mm. The specimens were prepared individually. A list of the grinding parameters used is shown in Table 4. 3.3. Polishing Table 5 summarizes the polishing parameters used. As in the case of the grinding process, the polishing forces and times listed in Table 5 are only approximate values that must be adjusted to suit the actual conditions. When polishing higher strength aluminium materials, it is often possible to dispense with the second stage of the polishing process (diamond, 1 m). However, the quality of the surface should be checked after completing the first polishing stage. If the specimen is to be etched immediately after preparation, final polishing with the suspension OPS is recommended. If the state of the precipitates is to be investigated, final polishing with OP-U is to be preferred, as OP-S has been

Parameter Surface Abrasive Grain/grit size Lubricant Direction of rotation Force (N) Time (min)

Plane grinding Grinding paper SiC 220 Water >> 25 3 (until flat)

Fine grinding Diamond 9 m DP-Green >> 150 30 5

MD-Largo

Table 4: Stages in the grinding process It may be necessary to adjust the grinding force and grinding time to suit the specimen material and geometry

Rotational speed (rpm) 300

Parameter Surface Abrasive Grin/grit size Lubricant Direction of rotation Force (N) Time (min)

Polishing 1 MD-DacMD-Nap Diamond 3 m DP-Red >> 25 3

Polishing 2

Final polishing MD-Chem SP-PoliCel1

Table 5: Stages in the polishing process

Diamond 1 m DP-Red >> 150 20 1.5

OP-S OP-U 0.04 m 0.04 m >> 150 20, Rinse: 10 2

Rotational speed (rpm) 150

found to attack the precipitates thereby altering their appearance. The SP-PoliCel polishing cloth, which is quoted in the Table as an alternative to MD-Chem, is particularly well-suited for the final polishing of very soft aluminium alloys. 4. Etching Excellent results can be achieved when specimens prepared using the technique described above are electrolytically etched with BarkGrasshopper intermetallic segregation in a cast aluminium alloy, 500 x

er's etchant and then viewed under polarized light illumination. However, this method of preparation requires electrical contact to be made with the specimen and this is often the source of difficulties (our experiences with commercially available electrically conductive hot mounting resins have been poor). For this reason an alternative etchant was sought.
Dinosaur intermetallic segregation in a cast aluminium alloy, 100 x

The ugly duckling intermetallic segregation in a cast aluminium alloy, 500 x

38
A Universal Method for the Mechanical Preparation of Aluminium Alloy Specimens with High Edge Retention and their Subsequent Colour Etching Structure of a wire of the alloy EN AW 7175, 200 x

Intercrystalline corrosion in a cast aluminium alloy, 1000 x

The aluminium colour etchant developed by Weck (4) is based on an alkaline potassium permanganate solution and is very wellsuited for etching aluminium cast alloys. As already mentioned, this alloy is comparatively harmless from a chemical point of view and has the additional benefit of not attacking intermetallic phases and precipitates, which are etched away by many other well-known etchants. The disadvantage of this etchant, however, is its exceedingly sensitive reaction with residual deformation layers in the surface of the prepared specimen. The immediate application of this etchant to specimens of a number of aluminium materials, in particular the wrought alloys, produced, as expected, unsatisfactory results. Despite final polishing with an oxide suspension, the specimens are still not completely deformationfree and thus unsuitable for use with this etchant. Longer final polishing using a variety of oxide suspensions did not significantly improve the result and led only to a reduction in the high level of edge retention achieved in the preceding preparative stages. A comprehensive series of experiments was therefore conducted in

Structure at the surface of the heat exchanger alloy EN AW 3103, starting liquid metal damage through solder metal penetration at the grain boundaries (the particles above the surface are residues of the solder material eutectic)

The aluminium wave burr at the solder connection of a heat exchanger

which the specimens were preetched with the aim of chemically removing residual deformations from the surface of the specimen. A range of different etching solutions and a variety of concentrations were examined; the best results being achieved by pre-etching the specimen with a 2 % aqueous solution of sodium hydroxide. As the results show, simple preetching with dilute sodium hydrox-

ide solution enables excellent microstructural contrasting to be achieved with Weck's etchant on nearly all the aluminium materials examined without impairing surface quality (edge retention, contrasting of precipitates). Examples of the results that can be achieved are shown in the three micrographs (Figures 1 to 3) of different aluminium alloys. One limitation of the method is

that it in the case of a very few wrought alloys e.g. EN AW 5083, (AlMg4.5Mn0.7) in a cold workhardened condition, it was not possible to achieve a satisfactory level of microstructural contrast using this procedure. The parameters used in the double etching procedure are presented in Table 6. A particular benefit of this double etching technique is that polarized light can be used for additional optical microstructure contrasting an advantage that is not generally realizable when etching is carried out using potassium permanganate alone. 5. Summary A universal method of mechanically preparing specimens of aluminium alloys has been developed in which the usual multi-stage grinding procedure using silicon carbide paper is replaced by a diamond fine-grinding stage using a Struers' MD-Largo grinding disc. The method is characterized by the very high level of edge retention that can be achieved - a feature that makes this technique particularly well suited to the preparation of surface-coated specimens. To etch specimens prepared in this way, a double etching procedure was developed involving a preetch with an aqueous 2 % sodium hydroxide solution and subsequent colour etching with Weck's alkaline potassium permanganate solution. As the results obtained so far demonstrate, this double etching procedure is almost as universal in its applicability as Barker's well-known electrolytic etching technique - without, however, requiring electrical contact to be made with the specimen.

Intermetallic segregation in a cast aluminium alloy, 250 x

Intercrystalline pitting corrosion in the alloy EN AW 6060, visible crystallographic corrosion attack, 200 x

Parameter Etchant

1st Etch 100 ml distilled water + 2 g sodium hydroxide

2nd Etch 100 ml distilled water + 4 g potassium permanganateonce dissolved: 1 g sodium hydroxide (4) RT 15 s Immersion etching. Dry etching. Always use fresh etchant. Etching is complete when the surface of the specimen has a yellow-green colour. Also see comments in Ref. (4)

Temperature Time Comments

RT 1 min Immersion etching. In some types of alloys the regions in the vicinity of precipitation are attacked. In such cases, the the etching time should be reduced to 30 s.

Table 6: Stages in the etching process

References (1) Petzow, G.: Metallographisches, Keramographisches, Plastographisches tzen Gebr. Borntraeger, Stuttgart 1994 (2) Beckert, M.; Klemm, H.: Handbuch der metallographischen tzverfahren DVG, Leipzig 1985 (3) Sperry, P.R.; Bankard, M.H.:

Metallographic Techniques for Aluminium Alloys, ASM Metals Handbook, 8th Edition, Vol.8, 1973 (4) Weck, E.; Leistner, E.: Metallographische Anleitung zum Farbtzen nach dem Tauchverfahren, Part III, DVS, Dsseldorf 1986 This article was first published in Praktische Metallographie, Vol. 38, No. 2, 2001