Cal Poly State University, SLO Materials Engineering Dept.

Mate 415

D. Niebuhr Fall 2001

Lab #1 Macroexamination
Learning Objectives: 1. 2. 3. 4. 5. Sketch a failed component by hand, including important dimensions and features of the object. Describe the important aspects of macro-photography. Photograph a component with the macrocamera showing important features. Describe and prepare a sulfur print using the standard ASTM specification. Discuss macro-etching, its procedure, and typical application. State and illustrate the proper procedure for performing dye penetrant inspection.

Preparation: Skim the material pertaining to macroexamination in Vander Voort, (pgs 1-60). Read the appropriate ASTM Methods, E-381 on Macroetching and E-1180 on Sulfur Printing, in the ASTM Standards book in the library in EW-12. This lab will involve working in 2-person teams. These teams will remain the same for the entire quarter. Procedure: 1. Visual Inspection/Macroexamination A. Each team will be given a part (broken sample) to examine visually. Make sketches in the notebook and measure "critical" dimensions. Prepare a good 2 - 3 plane view sketch, with dimensions, for your report. B. Take Polaroid photographs, one showing the entire part and one showing detail of fractured or otherwise failed area at a higher magnification (or an area that might be suspected of having "invisible" crack if none is visually apparent). Use Polaroid MP-4 or Low-Mag. Nikon for the "long-range" photo; use either of these cameras (with shorter-focal-length lens) or the Hi-Mag Nikon macro-camera for the detailed picture. Note the magnification or show a scale in the picture. 2. Macroetching Obtain one of the weld samples and grind through 600 grit paper. Macroecth the specimen using 5% nital until you can see the weld structure (fusion line and HAZ). Sketch or photograph to record. Record which sample you prepared, as you will use it again in a couple of weeks. 3. Sulfur Printing Obtain one sample of a low-sulfur steel and one of a high-sulfur steel from the instructor. Prepare sulfur prints of the two samples in accordance with published procedures (ASTM and Handout). 4. Dye Penetrant A. Examine the part used for visual inspection using visible dye-penetrant in accordance with instructions in the lab-procedure handout. Photograph any indication of crack or other flaw that you find at an appropriate magnification on one of the macro-cameras. A copy of the photo will appear in your notebook.

Cal Poly State University, SLO Materials Engineering Dept. Mate 415

D. Niebuhr Fall 2001

B. Do a fluorescent dye-penetrant test on one of the water-quenched 1090 steel bars from the MATE 215 lab. Note the presence of any quench-crack indications and sketch the surface where they are most prominent. A copy of the sketch should appear in your notebook.

Report: (50 points) Each team will write an engineering report discussing macroexamination, including macroetching, sulfur printing and dye penetrant, their applications, and limitations. The report is to include an Abstract, Introduction, Procedure, Results and Discussion. Include your sketches, photos, etc., and your macroetched section in a protective plastic sleeve that will be provided. The report is due___________.

Cal Poly State University, SLO Materials Engineering Dept. Mate 415

D. Niebuhr Fall 2001

Sulfur Printing Preparation of the Sample The surface to be sulfur printed should be flat and should not bear scratches coarser than those produced by a 120 grit SiC emery paper. Grind sample on the belt sander, use a fresh surface for each print. Papers Used Any unglazed and pliable photographic paper may be used. Matte (non-glossy) finish (Ad-type) paper has been found to be most suitable. Photostat paper is also satisfactory. Bromide-type papers are preferred to chloride-type papers. Concentration of Acid Any concentration between two and five (maximum) percent sulfuric acid may be used. Procedure Write name on non-emulsion side. Immerse the paper in the acid, emulsion side up*, and allow it to soak well (1 to 3 minutes), then remove it from the acid and allow the excess acid to drip off. The acid should be uniformly distributed over the surface of the paper by spreading with the gloved hand. If the sample is small, the paper may be placed, emulsion-side up, on a smooth glass plate, and the sample pressed carefully against it to insure good contact. Great care should be taken to prevent movement of the sample once it has come into contact with the paper. If the sample is large, the paper may be placed, emulsion-side down, over the surface and immediately smoothed with a print-roller or sponge or by a gloved hand to carefully move off the edge any entrapped air or hydrogen sulfide. The entire process can be conducted under room illumination without damage to the paper. Strong sunlight, however, should be avoided. When it is desired to compare the amount of sulfur in two or more samples, the operation should be timed from the instant the paper makes contact with the sample until it is removed, and the same time allowed in all cases. Follow similar procedure for each sulfur print to ensure a uniform comparison Good results are obtained using two percent sulfuric acid and allowing a time of one (1) (2 to 10 maximum) minute. The darker the print, the higher is the sulfur content. If for some reason a satisfactory print is not obtained, the sample must be re-ground before it can be sulfur-printed again, unless resulfurized steels or preetched with 10% nital. The prints should be washed in clear running water (about 15 minutes) and fixed** for a short time, 3 - 4 minutes (5 minutes (Vs. 15 to 20) maximum), then thoroughly washed (30 minutes) and dried. Do not dry in the dryer unit or the residual acid will attack it. Dry by pressing the print between paper towels and air dry. Pre-etching the surface of the steel samples with 10% nitric acid in water often helps to obtain quality sulfur prints. * ** Virgin paper curls when the emulsion side is up. Fixer is in a white plastic container ( 8x14x3) with silver ppt at the bottom.

Cal Poly State University, SLO Materials Engineering Dept. Mate 415

D. Niebuhr Fall 2001

Sulfur print technique is an exceptionally useful procedure for studying the heterogenity of steels. During solidification, most of the impurities, such as sulfur and phosphorus, are rejected into the interdendritiec liquid (coring). Thus, the last areas to solidify become highly enriched in impurities. This phenomenon is used to advantage in macroetching, where the corrosion rate difference between the dendritic and interdendritic regions, segregate and matrix, and so forth, allow the macrostructure to be observed. (Anything that causes inhomegenuity, causes an energy difference. Etching attackes the areas of highest energy more, eg., grain boundaries.) Because the solubility of solid sulfur in iron is very low, nearly all the sulfur is precipitated as sulfide inclusions. Sulfide distribution is influenced by the steel making process, with the degree of deoxidation being the primary factor. In steels with a very high oxygen content (low carbon content, no strong deoxidizers), most of the sulfides are found in the central portion of the ingot. In steels with low oxygen contents (medium or high carbon content, additions of silicon, aluminum, etc.), the sulfides are more uniformly distributed. Sulfur improves machinability, but cannot be used in steel unless there is sufficient manganese to combine with it to form manganese sulfide. Iron sulfide is liquid at temperatures well below the freezing point of iron. Liquid (low melting point) iron sulfide forms a grain-boundary film (network) that almost completely separates the iron crystals along the austenite grain boundaries. Steel in this condition is brittle and cannot be hot-worked without disintegrating. (See 2nd & 3rd paragraph in LECO Met-Tips No.21.) Mn added to ppt with the sulfur and thus prevent hot shortness. MnS exists as an isolated phase, rather than a network, and increases machinability by acting as an internal lubricant and chip breaker. H2SO4 + (Fe,Mn)S(inclusion) - H2S (g) + Fe SO4 + MnSO4 H2S + 2AgBr(emulsion) - Ag2S (brown) + 2HBr The liberated hydrogen sulfide gas can become entrapped in voids on the steel surface, and, thus leave a brown color on the paper, falsely indicating the presence of a gross sulfide segregate.

Macroetching Procedure Macroetching for ingot/billet structure will be done with the "Watertown Arsenal" etch, listed in Appendix A in Vander Voort, (38HCl-12H2SO4-50H2O at 80 C for approx. 10 minutes). Etching will be done in a Pyrex dish under the fume hood. Wear goggles and gloves if you are doing the etching. Wear safety glasses and stand well back if you are observing. Wear old clothes or lab coat/apron. When mixing the etchant add the sulfuric acid slowly to the water and allow to cool; then add the hydrochloric acid. Instructor will demonstrate the etch first. Then each team will etch a slice from a steel billet. When student teams are etching, there should be no more than 4 people at a time near the etch. When all teams are finished, let etch cool and carefully pour back into bottle.

Cal Poly State University, SLO Materials Engineering Dept. Mate 415

D. Niebuhr Fall 2001