Astm E3 Preparation of Metallographic Specimens1

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Designation: E 3 – 01
Standard Guide for

Preparation of Metallographic Specimens1
This standard is issued under the fixed designation E 3; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope E 1077 Test Method for Estimating the Depth of Decarbur-

1.1 The primary objective of metallographic examinations ization of Steel Specimens2
is to reveal the constituents and structure of metals and their E 1122 Practice for Obtaining JK Inclusion Ratings Using
alloys by means of a light optical or scanning electron Automatic Image Analysis2
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microscope. In special cases, the objective of the examination E 1245 Practice for Determining the Inclusion or Second-
may require the development of less detail than in other cases Phase Constituent Content of Metals by Automatic Image
but, under nearly all conditions, the proper selection and Analysis2
preparation of the specimen is of major importance. Because of E 1268 Practice for Assessing the Degree of Banding or
the diversity in available equipment and the wide variety of Orientation of Microstructures2
problems encountered, the following text presents for the E 1558 Guide to Electrolytic Polishing of Metallographic
guidance of the metallographer only those practices which Specimens2
experience has shown are generally satisfactory; it cannot and E 1920 Guide for Metallographic Preparation of Thermal
does not describe the variations in technique required to solve Sprayed Coatings2
individual specimen preparation problems. 3. Terminology
NOTE 1—For a more extensive description of various metallographic 3.1 Definitions:
techniques, refer to Samuels, L. E., Metallographic Polishing by Mechani-
3.1.1 For definitions used in this practice, refer to Termi-
cal Methods, American Society for Metals (ASM) Metals Park, OH, 3rd
Ed., 1982; Petzow, G., Metallographic Etching, ASM, 1978; and Vander- nology E 7.
Voort, G., Metallography: Principles and Practice, McGraw Hill, NY, 2nd 3.2 Definitions of Terms Specific to This Standard:
Ed., 1999. 3.2.1 castable mount—a metallographic mount generally
1.2 This standard does not purport to address all of the made from a two component castable plastic. One component
safety concerns, if any, associated with its use. It is the is the resin and the other hardener. Both components can he
responsibility of the user of this standard to establish appro- liquid or one liquid and a powder. Castable mounts generally
priate safety and health practices and determine the applica- do not require heat and pressure to cure.
bility of regulatory limitations prior to use. 3.2.2 compression mount—a metallographic mount made
using plastic that requires both heat and pressure for curing.
2. Referenced Documents 3.2.3 planar grinding—is the first grinding step in a prepa-
2.1 ASTM Standards: ration procedure used to bring all specimens into the same
A 90/A 90M Standard Test Method for Weight (Mass) of plane of polish. It is unique to semi or fully automatic
Coating on Iron and Steel with Zinc or Zinc-Alloy preparation equipment that utilize specimen holders.
Coatings 3.2.4 rigid grinding disc—a non-fabric support surface,
E 7 Terminology Relating to Metallography2 such as a composite of metal/ceramic or metal/polymer
E 45 Practice for Determining the Inclusion Content of charged with an abrasive (usually 6 to 15µm diamond par-
Steel2 ticles), and used as the fine grinding operation in a metallo-
E 340 Test Method for Macroetching Metals and Alloys2 graphic preparation procedure.
E 407 Test Methods for Microetching Metals and Alloys2 4. Significance and Use
E 768 Practice for Preparing and Evaluating Specimens for
Automatic Inclusion Assessment of Steel2 4.1 Microstructures have a strong influence on the proper-
ties and successful application of metals and alloys. Determi-
nation and control of microstructure requires the use of
1
This guide is under the jurisdiction of ASTM Committee E04 on Metallography metallographic examination.
and is the direct responsibility of Subcommittee E04.01 on Sampling, Specimen
Preparation, and Photography. 4.2 Many specifications contain a requirement regarding
Current edition approved April 10, 2001. Published July 2001. Originally microstructure; hence, a major use for metallographic exami-
published as E 3 – 21 T. Last previous edition E 3 – 95.
2
nation is inspection to ensure that the requirement is met. Other
Annual Book of ASTM Standards, Vol 03.01.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
Copyright ASTM International 1


E3
major uses for metallographic examination are in failure 5.4 Longitudinal sections taken parallel to the main axis of
analysis, and in research and development. the material are often used for revealing the following infor-
4.3 Proper choice of specimen location and orientation will mation:
minimize the number of specimens required and simplify their 5.4.1 Inclusion content of steel (see Practices E 45, E 768,
interpretation. It is easy to take too few specimens for study, E 1122, and E 1245),
but it is seldom that too many are studied. 5.4.2 Degree of plastic deformation, as shown by grain
distortion,
5. Selection of Metallographic Specimens
5.4.3 Presence or absence of banding in the structure (see
5.1 The selection of test specimens for metallographic Practice E 1268), and
examination is extremely important because, if their interpre- 5.4.4 The microstructure attained with any heat treatment.
tation is to be of value, the specimens must be representative of 5.5 The locations of surfaces examined should always be
the material that is being studied. The intent or purpose of the given in reporting results and in any illustrative micrographs. A
metallographic examination will usually dictate the location of suitable method of indicating surface locations is shown in Fig.
the specimens to be studied. With respect to purpose of study, 1.
metallographic examination may be divided into three classi-
fications: 6. Size of Metallographic Specimens
5.1.1 General Studies or Routine Work—Specimens should
6.1 For convenience, specimens to be polished for metallo-
be chosen from locations most likely to reveal the maximum
graphic examination are generally not more than about 12 to 25
variations within the material under study. For example,
mm (0.5 to 1.0 in.) square, or approximately 12 to 25 mm in
specimens could be taken from a casting in the zones wherein
diameter if the material is cylindrical. The height of the
maximum segregation might be expected to occur as well as
specimen should be no greater than necessary for convenient
specimens from sections where segregation could be at a
handling during polishing.
minimum. In the examination of strip or wire, test specimens
6.1.1 Larger specimens are generally more difficult to pre-
could be taken from each end of the coils.
pare.
5.1.2 Study of Failures—Test specimens should be taken as
6.1.2 Specimens that are, fragile, oddly shaped or too small
closely as possible to the fracture or to the initiation of the
to be handled readily during polishing should be mounted to
failure. Before taking the metallographic specimens, study of
ensure a surface satisfactory for microscopical study. There
the fracture surface should be complete, or, at the very least,
are, based on technique used, three fundamental methods of
the fracture surface should be documented. In many cases,
mounting specimens (see Section 9).
specimens should be taken from a sound area for a comparison
of structures and properties.
5.1.3 Research Studies—The nature of the study will dictate
specimen location, orientation, etc. Sampling will usually be
more extensive than in routine examinations.
5.2 Having established the location of the metallographic
samples to be studied, the type of section to be examined must
be decided.
5.2.1 For a casting, a section cut perpendicular to the
surface will show the variations in structure from the outside to
the interior of the casting.
5.2.2 In hot-worked or cold-worked metals, both transverse
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and longitudinal sections should be studied. Special investiga-
tions may require specimens with surfaces prepared parallel to
the original surface of the product.
5.2.3 In the case of wire and small rounds, a longitudinal
section through the center of the specimen proves advanta-
geous when studied in conjunction with the transverse section.
5.3 Transverse sections or cross sections taken perpendicu-
Symbol in
lar to the main axis of the material are often used for revealing Suggested Designation
Diagram
the following information:
5.3.1 Variations in structure from center to surface, A Rolled surface
5.3.2 Distribution of nonmetallic impurities across the sec- B Direction of rolling
C Rolled edge
tion,
D Planar section
5.3.3 Decarburization at the surface of a ferrous material E Longitudinal section perpendicular to rolled surface
(see Test Method E 1077), F Transverse section
5.3.4 Depth of surface imperfections, G Radial longitudinal section
5.3.5 Depth of corrosion, H Tangential longitudinal section
5.3.6 Thickness of protective coatings, and FIG. 1 Method of Designating Location of Area Shown in
5.3.7 Structure of protective coating. Photomicrograph.


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7. Cutting of Metallographic Specimens polishing, if possible. If etching is required, when studying the
7.1 In cutting the metallographic specimen from the main underlying steel in a galvanized specimen, the zinc coating
body of the material, care must be exercised to minimize should be removed before mounting to prevent galvanic effects
altering the structure of the metal. Three common types of during etching. The coating can be removed by dissolving in
sectioning are as follows: cold nitric acid (HNO3, sp gr 1.42), in dilute sulfuric acid
7.1.1 Sawing, whether by hand or machine with lubrication, (H2SO4) or in dilute hydrochloric acid (HCl). The HNO3
is easy, fast, and relatively cool. It can be used on all materials method requires care to prevent overheating, since large
with hardnesses below approximately 350 HV. It does produce samples will generate considerable heat. By placing the clean-
a rough surface containing extensive plastic flow that must be ing container in cold water during the stripping of the zinc,
removed in subsequent preparation. attack on the underlying steel will be minimized. More
7.1.2 An abrasive cut-off blade will produce a smooth information may be found in Test Method A 90/A 90M.
surface often ready for fine grinding. This method of sectioning NOTE 2—Picral etchant produces little or no galvanic etching effects
is normally faster than sawing. The choice of cut-off blade, when used on galvanized steel.
lubricant, cooling conditions, and the grade and hardness of NOTE 3—The addition of an inhibitor during the stripping of Zn from
metal being cut will influence the quality of the cut. A poor galvanized coatings will minimize the attack of the steel substrate. NEP
choice of cutting conditions can easily damage the specimen, (polethylinepolyamine) or SbCl3 are two useful inhibitors.
producing an alteration of the microstructure. Generally, soft 8.3 Oxidized or corroded surfaces may be cleaned as
materials are cut with a hard bond blade and hard materials described in Appendix X1.
with a soft bond blade. Aluminum oxide abrasive blades are 9. Mounting of Specimens
preferred for ferrous metals and silicon carbide blades are
preferred for nonferrous alloys. Abrasive cut-off blades are 9.1 There are many instances where it will be advantageous
essential for sectioning metals with hardness above about 350 to mount the specimen prior to grinding and polishing. Mount-
HV. Extremely hard metallic materials and ceramics may be ing of the specimen is usually performed on small, fragile, or
more effectively cut using diamond-impregnated cutting oddly shaped specimens, fractures, or in instances where the
blades. Manufacturer’s instructions should be followed as to specimen edges are to be examined.
the choice of blade. Table 1 lists the suggested cutoff blades for 9.2 Specimens may be either mechanically mounted,
materials with various Vickers (HV) hardness values. mounted in plastic, or a combination of the two.
7.1.3 A shear is a type of cutting tool with which a material 9.3 Mechanical Mounting:
in the form of wire, sheet, plate or rod is cut between two 9.3.1 Strip and sheet specimens may be mounted by binding
opposing blades. or clamping several specimens into a pack held together by two
7.2 Other methods of sectioning are permitted provided they end pieces and two bolts.
do not alter the microstructure at the plane of polishing. All 9.3.2 The specimens should be tightly bound together to
cutting operations produce some depth of damage, which will prevent absorption and subsequent exudation of polishing
have to be removed in subsequent preparation steps. materials or etchants.
9.3.3 The use of filler sheets of a softer material alternated
8. Cleanliness with the specimen may be used in order to minimize the
8.1 Cleanliness (see Appendix X1) during specimen prepa- seepage of polishing materials and etchants. Use of filler
ration is essential. All greases, oils, coolants and residue from material is especially advantageous if the specimens have a
cutoff blades on the specimen should be removed by some high degree of surface irregularities.
suitable organic solvent. Failure to clean thoroughly can 9.3.4 Filler material must be chosen so as not to react
prevent cold mounting resins from adhering to the specimen electrolytically with the specimen during etching. Thin pieces
surface. Ultrasonic cleaning may be effective in removing the of plastic, lead, or copper are typical materials that are used.
last traces of residues on a specimen surface. Copper is especially good for steel specimens since the usual
8.2 Any coating metal that will interfere with the subse- etchants for steels will not attack the copper.
quent etching of the base metal should be removed before 9.3.5 Alternatively, the specimens may be coated with a
layer of epoxy resin before being placed in the clamp in order
TABLE 1 Cutoff Blade Selection
to minimize the absorption of polishing materials or etchants.
Hardness HV Materials Abrasive Bond Bond Hardness
9.3.6 The clamp material should be similar in composition
up to 300 non-ferrous (Al, Cu) SiC P or R hard to the specimen to avoid galvanic effects that would inhibit
up to 400 non-ferrous (Ti) SiC P or R med. hard
up to 400 soft ferrous Al2O3 P or R hard etching. The specimen will not etch if the clamp material is
up to 500 medium soft ferrous Al2O3 P or R med. hard more readily attacked by the etchant.
up to 600 medium hard ferrous Al2O3 P or R medium 9.3.7 The clamp should preferably be of similar hardness as
up to 700 hard ferrous Al2O3 P or R&R med. soft
up to 800 very hard ferrous Al2O3 P or R&R soft the specimens to minimize the rounding of the edges of the
> 800 extremely hard ferrous CBN P or M hard specimens during grinding and polishing.
more brittle ceramics diamond P or M very hard 9.3.8 Exercise care in clamping the specimen. Excessive
tougher ceramics diamond M ext. hard
clamping pressure may damage soft specimen.
P—phenolic 9.4 Plastic Mounting:
R—rubber
R&R—resin and rubber 9.4.1 Specimens may be embedded in plastic to protect
M—metal them from damage and to provide a uniform format for both
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E3
manual and automatic preparation. This is the most common avoid boiling away the hardener. After the pressure has
method for mounting metallographic specimens. Mounting equilibrated, the resin is introduced into the mold and the
plastics may be divided into two classes—compression and vacuum is released and air admired to the chamber. Atmo-
castable. spheric pressure will force the resin into fine pores, cracks, and
9.4.2 The choice of a mounting compound will influence the holes.
extent of edge rounding observed during the grinding and 9.5.2 If a low-viscosity resin is used, the funnel and stop-
polishing operations. There are several methods available that cock may be eliminated. The specimen and resin are placed in
minimize rounding. The specimen may be surrounded by hard the mold prior to evacuation. The air in the specimen will
shot, small rivets, rings, etc., of approximately the same bubble out through the resin. Exercise care to ensure the
hardness or, when using a castable resin, a slurry of resin and hardening agent is not evaporated during evacuation. Dipping
alumina may be poured around the specimen. The specimen the specimen in the resin prior to placing it in the mold may
may also be plated before mounting (see Section 10). Many help in filling voids.
mounting procedures result in sharp edges on the mount 9.5.3 Vacuum impregnation is an effective method for
corners. The corners should be beveled to remove any plastic ensuring optimal results for porous metallographic mounts. It
mounting flash. is imperative that the specimens be completely dry prior to
9.4.3 Compression Mounting—There are four types of com- impregnation.
pression mounting plastics used predominantly in the metallo-
9.5.4 A more rapid technique but less effective method is to
graphic laboratory (see Table 2). These plastics require the use
lacquer the specimens with one of the formulations used by the
of a mounting press providing heat (140-180°C) and force
canning industry to line food containers. The formulations are
(27-30 MPa). Thermosetting plastics can be ejected hot but the
highly penetrating and the cure is a short time at low
best results are obtained when the cured mount is cooled under
temperatures. After lacquering, the specimens are mounted in
pressure. Thermoplastic compounds do not harden until cooled
the usual fashion.
and therefore should not be ejected while hot. Regardless of the
resin used, the best results are obtained when (1) the specimen
10. Plating of Specimens
is clean and dry, and (2) the cured mount is cooled under full
pressure to below 40°C before ejection from the press. This 10.1 Specimens such as fractures or those where it is
will ensure minimal shrinkage gap formation. necessary to examine the edges, are often plated to obtain good
9.4.4 Castable Plastics—Castable mounts are usually pre- edge retention. Plating can be done electrolytically or with
pared at room temperature. Some may require an external heat electroless solutions. These specimens are invariably mounted
source or applied pressure in order to cure. These resins consist prior to the grinding and polishing procedures. Electroless
of two or more components which must be mixed just prior to plating solutions can be purchased commercially.
use. There are four kinds of castable plastics in common use 10.2 Thoroughly clean the specimen surface prior to plating
(see Table 3). to ensure good adhesion of the plating. Avoid industrial
9.4.5 The molds for castable plastics are often simple cups cleaning treatments that are too harsh and may cause damage
that hold the resin until it cures. They may be reusable or not; to the specimen surface. Milder cleaning treatments that
the choice is a matter of convenience and cost. Handling involve detergents, solvents, mild alkaline, or acidic solutions
castable resins requires care. They all can cause dermatitis. are recommended.
Manufacturers’ recommendations for mixing and curing must 10.3 Chromium, copper, iron, nickel, gold, silver, and zinc
be followed to obtain best results. may be electrolytically deposited although copper and nickel
9.5 Mounting Porous Specimen: are predominantly used in metallographic laboratories.
9.5.1 Porous or intricate specimens may be vacuum impreg-
10.3.1 Ferrous metals are commonly plated electrolytically
nated in order to fill voids, prevent contamination and seepage,
with nickel or copper. A flash coat in a copper or electroless
and prevent loss of friable or loose components. Impregnation
nickel bath can be first applied for specimens that are difficult
is accomplished by placing the specimen in a mold in a vacuum
to electroplate.
chamber and then introducing the resin into the mold after the
chamber has been evacuated. The introduction of the resin into 10.3.2 Nonferrous metals may be plated with silver and the
the mold can be accomplished either by having a funnel or precious metals may be plated with nickel, gold, or silver.
stopcock fitted to the vacuum chamber or by having a basin of 10.4 The plating material should not react galvanically with
the resin present inside the chamber. A low-viscosity resin will the base metal of the specimen during plating, polishing, or
produce the best results. The pressure in the chamber must etching.
remain above the critical vapor pressure of the hardener to 10.5 Electroless plating is preferred to electrolytic plating
TABLE 2 Characteristics of Hot-Compression Mounting Compounds

Type of Compound Characteristics
Acrylic thermoplastic, cure time 10-15 min, optically clear, moderate shrinkage, low abrasion resistance, degraded by hot etchants
Diallyl phthalateA thermosetting, cure time 5-10 min, opaque, minimal shrinkage, good resistance to etchants, moderate abrasion resistance
EpoxyA thermosetting, cure time 5-10 min, opaque, very low shrinkage, good resistance to etchants, high abrasion resistance
PhenolicA (Bakelite) thermosetting, cure time 5-10 min, opaque, moderate shrinkage, degraded by hot etchants, moderate abrasion resistance
A
These compounds may be filled with wood flour, glass fiber or mineral particulate.
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E3
TABLE 3 Characteristics of Castable Mounting Compounds
Type of Compound Characteristics
Acrylic Cure time 8-15 min, moderate shrinkage, peak curing temperature can reach 90-120°C during polymerization, low abrasion
resistance, opaque to transparent
Polyester-acrylic (quartz-filled) Cure time 8-15 min, very low shrinkage, peak curing temperature can reach 90-120°C during polymerization, high abrasion
resistance, opaque
Polyester Cure time 30-60 min, high shrinkage, peak curing temperature can reach 90- 120 C during polymerization, moderate abrasion
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resistance, transparent
Epoxy Cure time 1⁄2-20 h, very low shrinkage, good adhesion, low heat generation during polymerization, moderate abrasion
resistance, low viscosity (good for vacuum impregnation), transparent
for specimens with rough, porous, or irregular surfaces, be- TABLE 4 European/USA Grit Grade Comparison Guide
cause the electroless solution provides better surface coverage FEPA ANSI/CAMI
and penetration. Grit Number Size (µm) Grit Number Size (µm)
10.6 Active metals such as zinc and aluminum are difficult P120 125.0 120 116.0
P150 100.0 180 78.0
to plate. Sometimes a flash cyanide copper plate can be P220 68.0 220 66.0
deposited, which then can be followed by normal plating from P240 58.5 ... ...
a sulfate bath. Evaporated coatings of copper, gold, or chro- P280 52.2 240 51.8
P320 46.2 ... ...
mium may also be used as starter coatings. P360 40.5 280 42.3
10.7 It is recommended that the plating thickness be at least P400 35.0 320 34.3
5µm. P500 30.2 ... ...
P600 25.8 360 27.3
P800 21.8 400 22.1
11. Grinding and Polishing P1000 18.3 500 18.2
P1200 15.3 600 14.5
General Information P1500 12.6 800 11.5
11.1 Many metals and alloys can be prepared using a similar P2000 10.3 1000 9.5
P2500 8.4 1500 8.0
sequence of grinding and polishing. Hard alloys may require P4000A 5.0 ... ...
greater pressure than soft alloys. The major differences will be A
Not found in the FEPA grading system.
in the final polishing. Some metals and alloys will require ANSI—American National Standards Institute
specific combinations of abrasive and support material, but a CAMI—Coated Abrasives Manufacturers Institute
surprising number can be handled by the same procedure. FEPA—European Federation of Abrasive Producers
Supplies and instructions for grinding, lapping, and polishing

are readily obtainable from laboratory supply houses. 11.2.3.4 Level the mount surface.
11.2 Grinding—Grinding can be done in a number of ways, 11.2.4 In fine grinding, damage to the specimen incurred
ranging from rubbing the specimen on a stationary piece of from the planar or rough grinding step must be removed. The
abrasive paper to the use of automatic devices. The choice of specimen is either ground on successively finer abrasive papers
method depends on the number and type of specimens to be (using water to wash away grinding debris and to act as a
done, financial considerations and requirements such as flat- coolant) or on a rigid disc or cloth charged with a suitable
ness and uniformity. abrasive.
11.2.1 Abrasive grit size designations in this practice are 11.2.5 After all grinding is done, the specimen must be
expressed in the ANSI (American National Standards Institute) cleaned thoroughly. Ultrasonic cleaning in a water/soap solu-
or CAMI (Coated Abrasives Manufacturers Institute) system tion containing a corrosion inhibitor may prove beneficial.
units with the corresponding FEPA (European Federation of 11.3 Polishing—Polishing is usually distinguished from
Abrasive Producers) numbers in parentheses. Table 4 provides grinding by the use of loose abrasive (#6µm) embedded in an
a correlation between these two systems and the approximate appropriately lubricated supporting surface. The choice of
median particle diameter for a given size in micrometres. abrasive, lubricant, and polishing surface support is often
11.2.2 Grinding should start with the finest paper, platen or specific to the metal and the object of the investigation.
stone capable of flattening the specimen and removing the Polishing can be divided into rough and fine (final) stages.
effects of prior operations, such as sectioning. The subsequent 11.3.1 Rough polishing is often sufficient for routine evalu-
steps should remove the effects of previous ones in a short ations like microindentation hardness and grain size.
time. Grinding consists of two stages- planar (rough) and fine. 11.3.2 When fine polishing is required, it may be performed
11.2.3 Planar or rough grinding [240 grit (P220) and with diamond or an oxide slurry step or both. The choice of
coarser] may be performed on belts, rotating wheels or stones. final polishing abrasive type and size is dictated by the
In some methods, diamond abrasives are used on rigid platens. hardness of the specimen. For instance, a lµm diamond final
Planar grinding may be used to accomplish the following: polish is often sufficient for many grades of steel, however,
11.2.3.1 Flatten an irregular or damaged cut surface, softer steels and non-ferrous materials often require an addi-
11.2.3.2 Remove sectioning damage, scale and other surface tional polishing step with an oxide slurry or suspension of SiO2
conditions prior to mounting, or Al2O3. Final polishing cloths are generally softer and higher
11.2.3.3 Remove substantial amounts of specimen material in nap than rough polishing cloths. Therefore, polishing time
to reach a desired plane for polishing, and force must be kept to a minimum to avoid artifacts such as


E3
edge rounding and relief. with abrasive so that the specimen follows an epicycloid path.
11.3.3 Careful cleaning of the specimen between stages is In some devices, the specimen rotates on its own axis as well.
mandatory to prevent contamination by coarser abrasive. The resulting scratch pattern now consists of randomly ori-
Ultrasonic cleaning may be effective. ented arcs. Deciding when the previous scratches have been
11.3.4 The polishing operations may be conducted by removed is more difficult than with directional (manual)
manual or by automated methods (preferred). grinding. The specimen surface should show uniform scratches
before proceeding to the next step. Cleaning between stages is
Manual (Hand-held) Methods required to prevent carryover of abrasives and contamination
11.4 When grinding manually, the specimen should be of subsequent preparation surfaces.
moved back and forth across the paper to allow for even wear. 11.10 Table 5 illustrates a traditional automated preparation
Between grinding steps, the specimen should be rotated 45- method. This method uses conventional SiC papers for grind-
90°. At the end of grinding on each paper, the surface of the ing and is suitable for all but the hardest of materials. Tables 6
specimen and its mount, if any, should be flat with one set of and 7 are preparation methods that utilize rigid grinding discs
unidirectional grinding scratches. or cloths for fine grinding. The method in Table 6 has been
11.5 Manual polishing methods consist of holding the shown to be effective for the preparation of materials harder
specimen by hand against an abrasive-charged rotating wheel than HRC45. The method in Table 7 may be used for the
and moving the specimen in a circular path around the wheel preparation of materials softer than HRC45. These procedures
against the direction of rotation of the wheel. The specimen may produce excellent results outside of the recommended
should be held firmly in contact with the wheel. hardness ranges.
11.6 The amount of force applied along with the rate of
movement of the specimen during grinding and polishing is a 12. Special Procedures
matter of personal preference and experience. In the prepara- 12.1 Occasionally, the metallographer is faced with the
tion of difficult materials such as thermally sprayed coatings or preparation of unfamiliar specimens or with special situations.
composites, the operating parameters must be strictly con- Anticipation of every possible situation is, of course, impos-
trolled. sible but some guidance can be offered.
11.7 A traditional manual preparation sequence consists of a 12.1.1 When used properly, electrolytic polishing can pro-
series of grinding and polishing steps and may be similar to duce near deformation-free surfaces but works best on solid
those listed in Table 5. solution alloys. Once the operating parameters are set, speci-
mens can be prepared quickly. See Guide E 1558.
Automated Methods 12.1.2 Vibratory polishing produces excellent results on
11.8 Many styles of automated specimen preparation ma- many materials. Although slow, a number of specimens can be
chinery are available. Most units can perform grinding and prepared simultaneously. It is especially advantageous for soft
polishing steps. Many use holders capable of accommodating materials.
multiple specimens. Major advantages of automated grinding 12.2 Porous Specimens—Specimens with continuous or
and polishing procedures are the consistent quality of specimen open pores can be vacuum-impregnated (see 9.5) with epoxy.
preparation and the substantial decrease in time. Therefore, Specimens with closed pores are mounted by a suitable
automated techniques are recommended over manual tech- method, ground through the fine grinding stage, cleaned, and
niques. dried thoroughly. The surface is then wiped with epoxy
11.9 Most of the devices for automated grinding and pol- mounting compound, usually the same material used to mount
ishing move the specimen around a rotating wheel covered the specimen, to seal the pores. After hardening, the last
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TABLE 5 Preparation Method 1 (General Use)
Surface Lubricant Abrasive Type/Size Time sec. ForceA Platen Rotation
ANSI (FEPA) N(lbf) RPMB
Planar Grinding
paper/stone water 120–320 (P120–400) 15–45 20–30 (5–8) 200–300C COD
grit SiC/Al2O3
Fine Grinding
paper water 240 (P220) grit SiC 15–45 20–30 (5–8) 200–300 CO
Rough Polishing
low/no nap cloth compatible lubricant 6µm diamond 120–300 20–30 (5–8) 100–150 CO
Final Polishing
med./high nap cloth compatible lubricant 1µm diamond 60–120 10–20 (3–5) 100–150 CO
synthetic suedeE water 0.04µm colloidal silica 30–60 10–20 (3–5) 100–150 CONTRAF
or 0.05µm alumina
A
Force per 30 mm (11⁄4 in.) diameter mount.
B
Power heads generally rotate between 25 and 150 rpm.
C
High-speed stone grinders generally rotate at greater than 1000 rpm.
D
Complimentary rotation, surface and specimen rotate in same direction.
E
Optional step.
F
Contra rotation, surface and specimen rotate in opposite directions.


E3
TABLE 6 Preparation Method 2 for Harder Materials $ HRC 45 (450 HV)
Planar Grinding
grit SiC/Al2O3
Fine Grinding
rigid disc compatible lubricant 6–15µm diamond 180–300 20–30 (5–8) 100–150 CO
Rough Polishing
low/no nap cloth compatible lubricant 3–6µm diamond 120–300 20–30 (5–8) 100–150 CO
Final Polishing
or 0.05µm alumina
A
B
C
D
E
Optional step.
F
TABLE 7 Preparation Method 3 for Softer Materials # HRC 45 (450 HV)

Planar Grinding
grit SiC/Al2O3
Fine Grinding
heavy nylon cloth compatible lubricant 6–15µm diamond 180–300 20–30 (5–8) 100–150 CO
Rough Polishing
low/no nap cloth compatible lubricant 3–6µm diamond 120–300 20–30 (5–8) 100–150 CO
Final Polishing
or 0.05µm alumina
A
B
C
D
E
Optional step.
F
fine-grinding stage is repeated to remove the excess material, 12.4.1.1 The problem of thin coatings can be handled by
and specimen preparation is continued as usual. The choice of using a taper mount. In this method, the specimen is mounted
epoxy for impregnation depends on the nature of the specimen. so that the plane of polish is at a small angle to the plane of the
It should be inert toward the specimen. surface. For example, a tapered plug is inserted in the mounting
12.3 Composite Materials—Composite materials, particu- press with the taper up. A blank tapered mount is prepared.
larly hard fibers in a soft matrix or wires in a soft insulation, Masking tape is wrapped around the circumference of the
can be particularly difficult to prepare. The best approach is to mount to make a well on the tapered end. A small amount of
first seal or impregnate pores or holes. Then grind carefully, epoxy mounting compound is mixed. The specimen, cut to fit
using copious lubrication. The grinding surface must be kept inside the well, is wetted with the epoxy and laid on the face of
flat and firm. In the polishing stages, the substrate should have the tapered mount, coated side up. Using a probe, the specimen
no nap and should be fairly hard. Diamond abrasive is is pressed down firmly onto the tapered face. The balance of
recommended. Both will minimize rounding of the hard the epoxy compound is added and allowed to harden. The
components. Sometimes, a compromise will have to be made mounted specimen is ground and polished on the epoxy face in
between accepting a few artifacts such as scratches or rounded the conventional manner exercising care that the plane of
edges. polish is perpendicular to the cylindrical axis of the mount.
12.4 Coated Materials: This is easily done with most automatic grinding machines.
12.4.1 Coated metals, such as galvanized steel, electro- 12.4.1.2 The problem of soft coatings can be solved by the
plated metal, enamel ware, and so forth, can be considered a use of a suitable backup. A piece of spring steel is useful to
variety of composite materials. They present problems of their hold the backup in place, or the backup may be cemented to the
own, such as flaking, chipping, and rounding. For example, specimen. The cement can act as an insulation to minimize
some coatings are so thin as to be unresolvable on simple cross galvanic effects. Caution: some cements will dissolve in epoxy
sections (tinplate). Other problems are the presence of a soft mounting compounds. A particularly suitable backup is another
coating on a harder substrate (galvanized steel) or a hard brittle piece of the same material, with the coating sandwiched in.
coating on a soft substrate (porcelain enamel on aluminum). Another solution is to add another coating, for example,
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E3
electroplate. However, this may introduce undesirable galvanic 12.6 Likewise, friable specimens can be bound together by
effects during etching. Galvanic problems may arise also from impregnation with plastic or by electroless nickel plating, or
the interaction of the coating and its substrate. The mounting both. Further guidance can be found in texts on preparation of
procedure used must result in excellent adhesion to the coated mineralogical specimens.
surface to minimize edge rounding. If edge rounding persists,
the polishing time and applied force may have to be decreased. 13. Precision and Bias
12.4.1.3 Hard coatings on softer substrates can be mounted
with a backup piece or a hard-filled mounting compound. 13.1 Because use of this practice does not produce numeri-
Diamond abrasives on a napless cloth will minimize surface cal results, no statement of precision or bias is possible.
relief during polishing.
12.5 Fragile specimens should be mounted in one of the 14. Keywords
castable mounting formulations. Vacuum impregnation will 14.1 alloys; grinding; metallography; metals; mounting;
ensure filling of holes and cavities (see 9.5). Thin walls can be polishing; sectioning; specimen preparation (metallographic)
reinforced by electroless nickel plating, which will alleviate the
rounding problem.
APPENDIXES
(Nonmandatory Information)
X1. CLEANING SPECIMENS
X1.1 Metallographers frequently need to clean specimens. a blast of compressed air to remove any loosely adherent
In some instances, the adherent debris, oxidation, or corrosion material. A soft camel-hair brush or a soft toothbrush may also
product must be collected for analysis, for example, by X-ray be useful for removing loosely adherent matter.
diffraction. In other cases, the adherent matter is of no interest, X1.3.1 If the techniques in X1.3 do not suffice, try aqueous
it merely needs to be removed. If the underlying surface is of solutions, organic solvents, or alcohol with an ultrasonic
no interest, the surface can be shot blasted, wire brushed, or cleaner. Aqueous solutions (8 g of Alconox per litre of warm
ground. However, if the underlying surface is important, for water) containing Alconox4, a detergent, have been found (1, 2)
example, a fracture surface, then the cleaning operation must to be effective. Follow the Alconox bath with rinsing under
do as little damage as possible. These different aims of the running water, then dry. Organic solvents, such as acetone,
cleaning operation must be kept in mind before formulating the ethyl methyl ketone, toluene, xylene, or alcohol (ethanol is
cleaning program. preferable to methanol because of potential health problems
with the latter) are also very effective. Before choosing one of
X1.2 When the adherent material is to be analyzed, a
these solutions, be sure that it will not adversely affect the
variety of procedures may be applied depending upon whether
material being cleaned. Avoid use of chlorinated organic
or not the underlying surface can or cannot be damaged.
solvents (such as trichlorethylene or carbon tetrachloride) due
X1.2.1 In the case of debris or corrosion product on the to their carcinogenic nature. Repeated replication, as described
surface of a part, a stylus, scalpel, or other sharp object can be in X1.2.2, is an effective method for cleaning fractures (3, 4).
used to scrape off or pry off enough material for analysis. This X1.3.2 When the procedures in X1.3 and X1.3.1 are unsuc-
will do some damage to the surface, but it will be localized. cessful, more drastic methods are required. Electrolytic clean-
X1.2.2 As an alternative, use cellulose acetate replicating ing solutions (Table X1.1), have been found to be quite useful.
tape to remove surface debris by the extraction replica ap- An inert material (stainless steel, graphite, or platinum, for
proach. A number of approaches have been developed and are example) is used as an anode, while the specimen is the
described in STP 5473 as well as in many textbooks on electron cathode in the electrolytic cell. Some of these solutions can
microscopy. Generally, thick (0.127 mm or 0.005 in.) tape is generate dangerous fumes, hence they should be used under a
employed. One surface is moistened with acetone and then hood with care. Endox 2145 has been found (1) to be useful for
pressed against the debris-coated surface. After it dries, strip cleaning heavily rusted steel fractures.
off the tape in the same way as you would remove adhesive X1.3.3 Cathodic cleaning solutions or acid-inhibited baths
tape. The debris will adhere to the tape. have also been employed to clean fractures (3, 5). However, as
the degree of corrosion or oxidation increases, fracture features
X1.3 When the surface is to be examined, but the adherent
will be destroyed to a greater extent and cleaning, while it can
debris will not be analyzed, several approaches can be used.
Always try the simplest, safest methods first. For example, use
4
Alconox is available from Alconox, Inc., New York, NY 10003. An equivalent
can be used.
3 5
“Manual Electron Metallography Techniques,” 1973. Available from ASTM Endox 214 is available from Enthone, Inc., West Haven, CT 06516. An
Headquarters. Request STP 547. equivalent can be used.
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E3
TABLE X1.1 Cleaning Solutions for Use When Standard Methods Are Inadequate
6N HCl plus 2 g/L Immerse specimen in solution for 1 to 15 min. Good for steels. Cleaning action can be enhanced by
Hexamethylene tetramineA light brushing or by brief (5 s) periods in an ultrasonic cleaner.
3 mL HCl Use a fresh solution at room temperature. Use in an ultrasonic cleaner for about 30 s.
4 mL 2-Butyne-1, 4 diol inhibitor
50 mL waterB
49 mL water Wash specimen in alcohol for 2 min in an ultrasonic cleaner before and after a 2-min ultrasonic
49 mL HCl cleaning period with the inhibited acid bath.
2 mL Rodine-50 inhibitorC
6 g sodium cyanide Electrolytic rust removal solution. Use under a hood with care. Use 100-mA/cm2 current density for up
6 g sodium sulphite to 15 min.
100 mL distilled waterDEF
10 g ammonium citrate Use solution heated to 30°C (86°F).

100 mL distilled waterG
70 mL orthophosphoric acid Recommended for removing oxides from aluminum alloy fractures (some sources claim that only organic
32 g chromic acid solvents should be used).
130 mL waterH
8 oz endox 214 powder Use electrolytically at 250-mA/cm2 current density for 1 min with a Pt cathode to remove oxidation
1000 mL cold water (add small amount products. Wash in an ultrasonic cleaner with the solution for 1 min. Repeat this cycle several times
of Photo-Flo)I,J if necessary. Use under a hood.
A
deLeiris, H., et al, “Techniques for Removing Rust from Fractures of Steel Parts that are to be Examined by Electron Microfractography,” Mem. Sci. Rev. Met., Vol 63,
No. 5, May 1966, pp. 463–472.
B
Dahlberg, E. P., “Techniques for Cleaning Service Failures in Preparation for Scanning Electron Microscope and Microprobe Analysis,” Scanning Electron Microscopy,
1974, Part IV, pp. 911–918.
C
Brooks, C. E., and Lundin, C. D., “Rust Removal from Steel Fractures—Effect on Fractographic Evaluation,” Microstructural Science, Vol 3A, Elsevier, NY, 1975, pp.
21–33.
D
deLeiris, H., et al, “Techniques for Removing Rust from Fractures of Steel Parts That Are to be Estimated by Electron Microfractography,” Mem. Sci. Rev. Met., Vol
63, No. 5, May 1966, pp. 463–472.
E
Russ, J. C., and Miller, G. A.,“ Effect of Oxidization on the Electron Fractographic Interpretation of Fractures in Steel,” JISI, December 1969, pp. 1635–1638.
F
Pickwick, K. M., and Smith, E., “The Effect of Surface Contamination in SEM Fractographic Investigations,” Micron, Vol 3, No. 2, 1972, pp. 224–237.
G
Interrante, C. G., and Hicho, G. E., “Removal of Iron-Sulfide Deposits from Fracture Surfaces,” ASTM STP 610, 1976, pp. 349–365.
H
Beachem, C. D., The Interpretation of Electron Microscope Fractographs, NRL Report 6360, U.S. Government Printing Office, Jan. 21, 1966.
I
Yuzawich, P. M., and Hughes, C. W., “An Improved Technique for Removal of Oxide Scale from Fractured Surfaces of Ferrous Materials,” Prakt. Met., Vol 15, April 1978,
pp. 184–195.
J
Goubau, B., and Werner, H., “Microfractographic Investigation of Fracture Surfaces Coated With Magnetite,” Prakt. Met., Vol 17, No. 5, May 1980, pp. 209–219.
remove the surface deposits, cannot restore damaged fracture bombardment (6) or by use of a glow-discharge method (7, 8).
features. These methods require specialized equipment.
X1.3.4 A number of proprietary rust removal solutions have
been developed. These are premixed and used directly out of
the container. Two such products are described in Refs 6 and 7.
X1.3.5 Cleaning can also be accomplished by argon-ion
X2. APPLIED LOAD CONVERSIONS
X2.1 Automated preparation machines commonly display X2.2.1 Some automated machines apply force individually
force in either pound-force (lbf) or newtons (N). The ability to to each specimen. In this case it is necessary to divide the force
convert from one unit to the other may be necessary when by the contact area to determine the load per specimen.
trying to interpret a documented procedure.
X2.3 Caution should be taken when using automated
X2.1.1 To convert from pound-force to newton multiply the machines that display pressure in pound-force per square inch
pound-force value by 4.5. (psi). Typically, the machine is displaying the air pressure
X2.1.2 To convert from newton to pound-force multiply the within the loading cylinder and not the actual pressure applied
newton value by 0.225. to either the specimen holder or individual specimen.
X2.2 When multiple specimens of equal contact area are X2.4 When converting from a force to a pressure, the
held in a holder, the applied force must be divided by the surface area of the specimen(s) must be determined. The value
number of specimens in the holder to determine the load per of force is then divided by the contact area to determine the
specimen. required pressure.
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E3
X3. PROCEDURE IMPROVEMENT
X3.1 To improve the preparation of a particular material, X3.8.3 If after etching, the deformation is well defined
try one of the preparation methods described in Table 5, Table covering several grains or even the whole specimen, then it
6, or Table 7. Following are general guidelines that may help may have been recently introduced. Check and clean the
improve results. polishing cloth for possible contamination. Replace the cloth if
results do not improve (see section X.2.1.4 ). Repeat the
X3.2 If a material is being prepared for the first time, the previous step.
surface should be microscopically examined after every step. X3.8.4 If after etching, the deformation is in the form of
long, blunt lines covering several grains (with possible inter-
X3.3 Before proceeding to the next step, be sure that all
ruptions) then it may have been introduced from an earlier
deformation and artifacts from the previous step, such as
stage. Repeat the procedure starting from the fine grinding
scratches, pull-outs or embedded grains, are completely re-
stage.
moved. It is difficult to identify when an artifact was intro-
duced if the specimen is not examined prior to the final step. X3.9 Smearing—Smearing is the flow of material at the
You must know when the artifact was introduced in order to surface of the specimen. It is the result of material being
improve the method. “pushed” across the surface instead of being cut.
X3.4 Keep the preparation times as short as possible. X3.9.1 Check the amount of lubricant. Smearing most often
Excessive preparation wastes consumables and may introduce occurs when lubrication levels are too low. Increase or change
artifacts such as relief and edge rounding. the lubricant to eliminate smearing.
X3.9.2 Check the applied load. Excessive loads can result in
X3.5 New consumables such as polishing cloths or dia- smearing. Reduce the load to eliminate smearing.
mond grinding products may need to be “broken in” for a short X3.9.3 Check the abrasive size. Abrasives grains that are
period prior to use. too small may not be effective in material removal. Increase the
abrasive grain size.
X3.6 The following section lists common preparation
artifacts and prevention measures. X3.10 Edge Rounding—Edge rounding results when the
edge of the specimen abrades at a greater rate than the body of
X3.7 Scratches—Scratches are grooves in the surface of the the specimen.
specimen produced by the points of abrasive particles. X3.10.1 Mount the specimen. Unmounted specimens al-
X3.7.1 Make sure that after planar grinding the surface of ways exhibit greater edge rounding than mounted specimens.
all of the specimens in the holder exhibit the same uniform X3.10.2 Use the correct mounting compound. There should
scratch pattern over the entire specimen. Repeat the planar be minimal shrinkage of the mounting compound away from
grinding step if necessary. the specimen. Try to match the abrasion resistance of the
X3.7.2 Clean the specimens and holder carefully after each mounting compound closely to that of the specimen. See
step to avoid contamination. Section 9.
X3.7.3 If there are still scratches left over from the previous X3.10.3 If the edge rounding first occurred during grinding,
step after finishing the current step, increase the preparation consider changing the grinding substrate to a less resilient
time by 25 to 50 %. If this does not work then you should form. Also consider changing the abrasive type. Diamond
consider altering the method by inserting an intermediate step. abrasive is often more effective than SiC at cutting hard
materials.
X3.8 Deformation—Deformation can be classified by two X3.10.4 Reduce polishing times as much as possible. Long
types, elastic and plastic. Elastic deformation disappears when polishing procedures often result in excessive edge rounding.
the applied load is removed. Plastic deformation, often called X3.10.5 Reduce applied load. Normally lower loads result
cold work, can be induced during sectioning, mounting, in less edge rounding.
grinding, lapping or polishing. Residual plastic deformation X3.10.6 Change the polishing lubricant. Oil or water/oil
can first be seen after etching. Only deformation that was type lubricants may help preserve edges.
introduced during metallographic preparation can be elimi- X3.10.7 Change the polishing cloth. Less resilient cloths
nated with procedure modification. Deformation from manu- produce better edges.
facturing operations such as bending, drawing and stretching X3.10.8 If the preceding steps are ineffective then consider
are not considered because they cannot be removed by altering plating the specimen. See Section 10.
the preparation method.
X3.8.1 If the deformation is visible in brightfield in the X3.11 Relief—Relief results when material from different
unetched condition, please see X3.7.3 Scratches, for tips on phases is removed at different rates due to varying hardness or
how to improve the preparation. wear rate of individual phases.
X3.8.2 If after etching, the deformation is restricted to X3.11.1 Relief normally first occurs during polishing. How-
single or a few grains then it is minimal and may be removed ever, if there are extreme differences in the hardness between
by repeating the previous step. phases it may occur during grinding. If this is the case then an
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E3
alternative grinding method should be considered. See Tables 5 X3.13.5 Specimen height should be kept as low as practical
and 6. to minimize gaps when using hot compression mounting.
X3.11.2 Polishing time should be kept to a minimum. X3.14 Contamination—Contamination is material from a
X3.11.3 Polishing cloths that have less resiliency produce source other than the specimen itself which is deposited on the
less relief (see Edge Rounding in X3.10). specimen surface during grinding or polishing.
X3.11.4 The polishing abrasive should be at least 2.5 times
harder (on the Vickers scale) than the hardest phase being X3.14.1 Thoroughly clean the specimen between prepara-
polished. tion steps (see 11.2.5, 11.3.3).
X3.14.2 Store grinding and polishing discs in a clean,
X3.12 Pull-outs—Pullouts are the cavities left in the dust-free environment.
surface after grains or particles are torn out during preparation. X3.14.3 Change grinding or polishing substrate/abrasive if
X3.12.1 Avoid high loads during grinding and polishing. necessary.
X3.12.2 Do not use coarse abrasives for Planar or Fine X3.15 Embedded Abrasive—Embedded abrasive results
grinding steps. when loose grinding, lapping, or polishing abrasive sticks into
X3.12.3 Do not make large abrasive size jumps between the surface of the specimen.
preparation steps. Insert an intermediate step if necessary. X3.15.1 Embedded abrasive is most common with soft
X3.12.4 Napless polishing cloths produce less pull-out than non-ferrous materials.
napped cloths. X3.15.2 Change to a more resilient grinding substrate.
X3.12.5 Every step has to remove the damage from the X3.15.3 Use a block of paraffin or candle to “pick up” loose
previous step, and has to introduce as little damage as possible. SiC particles on fine grit papers. This is done by lightly passing
X3.12.6 Check the specimen after every step in order to find the paraffin block across the paper.
out when the pull-out occurs. X3.15.4 Change to a more resilient polishing substrate
X3.13 Gaps—Gaps are the voids between the mounting when using diamond abrasives that are less than 3µm in
compound and the specimen. Gaps can result in a variety of diameter.
preparation artifacts such as edge rounding, contamination and X3.15.5 Change to an oil or water/oil-based polishing
staining. lubricant.
X3.13.1 Clean and dry the specimen thoroughly prior to X3.16 Lapping Tracks—Lapping tracks are indentations on
mounting. the specimen surface made by abrasive particles moving freely
X3.13.2 Select a mounting compound with low shrinkage (rolling) on a hard surface. Lapping tracks can be produced
(see Section 9). during both grinding and polishing.
X3.13.3 For hot compression mounting, cool the specimen X3.16.1 Change to a more resilient grinding or polishing
under pressure. substrate.
X3.13.4 For castable mounting compounds, avoid high X3.16.2 Increase the applied load in 10 % increments until
curing temperatures. It may be necessary to cool the specimen the lapping tracks disappear.
during the curing. X3.16.3 Employ optimal dynamics.
REFERENCES
(1) Yuzawich, P. M., and Hughes, C. W.,“ An Improved Technique for (5) Lane, G. S., and Ellis, J., “The Examination of Corroded Fracture
Removal of Oxide Scale from Fractured Surfaces of Ferrous Materi- Surfaces in the Scanning Electron Microscope,” Corrosion Science,
als,” Practical Metallography, Vol 15, April 1978, pp. 184–195. Vol 11, September 1971, pp. 661–663.
(2) Zipp, R. D., “Preservation and Cleaning of Fracture for Fractography,” (6) Macmillan, J. W., and Flewitt, P. E. J., “Assessment of Methods for
Scanning Electron Microscopy, Part I, 1979, pp. 355–362. Cleaning Oxide from Fracture Surfaces for Examination in a Scanning
(3) Russ, J. C., and Miller, G. A., “Effect of Oxidation on the Electron Electron Microscope,” Micron, Vol 6, No. 3/4, 1975, pp. 141–146.
Fractographic Interpretation of Fractures in Steel,” Journal, Iron and (7) ASTM Task Group E24.02, “Clean Surfaces for Fractography,” ASTM
Steel Institute, Vol 207, December 1969, pp. 1635–1638. STP 600, ASTM, Philadelphia, PA, 1976, pp. 251–253.
(4) Pickwick, K. M., and Smith, E., “The Effect of Surface Contamination (8) Hajicek, D. J., et al, “Development of a Cleaning Method for SEM
in SEM Fractographic Investigations,” Micron, Vol 3, No. 2, 1972, pp. Fractographic Analysis of Impulsively Loaded Cylinders,” Micro-
224–237. structural Science, Vol 5, Elsevier, NY, 1977, pp. 413–421.
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E3
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Standard Guide for

1. Scope E 1077 Test Method for Estimating the Depth of Decarbur-

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TABLE 2 Characteristics of Hot-Compression Mounting Compounds

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Supplies and instructions for grinding, lapping, and polishing

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TABLE 7 Preparation Method 3 for Softer Materials # HRC 45 (450 HV)

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X1. CLEANING SPECIMENS

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10 g ammonium citrate Use solution heated to 30°C (86°F).

X2. APPLIED LOAD CONVERSIONS

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X3. PROCEDURE IMPROVEMENT

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