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METALLOGRAPHIC

SAMPLE PREPARATION
CUTTING. GRINDING. MOUNTING

@BUEHLER LTD., 1981-AII rights reserved.


INITIAL STAGESOF
METAllOGRAPHIC
SAMPLE PREPARATION

The purpose of metallographic sample preparation is to produce a polished


surface from which the true microstructure may be viewed by microscopic
examination. The simplest and most commonly used method of producing
the desired surface is abrasive preparation, consisting of a series of abrasive
steps of increasing fineness which, if correctly performed, will produce a
surface that is undamaged, flat, and free of scratches. The basic preparation
procedures are:

Initial Stages Final Stages


Sectioning Fine Grinding
Rough Grinding Rough Polishing
Mounting Final Polishing

All stages of metallographic preparation are important. Errors committed or


steps omitted will contribute to an unacceptable polished surface and may
lead to erroneous interpretations or measurements during microscopic
analysis. Since the Initial Stages are characteristically coarser than the
Final, the risk of altering the true microstructure is greater. An altered micro-
structure may be caused by mechanical deformation due to incorrectly
chosen abrasive material, excessive pressure, or inadequate removal of
normal damage produced by the previous step. Failure to select the correct
mounting technique for heat and pressure sensitive materials or overheating
during grinding, due to excessive application of pressure or inadequate
cooling, are sources of thermal damage. To assure valid microstructural
analysis, care must be taken at each stage of specimen preparation to avoid
damage which could alter the true microstructure.

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Figure 1. Use of a Polaroid MP-4
Macro-Camera to Document
Sample Location Before

~g?7~ Sectioning

{!,
@ . .~--: -
: - ~ Figure 2. A Simplified
Code for Metallographer
Sample Location (Arrow
indicates surface to be
prepared)

PREPARATION PROCEDURES
Although Sectioning is normally the Initial Stage in sample preparation, the
problem of sample identity must be considered first. Once a part has been
sectioned and the samples removed and polished, it may be difficult to ascertain
the relationship of the pOlished section to the original location. To circumvent
this, a sampling map is recommended. Areas to be cut should be marked with
waterproof ink, showing the location and orientation of the intended plane of
polish. Figure 2 illustrates one example of sample mapping, and others are pos-
sible. The location and orientation of each sample may be recorded manually,
with a sketch, or by taking a macrophotograph as shown in Figure 1.

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SECTIONING
Sectioning is performed to remove a suitably sized sample for subsequent
mounting and polishing. Since the intended plane of polishing is usually de-
termined by a sectioning operation, caution must be exercised to avoid exces-
sive damage to this surface. Abrasive cutting, the most often recommended
method of metallographic sectioning, produces minimal surface deformation
and is also the most economical, simple and rapid method available. When
samples must be removed from large parts by destructive methods such as
torches or hack-saws, the cuts should be made at a reasonable distance from
the area of interest. Subsequent cutting to remove the damaged areas should
be performed in the laboratory with an abrasive cutter.
The prerequisites for successful abrasive cutting are shown symbolically
in Figure 4.
Wheel Selection should be based on the chemical and physical properties
of the material to be cut. While aluminum oxide abrasive wheels are suggested
for cutting ferrous alloys, non-ferrous alloys and non-metals should be cut with
silicon carbide wheels. Abrasive wheels are rated according to their hardness.
The softer, pressed wheels (paper sided) are used to cut harder materials; the
harder, rolled wheels (rough sided) are preferred for softer materials. Special
resin or metal bonded diamond abrasive blades may be required for extremely
hard metals, carbides and ceramics.

Figure 3. The ABRASIMET'M Cutter


WHEEL
SELECTION

Figure 4. Prerequisites
for Successful
Abrasive Cutting

COOLANT TECHNIQUE

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Adequate, uniform coolant is important to prevent heat build-up during the
cutting process. Submerged cooling is very efficient, but cutters employing an
abundant stream of coolant directed at the cutting area may be equally effective.
If a cutter employs adjustable coolant nozzles, the distance from both nozzles
to the work piece must be equal, thereby preventing irregular wear of the abra-
sive wheel which may result in curved cuts and possible wheel failure.
Technique is another important aspect of metallographic cutting. Parts must
be clamped securely to prevent movement during cutting. A vise such as that
shown in Figure 5 ensures positive positioning and gripping of the work piece
and prevents broken wheels and inaccurately cut samples. Firm, but not ex-
treme, pressure should be applied to maintain a reasonable cutting action.
Excessive pressure could cause burning of the work piece and possible wheel
breakage. Resistance to free cutting could indicate a wrong choice of abrasive
wheels for the sample material or insufficient cooling. Drastic slowing down or
stalling of the cutter while in operation may indicate that the particular cutter
is not suited for the job.
Although conventional abrasive cutting is preferred for sectioning rigid
samples of steel and other common alloys, delicate components must be
sectioned using a low speed saw.The ISOMET~ shown in Figure 6, is employed
when cutting materials whose physical shape or microstructure would be altered
due to mechanical forces or heat normally produced by conventional abrasive
cutters.

Figure 5. A Work Piece Secured in the Figure 6. Cutting with the ISOMETTM Low
MET-KLAMP'IDVise Speed Saw

The ISOMETTMutilizes a thin, continuous rim blade which rotates at a low


speed (up to 300 rpm). Held by a pivoted specimen arm, the sample is gravity
fed by a pre-determined, dead-weight load. The cut may be accurately located
by means of a micrometer cross-feed and the superior quality of the cut sur-
face is such that the number of subsequent preparation steps may be reduced.

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Figure 7. Using a DUOMEP' Belt Surfacer for Two Stage Rough Grinding

ROUGH GRINDING
Rough Grinding is often used to remove coarse deformation produced by shop
saws or heavy oxide layers resulting from heat treatment. If the plane of interest
is too near the initial surface, it must be approached by rough grinding rather
than by abrasive cutting. Burrs and specimen mounting resin flash may also be
removed rapidly by rough grinding.
Equipment used for this Stage includes both belt surfacers and disc grinders.
Because abrasive belts normally wear longer than comparable discs, convenient
belt surfacers such as the DUOM~ 11shown in Figure 7 are widely used.
CARBIMET<8J METSPLlCE@(Silicon Carbide) Belts are available in grit sizes
50 to 600, however, rough grinding is usually confined to the range of 50-180
grit. ZIRMEfTMMETSPLlCE@(Zirconia Alumina Ceramic Composite) Belts offer
an alternative, particularly for grinding harder materials such as wt)ite iron.
These belts have a higher cutting rate, cooler action, and longer life than
comparable silicon carbide belts.
Dry grinding may be preferred in special cases where coolant might produce
contamination. The VACUMETTMDust Removal System, used in conjunction
with a belt surfacer, removes dust and residue caused by dry grinding.
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A higher degree of surface flatness and stock removal may be obtained by
using a disc grinder such as the SUPERMET,@which operates at higher speeds
(5700 SFM*) than (1600 SFM) belt surfacers. Regardless of the type of grinder
used, the specimen should be continually moved across the available surface to
prolong abrasive life and prevent grooving of the belt platen or grinding wheel.

*Surface feet per minute.

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MOUNTING
Mounting provides a safe,convenient means of holding metallographic samples
during the Final Stages of preparation and protects the sample edge from the
destructive attack of abrasive materials. Encapsulants for metallography fall
into two major categories, Compression Molding and Room Temperature
Curing, as shown in Figure 8. Compression molding resins are dry powders or
PREMOLDSTMwhich cure at 3,000 to 4,200 psi (3-4.2 Ksi) pressure and 150°C
temperature. They are ideally suited for mounting solid materials which are not
damaged by the required heat and pressure. While compression mOlding is
more economical and usually requires less time and effort, room temperature
curing resins are preferred for samples that are sensitive to damage from heat
and pressure.
Selection of a mounting technique must also take into consideration the
possible need of special edge protection, one of the principal functions of
metallographic mounting. There is a broad variation in the effectiveness of
different edge protecting media. Vital information such as case hardness depth,
plated layer thickness and adherence, and surface defects may be preserved
by the application of effective edge retention technology. A poorly protected
sample edge becomes a radius rather than a flat plane when attacked by
impinging abrasives. This might cause distortion and loss of important features
which may, due to the divergent reflection of light, lead to inaccurate analysis
or measurements as shown in Figure 9. If an edge is rounded, a surface layer
may appear shallower than it actually is.
Poor edge retention results from low hardness of the mounting material
compared to the sample and/or excessive shrinkage of the encapsulant from the
sample surface.

Mounting Resins for Metallography


HeatandPressure
Thermosetting Thermoplastic
Phenollcs Dlallyls Epoxies Acrylics
FASTCYCLE HIGHHARONESS HIGHHARDNESS TRANSPAROO
ECONOMICAL CHEMICAllY RESISTAm' lOW SHRINKAGE lOWINITIAlPRESSURE
EASYTOUSE MODERATESHRINKAGE CHEMICALLY
RESISTAm' SLOWCURE
HIGHSHRINKAGE FAIRHARONESS
lOW HARDNESS DEFECTPRONE
POOREDGERETEm'ION lOW CHEMICAL
RESISTANCE

RoomTemperatureCuring
Acrylics Epoxies POlyesters
RAPID
CURE HIGH
EXOTHERM lOW SHRINKAGE TRANSPAREm' SLOW CURE
TRANSLUCOO HIGH SHRINKAGE SEMITRANSPAROO FAIR
HARDNESSSOLVEm' SENSITIVE
MOD.
HARDNESSSTRONG OOOR MOD.HARONESS lOWSHRINKAGESTRONG DOOR
DEMOUm'ABlE SOlVOORESISTAm
SLOWCURE

Figure 8. Mounting Resins for Metallography

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L
Edge rounding may be ideally controlled by choosing a low shrinkage
mounting material containing a hard filler (EPOMETTM)or adding a hard filler
to a low shrinkage (Epoxide) Room Temperature Mounting Resin. Another
effective edge preservation technique utilizes an electroless nickel coating,
EDGEMET~)which forms an intimate, hard protective layer on certain sample
materials.
Compression molding resins are the preferred choice for mounting samples
that can safely withstand pressures up to 4200 psi and temperatures as high as
150°C. Although a mounting press such as the SIMPLlMET"" 11is required, the
cost per mount is considerably less than for a sample mounted in any of the
room temperature curing resins. Compression molding resins are available in
several types (Figure 8) depending on the particular sample to be mounted.
Phenolics are the most economical for routine work where edge retention is
not critical. EPQMETTMMolding Compound, an epoxy containing a hard filler,
provides maximum edge retention. Maximum efficiency and convenience are
achieved by using an air activated mounting presssuch as the PNEUMET<B> I
shown in Figure 10.

-11- -11-

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Edges
not
protected
\\
C -::J Objective
lens
///
C =:J
Edges
protected

Light
t t
Specimen

Mount

Rounded Retained

Figure 9. How Edge Rounding Produces Inaccurate Information

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Room temperature curing resins are recommended when metallographic
samples are sensitive to damage from heat or pressure. Epoxies and polyesters
are two-liquid systems which must be measured and carefully mixed. Except
for EPo-KWICK@which cures in 30-40 minutes, epoxies and polyesters cure
slowly (4-8 hours), have virtually no exotherm and adhere well to the sample
surface. Epoxies have higher hardness and greater resistence to solvents and
mineral acids than other room temperature curing resins. Acrylics consist of a
powder and a liquid which are easy to mix, cure rapidly (SAMPL-KWICKTMin
5-6 minutes and PLASTIC KIT in 20-30 minutes) but produce an exotherm of
OO~~~ .
The choice of molds for casting room temperature curing mounts depends
on the resin system used, the mount size desired and the subsequent polishing

Figure 10. PNEUMET" Air Activated Press Used for Compression Molding

@
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Figure 11. SAMPL-KUP;" Phenolic, Metal and Glass Molds for Room Temperature Curing
Mounting Resins

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techniques employed. Mold types vary from consumable Phenolic Ring Forms
to re-usable Aluminum Ring Forms as shown in Figure 11. For further informa-
tion consult the BUEHLER ANALYST~ Section 7, pages 12-14.
Prior to further sample preparation (METAL DIGEST,@Volume 20, No. 3-
"Final Stages of Metallographic Sample Preparation") sharp edges produced
by the molding process should be removed by grinding. If the sample protrudes
from the surface of the mount due to normal differences in the coefficients of
expansion of the sample and the resin, a light rough grinding may again be
required.
Although the Initial Stages of metallographic sample preparation are coarser
and dirtier than the Final Stages, no less care in their performance should be
considered. Failure to be thorough and careful in these operations could result
in microstructural damage which may not be evident until the final pOlish is
completed.

Table I. Guide to Abrasive Cut-Off


Wheel Selection
9"Dia.
(22.9cm)
Aluminum Oxide Abrasive with Resin/Rubber Bond
Tool Steel Rc 60 & 10-41110 0.070" 1Q-44110 0.100"
Above, Carburized Steel (1.8mm) (2.5mm)
Hard Steel 10-4112-010 0.070" 10-4412-010 0.100"
Rc 50-60 (1.8mm) (2.5mm)
Medium Hard Steel 10-4116-010 0.070" 10-4416-010 0.100"
Rc 35-50 (1.8mm) (2.5mm)
Aluminum Oxide Abrasive with Rubber Bond
Soft or Annealed Steel 10-41210 0.063" 1Q-44210 0.063"
Rc 15-35 Rb 45-90 (1.6mm) (1.6mm)
Delicate Cutting 10-4127-010 0.032" 10-4427-010 0.045"
(Ultra Thin Blade) (0.8mm) (1.1mm)
Aluminum Oxide Abrasive with Resin Bond
Dry Cutting of I 10-413~10
Soft Materials
Silicon Carbide Abrasive with Rubber Bond
Hard Non-Metallics, Glass,
Rocks and Other Hard 10-4140-010 0.063" 10-4440-010 0.063"
Materials (1.6mm) (1.6mm)
Medium Hard Non-Ferrous
Metals; Uranium, 10-4145-010 0.063" 10-4445-010 0.063"
Titanium, Zirconium, etc. (1.6mm) (1.6mm)
Soft Non-Ferrous Metals; 10-41510 0.063" 104450-010 0.098"
Aluminum, Brass, etc. (1.6mm) (2.4mm)
(Packaged 10 Wheels per Box)
1~" (3.2cm) ARBOR HIGH VOLUME AND PRODUCTION ABRASIVE CUT-OFF WHEELS
FOR BUEHLER CUTTERS
Thickness
RecommendedUses I (22.9cm)
9" Dia.
Aluminum Oxide Abrasive with Rubber Bond
Tool Steels, Carburized & 10-5110-010 0.063" 10-5410-010 0.063"
Hard Steels, Stellite (1.6mm) (1.6mm)
Soft or Annealed 10-5112-010 0.063" 10-541 2-01 0 0.063"
Steels (1.6mm) (1.6mm)
(Packaged 10 Wheels per Box)

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Table 11.Abrasive Cutting
Trouble Shooting Chart
PROBLEM POSSIBLE CAUSE SUGGESTED REMEDY
Burning Overheated Lighten cutting pressure.
(Bluish discoloration) specimen Choose wheel for harder material
Rapid wheel wear Wheel bond breaking Choose wheel for softer material
down too rapidly Lighten cutting pressure
Frequent wheel breakage Loose specimen Clamp the specimen
fixturing more rigidly
Resistance to cutting Slow wheel Choose wheel for harder material
breakdown Reduce coolant flow
Cutter stalls Cutter capacity Use cutter with greater HP
inadequate Limit sample size

Table Ill. Compression Molding


Trouble Shooting Chart
Phenolic Resins, Diallyl Phthalate and EPOMETTM
DEFECT CAUSE REMEDY
Radial Split Too large a section in the given Increase mold size.
mold area.

@ Sharp cornered specimens. Reduce specimen size.

Edge Shrinkage Excessive shrinkage of plastic Decrease molding temperature.


away from sample. Choose lower shrinkage resin.
Cool mold slightly prior to
ejection.
Circumferential Split Absorbed moisture. Preheat powder or Premolds.

@
Burst
Entrapped
molding.
gasses during

Too short a cure period.


Momentarily release
during fluid state.

L.engthen cure period.


pressure

Insufficient pressure. Apply sufficient pressure during


transition from fluid state to
solid state.

Unfused Insufficient molqing pressure. Use proper molding pressure.


Insufficient time at cure Increase cure time.
temperature.
Increased surface area of With powders-quickly seal mold
powdered materials. closure and apply pressure to
eliminate localized curing.

TRANSOPTICTM Powder
DEFECT CAUSE REMEDY
Cotton ball Powdered media did not reach Increase holding time at
maximum temperature. maximum temperature.
Insufficient time at maximum
temperature.
Crazing Inherent stresses relieved upon Allowcooling to a lower
or after ejection. temperature prior to ejection.
@ Temper mounts in boiling water.

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BUEHLER SAMPLE PREPARATION
RESEARCH AND TECHNICAL REPORTS
CUTTING · GRINDING · MOUNTING
These reports, published in the open literature by BUEHLER personnel and
users of BUEHLER equipment and supplies, are available as reprints, at no
charge, upon request.
REPRINT NO. TITLE/ORIGIN
2 J. A. Nelson and R. M. Westrich, "Abrasive Cutting in Metal-
lography," Metal/ographic Specimen Preparation, Proceed-
ings of the 1973 Metallographic Symposium, Beverly Hills,
Calif., pp. 41-54, Plenum Press, 1974.
8 "Low Speed Saw," Bodine Motorgram, Vo!. 55, No. 3, May-
June, 1975.
12 J. A. Nelson, "Modern Methods and Materials for Metallo-
graphic Mounting;' Microstructural Science, Vo!. 4, pp.
327-338, American Elsevier Publishing, 1976.
17 J. A. Nelson and E. D. Albrecht, "The Basics of Metallography"
(Part I), Heat Treating, pp. 19-23, April, 1976.
19 J. A. Nelson and E. D.Albrecht, "The Basics of Metallography"
(Part 11),Heat Treating, June, 1976.
20 J. A. Nelson and W. U. Ahmed, "Significance of the Coolant/
Lubricant in Low Speed Saw Sectioning;' Praktische Metal-
lographie, Vo!. XIII, pp. 297-305, J!Jne, 1976.
35 "Diamond Compounds Grind-Porish Steel;' Cutting Tool
Engineering, p. 72. May/June, 1978.
56 "Diamond Blade Sections Schlitz Ecology Lid;' Brewers
Digest, May, 1980.
60 P.Wellner, "Investigations on the Effect of the Cutting Opera-
tion on the Surface Deformation of Different Materials;'
Praktische Metal/ographie, Vo!.XVII, pp. 525-535, November,
1980.

BUEHLER
.)=.~II.=T.:-"'-'
41 WAUKEGAN ROAO .
LAKEBLUFF. ILLINOIS USA 60044

Form No. 10-81-99 Printed in U.S.A.

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