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 Sectioning Rough Grinding Mounting

Final Stages Fine Grinding Rough Polishing 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 microstructure 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. 2

~g?7~
@
:

Figure 1. Use of a Polaroid MP-4 Macro-Camera to Document Sample Location Before 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 possible. The location and orientation of each sample may be recorded manually, with a sketch, or by taking a macrophotograph as shown in Figure 1. 3

SECTIONING
Sectioning is performed to remove a suitably sized sample for subsequent mounting and polishing. Since the intended plane of polishing is usually determined by a sectioning operation, caution must be exercised to avoid excessive 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

4

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 abrasive 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 extreme, 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 MET-KLAMP'ID Vise

Figure 6. Cutting with the ISOMETTM Low 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 surface is such that the number of subsequent preparation steps may be reduced. 5

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 ETSPLlCE@(Silicon Carbide) Belts are available in grit sizes M 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. 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.

I

6

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 PREMOLDSTM which 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
Dlallyls
HIGHHARONESS CHEMICAllY RESIST Am' MODERATESHRINKAGE

Phenollcs
FAST CYCLE ECONOMICAL EASYTO USE HIGH SHRINKAGE lOW HARDNESS POOR EDGE ETEm'ION R

Epoxies
HIGH HARDNESS lOW SHRINKAGE CHEMICALLY RESISTAm'

Acrylics TRANSPAROO lOWINITIAl PRESSURE SLOW CURE
FAIRHARONESS DEFECT PRONE lOW CHEMICAL RESISTANCE

RoomTemperature Curing
Acrylics RAPIDURE C HIGHXOTHERM E TRANSLUCOO HIGHHRINKAGE S MOD. HARDNESS STRONG OOOR DEMOUm'ABlE Epoxies
lOW SHRINKAGE SEMITRANSPAROO MOD. ARONESS H SOlVOORESISTAm SLOW CURE

POlyesters TRANSPAREm' SLOW CURE FAIR HARDNESSSOLVEm' SENSITIVE lOWSHRINKAGE STRONG DOOR

Figure

8. Mounting Resins for Metallography

7 L

Edge rounding may be ideally controlled by choosing a low shrinkage mounting material containing a hard filler (EPOMETTM) r adding a hard filler o 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"" 11 required, the is 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. EPQMETTM Molding 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-

8
Edges not protected

\
C Rounded

-::J

Objective lens

C

///
=:J Retained

protected

Edges

Light

t t

Specimen Mount

Figure 9. How Edge Rounding Produces Inaccurate Information

8

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

8

@
9

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

techniques employed. Mold types vary from consumable Phenolic Ring Forms to re-usable Aluminum Ring Forms as shown in Figure 11. For further information 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 and dirtier than the Final Stages, no less care considered. Failure to be thorough and careful in microstructural damage which may not be completed. sample preparation are coarser in their performance should be in these operations could result evident until the final pOlish is

Table I. Guide to Abrasive Cut-Off
Wheel Selection
9"Dia.
(22.9cm) Aluminum Oxide Abrasive with Resin/Rubber
Tool Steel Rc 60 & Above, Carburized Steel Hard Steel Rc 50-60 Medium Hard Steel Rc 35-50 Soft or Annealed Steel Rc 15-35 Rb 45-90 Delicate Cutting (Ultra Thin Blade) 10-41110 10-4112-010 10-4116-010

Bond
0.070" (1.8mm) 0.070" (1.8mm) 0.070" (1.8mm) 0.063" (1.6mm) 0.032" (0.8mm) 1Q-44110 10-4412-010 10-4416-010 0.100" (2.5mm) 0.100" (2.5mm) 0.100" (2.5mm) 0.063" (1.6mm) 0.045" (1.1mm)

Aluminum Oxide Abrasive with Rubber Bond
10-41210 10-4127-010 1Q-44210 10-4427-010

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 Materials Medium Hard Non-Ferrous Metals; Uranium, Titanium, Zirconium, etc. Soft Non-Ferrous Metals; Aluminum, Brass, etc. 10-4140-010 0.063" (1.6mm) 0.063" (1.6mm) 0.063" (1.6mm) 10-4440-010 0.063" (1.6mm) 0.063" (1.6mm) 0.098" (2.4mm)

10-4145-010 10-41510

10-4445-010 104450-010

(Packaged 10 Wheels per Box) 1~" (3.2cm) ARBOR HIGH VOLUME AND PRODUCTION ABRASIVE CUT-OFF WHEELS FOR BUEHLER CUTTERS Thickness (22.9cm) RecommendedUses I 9" Dia.
Aluminum Oxide Abrasive & Tool Steels, Carburized Hard Steels, Stellite Soft or Annealed Steels (Packaged with Rubber Bond 10-5110-010 10-5112-010 0.063" (1.6mm) 0.063" (1.6mm) 10-5410-010 10-541 2-01 0 0.063" (1.6mm) 0.063" (1.6mm)

10 Wheels per Box)

10

Table 11.Abrasive

Cutting

Trouble Shooting
PROBLEM Burning (Bluish discoloration) Rapid wheel wear Frequent wheel breakage Resistance to cutting Cutter stalls

Chart
SUGGESTED REMEDY Lighten cutting pressure. Choose wheel for harder material Choose wheel for softer material Lighten cutting pressure Clamp the specimen more rigidly Choose wheel for harder material Reduce coolant flow Use cutter with greater HP Limit sample size

POSSIBLE CAUSE Overheated specimen Wheel bond breaking down too rapidly Loose specimen fixturing Slow wheel breakdown Cutter capacity inadequate

Table Ill. Compression Molding Trouble Shooting Chart
Phenolic DEFECT
Radial Split

Resins, Diallyl CAUSE

Phthalate

and EPOMETTM
REMEDY Increase mold size. Reduce specimen size. Decrease molding temperature. Choose lower shrinkage resin. Cool mold slightly prior to ejection. Preheat powder or Premolds.
Momentarily release during fluid state. pressure

@
Edge Shrinkage Circumferential Split

Too large a section in the given mold area. Sharp cornered specimens. Excessive shrinkage of plastic away from sample.

Absorbed moisture.
Entrapped molding. gasses during

@
Burst Unfused

Too short a cure period. Insufficient pressure.

L.engthen cure period. Apply sufficient pressure during transition from fluid state to solid state. Use proper molding pressure. Increase cure time. With powders-quickly seal mold closure and apply pressure to eliminate localized curing.

Insufficient molqing pressure. Insufficient time at cure temperature. Increased surface area of powdered materials.

TRANSOPTICTM Powder
DEFECT Cotton ball CAUSE Powdered media did not reach maximum temperature. Insufficient time at maximum temperature. Inherent stresses relieved upon
or after ejection.

REMEDY Increase holding time at maximum temperature.

Crazing

Allowcooling to a lower
temperature prior to ejection. Temper mounts in boiling water.

@

11

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. 2 TITLE/ORIGIN J. A. Nelson and R. M. Westrich, "Abrasive Cutting in Metallography," Metal/ographic Specimen Preparation, Proceedings of the 1973 Metallographic Symposium, Beverly Hills, Calif., pp. 41-54, Plenum Press, 1974. "Low Speed Saw," Bodine Motorgram, Vo!. 55, No. 3, MayJune, 1975. J. A. Nelson, "Modern Methods and Materials for Metallographic Mounting;' Microstructural Science, Vo!. 4, pp. 327-338, American Elsevier Publishing, 1976. J. A. Nelson and E. D. Albrecht, "The Basics of Metallography" (Part I), Heat Treating, pp. 19-23, April, 1976. J. A. Nelson and E. D.Albrecht, "The Basics of Metallography" (Part 11), eat Treating, June, 1976. H J. A. Nelson and W. U. Ahmed, "Significance of the Coolant/ Lubricant in Low Speed Saw Sectioning;' Praktische Metallographie, Vo!. XIII, pp. 297-305, J!Jne, 1976. "Diamond Compounds Grind-Porish Steel;' Cutting Tool Engineering, p. 72. May/June, 1978. "Diamond Blade Sections Schlitz Ecology Lid;' Brewers Digest, May, 1980. P.Wellner, "Investigations on the Effect of the Cutting Operation on the Surface Deformation of Different Materials;' Praktische Metal/ographie, Vo!.XVII, pp. 525-535, November, 1980.

8 12

17 19 20

35 56 60

BUEHLER
.)=.~II.=T.:-"'-'
41 WAUKEGAN ROAO

.

LAKEBLUFF. ILLINOIS USA 60044 Printed in U.S.A.

Form No. 10-81-99