Sample preparation Standard preparation methods for materialographic analysis
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1 Sample preparation Standard preparation methods for materialographic analysis Practical experience ATM-Lab
2 2 Table of Contents 1. General Information Grit conversion chart, Pressure parameters and specimen size... 3 Explanation of symbols Preparation methods Aluminum and wrought aluminum alloy... 5 Aluminum alloy... 6 Carbon/glass fiber reinforced composites (CFC/GFC)... 7 Cast iron (GJS/GJL)... 8 Soft to medium-hard steel (5-35 HRC/350HV)... 9 Medium-hard to hard steel (30-65 HRC/850HV) Stainless steel (austenitic/ferritic) Steel and welded steel (macro) Nitrided steel Ceramics Cobalt based alloy Nickel based alloy Spray coatings (metallic) Magnesium Printed circuit board (non assembled) Printed circuit board (assembled) Copper and copper alloy Titanium (commercial pure: grade 1-4) Titanium alloys NOTES: The preparation methods can be applied for proper sectioned and burred specimens. Parameters like pressure (given as force in newton) are referred to single pressure and depend on specimen size. For specimens 40mm these values have to be adjusted with the help of table Pressure parameters and specimen size. Instead of the Dia Complete diamond suspensions common diamond suspensions in combination with lubricants (water or alcohol based) can be used. Mind right dosage! The velocity of the sample holder is 100 rpm and can vary depending on the specific material. Due to the diversity of materials and examination aims the provided standard preparation methods might not cover all applications. In this case contact our application lab; our team will support you with customized preparation methods. lab@atm-m.com Advanced Materialography
3 General Information 3 Grit conversion chart FEPA (P) grain size [µm] ANSI/CAMI grain size [µm] Reference: Analytical Characterization of Aluminum, Steel and Superalloys D. Scott MacKenzie, George E. Totten October 10, 2005 by CRC Press ISBN: Pressure parameters and specimen size Specimen diameter [mm] Divergence in pressure used in the preparation methods - (5N 10N) - 5N 0 + 5N + (5N 10N) NOTES: The preparation methods can be applied for proper sectioned and burred specimen. Parameters like pressure (given as force in newton) are referred to single pressure and depend on specimen size. For specimens 40mm these values have to be adjusted.
4 4 Explanation of Symbols EXPLANATION OF SYMBOLS Symbol Meaning Symbol Meaning Cutting Single pressure Mounting Speed disc / Polishing Speed sample holder / Polishing Sample holder clockwise Etching Sample holder anti-clockwise Pre- Time Polishing / diamond Dosing lubricant Lubricant waterbased Lubricant alcohol based
5 Preparation 5 Aluminum ( 99,7%) and wrought aluminum alloy Cut-off wheel: corundum, resin bond Bakelite red/black KEM 20, KEM 30 ** P320 (280) O Until plane ** P600 (400) O :00 ** P1200 (600) Polishing GAMMA Dia Complete O :30 (change SiC paper/foil after 45sec) :00 LAMBDA/OMEGA Eposil F 0.1µm :00 ( Etching (electrolyt.) Barker s reagent 30V ** To reduce the contamination of the specimen by SiC particles, it should be coated with paraffin wax before
6 6 Preparation Aluminum alloy Cut-off wheel: corundum, resin bond Bakelite black/red KEM 20 P320 (280) O Until plane Pre- BETA Dia Complete Poly, 9µm :00 Polishing SIGMA Dia Complete :00 LAMBDA/OMEGA Eposil F 0.1µm :00 ( Etching (chem.) Kroll s reagent 0:30
7 Preparation 7 Carbon/glass fiber reinforced composites (CFC/GFC) Cut-off wheel: diamond, metal bond (bronze) Pressure vessel KEM 15 plus P320 (280) O Until plane Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 Polishing GAMMA/DELTA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :30 (
8 8 Preparation Cast iron (GJS/GJL) Cut-off wheel: corundum, resin bond Bakelite red/black KEM 30 P320 (280) O Until plane P600 (400) O :00 P1200 (600) O :00 Polishing SIGMA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :00 ( 10sec)* Etching (chem.) Nital 0:03-0:10 * Rinsing with water can cause corrosion
9 Preparation 9 Soft to medium-hard steel (<35 HRC/350HV) Cut-off wheel: corundum, resin bond Epo black, Bakelite red/black KEM 15 plus P320 (280) O Until plane Pre- BETA Dia Complete Poly, 9µm :00 Polishing SIGMA/GAMMA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :00 ( Etching (chem.) Nital (micro) Adler s reagent (macro)* 0:03 0:03 * For weld analysis
10 10 Preparation Medium-hard to hard steel (35-65 HRC/850HV) Cut-off wheel: corundum, resin bond Epo black KEM 15 plus GALAXY red O Until plane Pre- BETA Dia Complete Poly, 9µm :00 IOTA Dia Complete :00
11 Preparation 11 Stainless steel (austenitic/ferritic) Cut-off wheel: corundum, resin bond Epo black, Bakelite red/black KEM 15 plus P320 (280) O Until plane Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 Polishing GAMMA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :00 ( Etching (chem.) V2A reagent 0:05-0:30
12 12 Preparation Steel and welded steel (macro) Cut-off wheel: corundum, resin bond Epo black, Bakelite red/black KEM 15 plus P180 (180) O Until plane P320 (280) O :00 Etching (chem.) Adler s reagent (macro) 0:03-0:10
13 Preparation 13 Nitrided steel Cut-off wheel: corundum, resin bond Epo black** KEM 15 plus GALAXY green O Until plane Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 Polishing GAMMA/DELTA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :00 ( ** Before hot mounting the specimen should be wrapped in aluminum foil to stabilize the nitrided layer
14 14 Preparation Ceramics Cut-off wheel: diamond, metal bond (bronze) Vacuum KEM 90 (porous material) KEM 35 (high-density, solid material) GALAXY red O Until plane GALAXY blue O :00 Pre- BETA Dia Complete Poly, 9µm + diamond paste :00 GAMMA Dia Complete + diamond paste :00
15 Preparation 15 Cobalt based alloy Cut-off wheel: corundum, resin or rubber bond Epo black KEM 15 plus P320 (280) O Until plane Pre- BETA Dia Complete Poly, 9µm :00 Polishing GAMMA Dia Complete :00 Polishing ZETA/IOTA Dia Complete Poly, 1µm :00 LAMBDA/OMEGA Eposal 0.06µm :00 (
16 16 Preparation Nickel based alloy Cut-off wheel: corundum, resin or rubber bond Epo black KEM 15 plus GALAXY green O Until plane Pre- BETA Dia Complete Poly, 9µm :00 Polishing GAMMA Dia Complete :00 LAMBDA/OMEGA Eposal 0.06µm :30-2:00 (
17 Preparation 17 Spray coatings (metallic, ceramic) Cut-off wheel: diamond, resin bond Vacuum KEM 90 P180 (180) O Until plane P320 (280) O :30 Pre- ALPHA/BETA Dia Complete Poly, 9µm :00-8:00** Polishing GAMMA Dia Complete :00-8:00** Polishing ZETA Dia Complete Poly, 1µm :00 LAMBDA Eposal 0.06µm :30 ( ** Until constant porousity å next step
18 18 Preparation Magnesium Cut-off wheel: diamond, resin bond Bakelite red/black, Thermoplast, KEM 20 * P600 (400) O Until plane Polishing Polishing Polishing BETA SIGMA ZETA Diamond suspension (alcohol or oil based) 9µm, poly Diamond suspension (alcohol or oil based) 3µm, poly Diamond suspension (alcohol or oil based) 1µm, poly : : :00 Etching (chem.) OMEGA** Etosil E 0.06µm :00 (ethanol for last 3% nitric acid 0:03-0:10 (ethanol for * To reduce the contamination of the specimen by SiC particles, it should be coated with paraffin wax before ** Wet the cloth with ethanol before
19 Preparation 19 Printed circuit board (non assembled) Cut-off wheel: corundum, resin bond Pressure vessel KEM 20 P180 (180) P800 (500) P1200 (600) O Until plane (slightly before point of interest) O :00 (until point of interest) O :00 (until point of interest) Polishing GAMMA/DELTA Dia Complete :00 ZETA/LAMBDA Eposal 0.06µm :00 (LAMBDA: O for last
20 20 Preparation Printed circuit board (assembled) Cut-off wheel: diamond, metal bond Vacuum Pressure vessel KEM 90, KEM 20 P320 (280), GALAXY green** P600 (400), GALAXY blue** P1200 (600), GALAXY yellow** O Until plane O :00 O :00 Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 Polishing GAMMA/DELTA Dia Complete :00 ZETA/OMEGA Eposal 0.06µm :30 (LAMBDA: O for last ** For printed circuit boards with ceramic components
21 Preparation 21 Copper and copper alloy Cut-off wheel: corundum, resin bond Bakelite red/black, Thermoplast KEM 20, KEM 30 P320 (280) O Until plane ** P600 (400) O :30 ** P1200 (600) O :30 Polishing SIGMA Dia Complete :00 OMEGA Eposil F 0.1µm** :00 ( Etching (chem.) Klemm s I reagent 0:02 ** 50ml Eposil F + 1ml O 2 + 1ml NH 3
22 22 Preparation Titanium (commercial pure: grade 1-4) Cut-off wheel: corundum, resin bond Epo black KEM 20, KEM 15 plus P320 (280) O Until plane Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 LAMBDA Eposil F 0.1µm** :00 15:00* ( Etching (chem.) Kroll s reagent 0:45 * Depends on grade of titanium ** Eposil F has to be mixed with hydrogen peroxide (35%) in a ratio of 5:1 (safety advice: use personal protective equipment)
23 Preparation 23 Titanium alloy Cut-off wheel: corundum, resin bond Epo black KEM 20, KEM 15 plus P320 (280) O Until plane P600 (400) O :30 Pre- ALPHA/BETA Dia Complete Poly, 9µm :00 LAMBDA Eposil F 0.1µm** :00 10:00* ( Etching (chem.) Kroll s reagent 0:45 * Depends on the alloy ** Eposil F has to be mixed with hydrogen peroxide (35%) in a ratio of 5:1 (safety advice: use personal protective equipment)
24 2 Preparation ATM GmbH Emil-Reinert-Str Mammelzen Germany Telefon +49(0)2681/ Telefax +49(0)2681/ info@atm-m.com Internet Subject to technical modification and errors Stand 04_2018
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