Electropolishing Recipes

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Material Composition Solution Conditions Comment
Ag
pure
Sulfuric 6%; Acetic 6%; Methanol 88%; Thiorea Cyanide Solution 12 gms
25C, 10V, 18mA
Slightly etched
Al
Alloy 1100
Perchloric 93%; Sulfuric 6%; Hydrofluoric 1%
-25C, 15V
Must keep below -25C
Al
Alloy 1100
Nitric 10%; Methanol 90%
-10C, 10V, 200mA
 
Al
Alloy 2024
Nitric 10%; Methanol 90%
-10C, 10V, 200mA
 
Al
Alloy 5052
Nitric 10%; Methanol 90%
-10C, 10V, 200mA
 
Al
Alloy 6061
Nitric 10%; Methanol 90%
-10C, 10V, 200mA
 
Al
powder
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
8C, 30V, 50mA
 
Al
pure
Perchloric 10%; Ethanol 90%
0C, 7V, 80mA
Excellent result, retains precipitates
Al
 
Nitric 20-25%; Methanol 75-80%
 
Add LN2 to electrolyte until ice forms. Begin polishing as soon as it reliquefies.
Al Ag
Ag 5-25%
Nitric 33%; Methanol 67%
-30C, 8V, 40mA
 
Al Be
As Cast 50%
Nitric 10%; Methanol 90%
-15C, 10V, 200mA
 
Al Be
As Cast 90%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 35V
 
Al Be
Be 0.5-30%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 17V, 100mA
For higher Be concentrations, use higher voltage.
Al Be Ti
Be 1-30%, Ti 1-10%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 20V, 80mA
 
Al Be Ti
Be 7%, Ti 2%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 50V, 80mA
 
Al Cu
Cu 4%
Nitric 33%; Methanol 67%
-30C, 9V, 10mA
Very good result
Al Cu
Cu 4%
Sulfuric 20%; Methanol 80%
5C, 40V, 50mA
Excellent result
Al Cu
 
Nitric 33%; Methanol 67%
-30C to -50C
 
Al Cu Ti
Alloy 2000 series
Nitric 25%; Methanol 75%; Hydrofluoric (1-5 drops)
-20C
If oxide film is present, it may be removed by dipping specimen in solution of 16 grams Chromic Acid,  35 cc Phosphoric Acid, 65 cc Distilled H20 for 5 to 10 minutes at room temperature.
Al Cu Ti
Alloy 2219
Perchloric 20%; Ethanol 80%
-30C, 35V, 100mA
Fast electrolyte flow needed. Sample must be removed from holder as quickly as possible and rinsed in three beakers of ethanol to prevent oxide film.
Al Ge
 
Perchloric 10%; Glycerol 20%; Methanol 70%
-10C, 18V, 60mA
 
Al Li
Li 2-3%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 15V, 40mA
 
Al Mg
Mg 3%
Perchloric 10%; Butoxyethanol 20%; Methanol 70%
   
Al Mn
Mn 3-25%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 25V, 125mA
Very brittle, good polish
Al Mn S
Mn 33%, S 3%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
8C, 25V, 125mA
Very brittle, good polish
Al Ni
Ni 20-80%
Perchloric 5%; Butoxyethanol 20%; Methanol 75%
5C, 37V, 50mA
Very good, small change in voltage with composition.
Al Si
Si 0.2%
Nitric 33%; Methanol 67%
-22C, 12.5V, 30mA
 
Al Si
Si 6%
Nitric 33%; Methanol 67%
-5C, 20V, 200mA
 
Al Ti
Ti 30-50%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 55V, 40mA
 
Al Ti
Ti 50%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 25V, 40mA
Very good
Au Fe
Fe 25%
Hydrochloric 6%; Sulfuric 6%; H20 88%
25C, 10V, 60mA
 
Be
pure
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 30V, 40mA
Slight etch with respect to orientation
Be Ti
Ti 12%
Sulfuric 20%; Methanol 80%
-10C, 25V, 60mA
 
Be Ti
Ti 2%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 55V 40mA
 
Be V
V 50%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 55V, 40mA
 
Bi2Te3   Tartaric 2%; Sodium Hydroxide 9%; H2O 89%    
Cd
 
Nitric 33%; Methanol 67%
-30C, 7v, 180 mA
 
Co
various alloys
Perchloric 20%; Acetic 80%
   
Co Fe
Fe 5-8%
Perchloric 25%; Acetic 75%
25C, 20V, 80mA
 
Co Ni
 
Perchloric 25%; Acetic 75%
-30C, 25V
 
Co Ni
 
Perchloric 10%; Acetic 90%
80V
 
Cu
pure
Nitric 10%; Methanol 90%
-18C, 20V, 40mA
 
Cu
various alloys
Phosphoric 30%; H2O 70%
 
Increase voltage until bubbles form on specimen surface, then reduce voltage until bubbles just disappear.
Cu
 
Nitric 33%; Methanol 67%
-30C to -50C
 
Cu Au
Au 50%
Nitric 30%; Methanol 70%
-25C, 20V
 
Cu Be
Be 10%
Nitric 10%; Methanol 90%
-15C, 55V, 80mA
 
Cu Be
 
Nitric 33%; Methanol 67%
-30C to -50C
 
Cu Be Co
 
Nitric 33%; Methanol 67%
-50C, 65mA
Fast electrolyte flow needed. Rinse in methanol. Surface may oxidize rapidly.
Cu Cr
Cr 3.8%
Nitric 10%; Methanol 90%
0C, 35V, >100mA
Good result, slight etching at the grain boundaries.
Cu CuO
CuO <5%
Nitric 33%; Methanol 67%
-35C, <8V, 200mA
 
Cu Fe
Fe 30%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
-20C, 25V
 
Cu Ni Sn
Single Crystal
Nitric 10%; Methanol 90%
-10C, 20V, 45mA
 
Cu Ni Sn
Spinodal
Nitric 33%; Methanol 67%
-30C, 20V, 80mA
 
Cu Pd
Pd 30-50%
Perchloric 5%; Butoxyethanol 35%; Methanol 60%
0C, 40V, 200mA
 
Cu Si
 
Nitric 33%; Methanol 67%
-50C, 65mA
Fast electrolyte flow needed. Rinse in methanol. Surface may oxidize rapidly.
Cu Ti
Ti 1.6%
Nitric 15%; Methanol 85%
   
Cu Ti
 
Nitric 33%; Methanol 67%
-30C to -50C
 
Discaloy
gamma
Perchloric 20%; Acetic 80%
25C, 5V, 30-45mA
Use low electrolyte flow
Discaloy
 
Perchloric 20%; Methanol 80%
-30C, 5V, 30-45mA
Use low electrolyte flow
Fe
pure
Perchloric 10%; Acetic 90%
15C, 30V, 30mA
 
Fe various alloys Perchloric 10%; Acetic 90%    
Fe   Chromic 50%; Acetic 50% 27V  
Fe AI C
 
Perchloric 5%; Butoxyethanol 35%; Methanol 60%
-20C, 15V
 
Fe AI O
Al <1%; O <1%
Perchloric 10%; Acetic 90%
20C, 35-40V, 30mA
Good result
Fe Al
 
Nitric 33%; Methanol 67%
-30C to -50C
 
Fe Be
Be 25%
Perchloric 5%; Butoxyethanol 35%; Methanol 60%
10C, 15V
 
Fe C
C <1%
Nitric 33%; Methanol 67%
-10C, 10V
 
Fe Cr
Cr 40%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 30V, 65mA
 
Fe Cr
Cr 46%
Perchloric 10%; Acetic 90%
0C, 30V
 
Fe Cu
Cu 0.3%
Perchloric 33%; Acetic 33%; Butoxyethanol 34%
   
Fe MnS
MnS 2-5%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
10C, 20-30V, 200mA
 
Fe Ni
Ni 35%
Perchloric 10%; Methanol 90%
15C, 25V, 80mA
Slightly etched
Fe Pd
Pd 15-70%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
5C, 30V, 15mA
 
Fe Si
Si 3%
Nitric 80%; Methanol 20%
-35C, 20V, 50-60mA
Large thin areas.  Sample must be removed from holder as quickly as possible and rinsed in three beakers of ethanol to prevent oxide film.
Fe Si
Si 3%
Sulfuric 80%; Methanol 20%
-35C, 20V, 50-60mA
Large thin areas.  Sample must be removed from holder as quickly as possible and rinsed in three beakers of ethanol to prevent oxide film.
Fe Si O
Si <1%; O <1%
Perchloric 10%; Acetic 90%
20C, 35-40V, 30mA
Good result
FV 535
 
Perchloric 20%; Methanol 80%
-20C, 30mA
Use low to moderate electrolyte flow
Glass
 
Hydrofluoric 90%; Hydrochloric 10%
 
Chemical Polish Only
Inconel
Alloy 600
Perchloric 20%; Methanol 80%
-40C, 15-20V, 80-90mA
Use low to moderate electrolyte flow
Inconel
Alloy 690
Perchloric 20%; Methanol 80%
-40C, 40V, 150mA
Fast electrolyte flow needed
Inconel
Alloy 706 (cold worked)
Perchloric 20%; Methanol 80%
-40C, 150V, 90-100mA
Fast electrolyte flow needed
Mar M 509
 
Nitric 4%; Isobutanol 48%; Methanol 48%; Zinc Chloride 40 gms
-40C, 150V, 25-60mA
Fast electrolyte flow needed
Mg
 
Nitric 10%; Methanol 90%
20V
 
Mo
 
Sulfuric 13%; Methanol 87%
-40C, 80-100mA
 
Mo
 
Sulfuric 80%; Hydrofluoric 20%
   
Mo C
C <1%
Sulfuric 5%; Glycerol 30%; Methanol 65%
-30C, 35V, 65mA
 
Mo Hf N
 
Sulfuric 20%; Methanol 80%
25C, 17V, 95mA
Dip in phosphoric after polishing
Mo Hf N
 
Perchloric 5%, Butoxyethanol 15%; Methanol 80%
0C, 105V, 90mA
Slightly etched
Mo Hf N
 
Sulfuric 20%; Methanol 80%
25C, 70V, >100 mA
Good result, Fast electrolyte flow needed
Monel
 
Nitric 37%; Methanol 63%
-40C, 40-50V, 60mA
Fast electrolyte flow needed
Nb
pure
Hydrofluoric 1%; Sulfuric 6%; Methanol 93%
-40C, 40V, 40mA
Slightly etched
Nb
various alloys
Hydrofluoric 1%; Sulfuric 2%; Methanol 97%
-50C
 
Nb
 
Saturated Solution of Ammonium Fluoride in Methanol 13%; Methanol 87%
-30C, 150V
Thins at a rate of 5 microns/minute. Maintaining temperature is critical.
Ni
pure
Perchloric 20%; Acetic 80%
   
Ni Al
Al 50%
Perchloric 3%; Butoxyethanol 32%; Methanol 65%
0C, 35V, 50mA
Excellent result
Ni Al
 
Perchloric 10%; Methanol 90%
-45C, 18V, 70mA
 
Ni Cr
Cr 33%
Perchloric 10%; Acetic 90%
10C, 55V, 65mA
 
Ni Mo   Nitric 33%; Methanol 67% -30C to -50C  
Ni Nb
Nb 40%
Perchloric 10%; Ethanol 90%
8C, 35-40V
 
Ni V
V 2%
Perchloric 10%; Acetic 90%
10C, 55V, 60mA
 
Pd
pure
Perchloric 16%; Acetic 42%; Butoxyethanol 42%
-10C, 25-30V
Deforms easily
Pd Ni
Ni 20-50%
Perchloric 16%; Acetic 42%; Butoxyethanol 42%
-10C, 25-30V
 
Pt
pure
Saturated Solution of Calcium Chloride in H20
25C, 35V
 
Pt C
C <1%
Saturated Solution of Calcium Chloride in H20
25C, 20V
 
Pt Ga
Ga 4%
Saturated Solution of Calcium Chloride in H20
25C, 20V
 
Si
 
Hydrofluoric 91%; H20 9%; Potassium Permanganate 10.5 gms
-25C
Fast electrolyte flow needed
Si Cu
Alloy 2124
Nitric 25%; Methanol 75%
-30C
 
Stainless Steel
Alloy 302
Perchloric 10%; Ethanol 90%
-25C, 25V, 10 mA
 
Stainless Steel
Alloy 303
Perchloric 5%; Acetic 95%
15C, 30V, 80mA
 
Stainless Steel
Alloy 304
Perchloric 20%; Acetic 80%
25C, 10-15V, 60-90mA
Use low electrolyte flow
Stainless Steel
Alloy 308
Perchloric 20%; Acetic 80%
25C, 10-15V, 60-90mA
Use low electrolyte flow
Stainless Steel
Alloy 310
Perchloric 5%; Acetic 95%
25C, 35V, 80mA
 
Stainless Steel
Alloy 420
Sulfuric 40%; Phosphoric 60%
60C, 10V
 
Stainless Steel
Alloy 420
Perchloric 15%; Ethanol 85%
25C, 18V
 
Stainless Steel   Sulfuric 40%; Phosphoric 60%    
Steel
Low Carbon
Glacial Acetic 500 ml; Anhydrous Sodium Chromate 100 gms
   
Ta
pure
Hydrofluoric 3%; Sulfuric 10%; Methanol 87%
-25C, 35V, 80mA
Slightly etched
Ta lr
Ta 50%
Saturated Solution of Calcium Chloride in H20
25C, 20V, 200mA
Good result
Ti
various alloys
Perchloric 6%; Butoxyethanol 35%; Methanol 59%
-30C
 
Ti
 
Perchloric 6%; Butoxyethanol 35%; Methanol 59%
   
Ti
 
Sulfuric 3%; Hydrochloric 3%; Methanol 94%
-30C
 
Ti Al
 
Perchloric 5%, Butoxyethanol 15%; Methanol 80%
5C, 35V, 30mA
Slightly etched at grain boundaries
Ti Al
 
Perchloric 20%; Methanol 80%
-30C, 55V, 35-45mA
Fast electrolyte flow needed
Ti Al
 
Sulfuric 5%; Methanol 95%
-30C, 55V, 35-45mA
Fast electrolyte flow needed
Ti Al Be
 
Perchloric 5%, Butoxyethanol 15%; Methanol 80%
0C, 30V, 30mA
 
Ti Al Nb
 
Hydrofluoric 1%; Sulfuric 5%; Methanol 94%
   
Ti Al Si
as cast
Sulfuric 20%; Methanol 80%
5C, 50V, 80mA
Very good result
Ti Al V
Al 6%; V4%
Perchloric 6%; Butoxyethanol 34%; Methanol 60%
-30C, 35V, 9mA
Fast electrolyte flow needed
Ti B
B 7%
Perchloric 20%; Methanol 80%
-20C, 11V, 170mA
The colder, the better
Ti Be
Be 12%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
5C, 20V, 40mA
Good result
Ti Be
Be 35%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
-10C, 15V, 30mA
 
Ti C
C 1.5%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
25C, 11V, 150mA
 
Ti Fe
Fe 25-30%
Perchloric 8%; Butoxyethanol 10%; Methanol 70%; H20 12%
10C, 12V, 120mA
 
Ti Ge
 
Hydrochloric 3%; Sulfuric 3%; Methanol 94%
-30C
 
Ti Mo
Mo 10%
Sulfuric 10%; Methanol 90%
-18C, 32V, 90mA
 
Ti Nb Mo Si
 
Sulfuric 10%; Methanol 90%
10C, 10V, 500mA
 
Ti Ni Fe
Fe 1%
Sulfuric 10%; Methanol 90%
-15C, 10V
 
Ti Ni Fe
Ti 50%
Sulfuric 10%; Hydrofluoric 5%; Methanol 85%
20-25V
Slightly etched
Ti V
V 10%
Sulfuric 10%; Methanol 90%
-18C, 33V, 80mA
 
Ti V Be
Be 10%; V 40%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
-10C, 70-85V, 50mA
 
U
pure
Sulfuric 20%; Methanol 80%
0C, 45V
 
Udimet
Alloys 710-720
Perchloric 20%; Methanol 80%
-20C, 45-55V, 55-65mA
Use moderate electrolyte flow
V Be
Be 50%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
0C, 55V, 40mA
 
W
 
Sodium Hydroxide 2%; H2O 98%
 
Use low electrolyte flow
X-45
 
Nitric 4%; Isobutanol 48%; Methanol 48%; Zinc Chloride 40 gms
-40C, 150V, 25-35mA
Fast electrolyte flow needed. It takes 12 minutes to thin a 50 micron thick disk.
X-750
 
Perchloric 20%; Methanol 80%
-30C, 100mA
Fast electrolyte flow needed
Zr
 
Perchloric 20%; Methanol 80%
-40C, 35-45mA
Use moderate electrolyte flow
Zr
 
Perchloric 20%; Acetic 80%
25C, 35-45mA
Use moderate electrolyte flow
Zr
 
Perchloric 20%; Acetic 80%
   
Zr Be
Be 5%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
5C, 30V, 60mA
 
Zr Co Ni
Co 40%; Ni 10%
Perchloric 5%; Butoxyethanol 15%; Methanol 80%
-10C, 35V, 25mA
 
Zr Nb
Nb 80%
Sulfuric 10%; Methanol 90%
-5C, 25V, 85mA
Slightly etched
Zr Nb
Zr 50%; Nb 50%
Sulfuric 10%; Methanol 90%
-10C, 22V, 90mA
Good result

CAUTION: Perchloric acid can be very explosive. Only use electrolytes containing perchloric acid in a safety fume hood capable of handling perchlorics.

Selected recipes courtesy of Mark Wall - Lawrence Livermore National Laboratory, James Haugh - Westinghouse Electric Company & Mary Grace Burke - Bechtel Bettis, Inc.

For additional recipes, refer to Practical Methods in Electron Microscopy, Volume 11, Thin Foil Preparation for Electron Microscopy by Peter J. Goodhew, Elsevier Science Publishers B.V., 1985 and Transmission Electron Microscopy of Materials by Gareth Thomas and Michael J. Goringe, John Wiley & Sons, Inc., 1979

 

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