Surface Coatings;

Metallographic preparation and Analysis of coatings..

29 July 2020
Dr. Mike Keeble
Americas Technology & Laboratories manager
Are the audio and
video working
OK?
 Who are we?

Buehler is a premier manufacturer of scientific equipment

Metallographic preparation
• Sectioning
• Mounting
• Grinding & Polishing

Imaging and Analysis

• Imaging software
• Image analysis suite
• Nikon microscopes

Hardness Testing
• Hardness Testing Software
• Full range of hardness testing equipment

Buehler also provides expert applications and technical support.

 Preparation outline and goals of metallography

A “True Microstructure” is defined as one without ;

General Preparation Principles
Sampling

Sectioning • Cutting, grinding and

polishing related
Mounting
deformation (A)
Grinding and
Polishing • Artificial artefacts or (B)
damage
(Etching)
• Thermal damage (C)
Image
Analysis • Relief or edge rounding
Hardness
Testing • Smear Key:
(A) Gross deformation
• Pull-outs (B) Plastic deformed layer
(C) Unaffected material

Each step is equally important! • Scratches**

 Surface Coatings; Introductions…

 Surface engineering techniques are broadly classified

as those that; Coatings that will be explored/highlighted in this session
• Alter surface without changing the substrate chemically include;
• Alter the surface by change the surface chemistry
Thermal Spray coatings
• Alter the surface through the addition of different
HVOF coatings
materials by deposition as a thin or thick layers
Plasma coatings (APS)
Flame spray
 Aim is to change surface properties without changing
or altering the bulk material property Chemical and electrochemical techniques
• To improve component lifetime by increasing oxidation, Conversion coatings
corrosion, wear, erosion and abrasion, hardness, Plating’s
conductivity… Hot dip

 These can also be classified to Organic coatings

• Tradition processes Paint and coatings on polymeric or metallic
- Organic painting, electroplating, galvanising, materials
thermal/plasma spraying, nitriding, carburising…
• Technologically advanced Physical vapor deposited coatings
- Physical and chemical vapor deposited (PVD/CVD), EBPVDs
Ion implantation, laser treatment …
What types of coatings
do you work with?
 Outline will cover

Sectioning

Mounting
Some key considerations when carrying out:

Grinding &
Polishing

Optical examination

Image Analysis
Sectioning considerations

 Equipment type
• Abrasive – larger components
• Precision cutter – Small delicate components

 Blade/Wheel type
• Abradable; Al2O3, SiC
- Alumina >ferrous SiC >non-ferrous
- Grit size bond structure – thin/thick blades
• Non-abradable; CBN, diamond
- Grain size and concentration of gains

 Operating variables
• Load / Feed rate
• Cutting modes
• Speed
• Wheel thickness

 Clamping
• Causes of blade breakages and warping

 Coolant care!
Sectioning considerations – coatings – always in tension..

Delamination, cracks
at the interface

Thermal spray
coating

Section in tension Mount before section

Sectioning considerations – coatings – adjust for MAC

 What is MAC?
• Contact between the blade and workpiece during sectioning
• Must be minimised!!

 Why?
• Increases cutting efficiency
• Increased wheel life
• Reduced heat by cooler cutting
• Consistency in wheel performance characteristics

 Wheel selection, feed and speed might be optimised but still

difficult for some materials to complete the cut
• Specimen MUST be orientated to minimise MAC. That is
sample is cut along a reduced area of contact

 Some machines offer the possibility for reduced MAC via

specimen rotation or wheel oscillation
 Outline will cover

Sectioning

Mounting
Some key considerations when carrying out:

Grinding &
Polishing

Optical examination

Image Analysis
Mounting considerations; Do you go cold or hot?

Compression (Hot) Mounting Turbine blade; 50mm Ø

280 bar (4.1 ksi) at 150-180° C (300-350° F)
• High equipment cost, Low consumable cost
• Simplicity
• Better hardness and edge retention
• Fewer H&S handling and storage concerns
• No odour
• Not suitable for pressure and heat sensitive materials
• Simultaneous production limited by press design

Castable (Cold) Mounting

30-180° C
• A viscous polymer liquid is cast in a mount shape
• Low equipment cost, High consumable cost Incorrect
• Best method for delicate & sensitive materials
• Multiple samples can be mounted
• Some require careful measurement and mixing

Correct
Mounting considerations; what should the resin do?

Specimen Pressure Hot mounting resins

damage
Temp ºC
Distortion Thermosetting
Thermoplastic
Chemicals / Etchants use
solvents IPA, Acetone
hydrocarbons
Shrinkage Specimen resin interface
Filler addition
Viscosity Low or high
Heat
Cold mounting resins
Abrasion rate Resin wear vs sample

Polishing rate Epoxies

Acrylic
Thermoplastics
Conductivity SEM
Electropolish /Etch
Others
Transparency Targeted removal
 Mounting considerations; approaches for coatings and thin layers protection

Edge protection measures Thin layered samples

• Electro/electroless deposition of Ni or
Cu
• Support strips
• Use of ceramic fillers
• Use foil around samples - hot mounting

Conductivity
Addition of;
Al/Sn
• Graphite filler
• Nickel filler

Thin layers/coated sheets

• Tapered preparation
• Multiple sheets in one mount
• Cement sheets
• Mount-section-mount option
 Mounting considerations; Hot mounting resin details…

EpoMet

Probemet

PhenoCure KonductoMet ProbeMet Diallyl

TransOptic EpoMet F/G
-Wood filled Phthalate
Long cool time -Mineral filled -Conductive for -Conductive for
under pressure -Use as a SEM SEM -Mineral or glass
-Hard mount evaluations evaluations filled Phenocure
-Softer mount backfill
-Extremely low
-Moderate - Carbon/filled E.g. edge-High
-Copper/Metal protection
hardness
-Transparent shrinkage
shrinkage media filled media -Low shrinkage
-High hardness

KonductoMet
Mounting considerations; Cold mounting resin details…

Key considerations

- Low viscosity

- Low temperature capability

- Excellent shrinkage/adhesion properties

Acrylics Epoxies - Good hardness and specimen support

- Powder/liquid -Resin/hardener
-Fast curing at high -Slow curing at lower E.g. edge protection
temperatures 90-120°C/ temperatures 30-120°C/
5-15mins. 1,5-14h.
-Optimised under -Optimised under vacuum
pressure – Preferred for composites
due to
temperature/shrinkage/ad
hesion and hardness

Epoxy + filler Acrylic

 Mounting considerations; cold mounting – vacuum or no vacuum??

Porous, Friable, cracked samples...

Without
Cycling
- 1cycle
@9:00
min

Cycling is key..
With Cycling
- 9cyles
@
1:00min

EpoxiCure 2
 Mounting considerations; Abrasion/Polishing rates…

Polishing rate; relates to how easy it is to remove

Abrasion rate; relates to how a mounted specimen is scratches – still a material removal process
abraded away (material removal) compared to the test • Polishing - carried out in an elastically soft system (on
piece a soft cloth) charged with abrasives (1 – 10µm size
• Resin shouldn’t range)
✓ restrict material removal rate from the • Classified as
specimen • High – easy to remove scratches
✓ wear faster than the specimen • Low - not easy to remove scratches
• Impacts flatness of the specimen & more on • Higher polishing rates are achieved for most resins
edge retention with polycrystalline than monocrystalline diamond
• Addition of fillers reduces the polishing rate of resins

Relief effect

Compression Castable Comp/Cast

(graphite sample)
How do you carry out
mounting your samples?
 Outline will cover

Sectioning

Mounting
Some key considerations when carrying out:

Grinding &
Polishing

Optical examination

Image Analysis
 Grinding considerations

Initial grinding
• Remove the damage resulting from sectioning
• Establish a planar surface
• Reach a specific plane close to a desired area/feature

…. use the finest practical grinding stage

The extent of sectioning damage determines the selection of the initial abrasive
size
… 180-320grit is most common

Subsequent Grinding (if needed at all)

• Sequentially lower the remaining damage.
• Retain flatness
From grinding to a following grinding step
½ x Previous particles size/double the grit nµmber
180grit → 320 → 600grit
75µm → 35µm → 15µm

Don’t over-use SiC paper!

Dress Diamond Grinding Discs and Planar Grinding Stones regularly
 SumMet guidelines… what are they?
Rate of progress
• An in-depth overview Deformation of Abrasive
of traditional & particle size
contemporary

removal
z-axis
preparation routes A

• Assessment related Residual Stuctural

subsurface damage Damage
after each step
Time

A B D
C
• Develop optimised
preparation routines.. E
D
• How about
incorporating planar C
grinding? E
How does it all relate to your preparation method?
1. Traditional preparation following
all the grit line until polishing –
more material removal

2. Traditional preparation with

reduced times – less material
1 removal
4
3. Optimal 5 step procedure
- Surface selection, times &
material specific

2
5 4. Good sectioning, wrong grit
selection for step 1

5. Excellent sectioning > less

damage to remove – straight to
3 polishing.

Which one relates to me..?

How can I change…?
Grinding to polishing considerations

From grinding to first polishing step

1/5 x Previous particles size (typically 4-6min polishing step)
280 grit (45µm) SiC → 9µm Diamond Polishing
600 grit (15µm) SiC → 3µm Diamond Polishing

From polishing to following polishing step

1/3 x Previous particles size (typically 3-5 minutes)
Polishing 9µm → 3µm → 1µm
1µm stage can be omitted for ceramic coatings

Oxide polishing
0.02 – 0.06µm size particles
Alµmina or Silica?
 Factors affecting grinding/polishing efficiency; platen speeds and applied force
Ideal platen speeds??
Al Specimens - 9µm diamond, 5lb(22N) All Buehler methods default to 32mm/1.25" specimens
40 Force selection
11
 Starting point
35
• 5 lb

Removal rate (µm/min)

10
30 • Increase in force
Removal rate (µm/min)

9
25 UltraPol mean higher
HerculesH 8 material removal
20
UltraPad 7 • Also high
15
6 chance of
10
5
subsurface
5
0 5 10 15 20 25 damage for
Load (lb) coarser
0 abrasives
0 100 200 300 400 500
RPM

 Adjust based
Platen rotation speed on:
- Similar observations for steels • Surface area –
- Higher speeds – centrifugal force cause lubricant/suspension based on
off the platen sample size;
Guide: 25mm, 30mm…
- For polishing on cloths • Material type
➢ 100 – 200rpm
- For grinding with fixed abrasives
➢ 200 – 300rpm
Making it easy for you....
 Factors affecting grinding/polishing efficiency; lubricant amount and cloth surface selection

Same surface different dispense rates

30

25

20
Additional factors
µm/min

.33 ml/min
15
1.83 ml/min
- Used cloth
13.83 ml/min - Platen diameter 200-300mm
10 - Platen speed 150 – 300 rpm
- Pressure
5 - Amount of samples

0
Microcloth TexMet C Ultrapad Hercules S Hercules H
 Factors affecting grinding/polishing efficiency; combination of factors

Direction Effect of different parameters – e.g. Al 7xxx

80%

70%

Increase in Removal Rate (%)

60%

50%

40%

Contra Comp 30%

• Minimise contamination during polishing?
20%
• Gentle action on coating?
10%

0%

Central or Single force – Flatness? 1

Force RPM Direction Volume of Abrasive Surface Selection

Increase in material removal rate

- Surface selection is key and different parameters will vary depending on the
material type
- Increase in material removal is not necessarily related to melting point/hardness of
alloy
Cold mounted samples can be a challenge
- Gold low polishing rate, Al/Brasses – high polishing rates
- Hard alloys can have high polishing rates, whereas pure metals can have low
polishing rates
What issues do you have most
difficulty resolving?
Applications; Thermal coatings – APS and EBPVD coatings

Aluminised

Delamination Thermal spray coatings pose various challenges during

metallographic preparation as highlighted

Pull Outs • These are related to the type of coating being

Platinum Platinum/aluminised
investigated, where different damage types may
occur:
Smearing ➢ metallic
➢ ceramic
➢ metallic/ceramic
Edge
rounding • For Metallic type coatings, conventional methods
are typically sufficient, however, coating damage can
False porosity occur during sectioning and/or coarse grinding PVD coated

• For ceramic type coatings preparation can be EB-PVD coated

Feature relatively straight forward as long as concerns
breaks relating to porosity, cracks
Applications; Thermal spray coatings – Metallic coatings

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 40mm) (min:sec) (rpm) (rpm) Rotation Dosing
20thou
1 PlanarMet 300 120 Water 35N Fixed 120rpm Comp -/-
(0.5mm)

2 SiC Paper/DGD’s 280/320grit Water 35N 00:40 200rpm 60rpm Comp -/-

3 UltraPad 9µm Metadi Supreme MetaDi 35N 5:00 150rpm 60rpm Contra 3

4 VerduTex 3µm Metadi Supreme MetaDi 35N 4:00 150rpm 60rpm Comp 3

MasterMet**
5 ChemoMet Water 30N 2:00 150rpm 60rpm Contra -/-
Colloidal Silica

** - last 15 second run water only to aid with cleaning

In central force mode; the total force should be a multiple of sample and force per specimen (6 X 35 = 210N)

Notes
• Step 1; to remove 20thou (0.5mm) and depending on number of samples – takes 2-3minutes max.
• Step 2; should be done twice for 30-40 seconds
• Step 3; UltraPad, a hard napped surface with 9µm polycrystalline suspension
• Step 4; VerduTex, a medium hard woven surface with 3µm polycrystalline suspension
• Step 5; ChemoMet, a porous soft surface for final stage using oxide polishing suspension – MasterMet (silica)
Applications; Thermal spray coatings – Ceramic coatings

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 40mm) (min:sec) (rpm) (rpm) Rotation Dosing
20thou
1 PlanarMet 300 120 Water 35N Fixed 120rpm Comp -/-
(0.5mm)

2 SiC Paper/DGDs 280/320grit Water 30N 00:40 250rpm 60rpm Comp -/-

9µm Metadi
3 UltraPad MetaDi 30N 5:00 150rpm 60rpm Contra 3
Supreme

3µm Metadi
4 VerduTex MetaDi 30N 4:00 150rpm 60rpm Comp 3
Supreme

MasterMet**
5 ChemoMet Water 25N 2:00 150rpm 60rpm Contra -/-
Colloidal Silica
** - last 15 second run water only to aid with cleaning
In central force mode; the total force should be a multiple of sample and force per specimen (6 X 35 = 210N). Also check force sample size
relation chart

Notes
• Step 1; to remove 20thou (0.5mm) and depending on number of samples – takes 2-3minutes max.
- If damage from planar grinding, use Diamond Grinding Discs to replace Step 1 and 2
• Step 2; should be done twice for 30-40 seconds
• Step 3; UltraPad, a hard napped surface with 9µm polycrystalline suspension
• Step 4; VerduTex, a medium hard woven surface with 3µm polycrystalline suspension
• Step 5; ChemoMet, a porous soft surface for final stage using oxide polishing suspension – MasterMet (silica)
Applications; Thermal spray coatings – porosity development

Metallic Ceramic

9 25
Pull outs
8 Pull outs
7 20

Porosity in Area %
Go to next polishing step
6
15
5
4
Smearing Edge rounding 10
3 Edge rounding
2 5
Go to next polishing step
1
0 0
0 5 10 15 20 0 5 10 15 20
Polishing progress (min.) Polishing progress (min.)
 Same coating – Why consulting with us would help with being optimal in preparation...

1 2 3

35µm DGD 35µm DGD 35µm DGD

9µm UltraPad 9µm UltraPad 8µm DGD
3µm Trident 3µm Trident 3µm Trident
1µm Trident 1µm Trident 1µm Trident
0.05µm ChemoMet

Note: Polishing was done for short period (<6min).

– Aim is to see effect of surface selection on porosity and feature evaluation
Platen speed 150rpm – step 3/4 Platen speed 100rpm – step 3/4

4 5
35µm DGD
Recommended
35µm DGD practice:
8µm DGD 8µm DGD
3µm PoliCloth 3µm PoliCloth - For porosity
1µm PoliCloth 1µm PoliCloth assessment a final
polish with 0.05µm
 Customer requirement was; flatness, visibility of bond coating, porosity check

30µm - Hercules 9µm-Utrapad 3µm-VerduTex 1µm-VerduTex 0.05µm-ChemoMet

As-received sample
- Edge rounding
- Heavy scratches
- Relief polishing
Final polish
Hard coatings – Change of a surface and related damage

Al Key
- Aluminide
(Al/Pt)
coatings are
prone to
cracking
DGD UltraPad 3µm 0.05µm during coarse
PtAl grinding and/or
initial
sectioning

DGD Hercules H 3µm 0.05µm Pt

Showing damage
attributed to coarse
surface at 9um
Surface selection impact on coating integrity - EBPVD coatings
P180 P400 9µm 3µm 1µm 0.05µm

➢ EBPVD 7YSZ
TBC with
(Ni/Pt)Al bond
coats

Key to
preparation
- No damage to
columnar
structure
- Check the tips
if cracked) and
gaps between
the columnar
structure
Ex- service thermal spray coating - EBPVD 7YSZ coating
Component sectioning As sectioned vane guide
Cracks observed in the bond coat,
are they due to preparation???

Undamaged Damaged Ex-service

Method changed to use SiC paper to P1200 and a 3µm recovery Yes; aggressive second step after
initial grind
Surface selection impact on coating integrity – Bond coat + APS YSZ + EBPVD YSZ coating

What do
you see?

As received sample Re-prepared sample

P320 9µm - UltraPad 3µm - Trident 1µm - Trident 0.05µm - ChemoMet

 How about traditional SiC vs DGD?…

Tests done up to 3µm finish…

Traditional preparation
can be long and with
considerable SiC paper
waste
P180 + P240 + P400 +9µm UltraPad + 3µm Trident Solution:
- Use DGD’s
- Will require 1 or 2
recovery SiC steps.
depends on coating
type

DGDs (75 or 55µm) + P240 + P400 +9µm UltraPad + 3µm Trident

Approximately how often do you
have to repeat your preparation
routine?
Applications; Bearing alloy coatings

Bearing materials are made from a variety of

Edge metals Consideration during:
rounding • Metallographic preparation need to be 1. Sectioning
varied for different materials - Avoid excessive heat, sufficient
coolant to cutting point
2. Mounting
Pull outs • Most materials are bonded to steel or other - Cold mounting preferred due to
(harder) backing compared to the bearing the use of white metals as part of
coatings materials the coating materials
Embedding - Mount materials of similar group
to minimize electrochemical action
(pick-up) • Bearing materials are often at least a two-
3. Grinding
phase coating system - Start with as finest grit as you can
possibly start, if damage is less
Smearing • The two phases consists of from prior steps
- Use progressively finer SiC
- A soft low melting point matrix or papers
- A soft low melting point second phase 4. Polishing
Local
- Use cloth with low nap for initial polishing
anodic
corrosion • Thicknesses after final grinding

- Bearing linings can also be quite thin

<2µm (requires excellent preparation to
observe detail)
Soft coating – Bearing coatings
Steel +2µm Ni + 300µm Cu/Pb + 25µm Sn/Cu

 Multilayer profiles
• 2 – 5 layers are
typically applied

 Mix of soft and hard

phases
Steel +2µm Ni + 300µm Cu/Pb + 25µm Sn/Ni • Pick-up on Pb
observed
• Pull-outs

 Thin layers
• Edge retention is
key

Steel +2µm Ni + 300µm Al/Sn + 2µm Ag + 3µm Bi

Applications; Bearing alloys

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 30mm) (min:sec) (rpm) (rpm) Rotation Dosing
DGD Yellow
1 35µm Water 20N 00:40 250rpm 60rpm Comp -/-
SiC P320 /P400

2 PoliCloth 9µm Metadi Supreme Water 20N 4:00 150rpm 60rpm Comp -/-

3 Trident 3µm Metadi Supreme Water 20N 4:00 150rpm 60rpm Comp -/-

4 Trident 1µm Metadi Supreme MetaDi 20N 4:00 150rpm 60rpm Comp 3

MasterMet**
5 ChemoMet Water 20N 2:00 100rpm 60rpm Contra -/-
Colloidal Silica

** - last 15 second run water only to aid with cleaning

In central force mode; the total force should be a multiple of sample and force per specimen (6 X 20 = 120N)

Notes
• Step 1; to remove sectioning damage using fixed abrasives – diamond grinding disc
• Step 2; UltraPad, a hard napped surface with 9µm polycrystalline suspension
• Step 3; Trident, a medium hard woven surface with 3µm polycrystalline suspension
• Step 4; Trident, a medium hard woven surface with 3µm polycrystalline suspension
• Step 5; ChemoMet, a porous soft surface for final stage using oxide polishing suspension – MasterMet (silica)
Applications; Bearing alloys

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 30mm) (min:sec) (rpm) (rpm) Rotation Dosing

1 SiC Paper P320grit Water 20N 00:40 200rpm 60rpm Comp -/-

2 SiC Paper P600grit Water 20N 00:40 200rpm 60rpm Comp -/-

3 SiC Paper P1200grit Water 20N 00:40 200rpm 60rpm Comp -/-

4 PoliCloth 3µm Metadi Supreme MetaDi 25N 4:00 150rpm 60rpm Comp 3

MasterMet**
5 ChemoMet Water 20N 2:00 100rpm 60rpm Contra -/-
Colloidal Silica

** - last 15 second run water only to aid with cleaning

In central force mode; the total force should be a multiple of sample and force per specimen (6 X 20 = 120N)

Notes
• Step 1; to remove sectioning damage.
• Step 2/3; removal of damage from step 1 but also present surface ideal for polishing stage
• Step 4; Policloth, a medium hard woven surface with 3µm polycrystalline suspension
• Step 5; ChemoMet, a porous soft surface for final stage using oxide polishing suspension – MasterMet (silica)
 Soft coating – Bearing coatings – Behaviour of different coatings

A
Two different
coating using
same procedure
- Both showing
good preparation
DGD 35µm 9µm - UltraPad 3µm- Trident 1µm - Trident 0.05µm - ChemoMet - (A) – show pick
up/ and pull-out
B within the Cu/Pb
layer

P600 9µm - PoliCloth 3µm -Trident 1µm - Trident 0.05µm - ChemoMet New routine
- Target Cu/Pb
layer + metallic
organic coating
- Use SiC with
finest grit
possible till
planar
Applications; Electroplated coatings + Organic coatings

Selective Consideration during:

etching 1. Sectioning
- Avoid excessive heat and pressure, sufficient coolant
to cutting point

Embedding 2. Mounting
- Cold mounting should be used on organic coatings
- Cold or hot mounting can be used for electroplated
coatings

Smearing 3. Grinding
- Start with the finest grit as you can start if damage is
less from prior steps
- Use progressively finer SiC papers

Edge
4. Polishing
rounding - Use cloth with low nap for initial polishing after final
grinding
 Applications; Galvanised coatings

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 30mm) (min:sec) (rpm) (rpm) Rotation Dosing

1 SiC Paper P320 grit Water 25N 00:40 200rpm 60rpm Comp -/-

2 SiC Paper P600 grit Water 25N 00:40 200rpm 60rpm Comp -/-

2 SiC Paper P1200 grit Water 25N 00:40 200rpm 60rpm Comp -/-

4 PoliCloth 3µm Metadi Supreme MetaDi 25N 4:00 150rpm 60rpm Comp 3

5 ChemoMet MasterPrep Water 25N 2:00 150rpm 60rpm Contra -/-

Notes
• Step 1; to planarise the surface
• Step 2; SiC step to prepare surface for first polishing stage
• Step 3; PoliCloth, a mediµm hard woven wool surface with 3µm polycrystalline suspension
• Step 5; ChemoMet, a porous soft surface for final stage using oxide polishing suspension –
MasterPrep (alumina)
 Applications; non-aqueous preparations

Force
(Per Platen Head
Step Lubricant/ Specimen – Time Speed Speed Relative Burst
No. Surface Abrasive Extender 40mm) (min:sec) (rpm) (rpm) Rotation Dosing
1 SiC Paper P320/P600 grit Water 35N 00:50 200rpm 60rpm Comp -/-

2 UltraPad 9µm oil based -/- 35N 04:00 200rpm 60rpm Comp -/-

3 Trident 3µm oil based -/- 35N 03:00 200rpm 60rpm Comp -/-

4 Trident 1µm oil based -/- 35N 2:00 150rpm 60rpm Comp 3

5 ChemoMet Micropolish + glycol -/- 30N 2:00 150rpm 60rpm Contra -/-

Notes
• Step 1; to planarise the surface – can be done atleast twice
• Step 2; UltraPad, a hard napped surface with 9µm diamond suspension (or paste)
• Step 3; Trident, a mediµm hard woven surface with 3µm diamond suspension (or paste)
• Step 4; Trident, a mediµm hard woven surface with 1µm diamond suspension (or paste)
• Step 5; Optional ChemoMet, a porous soft surface for final stage using oxide polishing suspension
Galvanised steel – Zinc coating

P240 P600 P1200 3µm PoliCloth 0.05µm MasterMet

Key
• Edge rounding
• Zn sensitivity to water
• Localised etching due to reaction of zinc with
aqueous final polishing compound
• Use non-aqueous polishing suspension such
as MasterPolish
Oil based preparation; Galvannealed zinc coating
P400 9µm oil 3µm oil 1µm oil

1µm polish
Sample re-prepared using aqueous based – with addition 0.05µm masterprep

After etching with Nital

1% for <3 seconds
 Surface coatings; electroplated with cadmium + organic coating + metallic top coat

Request was to have both the

steel, plating, coating and top
coat visible.

Procedure used
Steps:
1. P320 SiC – till planar
2. UltraPad 9µm
3. Microfloc 3µm
High strength steel with cadmium plating, organic coating with a metallic top coat 4. TexMet C 1µm
5. ChemoMet 0.06

Surface selection key to having

all the phases prepared and as
flat as possible

High strength steel with cadmium plating, organic coating without a metallic top coat
 Tolerance wear coatings

Force
(Per Time Platen Head
Step Lubricant/ Specimen (min:sec Speed Speed Relative
No. Surface Abrasive Extender – 40mm) ) (rpm) (rpm) Rotation

1 DGD Red 75µm - Water 30N 00:40 200rpm 60rpm Comp

DGD Yellow
2 - Water 30N 00:40 200rpm 60rpm Comp
35µm

9µm Metadi
3 UltraPad MetaDi 30N 5:00 150rpm 60rpm Comp
Supreme

4 Trident 3µm Metadi MetaDi 30N 4:00 150rpm 60rpm Comp

5 ChemoMet MasterMet Water 30N 2:00 150rpm 60rpm Contra

Challenges
- Edge rounding
- Abrasive (CBN) particle pull out
What types of analysis
do you carry out?
 Sectioning

Mounting

Grinding & Polishing

Optical examination

Micro-hardness
testing (optional)

Etching (optional)

Image Analysis
 Analysis requirements

 Coating thickness assessment - Good preparation helps – Auto thresholding for different coatings.

Single coating Multiple coatings

Note:
➢ Analysis on either horizontal or vertical coating configuration
➢ Program can be made for single coating or multi-layered configurations
➢ Single click or interactive
 Analysis requirements

 Porosity measurement – how about automating the process

Ceramic
coating

Note:
Metallic Analysis by a single click – Play
coating Or it can be set to be interactive for more user control
➢ Set the regions of interest with new field of view
➢ Adjust threshold if all features are not captured
Analysis requirements; impurities, pores, unmelted particles….

Pull out or embedment Diffusion zone, second phase

particles…

Impurities

pores, splats

Unmelted particles

 There are many feature of interest in coatings

Thank you !

August webinar – Focus on indentation

hardness testing of materials

Website – www.buehler.com
•​ Technical updates​
• Buehler’s Guide to Materials Preparation
• Tech Notes​
• Sum Notes​

Email -
- lab.eu@buehler.com
- lab.us@buehler.com

• Ask a specific question directly to Buehler’s

lab personnel​

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