Struers Welcomes You To:

Microindentation Hardness Testing

We will begin todays session in 10 minutes

To join the audio portion, please call 1-855-299-5224

Enter the Meeting # or Access Code # 953 347 558

Struers Welcomes You To:

Microindentation Hardness Testing
We will begin todays session in 5 minutes

To join the audio portion, please call 1-855-299-5224

Enter the Meeting # or Access Code # 953 347 558

Welcome to Struers Webinar

Microindentation Hardness Testing

Presenter: George F. Vander Voort

Housekeeping Items
If you are experiencing technical difficulties, please
contact 866.347.6865.
Also, all participates will be in listen-only
mode during the webinar.

Q&A
Please feel free to submit questions using the
Q&A tool in the lower right corner of your
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questions within the one hour time frame.

Microindentation Hardness Testing

George F. Vander Voort
Consultant Struers Inc.
www.georgevandervoort.com

Historical Views of Hardness

Hardness is a hazily conceived conglomeration or
aggregate of properties of a material more or less related
to each other
L.B. Tuckerman, NBS
The hardness of metals, like the storminess of seas, is
easily appreciated but not readily measured for one would
like to express it in terms of fundamental units
Hugh ONeill
the indenter forced into that material comes to rest
when its indenting load is exactly supported by whatever it
is that resists further indentation
Charles H. Wilson
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So, What is Hardness?

Hardness is: resistance to abrasion, scratching,
cutting and plastic deformation; high modulus of
elasticity, high yield point, high strength,
brittleness, ability to cut, lack of ductility and
malleability, etc.
Resistance to Penetration
Indentation hardness: resistance of a solid body
to penetration by a second body of specified
shape and composition, and under prescribed
conditions (Peter Blau)
ASTM E7 does not define hardness!
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Microindentation Hardness Testing

The purpose of macro-load hardness testing is to
obtain a bulk, average hardness to meet a
specification for annealed or Q&T metals.
The purpose of micro-load hardness testing is to
define differences due to segregation, surface
hardening treatments or to help identify phases.
Specimen preparation for macro-loads requires a
ground surface; for micro-loads, a fully polished
surface is required and as the test force drops, all
of the preparation-induced damage must be
removed to get valid results.
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The Vickers Test

In 1925, Smith and Sandland of the UK developed a hardness test
using a square-based pyramidal shaped indenter made from
diamond to overcome the limitations of the Brinell test (developed
in 1900) that used a spherical hardened steel ball (metals harder
than about 48 HRC cannot be tested). The indenter shape chosen
produced hardness numbers similar to those obtained by the
Brinell test.
The first low-load Vickers tester was built by Lips and Sack in
1936.
HV = cL/d2 = 1854.4 L/d2
For micro-HV, c is 1854.4, L is the load in gf, and d is the mean
diagonal in m
Historically, HV units were reported as kgf/mm2, but units are no
longer used in reporting hardness numbers due to the SI system.
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Vickers Microindentation Hardness Test

Advantages:
Small specimens can be tested; indents can be placed precisely;
hardness changes can be plotted in relationship to phases, depth
or geometries; high sensitivity; one continuous scale for testing all
materials; correlates to strength and other properties
Disadvantages:
Operation requires training and skill; extensive specimen
preparation; manual operation is time consuming and arduous;
equipment is delicate and subject to environmental influences

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The Vickers Indenter

Square-Based
Diamond Pyramid
Indenter
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Measuring the Indent Diagonals

When measuring an indent,
first bring the filar lines of the
micrometer together until they
just touch; then zero the
micrometer. Then, adjust the
filar lines until the indent tips
just touch the insides of the
two lines. Then, make the
measurements of the two
diagonals, average the X and
Y values, and calculate the
hardness (or look up the
hardness in tables). Some
machines give a direct
readout of the hardness after
you measure the diagonals.
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Indent Image Contrast is Crucial!

Excellent Image Contrast

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Poor Contrast Where are

the Indent Corners?

To Etch, or Not to Etch, That is the Question!

Paragraph 7.1.1.2 of ASTM E 384-11 says: The specimen surface should not be
etched before making an indentation. But, in microindentation testing we usually
need to see the microstructure to know where to test. The answer: do not etch
deeply! As the examples above show, etching can be done.
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HV Calculated from L and the Mean d2

HV Versus Force and Diagonal
1200
1100
1000
900

Hardness, HV

The equation
relating HV to d
and L results in
very large changes
in hardness for
minor d variations
at low loads a
major problem
with the test

800

1000 gf

700
600
500

500 gf

400
300
200
100

10 gf

0
0

10

25 gf

20

100 gf

50 gf

30

40

200 gf

50

Mean Diagonal, m

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60

300 gf

70

80

Influence of 0.5 m Measurement Imprecision

Influence of 0.5 m Variation in d
HV Due to 0.5 m d

350
10 gf

300

25 gf

250

50 gf

200

100 gf

150

200 gf

100

500 gf

1000 gf

50
0
0

10

20

30

40

50

60

70

80

90

100

110

120

Mean Diagonal Length, m

Error in Vickers Hardness Due to a 0.5 m Variation in d for Metals

with a Maximum HV of 1100-1200 HV as a Function of Test Force
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The Knoop Test

In 1939, Frederick Knoop and his associates at NBS developed a
low-load test based on a rhombohedral-shaped diamond indenter.
The long axis is 7.114 times the short axis. This shape is claimed
to minimize or eliminate elastic recovery when the indenter is
withdrawn, but that does not actually occur. The Knoop indenter is
excellent for testing thin coatings and for specimens with a steep
hardness gradient.
HK = cL/d2 = 14229L/d2
The constant c is 14229, L is the load in gf and d is the long
diagonal length in m
Historically, HK units were kgf/mm2, but units are no longer used in
reporting hardness numbers due to use of the SI system.

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Knoop Microindentation Hardness Test

Advantages:
Easier to test thin coatings in cross section compared to
Vickers; indents in a traverse can be spaced closer to each other;
better for characterizing steep hardness gradients and banding
segregation than Vickers
Disadvantages:
Same as Micro Vickers; Knoop hardness does vary with test load;
more difficult to correlate HK with strength and other properties as
the load varies from 500 gf.

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The Knoop Indenter

RhombohedralShaped Diamond
Indenter

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HK Calculated from L and the Long d2

HK Versus Force and Diagonal
1200
1100
1000

Hardness, HK

The equation
relating HK to d
and L results in
large changes in
hardness for
minor d variations
at low loads a
somewhat less
serious problem
with the Knoop
test compared to
the Vickers test.

900
800
700

1000 gf

600
500

500 gf

400
300
200
100

10 gf

0
0

25

25
50

75

50
100

100 gf
125

200 gf

150

175

Long Diagonal, m

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300 gf
200

225

250

Influence of 0.5 m Measurement Imprecision

Influence of 0.5 m Variation in d
HK Due to 0.5 m d

180
10 gf

160
140

25 gf

120

50 gf

100
80

100 gf

60

200 gf

40

500 gf

20

1000 gf

0
0

25

50

75

100

125

150

175

200

Long Diagonal Length, m

Error in Knoop Hardness Due to a 0.5 m Variation in d for Metals

with a Maximum HK of 1100-1200 HK as a Function of Test Force
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The Indentation Size Effect (Vickers)

At loads of 100 gf and below, the Vickers hardness is different than
above 100 gf (this problem was claimed to not exist for MacroVickers tests, but it does). The problem was attributed to dislocation
interactions with the indenter at low test loads (forces).
Four trends have been reported (trends reported in more than 60
publications), from most common to least common:
HV will gradually decease as the load is decreased below 100 gf
HV increases slightly and then decreases as the load decreases
HV increases as the load is decreased
HV is constant with varying load (least common trend)
With the Knoop test, the indent cavity shape is not constant with test
load and depth, so HK will increase as the load is decreased.
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HV Microindentation Hardness Data

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Load, gf, - Hardness Relationship

800
700

Harndess, HV

Data obtained using 5 steel

Rockwell C test blocks that
were polished. Measurements
made with a 60X objective,
600X overall magnification, on
a Leitz Miniload II tester. More
than 60 publications claimed
that the change in hardness
as the load drops below 100 gf
is due to dislocation
interactions with the indenter.
Similar results were obtained
with the same test blocks at
loads from 1 to 50 kgf using
an Akashi tester at 100X.

600
500
400
300
200
100
0
0

100

200

300

Load, gf

400

500

600

ASTM E-4 Interlaboratory HV Test Results

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Ferrous No. 1 Specimen

1100

1000

Hardness, HV

One person made 5

HV indents at each
test load using a
standard tester on 3
ferrous specimens.
14 people in different
labs measured the
indents with the
results shown.
Analysis per ASTM E
691 determined that
Labs E, F, H, M and J
obtained outlier
data, while the
results of 9 labs were
in good agreement.

9 Good Labs

Lab E

Lab F

Lab H

Lab M

Lab J

900

800

700

600

500
0

100

200

300

400

500

Load, gf

600

700

800

900

1000

E-4 Round Robin, Good Data

E-4 Round-Robin Good Data - F1
900

Hardness, HV

850
800
750
700
650
600

Lab A
Lab D
Lab L

550

Lab B
Lab G
Lab N

Lab C
Lab K
Lab O

500
10

100

Load, gf
F1 Hardest Ferrous Specimen
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1000

E-4 Round Robin, Good Data

E-4 Round Robin - Good Data, F2
500

Hardness, HV

480
460
440
420
400
380
360

Lab A

Lab B

Lab C

340

Lab D

Lab G

Lab K

Lab L

Lab N

Lab O

320
300
10

100

1000

Load, gf
F2 Intermediate Hardness Ferrous Specimen

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ASTM E-4 Interlaboratory HK Test Results

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Ferrous No. 1 Specimen

1200

9 Good
Lab E

1100

Lab F

Hardness, HK

One person made 5 HK

indents at each test
load using a standard
tester on 3 ferrous
specimens and 4
nonferrous specimens.
14 people in different
labs measured the
indents with these
results. Analysis per
ASTM E 691
determined that Labs
E, F, H, M and J
obtained outlier data,
while the results of 9
labs were in good
agreement.

Lab H

1000

Lab M
Lab J

900

800

700

600
0

100

200

300

400

500

600

Load, gf

700

800

900

1000

E-4 Round Robin - Unusual Knoop Results!

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Nonferrous No. 1 Specimen

370

350

Hardness, HK

It is most common to
see HK increase with
load, particularly so at
loads <100 gf, as tip
visibility leads to
undersizing and
higher HK values. Plus
the Knoop indent
cavity shape is not
identical as the depth
changes. But, here we
see much different
results, even for the 9
good labs. Lab M
clearly has serious
problems!

330

310

9 Good Labs

290

Lab M
Lab U

270

250
0

100

200

300

400

500

Load, gf

600

700

800

900

1000

DuraScan-70 Tester 10 gf to 10 kgf

Struers DuraScan-70
Microindentation Hardness
Tester comes in several
configurations and can be
equipped with a 6-piece turret:
one for a Vickers indenter, one
for a Knoop indenter, and
places for 4 objectives from
10X to 100X, with automated
stage, programmability, and
computer interface for control,
indent measurement, and data
analysis. The automated stage
can hold 6 or 12 (this slide)
specimens.

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6-Position Turret for DuraScan-70 Tester

Turret for 2 indenters and 4 objectives

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Automated holder for 6 specimens

DuraScan Experiments HV Tests

Vickers Measurements:
64.2, 61.3, 60.7, 44.7 and 32.5 HRC Test
Blocks
Loads from 10 to 10,000 gf
Measurements made with 10, 20, 40, 60 and
100X Objectives.

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HV for the 64.2 HRC Test Block

Hardness, HV

Vickers Hardness for 64.2 HRC

Block
1000
900
800
700
600
10

100

1000

Load, gf
Excellent Results at All Loads

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10000

HV for the 61.3 HRC Test Block

Vickers Hardness of 61.3 HRC Block
800

Hardness, HV

750
700
650
600
550
500

100X Obj.

40X Obj.

20X Obj.

10X Obj.

450
400
10

100

1000

Load, gf
10 gf Results Low, Others Excellent
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10000

HV for the 61.3 HRC Test Block

Vickers Hardness - 61.3 HRC Block
Hardness, HV

800
700
600
500
400
10

100

1000

10000

Load, gf
100X Obj.

40X Obj.

20X Obj.

10 gf Data Not Plotted

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10X Obj.

HV for the 60.7 HRC Test Block

Vickers Hardness of 60.7 HRC Test Block
800

Hardness, HV

750
700
650
600
550
500

100X Obj

60X Obj

450

20X Obj

10X Obj

40X Obj

400
10

100

1000

Load, gf
10 gf Results Low, Others Excellent
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10000

HV for the 44.7 HRC Test Block

Vickers Hardness, HV

Vickers Hardness - 44.7 HRC Test Block

500
450
400
350
60C Obj.
20X Obj.

100X Obj.
40X Obj.

300
250
200
10

100

1000

Test Load, gf
10 gf Results Low, Others Excellent

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10000

HV for the 32.5 HRC Test Block

Vickers Hardness, HV

Vickers Hardness of 32.5 HRC Block

500
450
400
350
300
250
200
150
100

100X Obj.
40X Obj.
10

60X Obj.
20X Obj.
100

1000

Load, gf
Excellent Results at all Loads

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10000

Vickers Hardness, All Blocks

HV vs. Force for HRC Test Blocks
Hardness, HV

900
700
500
300
100
10

100

1000

10000

Applied Force, gf
64.2 HRC

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61.3 HRC

60.7 HRC

44.7 HRC

32.5 HRC

HK for the 64.2 HRC Test Block

Knoop Hardness of 64.2 HRC Block
Hardness, HK

1000
950
900
850
800
750
700
650
600
0

250

500

750

1000

1250

1500

1750

2000

Load, gf
Usual Increase in HK with decreasing test load.
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HK for the 61.3 HRC Test Block

Knoop Hardness, HK

Knoop Hardness - 61.3 HRC Test Block

900
100X Obj
40X Obj.

850
800

60X Obj.
20X Obj.

750
700
650
600
10

100

1000

Test Load, gf

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10000

HK for all 4 HRC Test Blocks

Hardness, HK

HK of HRC Test Blocks

1000
900
800
700
600
500
400
300
200
100
0
0

100

200

300

400

500

600

700

800

900

Test Force, gf
64.2 HRC

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60.7 HRC

44.7 HRC

32.5 HRC

1000

Application Examples

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Microindentation Hardness Tests Used to Evaluate

the Thermal Exposure to the Lower Head of Unit 2

Three-Mile Island Nuclear Reactors Before March 28, 1979

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The accident at the Three

Mile Island Unit 2 reactor,
built by Babcock &
Wilcox, began at 4 am on
Wednesday, March 28,
1979, after failures in the
non-nuclear secondary
system were followed by
a failure in the primary
system when a stuckopen pilot-operated
relief valve (PORV)
allowed large amounts of
reactor coolant to
escape.
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Sampling Plan For Lower Head

19,000 kg of core material
melted during the incident
and landed on the lower
head. What temperature did
the head experience?
Sampling began 30 January
1990 by remote controlled
EDM removing 15 boat
shaped specimens (and
continued to the end of
March).
The diagram shows the
location of the boat
specimens relative to the hot
spot location under the
debris pile (only K13 was not
under the debris pile).
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Red arrow points to the

dark feathery band
observed by the VIP team
at the fusion line

White arrow points to the

hardness data by the VIP
team Rockwell C
converted to HV (some
values were <20 HRC)
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300 gf HV Tests of Specimens Cut from Lower

Head of Midland, MI Reactor Never in Service
Midland Control Specimens
Fusion Line

HV - 300 gf

350
300
250
200
150
Cladding

100
-5

HAZ

Base Metal

10

15

20

Distance From Interface, mm

Mid-1

Mid-2

Two specimens randomly selected from the Midland lower head.

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K-13 Not Under the Debris Pile

Cladding

HAZ

Base Metal

The hardness of K-13 was very similar to that of the Midland

specimens that never were in service
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300 gf HV Used to Screen Specimens for Thermal

Exposure
300 gf Vickers indents
were made through the
cladding across the
fusion zone and well into
the base metal to detect
re-austenitization.
Results from a similar
size cancelled reactor
(Midland, MI) were used
for comparison. E-8 and
F-10 were heated in the
accident above the AC3
temperature and formed
bainite upon cooling.
In the diagram, 0 marks the fusion line between
the ER308L cladding and the A533B head.
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Specimen H-5 Did Experience Temperatures >AC3

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Specimen F-5 Experienced Temperatures <AC1

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Cartridge Brass, Cu 30% Zn

Annealed and Cold Rolled 50% (100X)

CR 50%, Then 1300 F 30 min. (50X)

Cartridge brass cold reduced (Klemms I) and CR and annealed

(Klemms III color reagent (both in polarized light and sensitive tint).
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HV of Cold Worked and Annealed Cu-30% Zn

HV of Cartridge Brass
70

% Readings

60
50

50% CR

40
30
20
10
0
50

100

150

200

250

HV, 100 gf load

Full Anneal

1300F-30 m

900F-30 m

800F-30 m

700F-30 m

500F-30 m

50% Cold Reduced

The fully annealed specimen was cold reduced 50% in thickness. Then, CR
specimens were annealed for 30 minutes at 500, 700, 800, 900 and 1300 F. Cross
sections were prepared metallographically and 100 HV indents at 100 gf load were
made in each. The plot shows the distribution of HV values for each specimen.
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HV of Cold Worked and Annealed Cu-30% Zn

HV of 50% CR Cu - 30% Zn
HV, 100 gf Load

250
200
150
100
50
0
0

200

400

600

800

1000

1200

1400

Annealing Temperature, F (30 min)

This is a plot of the mean Vickers hardness values starting with the
specimen cold reduced 50% at room temperature and then showing the
effect of 30 minutes time at temperatures from 500 to 1300 F.
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Gas Nitrided H13 Tool Steel

50 m

10 m

This mold performed well in service. There was no compound layer but we do
observe cementite grain boundary films (green arrows point to a few of many,
right). The black arrow shows the apparent maximum affected depth of
penetration. Etched with 2% nital.
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Hardness Profile of Nitrided H13 Mold

Nitrided H13 - No Compound Layer

1200

Nitrided H13 - No Compound Zone

1200
1100

1000

Hardness, HK

Hardness, HV

1100
900
800
700
600
500
400

1000
900
800
700
600
500

300

400

200
0

0.1

0.2

0.3

0.4

0.5

200 gf

300 gf

0.2

0.3

0.4

0.5

Depth, mm

Depth, mm
100 gf

0.1

500 gf

100 gf

200 gf

300 gf

500 gf

The Vickers hardness varied very little with test load, as expected, while the
Knoop hardness increased with decreasing test load. Both defined the effective
case depth very well. Knoop, because indents could be placed closer to the
surface, revealed a drop in hardness at the surface while Vickers did not.
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Microstructure of 1053 Carbon Steel Induction

Hardened Gear Tooth

Tooth surface

Klemms I, XP+ST, 50X

Case-Core Interface

Non-uniform induction hardening of 1053 Gear Tooth

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Induction Hardened 1053 Gear Teeth

Induction Hardened 1053

900

900

800

800

Hardness, HV

Hardness, HK

Induction Hardened 1053

700
600
500
400
300
200

700
600
500
400
300
200

Depth, mm
50 gf

200 gf

Depth, mm
100 gf

200 gf

Vickers testing at 100 and 200 gf gave nearly identical test results while
Knoop test results at 50 gf were greater than at 200 gf. Both defined the
lower surface hardness well and both revealed the effective case depth
and the core hardness well.
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Carburized, Q&T 1141 Steel

Surface to Core 100X

Berahas Sulfamic Acid Reagent

Core Segregation 200X

Microstructural Variability in 1141 Carburized, Q&T Gear Tooth

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Carburized and Hardened 1141

Carburized 1141, Q&T

900

900

800

800

Hardness, HV

Hardness, HK

Carburized 1141, Q&T

700
600
500
400

700
600
500
400
300

300
0

0.25

0.5

0.75

1.25

1.5

0.25

200 gf

300 gf

0.75

1.25

1.5

Depth, mm

Depth, mm
100 gf

0.5

500 gf

200 gf

300 gf

500 gf

Knoop tests revealed a drop in surface hardness because indents could be made
closer to the surface. As usual, HK increased with decreasing load. The 200 gf
HV results were slightly higher than the 300 and 500 gf results. Retained
austenite was visible to a depth of ~0.32 mm while grain boundary ferrite was
visible to a depth of ~1.25 mm.
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Evaluation of Banding Segregation

100X

2% Nital

500X

Offshore Plate Steel: 0.13% C 1.40% Mn 0.010% P 0.001% S 0.33% Si

0.06% Cr 0.026% Nb 0.028% Al 0.003% Ti 0.0006% B 0.0062 % N

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Evaluating Banding Segregation

HK25 Tests - Offshore Plate Steel

HV25 - Offshore Plate Steel

600

Hardness, HV25

Hardness, HK25

600
500
400
300
200

500
400
300
200
100

100
0

0.1

0.2

0.3

Distance, mm

0.4

0.5

0.1

0.2

0.3

0.4

0.5

0.6

Distance, mm

25-gf Knoop measurements revealed the segregation better than 25-gf Vickers

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Evaluating Banding Segregation

HK50 - Offshore Plate Steel

HV50 - Offshore Plate Steel

600

Hardness, HV50

Hardness, HK50

600
500
400
300
200

500
400
300
200
100

100
0

0.1

0.2

0.3

Distance, mm

0.4

0.5

0.1

0.2

0.3

0.4

0.5

0.6

Distance, mm

50-gf Knoop measurements revealed the segregation better than 50-gf Vickers

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Evaluating Banding Segregation

HK100 - Offshore Plate Steel

HV100 - Offshore Plate Steel

600

Hardness, HV100

Hardness, HK100

600
500
400
300
200

500
400
300
200
100

100
0

0.1

0.2

0.3

Distance, mm

0.4

0.5

0.1

0.2

0.3

0.4

0.5

0.6

Distance, mm

100-gf Knoop measurements revealed the segregation better than 100-gf Vickers

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Evaluating Banding Segregation

HK200 - Offshore Plate Steel

HV200 - Offshore Plate Steel

600

Hardness, HV200

Hardness, HK200

600
500
400
300
200
100

500
400
300
200
100

0.1

0.2

0.3

Distance, mm

0.4

0.5

0.1

0.2

0.3

0.4

0.5

0.6

Distance, mm

200-gf Knoop measurements revealed the segregation better than 200-gf Vickers

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Evaluating Banding Segregation

HK300 - Offshore Plate Steel

HV300 - Offshore Plate Steel

600

Hardness, HV300

Hardness, HK300

600
500
400
300
200
100

500
400
300
200
100

0.1

0.2

0.3

Distance, mm

0.4

0.5

0.1

0.2

0.3

0.4

0.5

0.6

Distance, mm

300-gf Knoop measurements revealed the segregation better than 300-gf Vickers

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Evaluating Banding Segregation

Banding in Offshore Plate Steel

600
550
500
450
400
350
300
250
200
150
100
0

100

200

300

Test Force, gf
HV

HK

400

500

Standard Deviation

Mean Hardness

Banding in Offshore Plate Steel

150
125
100
75
50
25
0
0

100

200

300

400

Test Force, gf
HV

HK

While the mean HK values at each load are slightly higher than the mean HV
values, and both increase as the load decreases, the standard deviation of
the Knoop data better reflects the variability in hardness due to the banding
segregation than the standard deviation of the Vickers data.
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500

Evaluating Banding Segregation

Offshore Plate Steel
Hardness

600
500
400
300
200
100
0

100

200

300

400

500

Test Force, gf
Max HK

Min HK

Max HV

Min HV

The minimum HK and HV values vary little with test load and are quite
similar. But, the maximum Knoop hardness at each load is considerably
greater than the maximum Vickers hardness at loads <300 gf.
These same trends were obtained for 4 different banded specimens.
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New areaMASTER on Struers DuraScan-70

Variation in hardness
due to banding in a
plate steel revealed
using a grid of 3432
Knoop indents (25 gf)
done automatically!

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Conclusions
Microindentation hardness testing is an exceptionally useful tool for
the metallurgist. Its goals are different than bulk hardness testing.
Specimen preparation must remove preparation-induced damage and
this becomes more critical as the test load decreases.
Knoop indents can be spaced closer than Vickers indents and, for a
given load, is better at detecting hardness variations in gradients.
Parallel hardness traces with the indents staggered yields excellent
data to characterize hardness gradients.
As the indent gets smaller, we must use higher magnification, highquality objectives with good illumination to minimize measurement
imprecision.
Knoop hardness does vary with load, but we can correct data to HK
500 test results, and then use ASTM E 140 to estimate equivalent
hardness values with other scales, such as HRC.
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Questions and Thank You

**A link to the recorded session and presentation will be sent to all
participants within 24-48 hours

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