Microindentation

Hardness Testing
Microindentation hardness testing is a very valuable tool for the materials
engineer, but it must be used with care and full understanding of
potential problems.

The purpose of microindentation hardness testing is to study fine scale changes in

hardness, either intentional or accidental. The technique is also commonly known
as microhardness testing, but this term is misleading because it implies that the
hardness is extremely low, which is not the case. The applied load and the
resulting indent size are small relative to bulk tests, but the same hardness
number is derived. Consequently, ASTM Committee E-4 on Metallography
recommends the term "microindentation hardness testing," which could be given
the acronym MHT.

This article describes the two most common microindentation tests -- the Vickers
and the Knoop tests, which are currently being updated as ASTM Standard E
384.

The Vickers test

In 1925, Smith and Sandland of the
United Kingdom developed a new
indentation test for metals that were
too hard to evaluate by the Brinell test,
whose hardened steel ball was limited
to steels with hardnesses below ~ 450
HBS (~ 48 HRC). In designing the new
indenter, a square-based diamond
pyramid (Fig. 1), they chose a
geometry that would produce hardness
numbers nearly identical to Brinell
numbers within the range of both tests.
Fig. 1- Schematic diagram showing the shape of the
This was a very wise decision, because Vickers indenter and impression. The Vickers
it made the Vickers hardness test very hardness number is calculated based on the surface
easy to adopt. area of the indent.

The ideal d / D ratio (d = impression diameter, D = ball diameter) for a spherical

indenter is 0.375. If tangents are drawn to the ball at the impression edges for d /
D = 0.375, they meet below the center of the impression at an angle of 136
degrees, the angle chosen for the Vickers indenter.
Diamond allows the Vickers test to evaluate any material and, furthermore, has
the very important advantage of placing the hardness of all materials on one
continuous scale. This is a major disadvantage of Rockwell type tests, for which
15 standard and 15 superficial scales were developed. Not one of these scales can
cover the full hardness range. The HRA scale covers the broadest hardness range,
but this scale is not commonly used.

In the Vickers test, the load is applied smoothly, without impact, and held in
place for 10 or 15 seconds. The physical quality of the indenter and the accuracy
of the applied load (defined in E 384) must be controlled to get the correct
results. After the load is removed, the two impression diagonals are measured,
usually with a filar micrometer, to the nearest 0.1 µm, and then averaged. The
Vickers hardness (HV) is calculated by:

HV = 1854.4L / d2

where the load L is in grams-force and the average diagonal d is in µm (although

the hardness number units are expressed in units of kgf / mm2 rather than the
equivalent gf / µm2).

The original Vickers testers were developed for test loads of 1 to 120 kgf, which
produce rather large indents. Recognizing the need for lower test loads, the
National Physical Laboratory (U.K.) experimented with lower test loads in 1932.
The first low-load Vickers tester was described by Lips and Sack in 1936.

Because the shape of the Vickers indentation is geometrically similar at all test
loads, the HV value is constant, within statistical precision, over a very wide test
load range, as long as the test specimen is reasonably homogeneous.

However, studies of microindentation hardness test results conducted over the

past several years on a wide range of loads have shown that results are not
constant at very low loads. This problem, called the "indentation size effect," or
ISE, has been attributed to fundamental characteristics of the material. In fact, the
same effect is observed at the low load test range of bulk Vickers testers.
Furthermore, an ASTM inter-laboratory "round robin" of indents made at one
laboratory but measured by twelve different people, reported all three possible
ISE responses for the same set of indents!

Since the 1960s, the standard symbol for Vickers hardness per ASTM E 92 and E
384, has been HV. This nomenclature is preferred to the older, obsolete symbols
DPN or VPN. The hardness is expressed in a standard format. For example, if a
300 gf load reveals a hardness of 375 HV, the hardness is expressed as 375
HV300. Note that ASTM recommends a "soft" metric approach in this case,
because rigorous application of the SI system would result in hardness units
expressed not in the standard, understandable kgf / mm2 values, but in GPa units,
which are entirely meaningless to engineers and technicians.

In the Vickers test, it is assumed that recovery is not

elastic after the load is removed. However, in
reality recovery is elastic, and sometimes its
influence is quite pronounced. Generally, the
impression (Fig. 2) appears to be square, and the
two diagonals have similar lengths.

Fig. 2 - Example of Properly formed As with the Brinell test, the Vickers hardness
indents with excellent image contrast number is calculated based on the surface area of
(400X) the indent rather than the projected area. However,
if the impression shape is distorted by elastic
recovery, a very common result in anisotropic
materials (Fig. 3), should the hardness be based on
the average of the two diagonals? It is possible to
calculate the Vickers hardness based on the
projected area of the impression, which can be
measured by image analysis. Although rigorous
Fig. 3 - Example of a distorted Vickers
studies of this problem are seldom found in the
indent in an austenitic stainless steel literature, it appears that the diagonal measurement
specimen (400X) is the preferred approach even for distorted indents.
The Knoop test
As an alternative to the Vickers test,
particularly for very thin layers, Fredrick
Knoop and his associates at the former
National Bureau of Standards (now NIST)
developed a low-load test with a
rhombohedral-shaped diamond indenter, Fig.
4. The long diagonal is seven times (7.114
actually) as long as the short diagonal. With
this indenter shape, elastic recovery can be
held to a minimum. Some investigators claim
no elastic recovery with the Knoop indent, but
this cannot be true, because measurements of
the ratio of long-to-short diagonal often Fig. 4 - Schematic showing the shape of the
reveal results substantially different than the Knoop indenter and impression.
ideal 7.114 value.

The Knoop test is conducted in the same manner, and with the same tester, as the
Vickers test. However, only the long diagonal is measured, except for the
projected area hardness (PAH) test recommended by Blau. This, of course, saves
some time. The Knoop hardness is calculated from

HK = 14229L / d2

where the load L is in gf and the long diagonal d is in µm. Again, the symbol HK
was adopt in the early 1960s while other terms, such as HKN or KHN, are
obsolete. The Knoop hardnness is expressed in the same manner as the Vickers
hardness: 375 HK300 means that a 300 gf load produced a Knoop hardness of 375
kgf / mm2.

Aside from a minor savings of time, one chief merit of the Knoop test is the
ability to test thin layers more easily. For surfaces with varying hardness, such as
case hardened parts, Knoop indents can be spaced closer together than Vickers
indents. Thus, a single Knoop traverse can define a hardness gradient more
simply than a series of two or three parallel Vickers traverses in which each
indent is made at different depths. Furthermore, if the hardness varies strongly
with the depth, the Vickers indent is distorted by this change; that is, the diagonal
parallel to the hardness change is affected by the hardness gradient, while the
diagonal perpendicular to the hardness gradient remains unaffected (both halves
of this diagonal are of the same approximate length).

The shortcoming of the Knoop indent is that the three-dimensional indent shape
changes with test load and, consequently, HK varies with load. In fact, HK
values may be reliably converted to other test scales only for HK values
produced at the standard load, generally 500 gf, that was used to develop the
correlations. However, at high loads the variation is not substantial. Note that all
hardness scale conversions are based on empirical data; consequently,
conversions are not precise but are estimates.

Accuracy, precision, and bias

Many factors (see Table) can influence the quality of microindentation test
results.

Table: Factors affecting precision and bias in microindentation hardness testing

Instrument Factors Measurement Factors Material Factors
Accuracy of the applied load Calibration of the
Heterogeneity in composition
Inertia effects, speed of loading. measurement system.
or microstructure.
Angle of indentation. Resolving power of the
Crystallographic texture.
Lateral movement of the objective.
Quality of the specimen
indenter or specimen. Magnification.
preparation.
Indentation time. Operator bias in sizing.
Indenter shape deviations. Inadequate image Low reflectivity or
Damage to the indenter. quality. transparency.
Insufficient spacing between Nonuniform illumination.
indents or from edges.

In the early days of low-load (<100 gf) hardness testing, it was quickly
recognized that improper specimen preparation can influence hardness test
results. Most texts state that improper preparation yields higher test results
because the surface contains excessive preparation-induced deformation. While
this is certainly true, improper preparation may also create excessive heat, which
reduces the hardness and strength of many metals and alloys. Either problem may
be encountered due to faulty preparation.

For many years, it was considered necessary to electrolytically polish specimens

so that the preparation-induced damage could be removed, thus permitting bias-
free low-load testing. However, the science behind mechanical specimen
preparation, chiefly due to the work of Len Samuels, has led to development of
excellent mechanical specimen preparation procedures, and electropolishing is no
longer required.

In addition, several operational factors must be controlled for optimum test

results. First, it is good practice to inspect the indenter periodically for damage;
for example, cracking or chipping of the diamond. If you have metrology
equipment, you can measure the face angles and the sharpness of the tip.
Specifications for Vickers and Knoop indenter geometries are given in E 384.

A prime source of error is the alignment of specimen surface relative to the

indenter. The indenter itself must be properly aligned perpendicular (±1°) to the
stage plate. Next, the surface must be perpendicular to the indenter. Most testers
provide holders that align the polished face perpendicular to the indenter (parallel
to the stage).

If a specimen is simply placed on the stage surface, its back surface must be
parallel to its polished surface. Tilting the surface more than one degree from
perpendicular results in nonsymmetrical impressions, and can produce lateral
movement between specimen and indenter.

However, in most cases, indenting procedures are not the major source of error.
For example, the writer has encountered units that were not applying the correct
load, as shown in Fig. 5. Tester A produced nearly constant results over the full
load range, while tester B produced the correct results only at 1000 gf. As the
applied load decreased, the hardness decreased to less than 25% of the correct
value! Apparently, the load being applied, for loads under 1000gf, must have
been substantially greater than specified. After such an evaluation, it is easy to
decide which tester to purchase!

As this experience shows, it is important to regularly check the performance of

your tester with a certified test block. The safest choice is a test block
manufactured for microindentation testing and certified for the test (Vickers or
Knoop) as well as the specified load. Strictly speaking, a block certified for
Vickers testing at 300 or 500 gf (commonly chosen loads) should
yield essentially the same hardness with loads from about 50 to 1000 gf. That is,
if you take the average of about five indents and compare the average at your
load to the average at the calibrated load (knowing the standard deviation of the
test results), statistical tests can tell you (at any desired confidence level) if the
difference between the mean values of the tests at the two loads is statistically
significant or not.

When considering a new tester, it is

prudent to perform a series of indents (five
is adequate) at each test load available (as
shown in Fig. 5). Then, plot the mean and
95% confidence limits (not shown in Fig.
5) of each test as a function of load.
Because of the method of defining HV and
HK, which involves dividing by d2,
measurement errors become more critical
as d gets smaller; that is, as L decreases
and the material's hardness increases.

Therefore, departure from a constant

hardness for the Vickers or Knoop tests as
a function of load becomes a greater
problem as the hardness increases. For the
Knoop test, HK increases as L decreases
because the indent geometry changes with
Fig. 5 - Load vs. Vickers hardness test results for
indent depth and width. But the change in two testers using a quenched and tempered 440C
HK varies with the test load -- at a higher martensitic stainless steel specimen. Tester A is
hardness, the change is greater as L red, tester B is blue.
decreases.

The greatest source of error is measuring the indent, as documented in an ASTM

inter-laboratory test. Place the indent in the center of the measuring field, because
lens image quality is best in the center. The light source should provide adequate,
even illumination to provide maximum contrast and resolution. The accuracy of
the filar micrometer, or other measuring device, should be verified by a stage
micrometer.

Specimen preparation quality becomes more important as the load decreases, and
it must be at an acceptable level. Specimen thickness must be at least 2.5 times
the Vickers diagonal length. Because the Knoop indent is shallower than the
Vickers at the same load, somewhat thinner specimens can be tested.

Spacing of indents is important because indenting produces plastic deformation

and a strain field around the indent. If the spacing is too small, the new indent
will be affected by the strain field around the last indent. ASTM recommends a
minimum spacing (center to edge of adjacent indent) of 2.5 times the Vickers
diagonal.

For the Knoop test, in which the long diagonals are parallel, the spacing is 2.5
times the short diagonal. The minimum recommended spacing between the edge
of the specimen and the center of the indent should be 2.5 times. Again, Knoop
indents can be placed closer to the surface than Vickers indents.

For more information: George F. Vander Voort is director of research &

technology, and Gabriel M. Lucas is a materials engineer at Buehler Ltd., 41
Waukegan Road, Lake Bluff, IL 60044; tel: 847 / 295-4590; fax: 847 / 295-7942;
e-mail: gfvandervoort@compuserve.com; Web site: www.buehlerltd.com.