Nodularity:

General Description:

The term “Nodularity” is generally used to determine the percent of nodularity, which means a
degree or percent of a roundness value as established by ASTM standards, as well as, the
nodule count per unit area (i.e., number of nodules per mm2). Generally, the nodularity values
are determined by measuring a captured image of graphite in nodular cast iron as viewed through
a optical microscope at 100X magnification.

Specific Description:

Both ductile and cast iron graphite’s can be measured using the ASTM standardized nodularity
rating system through the use of image analysis.

According to traditional ASTM standards, Nodularity is measured by factors of 5 and is evaluated

based on traditional wall charts using subjective visual interpretations. Not until advanced
software designed Image Analysis tools were introduced into the process did some of the
subjectivity go away. Normal readings for Nodularity range between 80 and 95 which represent
material that meets higher standards of acceptability.

Typical Nodularity is represented by the following picture.

Plating Thickness:

General Description:

Generally speaking, plating thickness refers to any material or materials that have been treated
with a protective coating of one material type or another.

In the example of electroplating, an electrodeposited tin-lead coatings on fabricated articles of

iron, steel, copper, and copper alloys, to protect them against corrosion, to improve and preserve
solderability over long periods of storage, can be measured in relation to depth of application on
the substrate materials.

An example of a plating deposit

Specific Description:

Some corrosion of tin-lead coatings may be expected in outdoor exposure. In normal indoor
exposure, tin-lead is protective on iron, copper, and copper alloys. Corrosion may be expected at
discontinuities (pits or pores, or Porosity) in the coating. Porosity decreases as the thickness is
increased. A primary use of the tin-lead coating (solder) is with the printed circuit industry as a
solderable coating and as an etch mask material which requires a measurement of a maximum
and/or minimum tolerance range of the application’s coverage.

However, when referring to Plating Thickness in a metallographic sense there are hundreds of
various materials associated with the substrate materials that also have hundreds of materials
available to be applied as the layered coatings. Plating Thickness refers to a material or materials
that are used as an application to cover the base material, which is referred to as the substrate
material, and these coatings, or plating layers require measurements of depth and coverage area
based on preset tolerance levels to ensure the integrity of the protection the coatings provide.

The following are two examples of a Plating Thickness treatment:

Electrodeposited coatings on threaded fasteners

This specification covers application, performance and dimensional requirements

for electrodeposited coatings on threaded fasteners with unified inch screw
threads. It specifies coating thickness, supplementary chromate finishes, corrosion
resistance, precautions for managing the risk of hydrogen embrittlement and
hydrogen embrittlement relief for high-strength and surface-hardened fasteners. It
also highlights the differences between barrel and rack plating and makes
recommendations as to the applicability of each process.

Fatigue of Nickel-Plated Copper

The fatigue life of nickel-plated copper depends upon the thickness of the nickel
coating. Increases in life from 150 to 450 percent were obtained by increasing the
thickness of the nickel from 0.0001 to 0.00025 in. (0.00254 to 0.00635 mm). A
further increase in thickness to 0.005 in. (0.0127 mm) resulted in an increase in life
of 200 percent. Interrupting the current during electroplating produces interfaces
within the coating and increases the fatigue life for a given thickness. Increases in
life of 110 percent were obtained by applying a 0.0005-in. thick coating in five
layers, rather than in a single layer.

Porosity

General Description:

Porosity can best be defined as any object determined to be a contaminant of foreign material, or
to the contrary, voids or lack of material as measured by size, shape, color, content, and/or count.
Porosity covers a wide range of materials even outside the metallographic domain. For example,
porosity can be identified in plastics, wood, fibrous materials, cement, chemical based materials,
among many others.

However, in manufacturing of metal or plastic parts and assemblies, porosity in the raw material
is a serious issue affecting the quality of the finished products. Porosity may be caused by
temperature control problems, material impurities, or other causes in the casting of metal or
plastic parts.
. An example of Porosity

Specific Description:

Porosity internal to cast parts may become external or surface pores when material is then
removed from the raw part material by machining, grinding or other manufacturing operations.

Surface pores, if not detected, may cause leakage to occur between the mating surfaces of parts
comprising an assembly or between cavities in an assembly in which substantial pressure
differentials are desired.

An example is the required pressure differential between the cylinders of an engine or between
the region above and below a piston or a valve in a cylinder. The ultimate result of undetected
and uncorrected porosity can include loss of performance, leakage of lubricants or fuel, and
contamination of various portions of the assembled mechanism or product.

Detection of surface porosity requires the use of some form of 2, or even 3-dimensional high-
definition optical microscopy or metrology, because pores of concern may be as small as 100
micrometers in diameter (roughly the diameter of an average human hair) and may occur
anywhere on the surface of a part.

Pores in machined metal or plastic vary significantly in shape, depth, size and the surface
characteristics (such as surface roughness) within the perimeter of the pore. If pores are not
detected prior to assembly of mating surfaces during the manufacturing process, then
considerable additional manufacturing cost is usually incurred as the resulting assembly has to be
disassembled or scrapped after pressure testing or other later performance tests reveal
deficiencies. Thus, a good image analysis system which can acquire, and quantitatively measure
the data, or degree of porosity in manufactured materials, is imperative to achieve the highest
level of control for quality assurance requirements.

Graphite Flake Analysis

General Description:
Graphite flake classifications as defined by international standards refer to charting scheme
classifying inclusions in various iron and steel products. Using this classification system, the
various inclusions are dealt with under the appropriate headings, or listings. Over the years
various testing and experiments have been conducted to define the nature and mode of
occurrences of these graphite particles.

Specific Description:

One should always begin microstructural investigations by examining the as-polished specimen
before etching. This is a necessity, of course, for cast iron specimens if we are to properly
examine the graphite phase. Brightfield vertical illumination will be our starting point, but the
benefits of crossed polarized light will also be explored.

The following graphics depict structural characteristics of various graphite flake structures and
represent just a few examples of their unique compositions.

In Grey Iron

Figure 1

Figure 1 shows interdendritic flake graphite in a hypoeutectic alloy. This type of graphite has been
given many names. In the US it is referred to as Type D (ASTM A247) or as undercooled
graphite. It was thought that the fine size of the graphite might be useful, but it is not technically
useful as it always freezes last into a weak interdendritic network.

Figure 2

Figure 2 shows more regularly-shaped graphite flakes in an alloy of higher carbon content,
although still hypoeutectic. While flake lengths in Figure 1 are roughly 15-30µm, flake lengths in
Figure 2 are in the 60-120µm range.
 Figure 3

Figure 3 shows somewhat coarser flakes (250-500µm length range) in a higher carbon content
cast iron.

Figure 4

Figure 4 shows disheveled graphite flakes in a casting. Note that a few nodules are present. This
appears to be a mix of B- and D-type flakes.

Figure 5

Figure 5 shows a hypereutectic gray iron where very coarse flakes form before the eutectic which
is very fine. This is similar to C-type graphite.

Compacted Graphite

Figure 6

Compacted graphite is a more recent development made in an effort to improve the mechanical
properties of flake gray iron. Figure 6 shows an example where the longest flakes are in the 60-
120µm length range. Compare these flakes to those shown in Figures 2 and 3.
In Nodular Iron: (See Nodularity Above)

The addition of magnesium ('inoculation') desulfurizes the iron and causes the graphite to grow
as nodules rather than flakes. Moreover, mechanical properties are greatly improved over gray
iron; hence, nodular iron is widely known as 'ductile iron'.

Nodule size and shape perfection can vary depending upon composition and cooling rate.

Figure 7

Figure 7 shows fine nodules, about 15-30µm in diameter

Figure 8

Figure 8 shows coarser nodules (about 30-60µm diameter) in two ductile iron casts. Note that the
2 2
number of nodules per unit area is much different, about 350 per mm vs.125 per mm ,
respectively.

Grain Structure Types

The measurement of grain size, whether by the chart comparison method or by manual or
automated measurement methods, is complicated by the different types of grain structures
encountered and by the etched appearance of the grains. For example, as shown in Figure A,

Figure A Ferrite Grain

we may have ferrite grains in a non- heat treated or non-hardenable body-centered cubic (bcc)
metal or alloy. These do not contain annealing twins, but could contain deformation twins, and
second-phase constituents may be present. The example shown is ferrite in a low-carbon sheet
steel; carbides are present. This specimen was etched with nital and not all of the grain
boundaries are visible; those that are visible are variable in darkness and width. These factors
are a minor nuisance for manual rating and a significant problem for automatic rating.

Figure B depicts a single phase austenitic alloy that contains annealing twins.

Figure B Annealing Twins

Like the previous micrograph, it shows the boundaries as dark lines, a so-called "flat etch." The
austenitic alloy shown, L605, illustrates a common problem with such alloys, they are very difficult
to etch so that all of the grain boundaries are visible. This makes it very difficult to measure the
grain size with a high degree of precision. Also, when rating grain size the twin boundaries must
be ignored, which is not easy, especially by image analysis. Not all austenitic alloys will exhibit
annealing twins, aluminum alloys rarely are twinned.

Using Color Metallography:

Color has historically seen limited use in metallography, mainly due to the cost of film and prints
and the difficulty and cost of reproducing images in publications. However, with the growth of
digital imaging, capturing color images is much simpler and cheaper. Also, printing images in
color is inexpensive for in-house reports, and can be distributed cheaply on CDs, although
reproduction in journals is still expensive. Color does have many advantages over black and
white. First, the human eye is sensitive to only about forty shades of gray from white to black, but
is sensitive to a vast number of colors. Tint etchants reveal features in the microstructure that
often cannot be revealed using standard black and white etchants. Color etchants are sensitive to
crystallographic orientation and can reveal if the grains have a random or a preferred
crystallographic texture. They are also very sensitive to variations in composition and residual
deformation. Further, they are usually selective to certain phases and this is valuable in
quantitative microscopy.

The use of color in metallography has a long history with color micrographs published over the
past eighty-some years. Examples of natural color in metals are rare (Figure 1). Gold and copper
exhibit yellow color under bright field illumination. Color can be produced using optical methods,
as in dark field illumination (Figure 2), polarized light (Figure 3) and differential interference
contrast illumination (Figure 4). The microstructure of metals with non-cubic crystal structures can
be examined without etching using polarized light but color is not always observed. The specimen
must be prepared completely free of residual damage for color to be observed, and even then,
some non-cubic metals still exhibit little color. However, many metals and alloys can be etched
with reagents that deposit an interference film on the surface that cre- ates color in bright field
illumination. If it is difficult to grow such a film to the point where the color response is excellent,
the color can be enhanced by examination with polarized light, perhaps aided with a sensitive tint
filter (also called a lambda plate or first-order red filter).

Figures 1 (left) and 2 (right) showing natural reddish-purple color of the AuAl2 intermetallic (left)
in bright field and cuprous oxide¡¯s characteristic ruby red color in dark field illumination (tough-
pitch arsenical copper specimen). The magnification bars are 50 and 10 ¦Ìm, respectively.

Figures 3 (left) and 4 (right): Grain structure on high-purity Zr (left) that was hot worked and cold
drawn (note mechanical twins) and viewed in polarized light and of Spangold (Au¨C19Cu-5Al)
that was polished and cycled through the shape-memory effect to produce martensite and
Nomarski differential interference illumination was used to image the surface upheaval due to the
shear reaction at the free surface. The magnification bars are 100 and 50 ¦Ìm, respectively.

Austenitic alloys may also be etched with reagents that produce grain contrast or color variations
as a function of their crystallographic orientation. Figures 5 and 6 show the twinned austenitic
grain structure of cartridge brass that was etched producing grains with different colors and
contrast.

Figures 5 (left) and 6 (right) represent FCC twinned grain structure of cartridge brass under two
different etching methods, and viewed with polarized light plus a sensitive tint.

Note that unlike the flat etched L605 specimen, all of the grains are revealed. This structure is
easy to rate by the comparison method if the grain size chart depicts grains etched in the same
manner. This condition is virtually impossible to measure by automatic image analysis, however.
Again, twins are present but the coloration or contrast varies within the grains.

To measure twinned austenitic grain structures by image analysis, we need to either suppress the
etching of twins or be able to identify and ignore them. At the same time, all of the grain
boundaries must be revealed and be identifiable.

Anodizing
There are a number of electrolytic etching reagents that can be used to produce color. Second-
phase constituents can be colored and viewed with bright field. Anodizing aluminum specimens
with Barker¡¯s reagent, or similar solutions, does not produce an interference film, as color is not
observed in bright field. This procedure produces fine etch pitting on the surface. The grain
structure can be seen in black and white in polarized light, and in color if a sensitive tint plate is
added. Figure 7 shows an example of anodizing to reveal the grain structure of super-pure
aluminum.
Figure 7: Super-pure aluminum anodized with Barker¡¯s reagent (30 V dc, 2 minutes). The
magnification bar is 200 ¦Ìm long.