Elsevier Sequoia
27
S.A., Lausanne
A METHOD
OIL
~ Printed
in the Netherlands
IN LUBRICATING
W. W. SEIFERT
Massachusetts Institute of Technology, Cambridge, Mass. (U.S.A.)
V. C. WESTCOTT
Trans-Sonics, Inc., Burlington, Mass. (U.S.A.)
(Received
December
27, 1972)
SUMMARY
A new instrument has been developed which is capable of precipitating magnetic particles ranging in size from a few micrometers down to approximately 20
nm from liquids such as lubricating oils. With this instrument, designated a Ferrograph, particles are arranged according to size on a transparent substrate. The
particles recovered from lubricating oil exhibit an amazing complexity and range of
sizes and types. The density of the deposit may be measured optically, or the deposited particles may be examined with an optical or an electron microscope. Some of the
particles recovered from the lubricating oil of a typical machine are known to be associated with abrasive wear and others the result of adhesive wear. Corrosion products
are also observed.
The instrument is of use in research on lubricants, in the study of wear mechanisms, and as a device for the detection of the onset of abnormal wear as might occur
in the course of a ball bearing failure in a jet engine.
1. INTRODUCTION
3x
W. W. SEIFERT.
V. (.
Wt,STCOTl
AND
APPARATUS
The Ferrograph
resulted from an investigation
to find an improved method of
analysing the lubricating
oil of jet engines. The standard method for carrying out
such analyses is to use a spectrograph
to determine periodically
the amount of each
of a selected list of elements iron being the element greatest interest, in engine oil.
The object of the investigation
was to develop a method which would not
require as much apparatus as the existing systems and to obtain a system that would
provide earlier warning of an impending
failure.
A search of the field of analytical techniques4* showed that none of the standard methods was entirely suitable. In general, the simple methods were not sensitive
enough and the sensitive methods were not simple enough. Furthermore,
numerous
theories existed as to how the products of wear were held in the oil but no definitive
literature seemed to have been developed.
As an initial effort to develop a fuller understanding
of the types of contamination appearing in jet engine lubricating
oil, samples taken from several engines were
obtained. When these samples were examined under a high-powered
transmittedlight microscope a few particles could be seen, but their number and volume clearly
did not correlate with available spectrometric
data. The hypothesis was put forward
Weur, 21
(1972)
WEAR
PARTICLES
IN LUBRICATING
OIL
29
that the particles were smaller than could be seen in the microscope. An ultra microscope was, therefore, set up so that particles down to about 20 nm could be seen.
An astronomical number of particles was revealed.
Magnets were brought in the vicinity of the drop of oil while it was under the
microscope. None of the particles was attracted! Although from spectrographic
analysis the oil contained iron, the force exerted on such small particles was too small
to cause them to migrate toward the magnet*. The north and south poles of particles
as small as typically appear in lubricating oil are so close together that the repulsion
for one pole almost exactly equalled the attraction for the other. In addition, evidence
was obtained that additives in the oil caused oil to adhere to the particle. Thus it was
necessary to pull a small amount of oil along with each particle.
When the reasons for the failure of ordinary magnets to attract the particles
were elucidated, a special magnet was designed having a large field gradient. When
this magnet was located on the microscope stage, it did attract a small percentage of
particles from the oil. The rest of the particles were unaffected. Most of these nonmagnetic particles have since been shown to be of external origin, such as ingested sand,
sea salt, dust, carbon particles, etc.
Further studies of the oil showed that most of the small metallic particles
were permanent magnets due to their being so small that they had no more than one,
or at most, a few domains. On the other hand, a larger particle of iron that has not been
magnetized has thousands of domains oriented randomly. Consequently, its net
field will be zero. However, if there is only one domain all of the spin moments point
in the same direction and the particle is magnetically saturated.
When it was realized that most of the ferrous particles were permanent magnets, a new torsion magnetometer was developed to measure the bulk magnetic
moments of various oil samples. The moment of all of the particles was made to add
by solidifying the oil sample while it was stored in a magnetic field of 1000 gauss. The
external field oriented all of the particles so that their moments would add. Following
solidification, the sample was removed from the magnet and the resulting macroscopic
field measured with a torsion magnetometer. This equipment was simple and inexpensive and at first it was thought that it would form the basis for a practical oil
quality analysis system.
However, during the testing period, an oil sample was obtained from a jet
engine in which a gear had become loose on it shaft. Independent spectrometric
measurements indicated that the iron content of the oil had climbed from a few parts
per million to over 100 p.p.m. in a relatively short time. From the high iron content it
was predicted that a high magnetic moment would be observed. However, measurements with the torsion magnetometer indicated that the permanent magnetic moment
was less than for samples which were known to contain only 10 p.p.m. of iron. It was
reasoned, therefore, that the particles were not exhibiting permanent magnetism and
that, therefore, the particles must be multi-domained. This was interpreted as evidence
that large particles might appear in the lubricating oil prior to an engine failure.
It was obvious that new insights could be obtained if an instrument could be
developed which collected those wear particles exhibiting magnetic properties in
lubricating oil. To be effective the system should be capable of collecting particles
* Appendix
I.
Wear, 21 (1972)
30
Fig. 1. Photograph
W. W. SEIFERT.
V. (. WESTCOT
of the Ferrograph
having dimensions in the fractional micrometer range and should permit ready examination of particles once they were collected. A novel instrument,
designated a Ferrograph, was designed to achieve these goals.
The Ferrograph, Fig. 1, consists basically of a magnet designed to develop afield
having an extremely high gradient near the poles, a pump to deliver the oil sample at
a slow steady rate (feed rates in the order of l/4 cc per minute have been found to be
effective) and a substrate on which the magnetic particles are deposited and on which
they can be subsequently
examined by means of either an optical densitometer
or a
high performance
microscope. The substrate on which the particles are deposited is
treated by a proprietary process so that the oil runs down the center of the slide and so
that the particles will adhere to the slides surface upon removal of the oil. The slide
is mounted so that its axis is aligned with the gap between the pole pieces of the magnet.
The Ferrograph is adjusted so that edges of the pole pieces of the magnet lie in a horizontal plane as shown in Fig. 2. The slide in turn is mounted at a slight angle to the
horizontal.
The oil, which is first diluted with a special solvent which increases the
mobility of the contaminating
particles within the oil, is delivered to the higher end of
the slide, flows along the slide, confined by the barriers, and collected at the other end.
Because the distance from the surface of the slide to the pole faces is slightly
greater at the delivery than at the exit end, the magnetic field gradient is weaker at the
delivery than at the exit end. As a result, the particles are subjected to a continually
increasing force as they flow along the slide.
As discussed earlier, the nature of the force on small particles in a magnetic
field is dependent on their size. Particles sufficiently large to accommodate
at least a
few randomly oriented magnetic domains act essentially as small pieces of soft iron in
Weur. 21 (1972)
WEAR
PARTICLES
IN LUBRICATING
31
OIL
C011ect0r
Receptacle
Fig. 2. Schematic
diagram
Oil
Sample
of the Ferrograph.
a field. The force on them is determined by their size and the strength of the magnetic
field to which they are subjected and the field gradient. On the other hand, very small
particles appear to have the characteristics of permanent magnets4. The net force
exerted on such particles depends on their volume and the difference in the forces
on the two poles and thus on the rate of change of field strength with distance. Also,
the velocity with which a particle moves through a fluid when subjected to a force is
dependent or the viscosity of the fluid and the drag characteristics ofthe particle, which,
in turn, depend on its size and shape. Thus a combination of magnetic forces and drag
forces acts on the particles as they are carried by the oil as it flows along the slide.
The net effect is that of sorting the particles by size in the process of depositing them
on the slide. Large particles are deposited first, while the small particles tend to migrate
some distance along the slide before being deposited.
After a sample of approximately 5 cc has been pumped through the system,
a washing and fixing cycle removes the remaining oil and causes the particles to
adhere to the substrate. The liquids used for this purpose evaporate quickly leaving
the substrate dry. At this point the Ferrogram may be removed from the magnet for
observation. A typical pumping time for an oil sample is 20 min ; an additional 10 min
is required to wash and fix the particles on the slide. After the fixing operation the
particles are permanently attached to the Ferrogram.
Figure 3 shows a typical Ferrogram. The deposited particles appear as a dark
band along the center of the slide. The total weight of the deposit in this case is
approximately 13 micrograms. The end of the Ferrogram appearing on the left is
frllljilll li~~lll~lll~~ll~lll~ltf~i~tt~
60
da
!J
MM
Fig. 3. Photograph
Wear, 21 (1972)
of a Ferrogram.
32
W. W. SEIFERT.
V. C. WESTCOTT
the position to which the oil sample was delivered ; particle sizes become progressively
smaller from left to right. If the Ferrogram is viewed against a white background, variations in density are seen and may be quantitatively assessed.
3. OPTICAL
DENSITY
MEASUREMENTS
A convenient way to estimate the density of the deposit is to measure its diffuse
optical density by means of an optical densitometer. (See Fig. 4). Light from a small
aperture is passed through the Ferrogram onto the cathode of a photomultiplier
designed to generate accurately a voltage proportional to the logarithm of the light
intensity. The voltage is measured by an integral digital voltmeter which is adjusted
to read zero for a slide having no deposited material. As the optical density of the
deposit increases, the reading of the digital voltmeter increases and represents the
negative logarithm of the transmission x 103.A light reduction of 10P4 can be accommodated. The densitometer has two ranges, the Low range reads densities from 0.000
to 0.400. When switched to High the instrument covers the density range 0.00 to 4.00.
Typical readings vary from 10 to 100 (x 10e3) at the location where onemicrometer particles are normally deposited. If a wear process sets in which leads to
a failure of a wearing part, the density increases and often reaches values of 1,000 to
1,500 at the time when high iron content is usually detected spectrometrical~y. Actual
measurements obtained from wearing engines are discussed in a later section of this
paper.
The area sampled by the optical densitometer has been chosen to be 0.5 mm
in diameter. It is desirable to sample a large enough area to smooth out statistical
Fig. 4. Photograph
Wear, 21 (1972)
of Reader.
WEAR
PARTICLES
Fig. 5. Graph
IN LUBRICATING
of particle
OIL
33
density
variations in the deposit and, on the other hand, it is desirable to limit the size of the
sampled area so that variations in the distribution of the particles may be measured.
The selected aperture diameter is considered to meet these requirements since the
diameter is less than 1% of the total length of the Ferrogram and, on the other hand,
several hundred particles are often in the field of view. Figure 5 shows the relationship between the area covered by particles and optical density. This relationship
applies if the assumptions are made that all particles are opaque and that particles
are not piled one on another.
The first assumption is tantamount to the assumption that all of the particles
aremetal. This is the case in many, but not all, situations. Usually the area covered by
translucent particles is small and their effect on the absorption oflight is proportionally
less since they transmit a substantial fraction of the light impinging on them.
4. BICHROMATIC
MICROSCOPE
(1972)
SEIFERT.
Fig. 6. Microscope
illumination
Fig. 7. Photograph
of one version
I. c. WESTCOT-
schematic.
of the Bichromatic
microscope.
Kohler illumination.
The optical system has been designed to provide a numerical
aperture in the range between 0.85 and 0.95, the maximum being set by the objective
employed. This is important
in order to make certain spherical particles visible.
Colour balance was an important consideration
in the design of the microscope
and is achieved by independent
control of the intensities of Ll and L2 or by means of
neutral density filters. The use of this high contrast color combination
makes it
possible to distinguish the transmitted
from the reflected light. Opaque objects return
only reflected light and, therefore, appear red. Transparent
objects reflect very little of
the red light incident upon them but pass the green transmitted
light and, therefore,
appear green.
Objects which attenuate light but are not opaque appear various shades of
yellow-green.
Objects which are translucent
but have opaque inclusions
appear
yellow-green,
with the inclusions
appearing red.
Table I lists the extinction
coefficients of various metals and a few compounds7 - lo. The extinction coefficient is defined by
Wear. 21 (1972)
WEAR
PARTICLES
TABLE
IN LUBRICATING
35
OIL
Material
Iron
Nickel
Cobalt
Copper
Silver
Magnetite
Hematite
Wavelength
Extinction
Attenuation
(nm)
coefficient
1 pm
thickness (db)
of
589.1
589.1
650
650
589
546.1
546.1
1.63
1.86
1.85
7.4
20.6
0.12
0.3
151
172
155
621
1630
12
30
light for
Fe20,
Green
Hematite
Fe, 03
ray
17
13
where
5. SOME
PRELIMINARY
FINDINGS
Oil samples taken from a wide variety of machines such as automobile engines,
helicopter transmissions, gear boxes and gas turbines have been examined. Because of
the importance of being able to detect an incipient failure in an aircraft jet engine, the
majority of the initial samples examined have come from gas turbines. The particles
shown below are typical of those found in these engines.
Figure 8 is an example of a jet engine history chart; the abscissa indicates
operating hours, the left-hand ordinate scale represents readings of optical density
and the right-hand ordinate scale represents the quantity of iron in the oil as measured
by an emission spectrograph with a rotating carbon electrode. Readings from the
Ferrogram are plotted as crosses, while readings from a spectrograph appear as circles.
The quantity of iron as measured by the spectroanalysis does not appear to increase
Wear, 21 (1972)
A. W. SEIF-ERI.
NED
L. C. WFST(OT1
PARTICL
IARNING)
w
iINED
&
SPHERICAL
([IRS1
I I
FERROGRAM
EMlSSlON
6Ai iTIC
W[RNINGI,
READINGS
SPECTROGRAPH
,u_LLL
10
20
OPER,.TING
Fig. 8. Engine
history
READINGS
30
HOLJRS
40
chart.
until 20 operating hours have passed.At this point the indication increased from 2p.p.m.
to 3 p,p.m. Five hours later the indication
was in excess of 200 p.p_m.
A series of Ferrograms
shows a continuous
increase in optical density starting
with the 5-hour sample. This figure graphically illustrates the advantage of high resolution, since the spectrometric
data does not change by an amount in excess of the
normal scatter of readings until the iron content in the oil exceeds a few p.pm.
Figure 9 shows photomicrographs
of Ferrograms.
The long thin wire-like or
machined particles are typical of those found in oil samples taken from engines which
were later found to contain a failing part, such as a ball bearing or a gear.
It has been observed that oil samples taken from an engine in which a part
shows rapid wear often contain a variety of particles similar to those illustrated. Some
of these appear similar to lathe chips and turnings but are of micrometer size. Although
these wire-like turnings may be less than 5 pm across, they exhibit fissures and protrusions very much like actual lathe chips. The rapid build-up of such particles in
successive oil samples taken from an engine usually indicates incipient failure of a
part.
A particularly
interesting aspect of the slide from which Fig. 9(C) was taken
is that the oil was quite clean. There was relatively little background
of the nondescript
neur, 21 (1972)
Fig. 9. (A) Strings of particles resulting from adhesive wear. The particles are precipitated
in strings as a
result of the magnetic field. These particles were deposited at the 53 mm position on the Ferrogram
(see
Fig. 3 for scale). (B) Strings of small particles resulting from adhesive wear. This is the same Ferrogram
as
shown in (A). The field of view is located at the 10 mm position. (C)Small wire-like particles representative
of
abrasive wear. Note the coil spring and semi-loop. The source of these particles is not known but it is known
that as a consequence of ingesting a forgign object, the engine operated out of balance for a short time before
the sample was taken, (D) Heavy deposit of randomly shaped particles with a prominent wire-like machined
particle. Note the inclusions in the wire. Often cleavage faces will contain many such inclusions, while other
particles contain none. (E)A circular wire particle. Much more detail is observable by the eye. The tip facing
the center is composed of the same wire as the loop and consists of two twists with a flattened end. (F)
Very large particles observed on a Ferrogram
of oil taken from a jet engine. The oil was reported as having
high iron content as determined with a spectrograph.
Note the longitudinal
ridges as if the surface were
scuffed. (G) Particles adjacent to the field of view shown in (9F) and (9H). (I) Spherical particle found in oil
sample. Note the image of a pen point which has been projected on the particle. Only spheres appear to
reflect an undistorted
image. This oil was obtained from an engine which a few hours later was shut down
as a result of a main ball bearing failure.
particles characteristic ofoil which has been used for many hours in an engine showing
normal wear.
Spherical particles, as shown in Fig. 9(I), are also typical of high wear situations.
Although considerable controversy exists over how the spheres are produced. an
examination of a sphere on a Ferrogram by a scanning electron microscope indicated
that the surface was smooth as if the particle were produced by melting and subse-
r=5
T:ZO
hours
hours
2PPM
3PPM
Fe
Fe
r=25
hours
ZIOPPM
Fe
WEAR
PARTICLES
IN LUBRICATING
OIL
39
quent freezing in the oil. An alternate hypothesis holds that these spheres are produced
by fretting. Whatever the mechanism by which the spheres are produced, it has been
observed that the number of spheres increased rapidly during a ball bearing failure.
Most spheres observed up to the present time have ranged in diameter from 5 pm
down to the limit of visibility with the great majority less than 1 pm. Furthermore, most
have been metal, although occasionally oxide spheres are observed.
The spheres are unique in an optical sense in that they are so smooth that they
are difficult to observe with a microscope having a numerical aperture in the typical
range of 0.5 to 0.65. Because the angle of illumination corresponding to this aperture
results in illuminating only the top of the sphere, the object appears as a point of light
rather than a round body. When the numerical aperture is increased above 0.85 the
disc of illumination is much larger, and a sphere takes on the appearance of a round
body. It is quite possible that similar spheres were not discovered in lubricating systems at an earlier date because the illumination angle was insufficient to distinguish
them from many other particles that might, for example, appear on a filter.
Photomicrographs, Fig. 10, were taken from a series of Ferrograms made
from oil taken at intervals from a jet engine in which the main bearing ultimately
failed. Figure 10(B), taken after 10 h of operation, shows several of the machined
particles found to be characteristic of an incipient failure. After 20 h heavy (as large
as 10 by 40 pm) chips are also seen, while the Ferrogram taken after 25 h shows a very
dense deposit and includes spherical particles in addition to the lathe-like turnings
and the chips seen earlier.
Unfortunately, the black and white photographs reproduced here cannot
conve.y the true character of the images as viewed directly or even as reproduced in
color photographs. Actually the strings of particles show great detail and diversity
of color ranging from deep reds to bright greens, indicating that some particles are
free metal while others are oxides or other compounds.
6. APPLICATIONS
The Ferrograph represents a significant advance in the instrumentation available for the study of wear particles in lubricating oils. It promises to find wide application as a research tool in the study of wear phenomena and as a diagnostic tool for
detecting the onset of abnormal wear conditions in jet engines and other operational
equipment.
7. ACKNOWLEDGEMENTS
Direct observations have indicated that particles of the size typically found in
lubricating oil move very slowly under the influence of the fields from ordinary
Wear,21
(1972)
40
W. W. SEIFERT.
V. C. WESTCoT
magnets. This appendix presents the equations governing the force produced on such
particles by a magnetic field and the drag forces produced as particles move through
the oil.
The force exerted on a magnetic particle by an external magnetic field depends
on the magnetic moment of the particle and on the field gradient5,6. For particles in
the size range of interest with the Ferrograph, two cases apply.
First, there are small particles containing only one magnetic domain. Such
particles are saturated magnetically so that the force acting on them is given by the
equation :
(1)
F, = force in the X direction, kg m/set, M = magnetic moment of the particle, Wb m.
aH/iYx field gradient in the X direction, amp-turn/m.
Here, and throughout this appendix, units are expressed in the rationalized
mks system.
If the magnetic moment of the particle is expressed in terms of the volumetric
saturation moment of the material and the volume of the particle, eqn. (1) takes the
form
where I, = is the saturation moment, Wb m/m3 (see Table II), V = volume of the particle, m3.
Alternatively the equation can be written in terms of the mass of the particle
and its saturation moment per unit mass
(3)
where a,=saturation
moment, Wb m/kg (see Table II), W =mass of particle, kg.
If the particle is sufficiently large to support a number of domains and is soft
magnetically, the force on the particle may be expressed
^
F,=M
(4)
ax
TABLE II
~~~
_~
Mettrl
l,(Weber-m/m)
cr,(Weber-m/kg)
Iron
Cobalt
Nickel
1714 x 1om4
1422 x 1O-4
482 x 1O-4
218 x lo-
161 x IO-
544 x lo-
____
Wear, 21 (1972)
WEAR
PARTICLES
IN LUBRICATING
41
OIL
i = F&Jr
i = 5
and
KHV
1 = Cr
aH
Substitution of appropriate values into eqn. (6) will yield an approximate value
for the velocity at which a single domain particle would move through oil when a
magnet is brought into the vicinity of the oil sample. This was actually done by bringing a small Alnico magnet close to a drop of oil while it was under a microscope.
Table II lists the saturation moments for several magnetic materials in terms
of both volume and mass.
Typical particles of interest here have a radius of approximately one pm
and at 20C the viscosity of oil ranges from approximately 100 centipoise or 0.1 kg/m
set to the order of five times that value or 0.5 kg/m sec. We assume a value for the oil
diluted with developer of 0.1.
Measurements on the Alnico magnet used in this experiment, which was l/2 in.
diameter and 2 in. long, showed a field strength of approximately 350 gauss and a
gradient of approximately 500 gauss/cm at a distance of 8 mm from the pole face.
In free space we can write:
H=R
PO
Wb/m
amp-turn/m
Furthermore, one gauss is equivalent to 10m4 Wb/m. Substitution of the gradient as measured in gauss/cm, the permeability of free space and the necessary conversion from cgs to mks units yields for the dH/ax
Wb/m2
aHlax = 500 lo-
471x 1o-7
m
Wb/m
amp-turn/m
z 4x lo6 amp-turn/m.
Substitution
Wear,21
(1972)
of these values into eqn. (6) then yields for the particle velocity
(9)
(IO)
42
W. W. SEIFERT.
V. c. WESTCOTI
(1714x 10.4)($x
lo-s)
.C = P--.(o,1)
(fom6) ~--(4 x 10)
2 2Xx 10P mjsec.
The important conclusions to be drawn from this analysis are that particles in
the size range typically found in lubricating oil move very slowly under the influence of
the field from an ordinary magnet and that their velocity depends on the gradient of
the field and on the square of the radius of the particles.
REFERENCES
I D. C. Kittinger
2
3
4
5
6
I
Wear. 21 (1972)