TSG2100G 3 P 2

NOTES: The recipient of this standard shall undertake the following confidentiality obligations upon the receipt of this
standard.
Rev. 3
TOYOTA ENGINEERING STANDARD
TSG2100G
CONFIDENTIAL DO NOT REPRODUCE
5.2 General Concerns to Be Noted during Etching
(1) Make sure that the surface to be examined is free from lapping abrasive and foreign matter.
Also make sure that the surface is free from fingerprints, oil, or grease. Check how clean the
burnished surface is by wetting it with alcohol. If the alcohol spreads uniformly on the surface, it
may be assumed that the specimen will etch evenly. Two examples of non-uniformly etched
surfaces due to adhered oily substances are shown in Figs. 22 and 23.

Fig. 22 Non-Uniform Etching Caused by Adhered Oil
(Uniform Sorbite Structure Should Have Been Obtained.)

Fig. 23 Non-Uniform Etching Caused by Adhered Oil
(Uniform Sorbite Structure Should Have Been Obtained.)

(2) Shake the specimen frequently during etching in order to prevent bubbles from affecting the
reaction.
Pay careful attention to etching time. The specimen surface to be examined therefore is
oriented upward during immersion in some cases to allow progress to be observed.

- The recipient shall discard by shredding or fire, or return to Toyota Motor Corporation if appropriate, the documents contained in this standard when they
are no longer necessary due to the termination of the work concerned or the revision of current version of this standard,
- This standard and the technical information related thereto are owned by and under sole control of Toyota Motor Corporation. They shall not be disclosed
in whole nor in part to ant third party without prior written consent of Toyota Motor Corporation..
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NOTES: The recipient of this standard shall undertake the following confidentiality obligations upon the receipt of this standard.
Rev. 3
TSG2100G
(3) If no satisfactory result is obtained by etching, re-etching may be necessary. Note, however,
that etching quality usually deteriorates.
(4) If the surface has been over-etched, relap it or repeat the polishing process depending on the
surface condition.
(5) Etching level requirement depends on the objective of the examination and magnification. The
higher the magnification, the lower the required etching level.
(6) When etching has been completed, wash the surface in running water using clean cotton or
fabric until the reaction product made by the etching is completely removed. Then dry the
specimen by blowing heated air using a dryer (Fig. 21).
(7) Etching solutions are usually strongly acidic, poisonous, or deadly poisonous. Take special
care when handling them or diluting them with water during their preparation. If handled
carelessly, some etching solutions can even cause burns. For such solutions, take care also
during the etching operation.

6. Microscopy
6.1 Microscope for Metallography
Microscopes for metallography are divided into two types; the erected type and the inverted type.
Each type is further divided into monocular and binocular according to eyepiece.
Figs. 24 and 25 show typical microscopes widely used today.
The outstanding features of the erected and inverted types are as follows:
(1) In the erected type, the position of the surface to be examined can be easily determined, but it is
difficult to align the surface with the optical axis. In the inverted type, on the other hand, it is
difficult to position the surface to be examined. Since the surface can be maintained in a stable
position, this type is suitable for photography.
(2) The erected type has a maximum height of the specimen to be examined.
(3) The inverted type is more expensive than the erected type in general.

Fig. 24 Erected Type Microscope

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Fig. 25 Inverted Type Microscope (With Microphotography Equipment)

6.2 Construction of Metallurgical Microscope
The construction of an erected type is shown in Fig. 26.

Fig. 26 Construction of Microscope (Erected Type)

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6.3 Specimen Setting
(1) For the erected type microscope, place the specimen on the stage, aligning the surface to be
examined perpendicular to the optical axis (Fig. 29).
To adjust the horizontality of the surface to be examined, place synthetic resin clay on a
specimen plate. Put the specimen on the clay, and lightly press the surface to be examined,
using a hand press (Fig. 27).
It is advisable to cover the surface to be examined with a clean sheet of paper during the
pressing in order to keep the surface free from any dust and foreign matter.
(2) For the inverted type microscope, place the specimen on the stage, with the surface to be
examined facing downward. Choose a specimen plate with a proper opening that permits a
stable setting of the specimen (Fig. 28).
The specimen plate and other accessories should be cleaned in advance to keep the surface
free from any contaminants.

Fig. 27 Hand Press

Fig. 28 Inverted Type Microscope (Partial View)

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6.4 Specimen Positioning
The specimen can be positioned by adjusting the longitudinal positioning knob and the transverse
stage control (Fig. 29).
A heavy specimen may sometimes prevent smooth movement.

Fig. 29 Erected Type Microscope (Partial View)

6.5 Focusing
(1) To focus on the surface to be examined, use a lower magnification objective lens. Observing
the lens and the specimen from the side, bring the stage to a position closer to the lens than the
focus point.
Then view the surface through the eyepiece and gradually move the stage away from the lens by
manipulating the coarse focus adjustment.
When the surface is nearly in focus, manipulate the fine focus adjustment until the image can be
observed as clearly as possible.
If the focusing is done by raising the stage from a distant position from the lens, instead of by
lowering it from a position close to the lens, the lens may come into contact with the specimen,
causing damage to the lens or tilting the specimen (Fig. 30).

Fig. 30 Focusing

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(2) To look at the surface at higher magnification, focus the lens initially at lower magnification.
Then turn the lens revolver to the desired lens position. If the surface is out of focus, reposition
it by manipulating the fine focus adjustment.
Use of a high magnification objective lens at the beginning of focusing may cause it to come into
contact with the specimen due to the shorter focal distance, possibly damaging the lens.
Do not apply any force to the objective lens when changing the magnification, as it may misalign
the optical axis (Fig. 31).

Fig. 31 Revolver Operation

(3) An M12OX objective lens is used when the specimen is examined in the so-called "oil
immersion" method in which cedar oil (refraction index: 1.515) is fed between the lens and the
specimen.
Even for this method, use a lower magnification objective lens at first for coarse focusing. Then
change to the M12OX lens. Let the stage down and feed a drop of cedar oil. Bring the stage
close to the lens until the lens comes into contact with the oil, while observing the specimen from
the side (Fig. 32).
While viewing through the eyepiece, adjust the focus finely by manipulating the fine focus
adjustment.
If the cedar oil contains any bubbles, the image cannot be seen clearly. Cedar oil will solidify
itself if left on the stage for a long time. Completely remove the oil from both the lens and
specimen, using clean gauze saturated with xylene or benzene.

Fig. 32 Focusing by the Oil Immersion Method

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(4) Adjust the distance between the two eyepieces for comfort. If the visibility of the user differs
between right eye and left eye, adjust the eyepiece position by turning draw tube (Fig. 33).

Fig. 33 Adjustment of Eye-to-Eye Distance and Visibility

(5) The integrated magnification of the microscopic image is the product of the magnifications of the
objective lens and the eyepiece.
Ex.: When objective lens M48X and eyepiece WF10X are used, Integrated magnification
= 48 10 = 480.

6.6 Image Brightness Adjusting
6.6.1 Lamp Positioning
(1) Focus the lens on the surface to be examined, opening the brightness diaphragm to the "MAX"
position and maintaining the centerable auxiliary lens knob at "H" (high) (Fig. 34).
(2) Fully open the lamp field diaphragm and remove the eyepiece. While looking into the tube,
move the two entering knobs so that the bulb filament comes into alignment with the center
(optical axis).
This adjustment allows the brightest field and uniform lighting.
This adjustment can be performed correctly when a lower magnification lens is used.

Fig. 34 Lamp Housing

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6.6.2 Diaphragm Adjusting
(1) The brightness diaphragm, also called the aperture diaphragm, largely influences the resolution.
If the diaphragm is narrowed beyond a certain limit, the "numerical aperture" - an index for the
resolution of the objective lens - decreases, and resolution is actually reduced. In addition, the
image is diffracted. This may lead to erroneous conclusions (Figs. 35 and 36).

Fig. 35 Image Obtained from Properly Controlled Diaphragm

Fig. 36 Image Obtained from Excessively Narrowed Diaphragm

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(2) For proper diaphragm adjustment, follow the procedure described below.
Remove the eyepiece and look into the draw tube.
Narrow the brightness diaphragm gradually. The reflected image of the diaphragm will appear
from the circumference and gradually decrease its dimensions. The best position is the point
where the diaphragm image first appears. At this point, the resolution of the lens is at its
maximum. If the diaphragm is narrowed over this point, the contrast of the image will improve,
and thus image quality will appear to be improved. However, the actual resolution decreases.
Hence, it becomes difficult to detect fine crystal structures.
If the diaphragm is narrowed still further, diffraction will produce a false image. In this case the
correct structure cannot be detected.
The optimal position of the brightness diaphragm differs depending upon each objective lens.

6.6.3 Auxiliary Lens Adjusting
When using a low magnification objective lens, set the auxiliary lens knob to "L" (low). This is done
to illuminate every corner in the field.
When objective lens M6X is used for photographing, the circumference will darken. Be sure to adjust
the brightness using the auxiliary lens.
When using an objective lens other than M6X, leave the auxiliary lens knob set at "H" (high).

6.6.4 Light Source Adjusting
Lamp brightness can be controlled by adjusting the power transformer (Fig. 37). Correctly adjust the
light source position and two apertures to illuminate the specimen properly. Do not increase lamp
brightness excessively, or the lamp housing may overheat.

Fig. 37 Accessory (Power Transformer)

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6.7 Field Diaphragm Adjusting
(1) The field diaphragm is independent of resolution and field brightness. If the diaphragm is
opened excessively, however, the overspread light will reflect diffusely, and deteriorate image
contrast. Accordingly, the field diaphragm should be controlled according to the size of the area
to be observed.
(2) For normal microscopy, adjust the field diaphragm to a point just before the diaphragm image
can be seen from the circumference when viewed through the eyepiece (Fig. 38).
(3) As long as the same eyepiece is used, the field size will remain unchanged even if the objective
lens is replaced.
(4) To take photomicrographs, use minimal field to minimize foggy images resulting from diffused
reflection.

Fig. 38 (Optimum) Field Control

Applicable Standards
ISO 6344-1 Coated Abrasives -- Grain Size Analysis -- Part 1: Grain Size Distribution
Test
ISO 6344-2 Coated Abrasives -- Grain Size Analysis -- Part 2: Determination of Grain
Size Distribution of Microgrits P12 to P220
ISO 6344-3 Coated Abrasives -- Grain Size Analysis -- Part 3: Determination of Grain
Size Distribution of Microgrits P240 to P2500
JIS R 6010 Coated Abrasive Grain Sizes

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APPENDIX MICROSCOPIC STRUCTURE DETECTING METHOD FOR METAL
1. General Information on Metallurgical Microscopes
The Principle of Metallurgical Microscopes
As metal specimens are not transparent, a light is usually projected perpendicular to the surface of a
specimen, and the reflection is led into a metallurgical microscope to form an image.
In this respect microscopes for the examination of metals differ characteristically from biological
microscopes.
The light path of a metallurgical microscope is as shown in Appendix Fig. 1. The light emitted from a
light source reflects on the plane glass placed at an angle of 45 so that it turns by 90 . The
light then reaches the specimen surface passing through the objective lens. The light is reflected by
the specimen surface. Part of the reflected light that passed again through the objective lens goes
through the plane glass and the eye piece, then finally enters the naked eye.
The image of the specimen formed on the retina, as shown in Appendix Fig. 1, is a magnified virtual
image.
In the design of a biological microscope it is assumed that a cover glass is placed on the surface to be
examined, and the thickness of the cover glass is taken into consideration. In comparison with this,
the metallurgical microscope is designed assuming that no glass will be placed between the objective
lens and the surface to be examined.
Accordingly, the objective lens of every metallurgical microscope, differing from that of a biological
microscope, has the symbol "M" (short for Metallurgy) stamped as prefix to the magnification.

Appendix Fig. 1 The Principle of Erected Type Microscopes

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2. Objective Lens
2.1 The Aberration of a Lens
In forming an image with a lens, the image becomes unclear due to chromatic aberration and
spherical aberration.
An objective lens is designed so that the effect of these kinds of aberration is minimized.
(1) Chromatic aberration
A typical light is a mixture of rays of different wavelengths (different indexes of refraction) so that
a lens forms a series of images by a light passing through it at slightly deviating positions
depending on rays' refractive indexes.
In order to reduce chromatic aberration and obtain a clearer image, a method is used, in which a
convex lens system is made up using concave and convex lenses with different optical properties.
This is what is called achromatic lens.
Nonetheless, it is impossible to eliminate chromatic aberration with a light containing all
wavelengths. A lens system therefore is designed so that the image is formed at a position with
regard to rays of several kinds of wavelengths.
An achromatic lens is intended to form an image converging rays between green and red, as
shown in Appendix Fig. 2, while an apochromatic lens is designed so that rays in a range of red,
green, and purple converge to form an image.

Appendix Fig. 2 Schematic Diagrams of Differences in Aberration with Lens Systems

(2) Spherical aberration
In addition to chromatic aberration, another cause is involved in an unclear image. Even if the
light that enters a spherical lens is monochromatic, the image formed by rays brought to focus by
the central part does not coincide with that formed by rays focused by the outer portions of the
lens. Although some design considerations are given to correct the spherical aberration, it is
impossible to obtain an image perfectly free from the defect.
An achromatic lens corrects green light, and an apochromatic lens corrects green and purple
lights, as shown in Appendix Fig. 2.

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(3) Achromatic objective lens
Achromatic lenses are most commonly used as the objective lens of a microscope. They are
relatively free from aberration and are also inexpensive.
As objective lenses of metallurgical microscopes, those which are of various focal distances are
constructed.
Typical ones have a focal distance in a range between 32 and 1.8 mm with a magnification
varying from 4 to 97.
Achromatic objective lenses are made to correct both chromatic and spherical aberrations,
however, they cannot correct aberrations due to a light comprising all wavelengths.
Consequently, the use of a filter for mid-range wavelengths of visible light (yellow to green) is an
effective means of obtaining an image with no aberration.
Red and purple filters should not be used.
(4) Apochromatic objective lens
The apochromatic objective lens corrects aberration quite well, however, it has a drawback that it
is highly priced.
Lenses of this kind not only produce minimum aberration, but also are of a high numerical
aperture compared with achromatic lenses. Magnification by the apochromatic objective lens is
high. It therefore excels as an objective lens of a microscope.
(5) Plan lens
The image plane produced by a common lens is not a perfect plane, but is a slightly curved one.
As such, the focal point gradually varies in shifting the view from the central part of the visual
field to the outer portions.
This effect is inconvenient to the observation of an entire visual field, which is the reason of the
construction of objective lenses that correct the flatness of the image plane. Lenses of this type
are called "plan lens" and are marked as "M Plan X."
The plan lens is recommended especially for microphotography, as well as for general
examination.

3. Eyepiece
Eyepieces are intended to magnify the image formed by an objective lens. Their intrinsic
magnifications are such as 5, 7.5, 10, and 15, which are usually indicated on each lens.
Eyepieces are classified into the following three kinds.
(1) Huygens eyepiece
Constructed of two lenses plane and convex between which a diaphragm is placed. In
general, eyepieces of this kind are used together with an achromatic objective lens of low
magnifying power.
(2) Compensating eyepiece
In combination with an apochromatic objective lens, a compensating eyepiece corrects
aberration and forms a clear image, which the single use of an objective lens cannot manage
sufficiently.
The compensating eyepiece combined with an achromatic objective lens of a high magnification
yields a better result than the Huygens eyepiece.
(3) Projection eyepiece
Projection eyepieces, which minimize the curvature of the image plane, are used for
microphotography.

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4. Magnification
Each objective lens has its intrinsic magnification. The magnifying power is marked on each
objective lens.
The intrinsic magnification (N) of an objective lens is the magnifying power attained, without using any
eyepiece, solely by the objective lens at a distance equal to the length (L) of the fitting microscope's
cylinder, and is given by the equation: N = L/f
1
, where f
1
is the focal distance of the objective lens.
Metallurgical microscopes have slightly longer cylinders due to reasons related to illumination.
Accordingly, their lenses, even with the same focal distances as that of the lenses of biological
microscopes, are given a higher intrinsic magnification. As the eyepiece further magnifies the image
magnified by the objective lens, the magnification of an eyepiece is also an important factor. The
value is marked on the eyepiece according to microscope type. The intrinsic magnification (V) of an
eyepiece is given by the equation: V = S/f
2
, where S is the least distance of distinct vision (250 mm,
typically), and f
2
is the focal distance of the lens system.
The general magnification Vg of the microscope is determined by:

Vg = N V = L/f
1
S/f
2
(1)

N and V are indicated on the microscope so the magnification is obtained by multiplying N and V.
If, however, the least distance of distinct vision differs, the equation brings about a somewhat different
value.
The magnification involved in microphotography differs from the magnification of distinct vision in
general.
The magnification of microphotography N' is determined by:

N' = N b/S = N b/250S = 250 (mm) (2)

where, N: magnification of distinct vision
b: camera length (distance between eyepiece lens and ground glass)
S: least distance of distinct vision

If the camera length is 250 mm the magnification of microphotography equals the magnification of
distinct vision. A longer bellows produces a higher magnification, and a shorter one, a lower
magnification. One of the most readily available methods of determining the magnification of
microphotography is the use of a micrometer for that specific purpose. The micrometer is
constructed by graduating lines in intervals of 0.01 mm on a metal plane. By placing it under a
microscope instead of a specimen, forming its magnified image on the ground glass, and measuring
the line intervals in the image with a common scale, the magnification of the microphotograph under
that conditions is known. Next by replacing the micrometer with a specimen under the same settings
and focusing the image, it is possible to take a photograph of the same magnification as determined in
the previous procedure.

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5. Resolving Power
In attaining a higher magnification with a microscope, increasing the magnifying power of the eyepiece
is effective as illustrated by equations (1) and (2).
In so doing, however, it is intended to examine more minute structures, so simple enlargement of an
image is meaningless.
What is vital in the magnification by microscope of two close points on the specimen surface is the
limit that the microscope can clearly separate them.
The finer the limit of a microscope, the clearer the minute structures. This limit is called the resolving
power. A high resolving power means a finer limit. The resolving power is an important value that
reveals the property of a lens system. Factors that determine the degree of resolving power are the
wavelengths of light involved and a constant, called the numerical aperture of the objective lens.

6. Numerical Aperture
An object with a rough surface reflects light in all directions.
Of the reflected light, that enters the naked eye is only an extremely small flux of light. If a lens is
used, however, far more rays of light can be converged than with the naked eye.
The aim of importance with the objective lens is to form a magnified image, collecting more light than
the naked eye is capable of collecting.
Of the light reflected from a point on the specimen on the optical axis of the objective lens, that within
a cone defined by apical angle R
1
R
1
enter the lens as shown in Appendix Fig. 3.
Consequently, the numerical aperture of an objective lens is a figure that indicates the capacity of the
lens to collect the light.
The angle at which the light reflected by the specimen enters the lens depends on the refraction index
of the medium between the specimen and lens.
Appendix Fig. 3-a represents a case that air (n = 1.0) is present between the lens and specimen. If it
is assumed that a liquid with a higher refraction index than air is present in that space, the light
proceeds as shown in Appendix Fig. 3-b. If n = 1.5, where n is the refraction index of the medium,
the light that enters the lens equals that indicated by R
2
R
2
in Appendix Fig. 3-a, so more light enters
the lens than in the case of air.
The NA (Numerical of Aperture) is given by the equation below.

NA = n sin (3)

Appendix Fig. 3 Schematic Diagrams of the Numerical Aperture of Dry and Oil-Immersion Lenses

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In the example shown in Appendix Fig. 3-a, = 30 and n = 1.00, hence, NA = 1.00 sin 30
= 0.5. In the case of b, = 30 and n = 1.50, hence, NA = 0.75.
Oil-immersion systems are used as high-magnification objective lens for the reason explained above.
Cedar oil (oil extracted from a kind of cedar tree; n = 1.50) is usually used as the medium.
The numerical aperture value is marked on the lens together with its magnification.
The minimum distance on the specimen surface between two close points that can be separated
by a microscope is obtainable from equation (4):

NA 2
=

----- (4)

As illustrated by equation (4), is proportional to the wavelength of the light involved and in inverse
proportion to the numerical aperture of the objective.
Hence the shorter the wavelength of the light involved and the greater the NA of the objective lens
used, the clearer the minute structures. If the numerical aperture and intrinsic magnification of the
objective lens used are 1.00 and 100, respectively, and green light ( = 0.00053 mm) is involved,
two points apart from each other by at least = 0.000265 mm are distinct, but points within this
distance cannot be separated.
To the naked eye and at a distance of 250 mm, two points are not identified unless they are separated
from each other at least by 0.11 mm.
In order for the naked eye with an objective lens with an intrinsic magnification of 100 to identify two
points separated from each other by 0.000265 mm, an eyepiece with at least 4 intrinsic
magnification is required since 0.11/(0.00026 100) 4.
In the above case, the use of the objective lens is effective only when a magnification of 400 at the
minimum is attained.
In general, in applications of objective lenses with different numerical apertures, magnification should
be 400 times or more the numerical aperture of the objective lens in use, in order to make best use of
the resolving power of the objective lens.
As narrowing the aperture too far reduces the numerical aperture, it is correct in using a microscope
not to let the aperture become smaller than its proper value.
Usually magnifications are set so that they are 500 to 1000 times greater than the numerical aperture,
however, it is recommended to keep magnifications below 1000 times greater than the numerical
aperture. Since the numerical aperture of the objective lens is limited, a light of shorter wavelengths,
namely, bluish light, should be used if it is intended to examine minute structures clearly with a higher
magnification.
Even if a longer cylinder is used, an eyepiece of higher magnification is set, or an enlarged photo is
taken, there is a certain limit to the visibility of minute structures. Enlargement of these kinds is
referred to as "idiot magnification."

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What are the main steps involved in metallographic sample preparation?

What are some important considerations when using an etching solution?

NOTES: The recipient of this standard shall undertake the following confidentiality obligations upon the receipt of this

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