Designation: F 110 – 00a
Standard Test Method for
Thickness of Epitaxial or Diffused Layers in Silicon by the
Angle Lapping and Staining Technique 1
This standard is issued under the fixed designation F 110; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers a procedure suitable for inter-
laboratory comparisons of layer thickness. This test method is
applicable for layers of any resistivity so long as the layer
differs from the silicon substrate under it either in conductivity
type or in resistivity by at least one order of magnitude. The
method described is destructive in nature but is more widely
applicable than the alternate infrared method, Test Method
F 95.
1.2 For layers with thicknesses between 1 and 25 µm, an
interlaboratory precision as defined in Practice E 177, of
6(0.15 T + 0.5 µm) (3S) can be achieved where T represents
thickness expressed in micrometres.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 8.
2. Referenced Documents
2.1 ASTM Standards:
E 177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods 2
F 42 Test Methods for Conductivity Type of Extrinsic
Semiconducting Materials 3
F 95 Test Method for Thickness of Lightly Doped Silicon
Epitaxial Layers on Heavily Doped Silicon Substrates
Using a Dispersive Infrared Spectrophotometer 3
2.2 SEMI Standard:
C 28 Specifications for Hydrofluoric Acid 4
C 30 Specification for Hydrogen Peroxide4
C 35 Specification for Nitric Acid4
3. Terminology
3.1 Definitions:
1
This test method is under the jurisdiction of ASTM Committee F1 on
Electronics and is the direct responsibility of Subcommittee F01.06 on Silicon
Materials and Process Control.
Current edition approved Dec. 10, 2000. Published February 2001. Originally
published as F110 – 69 T. Last previous edition F 110 – 00.
2
Annual Book of ASTM Standards, Vol 14.02.
3
Annual Book of ASTM Standards, Vol 10.05.
4
Available from the Semiconductor Equipment and Materials International, 805
E Middlefield Rd., Mountain View, CA 94043.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
1
3.1.1 diffused layer—a region of opposite conductivity type
formed near the surface of a silicon crystal as a result of the
introduction of impurities into the silicon crystal by means of
solid state diffusion.
3.1.2 epitaxial layer—in semiconductor technology, a layer
of semiconducting material having the same crystalline spacing
as the host substrate on which it is grown.
3.1.3 layer boundary—for the purpose of this test method,
the interface between the layer and substrate as revealed by this
test method.
4. Summary of Test Method
4.1 The specimen is lapped to obtain a section inclined at a
small angle to the original surface. The boundary of the layer
is revealed by a chemical stain and illuminated with mono-
chromatic light through a partially silvered optical flat to
produce interference fringes. A photomicrograph of the fringe
pattern and specimen is taken and the thickness is determined
from the number of fringes.
5. Significance and Use
5.1 Epitaxial growth and dopant diffusion processes are
used extensively in the manufacture of silicon electron devices.
Measurement of the resulting layer thickness is a key factor in
the control of these processes. Epitaxial and diffusion layer
thickness measurements are also used to determine the suit-
ability of silicon wafers for subsequent steps in electron-device
manufacture.
5.2 The thickness as determined by various methods de-
pends on the impurity profile in the layer. Therefore, the layer
thickness determined by this test method may not be equal to
the layer thickness determined in accordance with Test Method
F 95 or to the depth of the electrical junction below the surface.
5.3 The test method is suitable for process control, research
and development, and materials acceptance purposes.
6. Apparatus
6.1 Angle Lapping— A plug and plug holder which hold the
specimen at an angle of 1 to 5° (Fig. 1), flat frosted-glass
lapping plate, a hot plate, a diamond scriber, and tweezers are
required.
6.2 Etching—Containers of polyethylene or polypropylene
suitable for use with hydrofluoric acid. A low-power micro-
scope is required for checking the progress of the etch in
 F 110
FIG. 1 Lapping Plug and Holder
staining the specimen.
NOTE 1—Special consideration is necessary in choosing a microscope
used in the staining procedure. The etches used contain hydrofluoric acid,
the vapors of which will fog glass lenses. An objective lens with a long
working distance is recommended to retard this effect.
6.3 Optical Measurements:
6.3.1 A research microscope adapted for use in this proce-
dure or a special purpose two-beam interferometer is required.
Several partially silvered optical flats or microscope slides of
different transmission values, and a source of monochromatic
light such as a mercury or sodium-vapor lamp are required if a
microscope is to be adapted (Fig. 2).
6.3.2 A camera for photomicrography of the fringe pattern.
7. Reagents and Materials
7.1 Purity of Reagents—All chemicals for which specifica-
tions exist shall conform to Grade 1, SEMI specifications for
those specific chemicals. Reagents for which SEMI specifica-
tions have not been developed shall conform to the specifica-
FIG. 2 Interference Microscope
2
tions of the Committee on Analytical Reagents of the American
Chemical Society, 5 where such specifications are available.
Other grades may be used provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
7.2 Purity of Water— Reference to water shall be under-
stood to mean either distilled water, or deionized water, having
a resistivity greater than 2 MV·cm.
7.3 Compressed Air or Nitrogen—Oil free and suitable for
drying.
7.4 Etch A—Add 8 drops of nitric acid (HNO3) to 50 mL of
hydrofluoric acid (HF).
7.5 Etch B—Mix 30 mL of hydrofluoric acid (HF) and 15
mL of hydrogen peroxide (H2O 2).
7.6 Etch C—Add to 10 mL of hydrofluoric acid (HF), 4
drops of nitric acid (HNO3) and 2 drops of silver nitrate
solution.
7.7 Etch D—Add 1 to 3 drops of nitric acid (HNO3) to 20
mL of hydrofluoric acid (HF).
7.8 Glycerin.
7.9 Lapping Compound— Alumina or silicon carbide hav-
ing particle sizes in the range from 6 to 12 µm.
7.10 Mounting Wax— Glycol phthalate or a suitable wax
can be prepared from a mixture of 500 parts carnauba wax, 225
parts cherry-bark rosin, and 25 parts bee’s wax, by weight.
7.11 Polishing Compound—Alpha-phase alumina having
an average particle size of 0.3 µm.
7.12 Silver Nitrate Solution—Dissolve 2.0 g silver nitrate
(AgNO3) in water and dilute to 100 mL with water.
7.13 The recommended chemicals shall have the following
nominal assays:
Hydrofluoric acid, % 496 0.25
Hydrogen peroxide, stabilized % 30
Nitric acid, % 70 to 71
8. Safety Hazards
8.1 The acids used in this test method are extremely
hazardous. All precautions normally used with these chemicals
should strictly be observed. They should not be used by anyone
who is not familiar with the specific precautions and first aid
treatments given in the appropriate Material Safety Data
sheets.
9. Sampling
9.1 The thickness of epitaxial and diffused layers may vary
across a wafer. Initial material sampling should be such that the
details of the variation are revealed. Adequate samples may
then be taken to characterize subsequent wafers.
10. Specimen Preparation
10.1 Mounting:
10.1.1 Scribe a wafer and break a piece at least 3 by 6 mm
in size from the area of interest.
5
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
 F 110
10.1.2 Heat the plug on the hot plate. Apply a thin smooth
coat of wax to the plug in the area where the specimen is to be
mounted.
10.1.3 Firmly press the specimen into the wax, front side up,
and position it with the edge to be sectioned parallel to the apex
of the plug’s bevel surface.
10.1.4 Cool the plug by lowering it into a beaker filled with
water at room temperature.
10.2 Lapping:
10.2.1 Make a slurry by adding glycerin to the polishing
compound or lapping compound on the lapping plate. If too
much glycerin is added, the slurry will become slimy and the
lapping speed will be reduced.
NOTE 2—The polishing compound is finer and particularly suited for FIG. 3 Specimen with Superimposed Fringe Pattern
measurements of the shallowest diffusion layers where a smoother surface
is advantageous. The lapping compounds are courser, lap faster, and the
11.2 Place a partially silvered optical flat on top of the
resulting rougher surface usually stains darker. Sometimes the specimen is
polished after lapping to provide a smooth surface. specimen, silvered side down, and focus the image of the
specimen (Fig. 2).
10.2.2 Insert the plug into its holder and lap the specimen 11.3 Illuminate the specimen with monochromatic light to
using strokes only in the direction shown in Fig. 1. Continue produce a pattern of interference fringes. 6
lapping until the exposed section is approximately 1 mm wide. 11.4 Adjust the pattern of the interference fringes by mov-
10.2.3 To remove all lapping compound, rinse the plug ing the partially silvered optical flat until the fringe pattern is
thoroughly in water and dry under compressed air or nitrogen. similar to the pattern in Fig. 3.
10.3 Staining the Specimen:
10.3.1 Place the plug under a low-power microscope, illu- NOTE 4—The relative intensity of the specimen image and the fringe
minate the specimen with the microscope light so that the pattern depends on the degree of silvering on the optical flat. If the
specimen image and the fringe pattern are not both distinguishable, choose
brightness of the lapped surface is maximized, and position the an optical flat with a different degree of silvering until they can be seen as
plug. in Fig. 3.
10.3.2 Select an etch appropriate for the combination of
11.5 Take a photomicrograph of the fringe pattern and
layer and substrate conductivity types as determined by any of
specimen.
the methods of Test Methods F 42 (see Table 1).
11.6 Draw a straight line on the photomicrograph parallel to
10.3.3 Using a suitable dropping bottle, apply a drop of the
the fringes on the surface and extend the line into the lapped
selected etch to the exposed section. Watch the sample through
section to the layer boundary revealed by the stain.
the lower-power microscope to observe the staining which
11.7 Count the number of fringes which intersect the line
should be visible within a few seconds. Illuminate the speci-
between the edge of the lapped area and the layer boundary and
men continuously with the microscope light while staining is
record the number of intersections.
occurring.
10.3.4 Immerse the plug and specimen in water to stop the 12. Calculation
staining reaction immediately after the stain has revealed the
12.1 Calculate the thickness as follows:
layer boundary. Thoroughly rinse the specimen in water and
dry it in compressed air or nitrogen. If the layer boundary is t 5 n ~l/2!
distinct, proceed with the measurement of layer thickness. If
where:
the layer boundary is indistinct, repeat the lapping and staining t = thickness, µm,
procedures beginning at 10.2.2. n = number of intersections, and
NOTE 3—An indistinct boundary can result from understaining or l = wavelength of monochromatic light, µm.
overstaining. Understaining results when the staining time is too short, the
light is too dim, or the etch is too old. Overstaining results when staining 13. Precision and Bias
time is too long. Insufficient lapping which does not expose the layer 13.1 For layers between 1 and 25 µm in thickness the
boundary will also cause failure in staining.
multilaboratory precision of the measurement, as determined
11. Measurement Procedure by a round robin, in which the recommended etches were used,
was 6(0.15 T + 0.5 µm) (3S) where T is thickness. The
11.1 Place the mounted specimen on the stage of the
multilaboratory precision of the measurement when the alter-
interferometer or modified microscope (Fig. 2).
native etches are used has not been determined; however,
TABLE 1 Etch Selection Guide single laboratory precisions of 60.45 µm (3S) when the layer
Specimen Conductivity Recommended Alternative
Types Etches Etches
6
n on p or p on n A hydrofluoric acid (HF) Bond, W. L., and Smits, F. M., “The Use of an Interference Microscope for
n on n or p on p B or C D Measurement of Extremely Thin Surface Layers,” Bell System Technical Journal,
Vol 35, 1956, pp. 1209–1221.

3
 F 110
and substrate were of opposite conductivity types and6 0.9 µm 14. Keywords
(3S) when the layer and substrate were the same conductivity
14.1 angle lapping; diffused layer; epitaxial layer; etching;
type have been reported.
fringe count; staining; thickness
13.2 The bias of this test method cannot be evaluated
because there are no available reference standards suitable for
evaluating bias.

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