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Designation: E 986 – 97

AMERICAN SOCIETY FOR TESTING AND MATERIALS


100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Practice for


Scanning Electron Microscope Beam Size Characterization1
This standard is issued under the fixed designation E 986; 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 4. Significance and Use


1.1 This practice provides a reproducible means by which 4.1 The traditional resolution test of the SEM requires, as a
one aspect of the performance of a scanning electron micro- first step, a photomicrograph of a fine particulate sample taken
scope (SEM) may be characterized. The resolution of an SEM at a high magnification. The operator is required to measure a
depends on many factors, some of which are electron beam distance on the photomicrograph between two adjacent, but
voltage and current, lens aberrations, contrast in the specimen, separate edges. These edges are usually less than one millime-
and operator-instrument-material interaction. However, the tre apart. Their image quality is often less than optimum.
resolution for any set of conditions is limited by the size of the Operator judgment is dependent on the individual acuity of the
electron beam. This size can be quantified through the mea- person making the measurement and can vary significantly.
surement of an effective apparent edge sharpness for a number 4.2 Use of this practice results in SEM electron beam size
of materials, two of which are suggested. This practice requires characterization which is significantly more reproducible than
an SEM with the capability to perform line-scan traces, for the traditional resolution test using a fine particulate sample.
example, Y-deflection waveform generation, for the suggested
materials. The range of SEM magnification at which this 5. Suggested Materials
practice is of utility is from 1000 to 50 000 3 . Higher 5.1 SEM resolution performance as measured using the
magnifications may be attempted, but difficulty in making procedure specified in this practice will depend on the material
precise measurements can be expected. used; hence, only comparisons using the same material have
1.2 This standard does not purport to address all of the meaning. There are a number of criteria for a suitable material
safety concerns, if any, associated with its use. It is the to be used in this practice. Through an evaluation of these
responsibility of the user of this standard to establish appro- criteria, two samples have been suggested. These samples are
priate safety and health practices and determine the applica- nonmagnetic; no surface preparation or coating is required;
bility of regulatory limitations prior to use. thus, the samples have long-term structural stability. The
sample-electron beam interaction should produce a sharply
2. Referenced Documents rising signal without inflections as the beam scans across the
2.1 ASTM Standards: edge. Two such samples are:
E 7 Terminology Relating to Metallography2 5.1.1 Carbon fibers, NIST—SRM 2069B.3
E 766 Practice for Calibrating the Magnification of a Scan- 5.1.2 Fracture edge of a thin silicon wafer, cleaved on a
ning Electron Microscope2 (111) plane.
3. Terminology 6. Procedure
3.1 Definitions: For definitions of terms used in this prac- 6.1 Inspect the specimen for cleanliness. If the specimen
tice, see Terminology E 7. appears contaminated, a new sample is recommended as any
3.2 Definitions of Terms Specific to This Standard: cleaning may adversely affect the quality of the specimen edge.
3.2.1 Y-deflection waveform—the trace on a CRT resulting 6.2 Ensure good electrical contact with the specimen by
from modulating the CRT with the output of the electron using a conductive cement to hold the specimen on a SEM
detector. Contrast in the electron signal is displayed as a stub, or by clamping the specimen on the stage of the SEM.
change in Y (vertical) rather than brightness on the screen. This Mount the specimen rigidly in the SEM to minimize any image
operating method is often called Y-modulation. degradation caused by vibration.
6.3 Verify magnification calibration for both X and Y direc-
tions. This can be accomplished by using Practice E 766.
6.4 Use a clean vacuum of 1.33 by 10− 2 Pa (10− 4 mm Hg)
1
This practice is under the jurisdiction of ASTM Committee E-4 on Metallog- or better to minimize specimen contamination resulting from
raphy and is the direct responsibility of Subcommittee E04.11 on X-Ray and
Electron Metallography.
Current edition approved Oct. 10, 1997. Published December 1997. Originally
published as E 986 – 84. Last previous edition E 986 – 92. 3
Available from National National Institute of Standards and Technology,
2
Annual Book of ASTM Standards, Vol 03.01. Gaithersburg, MD 20899.

1
E 986
electron beam and residual hydrocarbons interacting during 6.13 Rotate the specimen, not the scan, and shift the field of
examination. The presence of a contamination layer has a view on the specimen so that the desired edge is oriented
deleterious effect on image-edge quality. perpendicular to the horizontal scan direction near the center of
6.5 Allow a minimum of 30 min for stabilization of elec- the CRT.
tronic components. The selection of optimum SEM parameters 6.14 Make sure that no gamma or derivative processing is
is at the discretion of the operator.4 employed.
6.6 Select electron gun voltage within the desired range of 6.15 Obtain a line-trace photograph across the desired edge
operating conditions. using a recording time of at least 2 s and a bandwidth of 4 kHz
(if SEM is equipped with bandwidth control). (See Fig. 2.)
NOTE 1—The performance measurement must be repeated for each kV
setting used. 6.15.1 Caution—Slow scan rates in the line-trace mode
may cause burning of the CRT-screen phosphor for improperly
6.7 Saturate the filament and check both filament and gun adjusted SEM-CRT screens.
alignment for any necessary adjustment. 6.16 Locate the maximum and minimum Y-axis deflections
6.8 Set all lens currents at a resettable value with the aid of across the edge of the specimen in the line-trace photograph.
a suitable digital voltmeter, if available. (See Fig. 2.)
6.9 Cycle lens circuits OFF-ON two to three times to 6.17 The difference between these values is the full-edge
minimize hysteresis effects. An alternate procedure may be contrast produced in the line trace. From this contrast value,
used to drive the lens through a hysteresis loop—increase compute the Y-axis positions that correspond to contrast levels
current above operating current, decrease below operating of 20 and 80 % of the full-contrast value.
current, then back up to operating current.
6.10 Adjust lens apertures and stigmator for optimum reso- 20 % level 5 0.2 3 ~gmax 2 gmin ! 1 gmin (1)
lution (minimum astigmatism). Because of its higher resolu- 80 % level 5 0.8 3 ~gmax 2 gmin ! 1 gmin (2)
tion, the secondary electron imaging mode is most commonly 6.17.1 These levels are illustrated schematically on Fig. 2.
used. This procedure may also be used to characterize SEM Locate these positions in the line-trace photograph and mea-
performance in the backscattered electron imaging mode. sure the horizontal distance (D) in mm on the photograph
6.11 Locate a field on the chosen specimen that shows the between these points. The slope of the line trace should have a
desired edge detail. (See Fig. 1.) ratio (Y/D) of 2 to 4. The distance (D) should range between 2
6.12 Select the highest magnification that is sufficient to to 4 mm. The performance parameter (P), expressed in
allow critical focusing of the image and shows image-edge nanometres, is then defined as follows:
transition from white to black contrast (for example, fuzziness)
of at least 5-mm horizontal width in the photographed image. P 5 ~D 3 106!/M (3)
where M is the SEM calculated and corrected magnification
4
using an acceptable standard.
Newbury, D. E., “Imaging Strategy for the SEM–A Tutorial,” SEM, Vol. 1,
1981, pp. 71–78.
6.18 Photograph the field selected for later reference to aid
in the location of the image edge used for the performance
measurement.
6.19 Repeat the line-trace photograph and measurement
process outlined in 6.15 through 6.17 at two additional edges in
the material studied. Three waveform traces using a graphite-
fiber edge are shown in Fig. 3.
6.20 Average the three results to produce the performance
parameter (P).

FIG. 1 Edge of Graphitized Natural Cellulose Fiber Used to FIG. 2 Typical Waveform With 20 and 80 % Contrast Levels
Produce Line Traces (Fig. 3) Illustrated

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E 986
value for the precision and bias of the performance test based
on extensive experience. However, the sources of error and
their best estimates of uncertainties at a SEM magnification of
80 to 100 000 3 under controlled operating conditions and
with experienced operators, are as follows:
Source Uncertainty, %

SEM magnification (M) 610


Measurement variation between 62
operators
Measurement of waveform (D) 62
Approximate overall uncertainty 11

8. Reproducibility
8.1 Reproducibility of the performance parameter may be
determined by repeating the steps in Section 6 at intervals
determined by the user’s requirements. Measurement of per-
formance is recommended after repair or realignment of the
electron optical functions or after major changes in instrument-
operating parameters, for example, beam voltage or lens
settings, or both. A listing of instrument parameters that
influence the performance is included in the Annex of Practice
FIG. 3 Set of Waveforms Measured to Determine Performance E 766.
Parameter (P) (Eq 1)
9. Keywords

@P 5 ~P1 1 P2 1 P3!#/3 (4)


9.1 edge sharpness; electron beam size; E766; graphite
fiber; magnification; NIST–SRM 2069B; performance; SEM;
7. Precision and Bias specimen interaction; waveform
7.1 At the present time, it is not possible to give a specific

The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

3
SI QUICK REFERENCE GUIDE:
International System of Units (SI)
The Modernized Metric System*
UNITS
The International System of Units (SI) is based on seven fundamental (base) units:
Base Units
Quantity Name Symbol
length metre m
mass kilogram kg
time second s
electric current ampere A
thermodynamic temperature kelvin K
amount of substance mole mol
luminous intensity candela cd

and a number of derived units which are combinations of base units and which may have special
names and symbols:
Examples of Derived Units
Quantity Expression Name Symbol
acceleration
angular rad/s2
linear m/s2
angle
plane dimensionless radian rad
solid dimensionless steradian sr
area m2
Celsius temperature K degree Celsius °C
density
heat flux W/ m 2
mass kg/m3
current A/ m2
energy, enthalpy
work, heat N•m joule J
specific J/ kg
entropy
heat capacity J/ K
specific J/ (kg•K)
flow, mass kg/s
flow, volume m3 /s
force kg • m/s2 newton N
frequency
periodic 1/s hertz Hz
rotating rev/s
inductance Wb/A henry H
magnetic flux V •s weber Wb
mass flow kg/s
moment of a force N•m
potential,electric W/A volt V
power, radiant flux J/s watt W
pressure, stress N/ m2 pascal Pa
resistance, electric V/A ohm Ω
thermal conductivity W/(m • K)
velocity
angular rad/s
linear m/s
viscosity
dynamic (absolute)(µ) Pa • s
kinematic (ν) m2 /s
volume m3
volume, specific m3 / kg

*For complete information see IEEE/ASTM SI-10.


SI QUICK REFERENCE GUIDE

SYMBOLS
Symbol Name Quantity Formula
A ampere electric current base unit
Bq becquerel activity (of a radio nuclide) 1/s
C coulomb electric charge A• s
°C degree Celsius temperature interval °C = K
cd candela luminous intensity base unit
F farad electric capacitance C/ V
Gy gray absorbed dose J / kg
g gram mass kg / 1000
H henry inductance Wb/A
Hz hertz frequency 1/s
ha hectare* area 10 000 m2
J joule energy, work, heat N•m
K kelvin temperature base unit
kg kilogram mass base unit
L litre volume m3/1000
lm lumen luminous flux cd • sr
lx lux illuminance lm /m 2
m metre length base unit
mol mole amount of substance base unit
N newton force kg • m /s2
Ω ohm electric resistance V/A
Pa pascal pressure, stress N/m2
rad radian plane angle m/m (dimensionless)
S siemens electric conductance A/ V
Sv sievert dose equivalent J/ kg
s second time base unit
sr steradian solid angle m 2 /m 2 (dimensionless)
T tesla magnetic flux density Wb / m 2
t tonne, metric ton mass 1000 kg; Mg
V volt electric potential W/A
W watt power, radiant flux J/s
Wb weber magnetic flux V •s
*allowed with SI

Use of Symbols Exception: No space is left between the numerical value


The correct use of symbols is important because an incorrect sym- and symbol for degree of plane angle.
bol may change the meaning of a quantity. Some SI symbols are Examples: 73°, not 73 °
listed in the Symbol table. Note: Symbol for for coulomb is C; for degree Celsius it is °C
SI has no abbreviations—only symbols. Therefore, no periods
follow a symbol except at the end of a sentence. Do not mix symbols and names in the same expression.
Examples: A, not amp; s, not sec; SI, not S.I. Examples: radians per second or rad /s
not radians /second; not radians /s
Symbols appear in lower case unless the unit name has been taken m/s or metres per second,
from a proper name. In this case the first letter of the symbol is not metres /second; not metres /s
capitalized. J/kg or joules per kilogram,
Examples: m, metre; Pa, pascal; W, watt not joules /kilogram; not joules /kg
Exception: L, litre Symbol for product—use the raised dot ( • )
Symbols and prefixes are printed in upright (roman) type regard- Examples: N • m; mPa • s; W/(m2 • K)
less of the type style in surrounding text.
Symbol for quotient—use one of the following forms:
Example: . . . a distance of 73 km between . . .
Examples: m/s or m s or use negative exponent
Unit symbols are the same whether singular or plural. Note: Use only one solidus ( / ) per expression and parentheses to
Examples: 1 mm, 100 mm; 1 kg, 65 kg avoid any ambiguity.
Leave a space between the value and the symbol. Do not use modifying terms such as electrical, alternating
Examples: 115 W, not 115W; 0.75 L, not 0.75L current, etc.
88 °C, not 88°C or 88° C Examples: kPa (gage); MW (e); V (ac)
SI QUICK REFERENCE GUIDE

PREFIXES Exponential Powers. An exponent attached to a symbol containing


a prefix indicates that the multiple (of the unit with its prefix) is
Most prefixes indicate orders of magnitude in steps of 1000 and raised to the power of 10 expressed by the exponent.
provide a convenient way to express large and small numbers and to
Examples: 1 mm3 = (10 -3 m) 3 = 10 -9 m3
eliminate nonsignificant digits and leading zeros in decimal fractions.
1 ns-1 = (10 -9 s) -1 = 10 9 s -1
Examples: 64 000 watts is the same as 64 kilowatts* 1 mm2 /s = (10 -3 m)2/s = 10 -6 m2/s
0.057 metre is the same as 57 millimetres
16 000 metres is the same as 16 kilometres*
*except for intended accuracy
Prefix Symbol Represents
NUMBERS
yotta Y 1024 International practice separates the digits of large numbers into
zetta Z 1021
exa E 1018 groups of three, counting from the decimal to the left and to the
peta P 1015 right, and inserts a space to separate the groups. In numbers of four
tera T 1012 digits, the space is not necessary except for uniformity in tables.
giga G 109
mega M 106 Examples: 6.358 568; 85 365; 51 845 953; 88 000;
kilo k 103 0.246 113 562; 7 258
hecto h* 102
deka da* 101 Small Numbers. When writing numbers less than one, always put
deci d* 10-1 a zero before the decimal marker.
centi c* 10-2 Example: 0.046
milli m 10-3
micro µ 10-6 Decimal Marker. The recommended decimal marker is a dot on
nano n 10-9 the line (period). (In some countries, a comma is used as the
pico p 10-12
decimal marker.)
femto f 10-15
atto a 10-18 Because billion means a million million in most countries but a
zepto z 10-21
thousand million in the United States, avoid using billion in
yocto y 10-24
technical writing.
To realize the full benefit of the prefixes when expressing a quan-
tity by numerical value, choose a prefix so that the number lies be-
tween 0.1 and 1000. For simplicity, give preference to prefixes rep-
resenting 1000 raised to an integral power (i.e., µm, mm, km). DO’S AND DON’TS
*Exceptions: The units in the international system of units are called SI units—
In expressing area and volume, the prefixes hecto, deka, not Metric Units and not SI Metric Units.
deci, and centi may by required; for example, cubic
decimetre (L), square hectometre (hectare), cubic Non-SI units in the US are called Inch-Pound units (I-P units)—not
centimetre. conventional units, not U.S. customary units, not English units, and
not Imperial units.)
Tables of values of the same quantity.
Comparison of values. Treat all spelled out names as nouns. Therefore, do not capitalize
the first letter of a unit except at the beginning of a sentence or in
For certain quantities in particular applications. For example,
capitalized material such as a title.
the millimetre is used for linear dimensions in architectural
and engineering drawings even when the values lie far Examples: watt; pascal; ampere; volt; newton; kelvin
outside the range of 0.1 mm to 1000 mm; the centimetre is Exception: Always capitalize the first letter of Celsius.
usually used for anatomical measurements and clothing Do not begin a sentence with a unit symbol—either rearrange the
sizes. words or write the unit name in full.
Compound units. A compound unit is a derived unit expressed with Use plurals for spelled out words when required by the rules of
two or more units. The prefix is attached to a unit in the numerator. grammar.
Examples: V/m not mV/mm
MJ/kg not kJ/g Examples: metre—metres; henry—henries;
kilogram—kilograms; kelvin—kelvins
Compound prefixes formed by a combination of two or more pre- Irregular: hertz—hertz; lux—lux; siemens—siemens
fixes are not used. Use only one prefix.
Do not put a space or hyphen between the prefix and unit name.
Examples: 2 nm not 2 mµm
6 m3 not 6 kL Examples: kilometre not kilo metre or kilo-metre;
6 MPa not 6 kkPa milliwatt not milli watt or milli-watt
SI QUICK REFERENCE GUIDE

When a prefix ends with a vowel and the unit name begins with a Multiply By To Obtain
vowel, retain and pronounce both vowels. ft lbf (work)
• 1.36 J
Example: kiloampere ft • lb f / lb (specific energy) 2.99 J/kg
Exceptions: hectare; kilohm; megohm ft • lb f / min (power) 0.0226 W
gallon, US (*231 in 3) 3.785 L
When compound units are formed by multiplication, leave a space gph 1.05 mL/s
between units that are multiplied. gpm 0.0631 L /s
gpm /ft 2 0.6791 L /(s • m2 )
Examples: newton metre, not newton-metre; gr /gal 17.1 g /m3
volt ampere, not volt-ampere horsepower (550 ft • lbf / s) 0.746 kW
inch *25.4 mm
Use the modifier squared or cubed after the unit name. in of mercury (60°F) 3.377 kPa
Example: metre per second squared in of water (60°F) 248.8 Pa
in •lbf (torque or moment) 113 mN • m
Exception: For area or volume the modifier may be placed
in2 645 mm2
before the units. in3 (volume) 16.4 mL
Example: square millimetre; cubic metre in3 (section modulus) 16 400 mm3
in4 (section moment) 416 200 mm4
When compound units are formed by division, use the word per, not km / h 0.278 m/ s
a solidus ( / ). kWh *3.60 MJ
Examples: metre per second, not metre / second; watt per kip / in2 (ksi) 6.895 MPa
square metre, not watt / square meter litre *0.001 m3
micron (µm) of mercury (60°F) 133 mPa
Do not use modifying terms such as electrical, alternating current, mil (0.001 in.) *25.4 µm
etc. after the symbol. mile 1.61 km
mile, nautical 1.85 km
Examples: kPa (gage); MW (e); V (ac) mph 1.61 km/ h
mph 0.447 m /s
millibar *0.100 kPa
mm of mercury (60°F) 0.133 kPa
mm of water (60°F) 9.80 Pa
SELECTED CONVERSION FACTORS ounce (mass, avoirdupois) 28.35 g
ounce (force of thrust) 0.278 N
CAUTION: These conversion values are rounded to three or four significant
ounce (liquid, US) 29.6 mL
figures, which is sufficiently accurate for most applications. When making
ounce (avoirdupois) per gallon 7.49 kg/m 3
conversions, remember that a converted value is no more precise than the
original value. Round off the final value to the same number of significant pint (liquid, US) 473 mL
figures as those in the original value. See ANSI SI 10 for additional conver- pound
lbm (mass) 0.4536 kg
sions with more significant figures.
lbm (mass) 453.6 g
lbf (force or thrust) 4.45 N
Multiply By To Obtain lbm / ft (uniform load) 1.49 kg/m
acre 0.4047 ha lbm /(ft • h) (dynamic viscosity, µ ) 0.413 mPa •s
atmosphere, standard *101.325 kPa lbm / (ft • s) (dynamic viscosity, µ) 1490 mPa •s
bar *100 kPa lbf • s / ft2 (dynamic viscosity, µ) 47 880 mPa •s
barrel (42 US gal, petroleum) 159 L lbm /min 0.00756 kg/s
Btu, (International Table) 1.055 kJ lbm / h 0.126 g/s
Btu / lb •°F (specific heat, c p ) 4.184 kJ/(kg • K) lbf / ft2 47.9 Pa
bushel 0.03524 m3 lbm / ft2 4.88 kg/m 2
calorie, kilogram (kilocalorie) 4.187 kJ lbm / ft3 (density, ρ) 16.0 kg/m 3
candle, candlepower *1.0 cd lbm / gallon 120 kg/m 3
centipoise, dynamic vicosity, µ *1.00 mPa •s ppm (by mass) *1.00 mg/kg
centistokes, kinematic viscosity, ν *1.00 mm2/s psi 6.895 kPa
ft *0.3048 m quad (1015 Btu) 1.06 EJ
ft *304.8 mm quart (liquid, US) 0.946 L
ft / min, fpm *0.00508 m/ s rpm 0.105 rad / s
ft / s, fps *0.3048 m /s tablespoon (approx.) 15 mL
ft of water 2.99 kPa teaspoon (approx.) 5 mL
ft 2 0.09290 m2 therm (100,000 Btu) 105.5 MJ
ft 2/s, kinematic viscosity, ν 92 900 mm2 /s ton, short (2000 lb) 0.907 Mg; t (tonne)
ft 3 28.32 L yd *0.9144 m
ft 3 0.02832 m3 yd2 0.836 m2
ft 3/h, cfh 7.866 mL/s yd3 0.7646 m3
ft 3/min, cfm 0.4719 L/s
ft3 /s, cfs 28.32 L/s
footcandle 10.76 lx *Conversion factor is exact.
ft • lb f (torque or moment) 1.36 N •m Note: In this list the kelvin (K) expresses temperature intervals.
The degree Celsius symbol (°C) may be used for this purpose as well.

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