ASTM F358-83(1996)e1
(Test Method)Standard Test Method for Wavelength of Peak Photoluminescence and the Corresponding Composition of Gallium Arsenide Phosphide Wafers
Standard Test Method for Wavelength of Peak Photoluminescence and the Corresponding Composition of Gallium Arsenide Phosphide Wafers
SCOPE
1.1 This test method covers the techniques used to determine the wavelength of the photoluminescence peak and the mole percent phosphorus content of gallium arsenide phosphide, GaAs(1 x)Px.
1.2 Photoluminescence measurements indicate the composition only in the illuminated region and only within a very short distance from the surface, a distance limited by the penetration of the radiation and the diffusion length of the photo-generated carriers, as contrasted to X-ray measurements which sample a much deeper volume.
1.3 This test method is limited by the surface preparation procedure to application to epitaxial layers of the semiconductor grown in a vapor-phase reactor on a flat substrate. It is directly applicable to n-type GaAs(1x)Px with the wavelength, PL, of the photoluminescence peak in the range from 640 to 670 nm, corresponding to mole percent phosphorus in the range from 36 to 42 % ( x = 0.36 to 0.42). The calibration data provided for the determination of x from P L is applicable to material doped with tellurium or selenium at concentrations in the range from 1016 to 1018 atoms/cm3.
1.4 The principle of this test method is more broadly applicable. Other material preparation methods may require different surface treatments. Extension to other dopants, doping ranges or composition ranges requires further work to relate PL to the phosphorus content as determined by X-ray measurements of the precise dimensions of the unit cell upon which the calibration data are based. It is essential that calibration specimens have uniform composition in the volume sampled.
1.5 This test method is essentially nondestructive. It requires a light etching of the sample to be measured. The removal of a layer of material approximately 0.5 to 1.0 m in thickness is required. This etching does not degrade the specimen in that devices can still be fabricated from it.
1.6 This test method is applicable to process control in the preparation of materials and to materials acceptance.
1.7 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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
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e1
Designation: F 358 – 83 (Reapproved 1996)
Standard Test Method for
Wavelength of Peak Photoluminescence and the
Corresponding Composition of Gallium Arsenide Phosphide
Wafers
This standard is issued under the fixed designation F 358; 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.
e NOTE—Keywords were added editorially in February 1997.
1. Scope 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the techniques used to deter-
responsibility of the user of this standard to establish appro-
mine the wavelength of the photoluminescence peak and the
priate safety and health practices and determine the applica-
mole percent phosphorus content of gallium arsenide phos-
bility of regulatory limitations prior to use. Specific hazard
phide, GaAs P .
(1x) x
statements are given in Section 7.
1.2 Photoluminescence measurements indicate the compo-
sition only in the illuminated region and only within a very
2. Referenced Documents
short distance from the surface, a distance limited by the
2.1 ASTM Standards:
penetration of the radiation and the diffusion length of the
D 1125 Test Methods for Electrical Conductivity and Re-
photo-generated carriers, as contrasted to X-ray measurements
sistivity of Water
which sample a much deeper volume.
E 177 Practice for Use of the Terms Precision and Bias in
1.3 This test method is limited by the surface preparation
ASTM Test Methods
procedure to application to epitaxial layers of the semiconduc-
E 275 Practice for Describing and Measuring Performance
tor grown in a vapor-phase reactor on a flat substrate. It is
of Ultraviolet, Visible, and Near-Infrared Spectrophotom-
directly applicable to n-type GaAs P with the wavelength,
(1x) x
eters
l , of the photoluminescence peak in the range from 640 to
PL
2.2 SEMI Standard:
670 nm, corresponding to mole percent phosphorus in the
C1 Specifications for Reagents
range from 36 to 42 % (x 5 0.36 to 0.42). The calibration data
provided for the determination of x from l is applicable to
PL
3. Summary of Test Method
material doped with tellurium or selenium at concentrations in
16 18 3
3.1 The photoluminescence spectrum is recorded for the
the range from 10 to 10 atoms/cm .
wavelength range from 600 to 750 nm and the wavelength,
1.4 The principle of this test method is more broadly
l , at which maximum luminescence occurs is determined by
PL
applicable. Other material preparation methods may require
means of a graphical construction. The phosphorus content is
different surface treatments. Extension to other dopants, doping
then determined by means of a calibration curve relating l to
PL
ranges or composition ranges requires further work to relate
the amount of phosphorus as determined by X-ray measure-
l to the phosphorus content as determined by X-ray mea-
PL
ment of the precise dimension of the unit cell.
surements of the precise dimensions of the unit cell upon which
the calibration data are based. It is essential that calibration
4. Interferences
specimens have uniform composition in the volume sampled.
4.1 The apparent position of the photoluminescence peak
1.5 This test method is essentially nondestructive. It re-
can be distorted by the spectral response characteristics of the
quires a light etching of the sample to be measured. The
detection system, and, in particular, by the spectral response of
removal of a layer of material approximately 0.5 to 1.0 μm in
the photomultiplier. Therefore, the detector to be used for
thickness is required. This etching does not degrade the
measurements on a specific range of alloy compositions should
specimen in that devices can still be fabricated from it.
be chosen so that the corresponding range of l falls in a
PL
1.6 This test method is applicable to process control in the
region where the detector response is changing slowly.
preparation of materials and to materials acceptance.
Annual Book of ASTM Standards, Vol 11.01.
1 3
This test method is under the jurisdiction of Committee F-1 on Electronics and Annual Book of ASTM Standards, Vol 14.02.
is the direct responsibility of Subcommittee F01.15 on Gallium Arsenide. Annual Book of ASTM Standards, Vol 03.06.
Current edition approved Nov. 28, 1983. Published July 1984. Originally Available from Semiconductor Equipment and Materials Institute, 625 Ellis St.,
published as F 358 – 72 T. Last previous edition F 358 – 73 (1983). Suite 212, Mountain View, CA 94043.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
F 358
4.2 The presence of strong background radiation and, in by filtration or by positioning of the specimen with respect to
particular, of background radiation which changes rapidly with the illuminating radiation so that the specularly reflected rays
wavelength can displace the apparent position of the photolu- do not enter the collection system, or both. Fig. 1 shows a
minescence peak. Users should, therefore, assure themselves schematic diagram of a system in which the effects of the
that the background radiation is small by replacing the sample reflected illumination are minimized by suitable positioning.
with a mirror and scanning through the wavelength range of
5.2.4 Monochromator, designed to operate in the 600 to
interest. The resulting trace should be a small fraction of the
750-nm wavelength range with wavelength accuracy and
photoluminescence signal.
repeatability of 0.5 nm as determined in accordance with
4.3 Since the energy of the band gap of most semiconduc-
Practice E 275.
tors, and of GaAs P in particular, varies with temperature,
(1x) x 5.2.5 Detector—A photomultiplier tube with constant or
the measurement of l can be perturbed if the incident power
PL slowly varying spectral sensitivity throughout the range of
density from the illuminator is high enough to locally heat the
interest.
specimen. Users of this technique should, therefore, assure
NOTE 1—In the absence of data to the contrary, a variation of no more
themselves that they are not using too high a power density by
than 10 % in sensitivity in any 10-nm region of the spectral range of
measuring l as a function of incident power, by using neutral
PL
interest as determined from the manufacturer’s published sensitivity
density filters or other means. There should be no variation if
curves for the tube shall be deemed acceptable.
the power level is low enough; l will shift to longer
PL
5.2.6 Detector Electronics—Electronics capable of supply-
wavelengths with increasing power if power is excessive.
ing the high voltage required by the photomultiplier and of
5. Apparatus
detecting and amplifying the anode current from the photomul-
tiplier so that it can drive the chart-recorder electronics.
5.1 For Specimen Preparation—Chemical laboratory appa-
ratus such as plastic beakers, plastic-coated tweezers suitable 5.2.7 Detection System Sensitivity—The detection system,
for use with acids, and adequate facilities for handling and consisting of collection optics, monochromator, detector, and
disposing of acids and their vapors must be provided. detector electronics, should be capable of responding to a
−6
5.2 For Measurement of Specimen Photoluminescence (see luminescence signal of 10 mW/nm or less as calculated from
Fig. 1): the following equation:
5.2.1 Light Source, a 200-W mercury or xenon arc lamp, a
B 5 Sf /~WmTDG!
laser, or other source, with suitable filtration and focusing lens
to illuminate the specimen with radiation at a wavelength
where:
shorter than 600 nm with a total incident energy of at least 1 B 5 luminescence signal, mW/nm,
mW in an area 1 mm or less. S 5 minimum detectable signal at the output electronics,
typically 10 times the detector dark current, mA,
5.2.2 Specimen Support—A holder that can support the
f 5 the lesser of the speeds (f numbers) of the collection
specimen in such a position that the incident radiation strikes it
optics or the monochromator,
in a position t
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