AlllQS IStSSfi PUBLICATIONS

NIST SPECIAL PUBLICATION 400-99

U.S. DEPARTMENT OF COMMERCE/Technology Administration

National Institute of Standards and Technology

Semiconductor Measurement Technology:

The Results of an Interlaboratory Study

of EUipsometric Measurements

of Thin Film Silicon Dioxide on Silicon

QQ Barbara J. Belzer and David L. Blackburn

100

.U57

NO.W-99

1997

Semiconductor Measurement Technology:

The Results of an Interlaboratory Study of Ellipsometric

Measurements of Thin Film Silicon Dioxide on Silicon

Barbara J. Belzer and David L. Blackburn

Semiconductor Electronics Division

Electronics and Electrical Engineering Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

May 1997

U.S. DEPARTMENT OF COMMERCE, William M. Daley, Secretary

TECHNOLOGY ADMINISTRATION, Mary L. Good, Under Secretary for Technology

NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, Robert E. Hebner, Acting Director
National Institute of Standards and Technology Special Publication 400-99

Natl. Inst. Stand. Technol. Spec. Publ. 400-99, 30 pages (May 1997)

CODEN: NSPUE2

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 1997

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402-9325
TABLE OF CONTENTS

Page

Abstract 1 Key Words 1 Introduction 1 Sample Handling and Preparation 2

Results 3

Discussion 4

Conclusion 5 References 6

LIST OF TABLES

Page

1 Sample #1019-01 8

2 Sample #1019-02 11

3 Sample #1017-20 14

4 Sample #1017-23 17

5 Sample #1004-14 20

6 Sample #1004-17 23

7 Summary of the Statistical Analysis as Performed by the ASTM E69 1 Program and

as Performed Independently in the Spreadsheet 26

LIST OF FIGURES

Page

la Sample 1019-01 Thickness as Reported by the Participant 9

1 b Sample 1019-01 Thickness as Calculated by NIST 9

1 c Sample 1019-01 Measured Psi Values 10

1 d Sample 1019-01 Measured Delta Values 10

2a Sample 1019-02 Thickness as Reported by the Participant 12

2b Sample 1 0 1 9-02 Thickness as Calculated by NIST 12

2c Sample 1019-02 Measured Psi Values 13

2d Sample 1019-02 Measured Delta Values 13

3a Sample 1017-20 Thickness as Reported by the Participant 15

3b Sample 1 0 1 7-20 Thickness as Calculated by NIST 15

3c Sample 1017-20 Measured Psi Values 16

iii
LIST OF FIGURES (Cont'd.)

Page

3d Sample 1017-20 Measured Delta Values 16

4a Sample 1017-23 Thickness as Reported by the Participant 18

4b Sample 1017-23 Thickness as Calculated by NIST 18

4c Sample 1017-23 Measured Psi Values 19

4d Sample 1017-23 Measured Delta Values 19

5a Sample 1004-14 Thickness as Reported by the Participant 21

5b Sample 1 004- 1 4 Thickness as Calculated by NIST 21

5c Sample 1004-14 Measured Psi Values 22

5d Sample 1004-14 Measured Delta Values 22

6a Sample 1004-17 Thickness as Reported by the Participant 24

6b Sample 1 004- 1 7 Thickness as Calculated by NIST 24

6c Sample 1004-17 Measured Psi Values 25

6d Sample 1004-17 Measured Delta Values 25

iv
Semiconductor Measurement Technology:

THE RESULTS OF AN INTERLABORATORY STUDY OF ELLIPSOMETRIC

MEASUREMENTS OF THIN FILM SILICON DIOXIDE ON SILICON

Barbara J. Belzer and David L. Blackburn

Semiconductor Electronics Division

National Institute of Standards and Technology

Gaithersburg, MD 20899

Abstract

The results of an interlaboratory study for the measurement of thin film oxides on

silicon are presented. The study was performed by nine different laboratories using

six different types of ellipsometers made by three different manufacturers. The

purpose of the study was to establish a baseline of agreement between laboratories

for single-wavelength ellipsometric thin-film measurements. The maximum standard

deviation of the thickness calculated between laboratories using a common data

reduction method was 0.22 nm for 10 nm oxides, 0.43 nm for 50 nm oxides, and 0.32

nm for 100 nm oxides.

Key words: ellipsometry; interlaboratory; metrology; silicon; silicon dioxide; single

wavelength; thin films

Introduction

The interlaboratory study consisting of a series of controlled measurements on a selected set of SiOj on Si wafers was performed by nine different laboratories using six different types of ellipsometers

made by three different manufacturers. The purpose of the study was to establish a baseline of

agreement between laboratories for ellipsometric thin-film measurements. National Institute of

Standards and Technology (NIST) measurements were made on the High-Accuracy Ellipsometer

designed and built at NIST [1]. The measurements were made over a period of approximately 6

months, beginning in mid-August of 1993 and ending in mid-February 1994. The laboratories

reported their measured ellipsometric parameters A and the angle of incidence (nominally 70° for

all measurements), and the derived thickness of the silicon dioxide using the particular analysis

technique usually employed by the laboratory and each laboratory's "preferred" material parameters.

All measurements reported here were made at a wavelength of 633 nm. Included in this report are

1
the derived thicknesses using a common procedure and material parameters. The laboratories

participating in the study were Rudolph Research (Flanders, NJ), IBM (Essex Junction, VT),

Motorola, Inc. (Mesa, AZ), VLSI Standards (San Jose, CA), SEMATECH (Austin, TX), J.A. Woollam Co. (Lincoln, NE), Digital Equipment Corporation (Hudson, MA), Gaertner Scientific

(Chicago, IL), and NIST (Gaithersburg, MD).

Sample Handling and Preparation

The study consisted of measurements made on two wafers each of three different nominal

thicknesses (six wafers total) circulated in series from laboratory to laboratory. The nominal

thicknesses were 100 nm, 50 nm, and 10 nm. After each laboratory was finished with its measurements, the samples were sent back to NIST where a brief series of measurements were done

to assure that there were no significant changes or anomalies in the properties of the samples

throughout the study. The only cleaning of the samples was performed at NIST using a procedure

that is recommended for the NIST-produced SRMs consisting of an ethanol rinse and nitrogen blow

dry, followed by a deionized water rinse and nitrogen blow dry. The samples were routinely cleaned

after it was determined that no changes had occurred in the samples and before they were sent to the

next participating laboratory. The other participating laboratories did not clean the wafers prior to

their measurements. This procedure was used to eliminate any changes or anomalies that might be

introduced into the samples due to different cleaning procedures at the different laboratories or due

to other unforeseen occurrences. There were no significant changes in the samples observed over

the duration of the study.

The oxides on the 10 nm and 50 nm samples were grown at 950 °C in dry oxygen and annealed in

nitrogen for approximately 1 h at 1050 °C. The 100 nm oxides were grown at 1050 °C in dry

oxygen. The anneal of the 10 nm and 50 nm oxides was done in an attempt to remove differences

in the optical properties of the oxide and/or SiOj-Si interface region due to the different growth

temperatures. It was not the intent of this study, though, to investigate any such possible differences.

Each participating laboratory agreed to perform the measurements on the sample set according to the guidelines set forth as follows: The wafers were sent to each laboratory for measurement via

overnight mail from NIST only after the participant had confirmed that the wafers could be measured

within a day or two of receipt. About a one to one-and-a-half week total time frame for the "receiptto-return" cycle was requested from each participant. The wafers were returned to NIST via

overnight mail after each laboratory had completed its measurements. The wafers were not to be

cleaned by the receiving laboratory. Four replicate measurements of each wafer, with removal and

remount of the sample between replications, were to be made at the approximate center of the wafer.

There were a total of 24 individual measurements requested from each participant for this study.

Each laboratory recorded the following basic information: A, A (633 nm), angle of incidence

(70°), calculated thickness, optical constants (fixed and/or derived), and equipment type. All

participants were encouraged to provide any ancillary information which was within the scope of

their operation. Information suggested for inclusion were the calculated thickness and refractive

2
index of the film using the method and constants preferred by the participant and, if possible, the

method and constants preferred by NIST, spectroscopic ellipsometry results (A, A, and thickness

calculations), and multiple angle and/or principal angle measurements. The individually preferred

method is reported in the tables (As-Reported Thickness Values).

Results

The purpose of the study was to determine a baseline level of agreement in one-layer oxide thickness

determinations between the nine participating laboratories using as tight a control as possible on the

measurement procedure, sample preparations, and sample handling. The one-layer model of

calculated oxide thickness based on ellipsometric measurements assumes a single, homogeneous

layer of thermally grown silicon dioxide atop the silicon substrate. It is not to be implied that the

measurement, model, or handling procedures that were employed are necessarily the best or yield

the most accurate results for these measurements. The goal was to eliminate, as much as possible,

variations in results due to differences in procedures and handling. For the sake of this study, NIST

calculated individual thicknesses from the data presented by the participants using a math program

and the standard ellipsometric equations.

The measured and calculated results for the single wavelength measurements are presented in the

tables and graphs which appear at the end of the report. These results are discussed in the next

section. Each of the six tables contains the data for one sample from all of the participating

laboratories. The tables are divided into sections which list the derived thickness (As-Reported)

using each laboratory's preferred procedure and constants, the derived thickness (NIST Calculated)

using a common analysis procedure and common, fixed, optical constants for the SiOj (n = 1.461)

and Si (n = 3.875, k = 0.0156), and the measured ellipsometric parameters A and i|/ reported by each

laboratory, except for lab F which employed an ellipsometer for which individual A and ij; values

are not indicated to the instrument user.

Also included in Tables 1 through 6 are the average and the standard deviation of each laboratory's

set of four measurements on each sample, and the "grand" average and standard deviation of all laboratory average values on each sample. The average and standard deviation values that are highlighted for a few samples for a few laboratories are values that lie far enough from the values

of the other laboratories that the data "may require further investigation" according to ASTM

Standard Practice E 691 [2]. A cursory examination of these values was carried out, and it was

decided to keep all of them for the final analysis. The data in the tables are plotted in Figures 1 through 6, where each laboratory's derived or measured value is shown as a data point, the

laboratory's average values are connected by a line, and the grand average (GA) and GA ± 3s are shown.

Table 7 summarizes the statistical analysis as performed by the ASTM E 691 Interlaboratory Data

Analysis Software [3] and as performed in the spreadsheet used to tabulate the data. The column

headings in this table are defined as follows:

3
Column Heading Column Contents

Specimen ID Sample Serial Number

t nom (nm) Nominal thicknesses expressed in nanometers

Method Thickness calculation method, i.e., participant vs. NIST's

Standard method

t GA (nm) Thickness Grand Average (ASTM E 691) average of the cell

averages

s (nm) Standard deviation in nanometers of the cell averages as determined from the spreadsheet

Sr Within-laboratory Repeatability standard deviation (ASTM E

691)

SR Between-laboratory Reproducibility standard deviation

(ASTM E 691)

r (2.8 X Sr) Repeatability limits, 95% probability (ASTM E 691)

R (2.8 X SR) Reproducibility limits, 95% probability (ASTM E 691)

Discussion

Tables 1 through 6 summarize each laboratory's reported data. In the following discussion, it should

be remembered that this study was undertaken only to determine the baseline agreement between

laboratories and not to determine accuracy or preference of measurement methods.

Laboratory B was unable to complete the measurements as originally agreed upon. They were able

to complete only three replications on one wafer of each nominal thickness using single-wavelength

ellipsometry. A fourth result which was taken from spectroscopic measurements was also provided.

The information listed in the tables for Laboratory B is taken from the reported single-wavelength

data, with the fourth point being the average of the other three. While this is not as prescribed and

almost certainly affected the reproducibility statistic for the study, it was felt that the measurement

could not be discounted entirely.

An equipment problem affected the outcome of the measurements for Laboratory D, especially for

Sample #1019-01 . This participant was unable to use the ellipsometer specified for calibrations and

careful scientific procedure, but did have access to one installed in a fabrication environment. Thus,

the ellipsometer was not optimized for the type of flexibility necessary for a best scientific effort in

that its calibration and operational control were not under the direct control of the individual

participant and was therefore, not necessarily known.

Laboratory H used the wavelength, A = 633, as selected from a monochromator while all others used

a helium-neon laser source for their measurements.

4
As can be seen in Table 7, agreement between the laboratories generally improves slightly when a common or standard procedure is used in calculating the layer thickness, especially for the 1 0 nm

SiOj. The repeatability limit, r, is described as the 95% probability limit for each laboratory's

measurement repeatability. The r value ranges from a minimum of 0.05 nm for one of the 100 nm

samples to 0.25 nm for a 50 nm sample. The reproducibility limit, R, is the 95% probability limit for

the reproducible measurement results between all the participants in this study. The R value ranges

from 0.5 1 nm for a 10 nm sample to 1 .22 nm for a 50 nm sample. Overall, the calculation method

used to analyze the ellipsometry data does not seem to affect the r value and affects the R value only

slightly.

The thicknesses that are calculated are dependent upon the method used. The grand average (GA)

changes by an average of 0.14 nm (thicker) when using the "standard" or common method. It is not

within the scope of this report to give any further interpretation regarding the calculation method

other than that differences in the optical constants used significantly affect the calculated thickness.

The standard deviation of the thickness calculation between laboratories when using the individual

laboratory's preferred method ranges from a minimum of 0.29 nm for a 10 nm oxide to a maximum

of 0.44 nm for a 50 nm sample. The standard deviation of the thickness calculation between

laboratories using a common or standard method produces standard deviations which range from

a minimum of 0. 1 8 nm for a 1 0 nm oxide to a maximum of 0.43 nm for one of the 50 nm oxides.

The ranges for the standard deviation reported in a recent European-based study [4] using single

wavelength ellipsometry (SWE) are from 0.93 nm and 0.99 nm for 10 nm oxides to 0.54 and 0.58

for their 120 nm samples. The spectroscopic ellipsometry results from that study had standard

deviations in the calculated thickness from 0.54 nm and 0.74 nm for the 10 nm samples, and 0.48

nm and 0.50 nm for the 50 nm oxides, to 0.29 nm and 0.54 nm for the 120 nm artifacts. It is interesting to note that the European-based study showed a decreasing magnitude in standard

deviation between labs as the oxide increased in thickness, whereas this study seems to show no

discernible trend in either direction.

Conclusion

The study has demonstrated the within-laboratory and between-laboratory agreement that can be

achieved for thin oxide on silicon measurements using single-wavelength ellipsometry. The good

agreement that is demonstrated is likely influenced by the carefully controlled and monitored

samples (particularly as regards their cleaning), the specific measurement instructions given each

participant, and the selection of participants (calibration labs, instrument manufacturers, and others

known to understand and make careful measurements). The next task should be to determine if this

agreement can be extended into fabrication facilities where excellent tool-to-tool reproducibility is necessary.

The recent study done in Europe concluded that the "results of SWE carmot be trusted for silicon

oxide thicknesses below 20 nm" [5]. The results ofNIST's interlaboratory study do not support that

conclusion. This study shows that the magnitude in difference between thickness measurements

5
among laboratories does not need to degrade as oxide thickness decreases down to at least 1 0 nm.

It demonstrates that single-wavelength ellipsometry can be used to reliably measure oxide

thicknesses as thin as 1 0 nm if care is taken.

The Semiconductor Industry Association reported in 1994 in the Semiconductor Technology

Workshop Working Group Reports (National Technology Roadmap for Semiconductors or NTRS)

that process tolerance requirements for 9 nm gate oxides were ±0.5 nm (3 a) in 1992 and ±0.3 nm

(3a) for 6.5 rmi gate oxides in 1995. The same report projected a need in 1998 for a ±0.2 nm (3a)

process tolerance for 4.5 nm gate dielectrics [6]. To best compare these semiconductor-industrystated requirements to the between-laboratory agreement found here, one should look at the SR

and R columns of Table 7 for the 10 nm samples, Stnd (Method) row. The SR values are 0.18 nm

and 0.23 nm, and the R values are 0.51 nm and 0.63 nm for the two 10 nm samples. To best

compare the stated requirements to the within-laboratory agreement found here, one should look

at the Sr and r columns of Table 7 for the 10 nm samples, Stnd (Method) row. The Sr values are 0.03 rmi and 0.05 nm, and the r values are 0.08 nm and 0.15 nm.

The within-lab measurements here satisfy all the projected NTRS requirements through 1998

(assuming that the "absolute" measurement precision at 1 0 nm does not degrade upon going to 6 nm

thicknesses). The between-lab measurements do not meet the NTRS requirements, with both 10 nm

samples falling only slightly outside the 3 a limits stated for 9 nm gate oxides. Further work is needed on thinner samples to determine if this trend continues.

Note should be made of a round robin on oxide-thickness measurements by ellipsometry conducted

by ASTM Committee F-1 several years ago [7]. There were 1 1 laboratories involved in that study,

and the samples ranged in nominal thickness from 5 nm to 50 nm. The between-laboratory standard

deviations in thickness (Table A 1 .4 of reference 7) for that study were comparable to those found

in this study.

References

[1] Candela, G.A. and Chandler-Horowitz, D., An Ellipsometry System for High Accuracy

Metrology of Thin Films, Proc. Soc. Photo-Optical lustrum. Engrs., Integrated Circuit

Metrology II 480, 2-8 (1984).

[2] Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a

Test Method, Designation: E 691-92, American Society for Testing and Materials Committee

E-ll,May 1992.

[3] Certain commercial equipment, instruments, or materials are identified in this paper in order

to adequately specify the experimental procedure. Such identification does not imply

recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best available for

the purpose.

6
[4] Vanhellemont, J., et al.. Round Robin Investigation of Silicon Oxide on Silicon Reference

Materials for Ellipsometry, Appl. Surface Sci., 63, 45-49 (1993).

[5] Ibid., 50-51 (1993).

[6] The National Technology Roadmap for Semiconductors, Semiconductor Industry

Association, San Jose, CA, 1994.

[7] Standard Test Method for Measurement of Insulator Thickness and Refractive Index on

Silicon Substrates by Ellipsometry, Designation: F 576-90, American Society for Testing and

Materials Committee F-1, November 1990.

7
TABLE 1. SAMPLE #1019-01

Thickness (nm)

As Reported

Lab A LabB LabC LabD LabE LabG-1 LabH Labi Lao r

10.820 10.400 10.500 9.790 10.700 10.860 11.040 10.786 iU.O/U 10.836 10.400 10.600 9.850 10.800 10.840 11.050 10.640 lU.ooU 10.830 10.500 10.600 9.850 10.800 10.840 in i'xn 11.050 10.660 10.670 10.817 10.433 10.600 9.850 10.800 10.840 in R'in 11.070 10.713 in <0A

Average 10.826 10.433 10.575 10.775 10.845 1 A CI "3 J.U.5JJ 11.053 10.700- 10.678

Stnd. Dev. 0.009 0.047 0.050 0.030 0.050 0.010 0.013 0.065 0.010 GrAvg/SD 10.655 0.f33

'

NIST Calculated (one-layer) Si02 n=1.461 UbA UbB LabC LabD LabE UbG-1 LabG-2 UbH Labi

10.856 10.509 10.640 11.102 10.926 10.905 10.827 11.040 10.786 10.867 10.524 10.675 11.053 10.986 10.885 10.832 11.018 10.640 10.864 10.489 10.677 11.053 10.958 10.891 10.837 11.006 10.660 10.851 10.508 10.709 11.053 10.979 10.887 10.859 11.071 10.713 Average 10.860 10.508 10.675 11.065 10.962 10.892 10.839 11.034 10.700

Stnd. Dev. 0.007 0.014 0.028 0.025 0.027 0.009 0.014 GrAvg/SD 10.837 0.182

Lab A LabB LabC LabD UbE LabG-1 LabG-2 LabH Labi

11.512 11.500 11.540 11.400 11.550 11.512 11.538 11.500 11.509 11.518 11.470 11.500 11.400 11.510 11.517 11.539 11.480 11.524 11.514 11.520 11.540 11.400 11.510 11.517 11.541 11.470 11.548 11.510 11.497 11.540 11.400 11.520 11.520 11.544 11.460 11.520 Average 11.513 11.497 11.530 wmmm 11.523 11.517 11.541 11.478 11.525

Stnd. Dev. 0.003 0.021 0.020 0.000 0.019 0.003 0.003 0.017 0.016 GrAVG/SD 11.502 0.043 k^f'Delta (degree ^ LabA UbB LabC LabD LabE LabG-1 LabG2 LabH Labi

149.858 150.700 150.380 149.240 149.680 149.728 149.921 149.400 150.020

149.823 150.660 150.290 149.360 149.530 149.778 149.909 149.450 150.378 149.830 150.750 150.290 149.360 149.600 149.763 149.897 149.480 150.331 149.860 150.703 150.210 149.360 149.550 149.773 149.844 149.320 150.198 Average 149.843 150.703 150.293 149.330 149.590 149.761 149.893 149.413 150.232

Stnd. Dev. 0.019 0.037 0.069 0.060 0.067 0.023 0.034 0.070 \ GrAVG/SD 149.8*95 6!446 *

8
Sample 1019-01 Thickness as Reported by the Participant

11.9

11.4

uH

10.9

10.4 -

UbA UbB UbC Ub D Ub E Ub G-1 Lab G-2 Laboratory Code

Figure la

Ub H Ub I UbF

B

Meas. 1 Meas. 2

- - - Meas. 3 — O- • Meas. 4 — —Grand Average +3 s

-3 s

Sample 1019-01 Thickness as Calculated by NIST

11.2

E^ 10.8

Si I

| 10.6

10.2

10UbA UbB

1

1

i

1

1

1 1

1 ! ^ J

1 k 1

i

V

V

' \

1 UbC UbD

Laboratory Code

Figure lb

UbE UbG-l UbG-2 Ub H UbI

B

Meas. 1 - -A — Meas. 2

- - - Meas. 3 — o- . Meas. 4 +3s — —Grand Average

-3 s
Sample 1019-01 Measured Delta Values

151.5 T

^

i

:

151 -

148.5 -

148 - • • •

147.5 - t

'

t

147 -I 1i i

1

i i i UbA UbB UbC Ub D Lab E LabG-1 LabG2 Lab H Labi

Laboratory Code

Figure Id

10
TABLE 2. SAMPLE #1019-02

Thickness (nm)

As-Reported

Lab A LabB LabC LabD UbE LabG-1 LabG-2 LabH UbI LabF

10.885 10.400 10.500 10.200 10.700 11.080 11.050 11.050 11.004 10.680 10.870 10.400 10.500 10.200 10.700 11.060 11.070 11.060 10.830 10.740 10.862 10.500 10.600 10.200 10.700 11.070 11.060 11.010 10.898 10.690 10.866 10.433 10.600 10.200 10.700 11.070 11.060 11.050 10.979 10.710 Average 10.871 10.433 10.550 10.200 10.700 11.070 11.060 11.043 10.928 10.705 Stnd Dev. 0.010 0.047 0.058 0.000 0.000 0.008 0.008 0.022 0.026 GrAvg/S 10.756 0.294 ! NLST Calculated (one-layer) Si02 n = 1.461 Lab A UbB UbC LabD LabE LabG-1 LabG-2 LabH Labi

10.914 10.509 10.557 11.169 10.855 11.129 11.061 10.921 11.004

10.899 10.524 10.574 11.186 10.897 11.112 11.074 10.824 10.830

10.894 10.489 10.659 11.186 10.884 11.121 11.064 11.011 10.898

10.894 10.508 10.660 11.186 10.885 11.118 11.069 10.737 10.979 Average 10.900 10.508 10.613 11.182 10.880 11.120 11.067 iU.o / J in ooR

Stnd. Dev. 0.009 0.014 0.055 0.009 0.018 0.007 0.006 n n70 GrAvg/S To.897 0.222 1 Psi (degrees)

Lab A LabB LabC LabD LabE UbG-1 UbG-2 LabH Labi

11.529 11.500 11.500 11.440 11.530 11.557 11.583 11.520 11.567

11.526 11.470 11.500 11.440 11.540 11.562 11.590 11.540 11.590

11.521 11.520 11.500 11.440 11.520 11.562 11.580 11.510 11.593 11.528^ 11.497 11.540 11.440 11.550 11.562 11.584 11.390 11.564 Average 11.526 11.497 11.510 11.440 11.535 11.561 11.584 11.490 11.579

Stnd. Dev. 0.003 0.021 0.020 0.000 0.813 0.003 0.004 0.015 GrAvg/S 11.525 \0~Q46

1019-02 Delta (degrees)

Lab A LabB LabC LabD LabE LabG-1 LabG-2 UbH Labi

149.708 150.700 150.580 149.080 149.780 149.188 149.355 149.690 149.491 149.745 150.660 150.540 149.040 149.750 149.228 149.324 149.930 149.917 149.758 150.750 150.330 149.040 149.780 149.208 149.347 149.470 149.752 149.758 150.700 150.330 149.040 149.780 149.213 149.336 150.130 149.553 Average 149.742 150.703 150.445 149.050 149.773 149.209 149.341 149.805 149.678

Stnd. Dev. 0.024 0.037 0.134 0.020 0.015 0.017 0.013 0.194 GrAvg/S 149.749 0.542 1

11

I

I
Sample 1019-02 Thickness as Reported by the Participant

12 -I

:

i 1

i

1

i

:

9

-

8.5 -1

i i i i i i

1

i Lab A UbB Lab C Ub D Ub E UbG-1 Ub G-2 Ub H Labi Ub F Laboratory Code

Figure 2a

Sample 1019-02 Thickness as Calculated by NIST

11.8 -| 1

i

: : ^

1

Laboratory Code

Figure 2b

12
Laboratory Code

Figure 2d

13
TABLE 3. SAMPLE #1017-20

Thickness (nm)

As Reported

Lab A LabB LabC LabD UbE UbG-1 UbG-2 UbH Labi LabF

52.574 51.700 52.400 52.200 53.200 52.790 52.810 52.600 53.059 53.020 52.550 51.700 52.400 52.200 53.200 52.770 52.780 52.220 52.812 52.950 52.557 51.700 52.300 52.100 53.200 52.750 52.750 52.250 52.577 52.980 52.636 51.700 52.300 52.200 53.200 52.750 52.900 52.260 52.805 53.110 Average 52.579 51.700 52.3d0 52.175 51200 52.765 52.«i0 52.333 52.813 53.015 Stnd Dev 0.039 0.000 • 0.058 0.050 0.000 0.019 0.065 0.179 0.070 GrAVG/S 52.574 0.443 1 NIST Calculated (one-layer) Si02 m = 1,461 UbA Ub B LabC LabD LabE UbG-1 UbG-2 UbH Labi

52.709 51.675 52.536 53.044 52.573 52.972 52.852 52.923 52.694 51.697 52.487 53.166 52.555 52.953 52.827 52.695 jl.aiZ

52.691 51.578 52.301 53.117 52.555 52.938 52.795 52.797 JZ.J / / 52.764 51.650 52.350 53.117 52.567 52.932 52.952 52.852 CO one

Average 52.715 iliiSM 52.419 53.111 52.563 52.949 52.857 52.817 52.813

Stnd. Dev 0.034 0.052 0.111 0.050 0.009 0.018 0.068 0.096 GrAVG/S 52.655 0.428 Psi(degrees)

Ub A UbB LabC LabD LabE UbG-1 UbG-2 LabH Labi

23.601 23.430 23.630 23.600 23.630 23.682 23.715 23.730 23.570

23.591 23.470 23.630 23.600 23.620 23.682 23.710 23.630 23.580

23.596 23.450 23.580 23.600 23.620 23.677 23.701 23.660 23.536

23.623 23.450 23.580 23.600 23.620 23.677 23.747 23.670 23.560 Average 23.603 23.450 23.605 23.600 23.623 23.680 23.718 23.673 23.562

Stnd. Dev 0.014 0.016 0.029 0.000 - 0.005 0.003 0.020 ^iHH 0.019 GrAVG/S 23.62ri 0.078 Delta (degrees)

Lab A LabB LabC LabD UbE UbG-1 LabG-2 LabH Labi

93.635 94.410 93.790 93.400 93.760 93.458 93.571 93.520 93.334

93.643 94.410 93.880 93.400 93.770 93.473 93.589 93.660 93.540

93.648 94.500 93.960 93.360 93.770 93.483 93.611 93.590 93.713 93.600 94.410 93.920 93.400 93.760 93.488 93.505 93.550 93.540 Average 93.631 0.045

93.888 93.390 93.765 93.476 93.569 93.580 93.532

Stnd. Dev 0.021 0.073 0.020 0.006 0.013 0.046 GrAVG/S 93.696 0.314

14
Sample 1017-20 Thickness as Reported by the Participant

54.5

53.5

53 -

S 52.5

H 52

51.5

51

50.5

—

\ -9

/j i

^'"^ r

1

j

j

1 i

1

1

i i i

—a—Meas, I

• — Meas. 2

- - - Meas. 3

• o- • Meas. 4 - - +3s - ~Grand Average — - -3 s

Lab A UbB Lab C Ub D Ub E UbG-1 Ub G-2 UbH Labi UbF

Laboratory Code

Figure 3 a

Sample 1017-20 Thickness as Calculated by NIST

54.5

54

53.5

53

IsH 52 I

51.5 -

51

50.5

1

X f-v!''

— ^-*-<

[-"

Ay

1

~ 1

, 1

1 1 1

s—Meas. 1 -A - Meas. 2

• -Meas. 3 o- - Meas. 4

• - +3s —Grand Average

- -3 s

Lab A Lab B Lab C Ub D Ub E UbG-1 UbG-2 UbH UbI

Laboratory Code

Figure 3b

15
Sample 1017-20 Measured Psi Values

24

Sample 1017-20 Measured Delta Values

92.5 -

92 -

91.5 -I 1i i i i i i UbA UbB UbC Ub D Lab E UbG-1 UbG-2 Ub H Ub I

Laboratory Code

Figure 3d

16
TABLE 4. SAMPLE #1017-23

Thickness (nm)

As-Reported

LabA UbB UbC UbD UbE UbG-1 UbG-2 UbH UbI UbF

52.484 51.700 52.200 52.100 53.100 52.590 52.550 52.430 52.758 52.570 52.496 51.700 52.100 52.300 53.000 52.570 52.550 52.370 52.646 52.670 52.452 51.700 52.300 52.300 53.100 52.590 52.520 52.400 52.672 52.620 52.480 51.700 52.200 52.300 53.000 52.590 52.570 52.330 52.670 52.660 Average 52.478 51.700 52.200 52.250 53.050 52.585 52.548 52.383 52.687 52.630 GrAvg/S~ 52.451 1 0.357 NIST Calculated (one-layer) Si02 n = 1.461 Ub A UbB UbC UbD UbE UbG-1 UbG-2 UbH UbI

52.625 51.675 52.253 52.995 52.507 52.775 52.594 52.718 52.758 52.628 51.697 52.230 52.995 52.526 52.752 52.592 52.755 52.646 52.589 51.578 52.398 53.044 52.507 52.772 52.570 52.748 52.672 52.597 51.650 52.051 52.995 52.517 52.775 52.614 52.737 52.670 Average 52.610 5L650 52.233 53.007 52.514 52.769 52.593 52.740 52.687

Stnd. Dev 0.020 0.052 0.024 0.009 0.011 0.018 0.016 0.049 GrAvg/S 52.533 0.391 ^ Psi (degrees)

Ub A UbB UbC UbD UbE UbG-1 UbG-2 UbH UbI

23.571 23.430 23.580 23.600 23.630 23.617 23.631 23.650 23.554

23.578 23.470 23.540 23.640 23.620 23.620 23.636 23.650 23.540

23.563 23.450 23.580 23.640 23.620 23.622 23.631 23.660 23.543 23.576 23.450 23.500 23.640 23.620 23.627 23.634 23.640 23.537 Average 23.572 23.450 23.550 23.630 23.623 23.622 23.633 23.650 23.544

Stnd. Dev 0.007 0.016 0.020 • 0.005 0.004 0.002 0.008 0.007 GrAvg/S 23.586 0.064 Delta (degrees)

Ub A UbB UbC UbD UbE UbG-1 UbG-2 UbH UbI

93.690 94.410 94.000 93.360 93.800 93.588 93.743 93.650 93.563 93.690 94.410 94.000 93.280 93.780 93.608 93.747 93.620 93.657

93.715 94.500 93.880 93.320 93.800 93.593 93.763 93.630 93.638

93.715 94.440 94.130 93.320 93.790 93.593 93.728 93.630 93.635 Average 93.703 94.440 94.003 93.320 93.793 93.596 93.745 93.633 93.623

Stnd. Dev 0.014 0.042 0.033 0.010 0.009 0.014 0.013 0.041 GrAvg/S 93.762 0.313 ,

17
Sample 1017-23 Thickness as Reported by the Participant

54

53.5

53

52.5

« 52

laH 51.5 -

51 -

50.5 -

i

1i

1 /i

TM .m...^mm...m...!m m...m...mnm,..m..

i

i

,//

///

...^yff^.*^. \ 1 4

X i \ '

\

1

i

I

i

—e

Meas. 1 - -A- Meas. 2

• • - Meas. 3 — -O- - Meas. 4 +3s — —Grand Average

-3 s

50UbA LabB Lab C Lab D Lab E LabG-1 LabG-2 Lab H Labi Lab F

Laboratory Code

Figure 4a

Sample 1017-23 Thickness as Calculated by NIST

54

53.5

53 -

^515

B

V)

52 52

StH 51.5

51

50.5 -

>^ ' ITS >

1

' 1

1

1 50 1 Lab A LabB Lab C Lab D Ub E UbG-1 LabG-2 Ub H

Meas. 1 - -A - Meas. 2

- - • Meas. 3 — -O- Meas. 4 +3s ~~ "Grand Average

-3 s

UbI

Laboratory Code

Figure 4b

18
Sample 1017-23 Measured Psi Values

23.8

23.7

23.6 -

u 23.5

23.4 -

23.3

23.2Ub A UbB UbC LabD Ub E Lab G-1 Ub G-2 Laboratory Code

Figure 4c

Sample 1017-23 Measured Delta Values

. •>

.- ^/

•/ V ^ ^ _.(

{

/

--

;

1

i

UbH UbI

—s

Meas. 1 - -A — Meas. 2

• - • Meas. 3 - O- - Meas. 4 +3 s Grand Average

-3 s

95

94.5

94

u

u 93

92.5

92

91.5

*

1

1

.i .

i

^ 1 ^

1

1 ^

Jr

-r 11 1

'

B

Meas. 1 — -A- Meas. 2

- • - Meas. 3 - O- - Meas. 4 +3 s — —Grand Average

-3 s

Ub A UbB UbC UbD Ub E Ub G-1 Ub G-2 UbH UbI

Laboratory Code

Figure 4d

19
TABLES. SAMPLE #1004-14

Thickness (nm)

As-Reported

Lab A LabB UbC UbD UbE UbG-1 UbG-2 UbH UbI UbF

101.356 100.700 101.500 100.600 101.300 101.360 101.370 101.540 101.149 101.240 101.323 100.600 101.600 100.800 101.300 101.380 101.360 101.650 101.154 101.240 101.448 100.600 101.500 100.800 101.300 101.360 101.380 101.560 101.145 101.210 101.496 100.633 101.600 100.900 101.300 101.370 101.390 101.560 101.156 101.120 Average 101,406 100.633 101.550 100.775 101.300 101.368 101.375 101.578 10L151 101.203 Stnd._Dev 0.080 0.047 0.058 ^ '%m 0.000 0.010 0.013 0.049 0.005 0.057 GrAvg/S~ "roT.23~4~ 0.311 1 NIST Calculated (one-layer) Si02 n = 1.461 Lab A LabB LabC UbD UbE UbG-1 UbG-2 UbH UbI

101.178 100.681 101.516 101.170 101.364 101.407 101.444 101.902 101.149 101.146 100.716 101.558 101.370 101.364 101.430 101.435 t A 1 A'^A

101.970 101.154 101.275 100.749 101.508 101.312 101.294 101.472 101.457 1 A 1 OOA 101.880 101.145 101.324 100.710 101.566 101.445 101.378 101.424 101.466 lUl.SSU 101.156 Average 101.231 100.714 101.537 101.324 101.350 101.433 101.451 101.908 101.151 Stnd.Dev 0.083 0.028 0.029 0.038 0.028 0.014 A A/11 A AAf 0.005 GrAvg/S 101.344 0.321 Psi (degrees)

Lab A LabB LabC UbD UbE UbG-1 UbG-2 LabH UbI

41.970 41.640 42.130 42.000 42.070 42.112 42.117 42.390 41.984 41.952 41.660 42.170 42.120 42.070 42.123 42.113 42.430 41.987

42.023 41.660 42.130 42.080 42.030 42.115 42.123 42.370 41.983 42.050 41.653 42.170 42.160 42.080 42.120 42.130 42.370 41.989 Average 41.999 41.653 42.150 42.090 42.063 42.118 42.121 42.390 41.986

Stnd. Dev 0.045 0.009 0.023 0.022 0.005 0.007 0.028 0.003 GrAvg/S 42.063 0.193 Delta (degrees)

Lab A LabB LabC LabD UbE UbG-1 UbG-2 LabH UbI

79.008 79.370 79.330 78.720 79.090 78.963 79.094 79.110 78.755 79.010 79.370 79.210 78.720 79.090 78.983 79.087 79.120 78.755 79.048 79.540 79.290 78.760 79.080 78.968 79.109 79.160 78.739 79.063 79.427 79.250 78.760 79.080 78.978 79.097 79.160 78.744 Average 79.032 79.427 79.270 78.740 79.085 78.973 79.097 79.138 78.748

Stnd. Dev 0.027 0.052 0.023 0.006 0.009 0.009 0.026 0.008 GrAvg/"S 79.057 0.222 !

20
Sample 1004-14 Thickness as Reported by the Participant

Laboratory Code

Figure 5a

Sample 1004-14 Thickness as Calculated by NIST

Laboratory Code

Figure 5b

21
Sample 1004-14 Measured Psi Values

42.8

42.6

42.4

42.2 -

1^ 42 u

u

«^41.8

•o

'5

41.6

41.4

41.2

41

40.8Ub A

V ^

— —

^*<^ • - 7" "* —J

1. ^ _

' , N."

11

'

1 UbB UbC LabD Ub E Ub G-1 UbG-2 Ub H Laboratory Code

Figure 5 c

Sample 1004-14 Measured Delta Values

UbI

Meas. 1 Meas. 2

- - - Meas. 3 — -o- - Meas. 4 +3s — —"Grand Average

-3 s

80.25

22
TABLE 6. SAMPLE #1004-17

Thickness (nm)

As-ReportedLab A LabB LabC LabD LabE UbG-1 UbG-2 UbH UbI UbF

101.409 100.700 101.100 100.500 100.900 101.260 101.300 100.850 101.122 101.030

101.418 100.600 101.400 100.400 101.000 101.270 101.280 100.840 101.132 101.070

101.412 100.600 101.500 100.500 100.900 101.270 101.310 100.850 101.143 101.090

101.423 100.633 101.400 100.400 101.000 101.280 101.320 100.850 101.143 101.090 Average 101.416 100.633 101.350 100.450 100.950 101.270 101.303 100.848 101.135 101.070

Stnd. Dev. 0.006 0.047 0.058 0.058 0.008 0.017 0.005 0.010 0.028 GrAvg/5D 101.042 0.321

' NIST Calculated (one-layer) Si02 n= 1.461 Ub A UbB LabC LabD LabE UbG-1 UbG-2 UbH UbI

101.198 100.681 101.361 101.262 101.169 101.311 101.373 101.364 101.122

101.207 100.716 101.361 101.196 101.187 101.321 101.354 101.345 101.132

101.204 100.749 101.389 101.204 101.171 101.324 101.382 101.345 101.143 101.219 lUO.VlU 101.370 101.196 101.187 101.329 1U1.J99 —nil 'i"7A

III 1 1 j'l 101.143^ Average 101.207 m>mm

0.028

101.370 101.215 101.179 101.321 101.377 1 A1 1 TC lUl. 1 JJ

Stnd. Dev. 0.009 0.013 0.032 0.010 0.008 0.019 0.015 0.010 GrAvg/SD 101.208 0.206 Fsi (degrees)

Lab A LabB LabC LabD UbE UbG-1 UbG-2 UbH UbI

42.005 41.640 42.080 42.080 41.980 42.077 42.099 42.090 41.989

42.010 41.660 42.080 42.040 41.990 42.082 42.089 42.080 41.995

42.006 41.660 42.080 42.040 41.980 42.085 42.102 42.080 42.000

42.013 41.653 42.080 42.040 41.990 42.087 42.112 42.100 41.998 Average 42.008

0.009

42.080 42.050 41.985 42.083 42.101 42.088 41.996

Stnd. Dev. 0.003 0.006 0.004 0.009 0.010 0.005 GrAvg/SD 42.005 0.139 Delta (degrees)

Lab A UbB LabC LabD UbE UbG-1 UbG-2 UbH UbI

78.818 79.370 79.000 78.520 78.880 78.783 78.905 78.930 78.571 78.823 79.370 79.000 78.520 78.890 78.788 78.891 78.920 78.571 78.838 79.540 79.130 78.560 78.890 78.778 78.922 78.920 78.586 78.860 79.427 79.040 78.520 78.890 78.788 78.921 78.910 78.603 Average 78.834 79.427 79.043 78.530 78.888 78.784 78.910 78.920 78.583

Stnd. Dev. 0.061 0.020 0.005 0.005 0.015 0.008 0.015 GrAvg/SD 78.880 1 0.262

23
Laboratory Code

Figure 6a

Sample 1004-17 Thickness as Calculated by NIST

102.2

102.

101.$

101.6

100.4 -

I

i I- i >

100.2 -I i

, 1 , , i, UbA UbB UbC Ub D UbE UbG-1 UbG-2 LabH Ub I Laboratory Code

Figure 6b

24
Sample 1004-17 Measured Psi Values

42.6

42.4

42.2

g42. u

DO«

•S 41.8

41.6

41.4

41.2 LabA LabB Lab C Lab D Lab E UbG-1 LabG-2 UbH Ub I Laboratory Code

Figure 6c

Sample 1004-17 Measured Delta Values

—B—-Meas. 1 - -A - Meas. 2

- • • -Meas. 3 — -o- - Meas. 4 — - +3s -~ —Grand Average

80

79.5

3 79

^78.5

78.

77.5

>

/a?

://

'v

'*• >s>. '•

1

, 1 1 1

G

-Meas. 1 Meas. 2

- • • Meas. 3 — -O- • Meas. 4 +3s

'Grand Average

-3 s

UbA LabB UbC UbD LabE UbG-1 UbG-2 UbH UbI

Laboratory Code

Figure 6d

25
26
! I

I

f

I

1

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