X-ray or gamma ray systems or devices – Specific application – Diffraction – reflection – or scattering analysis
Reexamination Certificate
2002-04-17
2003-11-04
Dunn, Drew A. (Department: 2882)
X-ray or gamma ray systems or devices
Specific application
Diffraction, reflection, or scattering analysis
Reexamination Certificate
active
06643354
ABSTRACT:
FIELD OF THE INVENTION
X-ray reflectometry is a technique for measuring the thicknesses of thin films in semiconductor manufacturing and other applications. In order to maximize accuracy with this technique, it is necessary to precisely calibrate and align elements of the X-ray reflectometry system and the present invention relates to methods for achieving this.
BACKGROUND OF THE INVENTION
There is considerable need to accurately measure the thicknesses of thin films, particularly in the semiconductor manufacturing industry. One method for making such measurements is an X-ray reflectometry technique (“XRR”) which relies on measuring the interference patterns of X-rays scattered from a thin film sample. With XRR the reflectivity of a sample is measured at X-ray wavelengths over a range of angles. These angles typically range from zero degrees, or grazing incidence along the surface of the sample, to a few degrees. From the X-ray interference pattern, properties of the sample such as material composition and thickness can be inferred.
In a recent development, simultaneous measurements of the sample reflectivity over a range of angles are accomplished by illuminating the sample with a focused beam and then detecting the reflected X-rays with a position sensitive detector such as a photodiode array.
XRR has several advantages over techniques using visible light. One such advantage is that XRR makes it possible to measure the thickness of ultra-thin films whose thicknesses are on the order of 30 angstroms or less. Visible light is not suitable for the study of such ultra-thin films using interference patterns because of its wavelength. However, an XRR system may preferably use radiation at wavelengths of about 1.5 angstroms, which radiation creates suitable interference patterns even when probing such ultra-thin films. In addition, XRR may suitably be used where the film is composed of a material that is opaque to light, such as a metal or metal compound. Finally, XRR may suitably be used to measure the density and thickness of films composed of materials that have a low dielectric constant and a correspondingly low index of refraction, such as certain polymers, carbon fluoride compounds, and aerogels.
A preferred XRR technique is described in U.S. Pat. No. 5,619,548, issued Apr. 8, 1997, which is hereby incorporated by reference in its entirety.
FIG. 1
illustrates this preferred technique.
Referring to
FIG. 1
, the preferred X-ray scattering system includes an X-ray source
31
producing an X-ray bundle
33
that comprises a plurality of X-rays shown as
35
a
,
35
b
, and
35
c
. An X-ray reflector
37
is placed in the path of the X-ray bundle
33
. The reflector
37
directs the X-ray bundle
33
onto a test sample
39
held in a fixed position by a stage
45
, and typically including a thin film layer
41
disposed on a substrate
43
. Accordingly, a plurality of reflected X-rays,
57
a
,
57
b
, and
57
c
concurrently illuminate the thin film layer
41
of the test sample
39
at different angles of incidence.
The X-ray reflector
37
is preferably a monochromator. The diffraction of the incident bundle of X-rays
33
within the single-crystal monochromator allows only a narrow band of the incident wavelength spectrum to reach the sample
39
, such that the Brag condition is satisfied for this narrow band. As a result, the plurality of X-rays
57
a
,
57
b
, and
57
c
, which are directed onto the test sample
39
, are also monochromatic. A detector
47
is positioned to sense X-rays reflected from the test sample
39
and to produce signals corresponding to the intensities and angles of incidence of the sensed X-rays.
FIG. 2
depicts an example of a graph of data from the detector
47
showing a normalized measure of the reflectivity of the sample as a function of the angle of incidence to the surface of the sample
39
. A processor is connected to the detector to receive signals produced by the detector in order to determine various properties of the structure of the thin film layer, including thickness, density and smoothness.
In order to maximize the accuracy of the X-ray measurements, it is necessary to precisely calibrate and align the XRR system. The present invention relates to techniques for doing this.
SUMMARY OF THE INVENTION
One object of the present invention relates to the calibration of the detector
47
. In order to properly interpret the raw data graphed in
FIG. 3
, it is necessary to determine which pixel C
0
lies on the extended plane of the sample
39
. In addition it is necessary to find the intensity of the incident, unreflected X-ray corresponding to each pixel in order to be able to normalize the reflected X-ray intensity readings on a point-by-point basis. An aspect of the present invention describes a method for accurately determining C
0
for each sample placement and for finding the incident X-ray intensity corresponding to each pixel and thus permitting an amplitude calibration of the reflectometer system.
Another object of the present invention relates to a method for aligning an angle-resolved X-ray reflectometer that uses a focusing optic, which may preferably be a Johansson crystal. In accordance with the present invention, the focal location may be determined based on a series of measurements of the incident beam profile at several different positions along the X-ray optical path.
Another object of the present invention is to validate the focusing optic. It is important that the focusing optic forms an X-ray beam of uniform and predictable convergence. This is necessary in order to achieve an accurate one-to-one correspondence between the pixel location on the detector and the angle of reflection of X-rays from the sample. A validation of the optics may be performed using a grid mask consisting of regularly spaced openings and opaque bars in order to observe the accuracy of optic shaping.
Another object of the present invention relates to the alignment of the focusing optic with the X-ray source. For example, in the case of an X-ray tube source, achieving the best angular resolution for the reflectometer requires that the line focus of the X-ray tube and the bend axis of the focusing optic be coaligned so as to be accurately parallel. A method for checking this coalignment is to place a fine wire between the X-ray source and the optic and observe the shadow of the wire in the beam profile formed by the optic.
Another object of the present invention concerns the correction of measurements errors caused by the tilt or slope of the sample.
Yet another object of the present invention concerns the calibration of the vertical position of the sample. Changes in the sample height lead to shifts in the location of the reflected beam, so that the vertical sample position must be calibrated if an accurate measurement is to be made.
REFERENCES:
patent: 5042951 (1991-08-01), Gold et al.
patent: 5412473 (1995-05-01), Rosencwaig et al.
patent: 5475728 (1995-12-01), Smith et al.
patent: 5619548 (1997-04-01), Koppel
patent: 5878106 (1999-03-01), Fujiwara
patent: 5923720 (1999-07-01), Barton et al.
patent: 6041098 (2000-03-01), Touryanski et al.
patent: 6069934 (2000-05-01), Verman et al.
patent: 144 956 (1980-11-01), None
patent: 2001116705 (2001-04-01), None
patent: WO 92/08104 (1992-05-01), None
K. Sakurai et al., “Fourier Analysis of Interference Structure in X-Ray Specular Reflection from Thin Films,”Jpn. J. Appl. Phys., vol. 31, 1992, pp. L113-L115.
K.N. Stoev et al., “Review on grazing incidence X-ray spectrometry and reflectometry,”Spectrochimica Acta Part B, vol. 54, 1999, pp. 41-82.
N. Wainfan et al., “Density Measurements of Some Thin Copper Films,”Journal of Applied Physics, vol. 30, No. 10, Oct. 1959, pp. 1604-1609.
J.P. Sauro et al., “Some Observations on the Interference Fringes Formed by X Rays Scattered from Thin Films,”Physical Review, vol. 143, No. 1, Mar. 1966, pp. 439-443.
K. Sakurai et al., “Analysis of thin films by X-ray scattering at grazing incidence,”SPring-8 User Experiment Report No. 2(1998 A), Mar. 1999, p. 162.
In re PC
Koppel Louis N.
Opsal Jon
Uhrich Craig E.
Dunn Drew A.
Kiknadze Irakli
Stallman & Pollock LLP
Therma-Wave, Inc.
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