Академический Документы
Профессиональный Документы
Культура Документы
Miho Yasaka*
1. Introduction
This is the fth article in the series of X-ray thin-lm
measurement techniques. The second, third and forth
articles of this series, previously published in the Rigaku
Journal, describe out-of-plane, high-resolution and in-
plane XRD measurements to obtain crystallographic Fig. 1. Reection and refraction of X-rays on material
information on crystal size, lattice strain and orientation surface.
relationship of a thin-lm material. These measurements
have been based on the premise of a crystalline thin lm. electromagnetic waves, the refractive index of a material
On the other hand, the X-ray reectivity (XRR) is slightly less than 1. Therefore, the X-rays undergo
measurement is not a technique to evaluate diffraction total reection when incident on a at surface of a
phenomenon. The XRR measurement technique material at a grazing angle is smaller than the critical
described in this article is used to analyze X-ray angle for total reection (q c). Thus X-ray reectivity is
reection intensity curves from grazing incident X-ray related to the values of refractive index and X-ray
beam to determine thin-lm parameters including wavelength. It should be noted that Cu-Ka X-rays is
thickness, density, and surface or interface roughness. used throughout this article.
This article will provide an overview of the principles of
X-ray reectivity, measurement procedures, and analysis
methods. It also discusses the procedural ow from
measurement to analysis, as well as precautions.
For the 300 nm thick lm, oscillations of X-ray 1. Set the 2q axis to 0 to detect the incident X-ray
reectivity cannot be observed using the optics system beam directly.
with a multilayer mirror. This is because the period of 2. Set the sample and retract the Z axis to the rear to
the oscillation changes depending on lm thickness. avoid blocking the incident X-ray beam. Check
With a larger lm thickness, the period of the oscillation intensity in this geometry.
is smaller, and the resolution of the X-ray optics used for 3. Scan and set the Z axis at which intensity is half the
measuring X-ray reectivity must be increased. Table 1 intensity measured in step 2.
provides an overview of the optics used in reectivity 4. Scan the sample rotation axis (the w axis) and
measurement and guidelines for lm thickness adjust the alignment incident X-ray beam to obtain a
measurement. maximum intensity.
5. Repeat the scans of both the Z and the w axes for
Table 1. Overview of optics used in a reectivity measurement two or three times to make sure these axes and the
and guide for lm thickness measurement. sample surface are properly aligned.
4. Set the w axis at the peak position on 3. component in the incident X-ray beam, potentially
5. Scan a sample swing axis (c, Rx or Ry axes). resulting in a higher measured intensity. If the sample is
6. Set the swing axis at the peak position on 5. not bent uniformly but is corrugated, both of the effects
7. Repeat steps 3 to 6 until the peak positions on the w above occur simultaneously. If the sample is bent as
and the swing axes agree with those in the previous above, a slightly larger receiving slit is recommended to
scan. detect all total reection X-rays. A slightly larger high-
limit slit is also recommended to obtain a more intense
The two types of halving adjustments described above X-ray reectivity curve for thin lm analysis.
can be done using an appropriate X-ray reectivity
curve. 4. X-ray reectivity measurement
To ensure a precise X-ray incidence angle also Following selective optics and sample alignment
requires various procedures for an accurate sample perform reectivity measurement, X-ray reectivity
alignment. To facilitate these complex procedures, the measurement is based on the angles of w and 2q , which
software enabling easy acquisition of an appropriate were obtained from the sample alignment, and each
reectivity curve has been developed, recently. This movement is scanned in the speed of 2 : 1 (i.e., the 2q /w
software is equipped with an innovative function which scan).
makes the measurements under the conditions The scanning range is measured from below the
determined based on the sample width and height, lm critical angle to the angle where the measured reection
thickness, optics, etc. intensity reaches the level of the background. Generally,
the scanning range is from 2q 0.10.2 to 412.
3.4. Precaution attributable to sample The sampling width is applied to width in which
The preceding paragraph indicated that the incident prole shape near the critical angle or the oscillation
optics and the height limiting slit size are dependent on in the reection intensity is clearly observed without
the lm thickness and the sample width. The precautions being squashed (0.001 to 0.01). It is suitable to
attributable to a sample are described below. approximately 1/5 to 1/7 of the minimum period of the
Rough sample surfaces may keep reectivity proles oscillation.
from exhibiting oscillations clearly because of diffused Scanning speed is set at the speed that statistical
reections. The reason is that diffused reections are uctuations can be suppressed to levels permitting a
observed through the receiving slit. Diffused reections clear observation of the oscillation in the reection
should be removed so that high angular resolution intensities, clear of noise (e.g., 0.01 to 2/min.).
capability can be achieved. In this case, depending on
the extent of the roughness, using a narrow receiving slit 5. Reectivity Analysis Method
and an analyzer crystal in the receiving optics may help The principles of the X-ray reectivity method for
to observe clearer oscillations. determining lm density, lm thickness, and surface and
If the sample is bent or corrugated, total reection interface roughness of a thin-lm sample from the
intensity may be stronger or weaker than that of the measured X-ray reectivity curve are described below.
incident X-ray beam, as shown in Fig. 11(a), (b).
5.1. Total reection and refractive index for X-
Rays
The X-ray refractive index of a substance is slightly
less than 1. If an X-ray beam strikes a substance with a
at surface at an incident angle equal to or less than the
critical angle for total reection, q c, and total reection
Fig. 11(a). Effects when sample is bent convexly. will occur as described in Section 2.1. The refractive
index n of a material for X-rays can be calculated using
the following equations:
n 1I iG (2)
r Q2
I e N0W
2U
x (Z f e) x M
i
i i i
i
i i
(3)
Fig. 11(b). Effects when sample is bent concavely.
r Q2
If the sample is bent convexly, X-ray beams reected
G e
2U
N0W
x ( Z f ee ) x M
i
i i i
i
i i
(4)
R j 1, j 2 Fj , j 1
R j , j 1 a 4j (8)
R j 1, j 2 Fj , j 1 1
g j g j 1 8U 2 gi g j 1X 2j 1
Fj , j 1 exp (9)
g j g j 1 Q2
a j exp(iU g j d j / Q ) (10)
( )
that the substance is assumed to be sufciently thick that
cos 4U d / sin 2 V 2I (7) no reectivity will occur from the bottom of the
substrate.
7. Concluding remarks
The principles of the X-ray reectivity method,
measurement procedures, and data-analysis methods
have been described. The X-ray reectivity method is
nondestructive and can be used for evaluating the layer
structure, thickness, density, and surface or interface
roughness of a multilayer lm.
In recent years, a working group has been set up to
share information and problem consciousness because of
diversication of target samples and highly-developed
and complicated analysis techniques(4). Recently many
articles on the applications of the X-ray reectivity
(2) The thin layer is presented at the interface between the Ta method have been published in the literature. For
and the NiFe layers. examples:
References (10) H. Shimizu, K. Kita, K. Kyuno and A. Toriumi: Jpn. Jour. Appl.
Phys., 44 (2005), 61316135.
( 1 ) H. Kiessig: Ann. Phys., 10 (1931), 715768. (11) S. Kobayashi, T. Nishikawa, T. Takenobu, S. Mori, T. Shimoda,
( 2 ) L. G. Parratt: Phys. Rev., 95 (1954), 359369. T. Mitani, H. Shimotani, N. Yoshimoto, S. Ogawa and Y. Iwasa:
( 3 ) S. K. Sinha, E. B. Sirota and S. Garoff: Phys. Rev., B38 (1988), Nature Materials, 3 (2004), 317322.
22972311. (12) T. Fukuyama, T. Kozawa, K. Okamoto, S. Tagawa, M. Irie, T.
( 4 ) http://www.nims.go.jp/xray/ref/ Mimura, T. Iwai, J. Onodera, I. Hirosawa, T. Koganesawa and K.
( 5 ) K. Omote and Y. Ito: Hyomen Kagaku (Japanese), 27 (2006), Horie: Jpn. Jour. Appl. Phys., 48 (2009), 06FC03-106FC03-3.
642648. (13) T. Fukuyama, T. Kozawa, S. Tagawa, R. Takasu, H. Yukawa, M.
( 6 ) A. Kurokawa, K. Odaka, T. Fujimoto and Y. Azuma: Shinku Sato, J. Onodera, I. Hirosawa, T. Koganezawa and K. Horie:
(Jour. Vac. Soc. Jpn.) (Japanese), 50 (2007), 199201. Appl. Phys. Express, 1 (2008), 065004-1065004-3.
( 7 ) T. Fujimoto, S. Yamagishi, Y. Azuma, T. Taketsuji and T. (14) Y. Ito: Material Stage (Japanese), 8 (2004), 2734.
Watanabe: Hyomen Kagaku (Japanese), 28 (2007), 494499. (15) T. Suzuki, K. Omote, Y. Ito, I. Hirosawa, Y. Nakata, I. Sugiura,
( 8 ) K. Omote and Y. Ito: Mater. Res. Soc. Symp. Proc., 875 (2005), N. Shimizu and T. Nakamura: Thin Solid Films, 515 (2006),
O8.2.1. 24102414.
( 9 ) H. Ohta, T. Mizoguchi and Y. Ikuhara: Material Integration (16) Y. Ito: Shinku (Jour. Vac. Soc. Jpn.) (Japanese), 49 (2006), 104
(Japanese), 22 (2009), No. 910, 3842. 108.