This invention relates to a system for measuring both linear birefringence and circular birefringence (magnitude and angle) in a transparent sample.
Many important optical materials exhibit birefringence. Birefringence means that different polarizations of light travel at different speeds through the material. These different polarizations are most often considered as two components of the polarized light, one being orthogonal to the other.
Birefringence is an intrinsic property of many optical materials, and may also be induced by external forces or fields. Retardation or retardance represents the integrated effect of birefringence acting along the path of a light beam traversing the sample. If the incident light beam is linearly polarized, two orthogonal components of the polarized light will exit a linearly birefringent sample with a phase difference, called the retardance. If the incident light beam is circularly polarized, two orthogonal components of the polarized light will exit a circularly birefringent sample with a phase difference, called the retardance. The fundamental unit of retardance is length, such as nanometers (nm). It is frequently convenient to express retardance in units of phase angle (waves, radians, or degrees), which is proportional to the retardance (nm) divided by the wavelength of the light (nm). An “average” birefringence for a sample is sometimes computed by dividing the measured retardation magnitude by the thickness of the sample.
The need for precise measurement of birefringence properties has become increasingly important in a number of technical applications. For instance, it is important to specify and control the residual linear birefringence (hence, the attendant induced retardance) in optical elements used in high precision instruments employed in semiconductor and other industries. The optics industry thus has a need for a highly sensitive instrument for measuring linear birefringence in optical components. This need has been largely unmet, especially with respect to measurements of low levels of retardance.
Linearly polarized light may also be characterized as the superposition of two components of circularly polarized light (right-hand and left-hand senses) having identical amplitude and frequency or wavelength. The relative phases of the two circular polarization components determines the polarization plane. The plane of polarization will be rotated in instances where the refractive indices of a sample are slightly different for the two senses of circular polarization. This rotation of the polarization plane is referred to as optical rotation. Optical rotation is also referred to as circular birefringence because it relates to the phase shifting of the circular polarization components that is attributable to the different refractive indices.
If linearly polarized light passes through chiral media, such as, for example a solution of chiral molecules, the polarization of the incident light will be rotated. This circular birefringence (or optical rotation) is often referred to as natural optical rotation to distinguish it from Faraday rotation in a magnetic field. The extent of optical rotation, therefore, is indicative of the molecular structure (the chirality) of such media. Thus, the precise detection and analysis of the optical rotation, or circular birefringence, imparted by sample of chiral medial is useful for analytical chemistry, pharmaceutical, and biological industries.
The complete description of each linear and circular birefringence requires two parameters. Both linear and circular birefringence of a sample along a given optical path require specifying the magnitude of the birefringence, or the amount of integrated phase retardation along the given optical path length. For linear birefringence, it is also required to specify the fast axis of the sample. The two orthogonal polarization components described above are parallel to two orthogonal axes, which are determined by the sample and are called the “fast axis” and the “slow axis.” The fast axis is the axis of the material that aligns with the faster moving component of the polarized light through the sample. For circular birefringence, the sense of optical rotation, in terms of clockwise or anticlockwise, should be specified. Therefore, a complete description of the linear and circular birefringence of a sample along a given optical path requires specifying both the magnitude of the birefringence, the relative angular orientation of the fast (or slow) axis, and the rotational direction (for circular birefringence).
The present invention is directed to a practical system and method for precisely measuring low-level linear and circular birefringence properties of optical materials. The retardance magnitude and orientation of the fast axis are precisely calculated, as well as the rotational direction. The system permits multiple measurements to be taken across the area of a sample to detect and graphically display variations in the retardance across the sample area.
In a preferred embodiment, the system incorporates a photoelastic modulator for modulating polarized light that is then directed through a sample. The beam propagating from the sample is separated into two parts. These separate beam parts are then analyzed at different polarization directions, detected, and processed as distinct channels. The detection mechanisms associated with each channel detect the light intensity corresponding to each of the two parts of the beam. This information is employed in an algorithm for calculating a precise, unambiguous measure of the retardance induced by the sample and the orientation of the fast axis.
As one aspect of this invention, the system includes a beam-splitting member and detector arrangement that permits splitting the beam into two parts with minimal contribution to the retardance induced in the beam. Moreover, the presence of any residual birefringence in the optical system (such as may reside as static birefringence in the photoelastic modulator or in any of the optical components of the system) is accounted for in a number of ways. For example, certain of the system components are arranged or mounted to minimize the chance that strain-induced birefringence may be imparted into the element. A reliable calibration technique is also provided.
The system permits the low-level linear and circular birefringence measurements to be taken at any of a plurality of locations across the area of the sample. The measurements are compiled in a data file and graphically displayed for quick analysis.
In one embodiment of the invention, the optical components of the system are arranged to measure the birefringence properties of a sample that is reflectively coated on one side, thereby permitting measurement of birefringence properties even though the sample is not completely light transmissive.
Other advantages and features of the present invention will become clear upon study of the following portion of this specification and drawings.
Linear Retardance Measurement
The diagram of
The source light beam “B” is directed to be incident on a polarizer 22 that is oriented with its polarization direction at +45° relative to a baseline axis. A high-extinction polarizer, such as a Glan-Thompson calcite polarizer, is preferred. It is also preferred that the polarizer 22 be secured in a precision, graduated rotator.
The polarized light from the polarizer 22 is incident on the optical element 25 of a photoelastic modulator 24 (
The PEM has its birefringent axis oriented at 0° and is controlled by a controller 84 that imparts an oscillating birefringence to the optical element 25, preferably at a nominal frequency of 50 kHz. In this regard, the controller 84 drives two quartz transducers 29 between which the optical element 25 is bonded with an adhesive.
The oscillating birefringence of the PEM introduces a time-varying phase difference between the orthogonal components of the polarized light that propagates through the PEM. At any instant in time, the phase difference is the retardation introduced by the PEM. The retardation is measurable in units of length, such as nanometers. The PEM is adjustable to allow one to vary the amplitude of the retardation introduced by the PEM. In the case at hand, the retardation amplitude is selected to be 0.383 waves (2.405 radians).
The beam of light propagating from the PEM is directed through the transparent sample 26. The sample is supported in the path of the beam by a sample stage 28 that is controllable for moving the sample in a translational sense along orthogonal (X and Y) axes. The stage may be any one of a number of conventional designs such as manufactured by THK Co. Ltd., of Tokyo, Japan as model KR2602 A-250. As will become clear, the motion controllers of the sample stage 28 are driven to enable scanning the sample 26 with the beam to arrive at a plurality of retardance and orientation measurements across the area of the sample.
The sample 26 will induce retardance into the beam that passes through it. It is this retardance value that is determined in accordance with the processing provided by the present invention, as explained more below. The present system is especially adapted to determine low levels of retardance. Low retardance levels are determined with a sensitivity of less than ±0.01 nm.
In order to obtain an unambiguous measure of the sample-induced retardance, the beam “Bi” that passes out of the sample is separated into two parts having different polarization directions and thereby defining two channels of information for subsequent processing.
Turning first to the preferred mechanism for separating the beam “Bi,” there is located in the path of that beam (hereafter referred to as the incidence path) a beam-splitting mirror 30. Part “B1” of the beam “Bi” passes completely through the beam-splitting mirror 30 and enters a detector assembly 32 for detection.
The diameter of the mirror 30 is slightly less than the diameter of the housing aperture. The aperture is threaded except for an annular shoulder that projects into the lowermost end of the aperture to support the periphery of the flat, round mirror 30. A retainer ring 40 is threaded into the aperture to keep the mirror in place in the housing 31 against the shoulder.
In a preferred embodiment, care is taken to select and mount the mirror 30 so that substantially no stress-induced birefringence is introduced into the mirror. In this regard, the mirror is preferably made of Schott Glass type SF-57 glass. This glass has an extremely low (near zero) stress-optic coefficient. The retainer ring 40 is carefully placed to secure the mirror without stressing the glass. Alternatively, flexible adhesive may be employed to fasten the mirror. No setscrews or other stress-inducing mechanisms are employed in mounting the mirror.
It is noteworthy here that, although a beam-splitting mirror is preferred, one can substitute other mechanisms (such as a flipper mirror arrangement) for separating the beam “Bi” into two parts.
The part of the beam “B1” that passes through the mirror 30 enters the detector assembly 32 (
The reflective surface 35 of the beam-splitting mirror 30 (
The reflected part of the Beam “Br” is incident upon another detector assembly 50. That assembly 50 is mounted to the post 36 (
The detector components are compactly integrated and contained in a housing 60 that has a flat front side 62. The remainder of the side of the housing is curved to conform to the curvature of the central aperture 56 of the base plate 52. Moreover, this portion of the housing 60 includes a stepped part 64 that permits the curved side of the housing to fit against the base plate 52 and be immovably fastened thereto.
A sub-housing 70 is fastened inside of the detector components housing 60 against the flat side 62. The sub-housing 70 is a generally cylindrical member having an aperture 72 formed in the bottom. Just above the aperture 72 resides a compact, Glan-Taylor type analyzer 74 that is arranged so that its polarization direction is 0°, parallel with that of the PEM 24.
Stacked above the analyzer 74 is a narrow-band interference filter 77 that permits passage of the polarized laser light but blocks unwanted room light from reaching a detector 76. The detector is preferably a photodiode that is stacked above the filter. The photodiode detector 76 is the preferred detection mechanism and produces as output a current signal representative of the time varying intensity of the received laser light. With respect to this assembly 50, the laser light is that of the beam “B2,” which is the reflected part “Br” of the beam that propagated through the sample 26.
The photodiode output is delivered to a preamplifier carried on an associated printed circuit board 78 that is mounted in the housing 60. The preamplifier 75 (
It is noteworthy here that the other detector assembly 32 (
The photodiode of detector assembly 32 produces as output a current signal representative of the time varying intensity of the received laser light. With respect to this assembly 32, the laser light is that of the beam “B1,” which is the non-reflected part of the beam “Bi” that propagated through the sample 26.
The photodiode output of the detector assembly 32 is delivered to a preamplifier 79, which provides its output to the lock-in amplifier 80 (
In summary, the lock-in amplifier 80 is provided with two channels of input: channel 1 corresponding to the output of detector assembly 32, and channel 2 corresponding to the output of detector assembly 50. The intensity information received by the lock-in amplifier on channel 1— because of the arrangement of the −45° analyzer 42—relates to the 0° or 90° component of the retardance induced by the sample 26. The intensity information received on channel 2 of the lock-in amplifier 80—as a result of the arrangement of the 0° analyzer 74—relates to the 45° or −45° component of the retardance induced by the sample. As explained below, this information is combined in an algorithm that yields an unambiguous determination of the magnitude of the overall retardance induced in the sample (or a location on the sample) as well as the orientation of the fast axis of the sample (or a location on the sample).
The lock-in amplifier 80 may be one such as manufactured by EG&G Inc., of Wellesley, Mass., as model number 7265. The lock-in amplifier takes as its reference signal 82 the oscillation frequency applied by the PEM controller 84 to the transducers 29 that drive the optical element 25 of the PEM 24. The lock-in amplifier 80 communicates with a digital computer 90 via an RS232 serial interface.
For a particular retardance measurement, such as one taken during the scanning of several locations on a sample, the computer 90 obtains the values of channel 1. The computer next obtains the values of channel 2. The intensity signals on the detectors in channels 1 and 2 are derived as follows:
where Δ is the PEM's time varying phase retardation; δ is the magnitude of the sample's retardance; and ρ is the azimuth of the fast axis of the sample's retardance.
The Mueller matrix for a linearly birefringent sample (δ, ρ) used in the derivation has the following form:
In equations (1), sin Δ (Δ=Δ0 sin ωt, where ω is the PEM's modulating frequency; Δ0 is the maximum peak retardance of the PEM) can be expanded with the Bessel functions of the first kind:
where k is either “0” or a positive integer; and J2k+1 is the (2k+1)th order of the Bessel function. Similarly, cos Δ can be expanded with the even harmonics of the Bessel functions:
where J0 is the 0th order of the Bessel function, and J2k is the (2k)th order of the Bessel function.
As seen from equations 1–3, it is preferable to determine the magnitude and angular orientation of retardance using the signal at the PEM's first harmonic. The useful signal for measuring linear birefringence at the PEM's 2nd harmonic is modified by sin2(δ/2), a value that is much smaller than sin δ. The 1F electronic signal on the detectors can be expressed in equation (4):
Ich1,1F=sin δ cos(2ρ)2J1(Δ0)sin(ωt)
Ich2,1F=sin δ sin(2ρ)2J1(Δ0)sin(ωt) Eqn. (4)
As noted, the 1F signal is determined using the lock-in amplifier 80 that is referenced at the PEM's first harmonic. The lock-in amplifier will exclude the contributions from all harmonics other than 1F. The output from the lock-in amplifier 80 for the two channels is:
Using the approximation of sin δ≈δ for low-level linear birefringence; and √2 results from the fact that the lock-in amplifier measures the r.m.s. of the signal, instead of the amplitude.
All terms appearing at a frequency other than the PEM's first harmonic are neglected in obtaining equations (5). The validity of equations (5) for obtaining the 1F VAC signal is further ensured from the approximation that sin2(δ/2)≈0 when δ is small. This applies for low-level retardance of, for example, less than 20 nm.
In order to eliminate the effect for intensity fluctuation of the light source, or variations in transmission due to absorption, reflection losses, or scattering, the ratio of the 1F VAC signal to the VDC signal is used. (Alternatively, similar techniques can be employed, such as dynamically normalizing the DC signal to unity.) Exclusion of the cos Δ terms in equation (1) can severely affect the VDC signal in channel I even though it has a minimal effect on the determination of the 1F VAC signal using a high quality lock-in amplifier. The DC term of channel 1 depends on J0(Δ0) as seen from equation (6).
Consequently, this DC term should be corrected as in equation (7):
where Rch1 and Rch2 are experimentally determined quantities from the two channels.
To correct the “DC” term caused by the cos Δ term in channel 1, one properly sets the PEM retardation so that J0(Δ0)=0 (when Δ0=2.405 radians, or 0.383 waves). At this PEM setting, the efficiency of the PEM for generating the 1F signal is about 90% of its maximum.
Finally, the magnitude and angular orientation of the linear birefringence is expressed in equations (8):
These equations (8) are compiled in a program running on the computer 90 and used to determine the magnitude and orientation of the retardance at any selected point on the sample.
Equations (8) are specifically developed for small linear birefringence. The approximation of sin δ≈δ used in deriving equations (8) has an error of ˜1% for δ=20 nm when the light wavelength is at 632.8 nm. For any larger retardation, sin δ should be used, instead of δ.
As noted above, best retardance measurement results are achieved when one minimizes the residual birefringence present in the optical components of the system. To this end, the present system employs a PEM 24 (
Notwithstanding efforts such as the foregoing to eliminate residual birefringence in the system components, the presence of at least some level of residual birefringence is inevitable. In the present system, highly accurate results are obtained by correcting the results of equations 8 to account for any remaining residual birefringence in the system, which residual may be referred to as the system offset. In practice, residual birefringence in the optical element of the photoelastic modulator and in the beam-splitting mirror substrate can induce errors in the resulting measurements. Any such errors can be measured by first operating the system with no sample in place. A correction for the errors is made by subtracting the error values for each channel.
The system offset is obtained by making a measurement without a sample in place. The results from both channels 1 and 2 are the system offsets at 0° and 45° respectively:
where the superscript “0” indicates the absence of a sample. The equation bearing the term ρ=0 corresponds to channel 1 (the −45° analyzer 42). The equation bearing the term ρ=π/4 corresponds to channel 2 (the 0° analyzer 74). The system offsets are corrected for both channels when a sample is measured. The system offsets for channels 1 and 2 are constants (within the measurement error) at a fixed instrumental configuration. Barring any changes in the components of the system, or in ambient pressure or temperature, the system should remain calibrated.
In principle, this procedure will provide a method of self-calibration of the system. It is, however, prudent to compare the system measurement of a sample with the measurement obtained using other methods.
One such calibration sample may be provided by a compound zero-order waveplate. The compound waveplate comprises two multiple-order waveplates (e.g., quartz) or two zero-order waveplates (e.g., mica) selected to have a very small retardance difference between them (e.g., less than 0.03 wavelengths). They would be combined with their axes at right angles so that the retardance of one is subtracted from the other to produce the sought-after low-level retardance, compound zero-order waveplate(s) for use in calibration. Such a configuration will provide a uniform retardance across the surface with a low temperature coefficient of retardance.
If the components of the present system are correctly set up, the magnitude of the measured, sample-induced retardance will be independent of the sample's angular orientation. This angular independence may be lost if: (1) the polarization directions of the polarizer 22 and analyzers 42, 74 are not precisely established, and (2) the maximum peak retardance of the PEM is not precisely calibrated. What follows is a description of correction techniques for eliminating the just mentioned two sources of possible “angular dependence” errors.
As respects the precise establishment of the polarization directions of the polarizer 22 and analyzers 42, 74, the correction technique applied to the polarizer 22 involves the following steps:
As respects the calibration of the PEM, the following technique may be employed:
As mentioned above, the motion controllers of the sample stage 28 are controlled in a conventional manner to incrementally move the sample 26 about orthogonal (X, Y) axes, thereby to facilitate a plurality of measurements across the area of a sample. The spatial resolution of these measurements can be established as desired (e.g., 3.0 mm), provided that the sought-after resolution is not finer than the cross section of the beam that strikes the sample. In this regard, the cross sectional area or “spot size” of the laser beam may be minimized, if necessary, by the precise placement of a convex lens with an appropriate focal length, such as shown as line 96 in
In some instances it may be desirable to enlarge the spot size provided by the laser source. To this end a lens or lens system such as provided by a conventional beam expander may be introduced into the system between the laser 20 and the polarizer 22.
The measured retardance values can be handled in a number of ways. In a preferred embodiment the data collected from the multiple scans of a sample are stored in a data file and displayed as a plot on a computer display 92. One such plot 100 is shown in
In a preferred embodiment, the just described retardance measurements are displayed for each cell as soon as that cell's information is computed. As a result of this instantaneous display approach, the operator observes the retardance value of each cell, without the need to wait until the retardance values of all of the cells in the sample have been calculated. This is advantageous for maximizing throughput in instances where, for example, an operator is charged with rejecting a sample if the birefringence value of any part of the sample exceeds an established threshold.
Also illustrated in
It will be appreciated that any of a number of variations for displaying the measured data will suffice. It will also be apparent from
Another approach to graphically displaying the retardance magnitude and orientation information provided by the present system is to depict the retardance magnitude for a plurality of locations in a sample via corresponding areas on a three-dimensional contour map. The associated orientations are simultaneously shown as lines or colors in corresponding cells in a planar projection of the three dimensional map.
The sample 124 (
As noted above, it is desirable to locate the beam-splitting mirror 30 as near as practical to the beam “B” so that the beam “Bi” reflected from the sample 124 is angled “R” only slightly away (for example 2° to 5°) from the beam “B” propagating from the PEM 24. To this end, the housing 31 may be modified to support a mirror that is semi-circular in shape such that the flat edge of the mirror is located adjacent to the beam “B.” The beam “Bi”, therefore, could be reflected to a location on the mirror that is very close to that edge, hence to the beam “B” as desired.
While the present invention has been described in terms of preferred embodiments, it will be appreciated by one of ordinary skill in the art that modifications may be made without departing from the teachings and spirit of the foregoing. For example a second lock-in amplifier may be employed (on for each channel) for increasing the speed with which data is provided to the computer.
Also, one of ordinary skill will appreciate that sequential measurement using a single detector may be employed for measuring the intensity signal in two different polarization directions and thereby defining two channels of information for subsequent processing. For example, a single detector assembly could be employed. This dispenses with the second detector assembly and the beam-splitter mirror. Such a set-up, however, would require either rotating the analyzer or switching between two polarizers of different orientations to ensure unambiguous retardance measurements and to ascertain the orientation of the fast axis. Alternatively, the sample and the analyzer may be rotated by 45°.
The preferred embodiment of the present invention uses a HeNe laser for a stable, pure, monochromatic light source. The HeNe laser produces a beam having a 632.8 nm wavelength. In some instances, retardance magnitude measurements using light sources having other frequencies are desired.
As another aspect of the present invention, one can develop and apply correction factors to convert the retardance magnitude measurement of the sample as measured by the HeNe laser to the retardance value that would occur in the sample at another source-light wavelength. In this regard,
The wavelength correction technique just described for fused silica can also be applied to other materials. For example,
As another approach to correcting the measured retardation magnitude at one source-light wavelength to relate to the retardation magnitude at another wavelength, one can refer to the stress-optic coefficient of the sample material being tested, which coefficient is known as a function of wavelength. The retardance magnitudes measured at two different wavelengths are directly proportional to the stress-optic coefficient of the material.
Circular Retardance Measurement
As noted above with respect to
The determination of the circular retardance employs, in a preferred embodiment, the optical components arrangement shown in the diagram of
The signal presented by the channel 2 detector assembly 50 (
where Δ is the PEM's time varying phase retardation (Δ=Δ0 sin ωt, where ω is the PEM's modulating frequency; Δ0 is the retardation amplitude of the PEM), and α is the magnitude of the circular retardance.
The light intensity signals at the detector for channel II are:
where I0 is the light intensity after the first polarizer.
The function of cos Δ in equation 10 can be expanded with the Bessel functions of the first kind:
where J0 is the 0th order of the Bessel function, and J2k is the (2k)th order of the Bessel function.
Substituting equation (11) into equation (10) and taking only up to the second order of the Bessel functions, we obtain:
As seen from equation 12, the detector signal of channel II contains “DC” terms, a 2F (cos(2ωt)) term and higher order harmonic terms. It is the 2F “AC” signal that is most useful for determining the circular birefringence. The 2F “AC” signal can be determined using a lock-in amplifier 80 that is referenced at the PEM's second harmonic frequency. For theoretical evaluation, we assume that a perfect lock-in amplifier will exclude the contributions from all other harmonics. The 2F signal measured by the lock-in amplifier for channel II is:
where we have used VCh2=KCh2ICh2 (VCh2 is the detector's electronic signal and KCh2 is an instrumental constant), and the small angle approximations (sin α=α); and √2 results from the fact that the output of a lock-in amplifier measures the root-mean-square, not the signal amplitude.
The “DC” signals for channel II can be derived from equation (12).
When the PEM retardation amplitude Δ0=2.405 radians (0.3828 waves) is chosen, J0(Δ0)=0. At this PEM setting, the 2F signal and the “DC” terms for channel II are:
In order to eliminate the effect of light intensity variations due to light source fluctuations and the absorption, reflection and scattering from the sample and other optical components, the ratio of the 2F “AC” signal to the “DC” signal is used. The ratios of “AC” signal to the “DC” signal for both channels are represented in equation (16):
Finally, the circular birefringence of the sample is expressed as:
here α, represented in radians, is a scalar that can be converted to degrees.
The mathematical sign of the α term calculated above is indicative of the direction of rotation of the polarization plane of the beam. For instance a positive value indicates rotation in the right-hand sense; negative meaning rotation in the left-hand sense.
A single lock-in amplifier 80 (
As indicated in
It will be appreciated that the various refinements described above with respect to the elimination of residual birefringence in the PEM and system offsets are applicable irrespective of whether linear retardance, circular retardance, or both are determined.
Similarly, the calibration techniques described above are also applicable when the system is used for calculating circular retardance. Moreover, it is contemplated that, depending on the characteristics of the sample, different light source frequencies (that is, other than the preferred 632.8 nm wavelength HeNe laser) may be desirable.
It will also be appreciated that the magnitude and rotation direction of each circular retardance measurement can be stored and displayed in a manner as described above with respect to linear retardance magnitude and angle (See
In some instances it may be desirable to determine the circular retardance of a sample having a reflective coating. Thus, the arrangement of optical components described above with respect to
It is also contemplated that the V12F signal transmitted on channel 1 (
Filing Document | Filing Date | Country | Kind | 371c Date |
---|---|---|---|---|
PCT/US02/09384 | 3/23/2002 | WO | 00 | 4/29/2003 |
Publishing Document | Publishing Date | Country | Kind |
---|---|---|---|
WO01/73385 | 10/4/2001 | WO | A |
Number | Name | Date | Kind |
---|---|---|---|
4306809 | Azzam | Dec 1981 | A |
4668086 | Redner | May 1987 | A |
4801798 | Lange | Jan 1989 | A |
4850710 | Mochida et al. | Jul 1989 | A |
5268305 | Ribi et al. | Dec 1993 | A |
5319194 | Yoshizumi et al. | Jun 1994 | A |
5457536 | Kornfield et al. | Oct 1995 | A |
5521705 | Oldenbourg et al. | May 1996 | A |
5536936 | Drevillon et al. | Jul 1996 | A |
5825492 | Mason | Oct 1998 | A |
5956146 | Nakagawa | Sep 1999 | A |
5956147 | Jellison et al. | Sep 1999 | A |
6473181 | Oakberg | Oct 2002 | B1 |
Number | Date | Country | |
---|---|---|---|
20030179375 A1 | Sep 2003 | US |
Number | Date | Country | |
---|---|---|---|
60193652 | Mar 2000 | US |