Systems and methods for characterizing high-scatter glass-based samples using light-scattering polarimetry
11035730 · 2021-06-15
Assignee
Inventors
Cpc classification
International classification
G01N21/00
PHYSICS
Abstract
Methods of characterizing an optical retardance or a stress-related property of a glass-bases sample include directing a light beam into the glass-based sample while varying the polarization of the light beam to generate scattered light for each polarization are provided. The scattered light for each polarization is captured with an image sensor, which has an exposure time and a frame rate. The scattered light has an intensity distribution at the image sensor. The sample is moved so that the image sensor averages two or more different intensity distributions per frame to form an averaged intensity distribution for each polarization. The averaged intensity distributions for multiple frames are then used to characterize the optical retardance. The optical retardance can turn be used to determine stress-related properties of the glass-based sample. Moving the substrate reduces measurement noise scattered light having no optical retardance information.
Claims
1. A method of using light-scattering polarimetry to characterize an optical retardance of a glass-based sample, comprising: a. directing a light beam from a light source into the glass-based sample while varying a polarization of the light beam between at least first and second polarization states to generate scattered light for each polarization state; b. for each of the at least first and second polarization states, capturing the scattered light with an image sensor having an exposure time t.sub.E and that captures frames at a frame rate FR, wherein the scattered light has an intensity distribution at the image sensor; c. moving the sample at a sample speed SS relative to at least one of the light beam and the image sensor so that for each of the at least first and second polarization states, the image sensor averages two or more of the intensity distributions per frame to form an averaged intensity distribution; and d. using the averaged intensity distribution for each of at least first and second polarization states to characterize the optical retardance.
2. The method according to claim 1, further comprising using the characterized optical retardance of act d) to determine at least one stress-related characteristic of the glass-based sample.
3. The method according to claim 2, wherein the at least one stress-related characteristic is selected from the group of stress-related characteristics comprising: a stress profile, a surface stress, a depth of compression, a center tension, and a birefringence profile.
4. The method according to claim 1, wherein the act c) of moving the glass-based sample at the sample speed SS relative to at least one of the light beam and image sensor comprises moving the glass-based sample while keeping the light beam and image sensor stationary.
5. The method according to claim 1, wherein the act c) comprises moving the glass-based sample at the sample speed SS≥K.Math.λ/t.sub.E, where λ is a wavelength of the light beam and K is in the range from 0.4 to 1.
6. The method according to claim 1, wherein the light beam resides in an incident plane and further comprising moving the glass-based sample in a direction perpendicular to the incident plane.
7. The method according to claim 1, wherein the act of moving the sample includes a translation, a rotation, or a combination thereof.
8. The method according to claim 1, wherein the act c) of moving the glass-based sample comprises moving one or both of the laser source and the image sensor while keeping the glass-based sample stationary.
9. A method of determining a stress-based characteristic of a glass-based sample using light-scattering polarimetry, comprising: operably arranging the glass-based sample in or relative to a polarimeter having an image sensing device, a light source that emits a light beam, and an optical compensator that defines at least first and second polarizations of the light beam; while moving the glass-based sample relative to the at least one of the light source and the image sensing device, directing the light into the glass based sample to generate scattered light that forms at the image sensing device a line image having a time-varying intensity distribution; for each of the first and second polarizations, detecting with the image sensing device at least two substantially different intensity distributions; forming an averaged intensity distribution from the at least two substantially different intensity distributions; calculating an optical retardation using the averaged intensity distributions for the at least first and second polarizations; and determining the at least one stress-based characteristic from the optical retardation.
10. The method according to claim 9, wherein forming the averaged intensity distribution comprises detecting the at least two substantially different intensity distributions within a frame of an image sensor that has a frame rate FR.
11. The method according to claim 10, wherein each of the at least two substantially different intensity distributions are detected within an exposure time t.sub.E of between 0.05 millisecond and 100 milliseconds and at the frame rate FR of between 10 and 200 frames per second.
12. The method according to claim 9, wherein the calculating of the optical retardation utilizes between two and two-hundred frames over a measurement time t.sub.M of between 0.1 seconds and 10 seconds.
13. The method according to claim 9, wherein moving the glass-based sample is performed at a speed of at least 0.75 millimeters per second.
14. The method according to claim 9, wherein the light beam resides in an incident plane and further comprising moving the glass-based sample in a direction perpendicular to the incident plane.
15. A method of measuring at least one stress-based characteristic of a glass-based sample having a body, comprising: a. performing a polarimetry measurement of the glass-based sample for at least first and second polarization states of light having a wavelength λ and transmitted into the body of the sample to generate scattered light; b. during act a), detecting for each of the at least first and second polarization states at least first and second light distributions of the scattered light from different portions of the body and averaging the at least first and second light distributions to form an averaged light distribution; c. using the averaged light distribution for each of the first and second polarization states to calculate an optical retardance as a function of depth into the body of the glass-based sample; and d. using the calculated optical retardance to determine the at least one stress-based characteristic of the glass-based sample.
16. The method according to claim 15, wherein said averaging is performed by detecting the at least first and second light distributions within a single frame of an image sensor.
17. The method according to claim 15, wherein the at least first and second light distributions are formed by taking respective at least first and second exposures each having an exposure time t.sub.E.
18. The method according to claim 15, further comprising during act a), moving the glass-based sample so that the different portions of the body are spaced apart by at least one half the wavelength of the light.
19. The method according to claim 18, wherein the movement of the glass-based sample has a sample speed SS≥K.Math.λ/t.sub.E, where t.sub.E is an exposure time for the first and second exposures used to capture the first and second light distributions, and K is in the range from 0.4 to 1.
20. The method according to claim 15, wherein the scattered light comprises a noise from a non-stress-related scattering feature of the body and a retardation signal from a stress-related scattering feature of the body, and wherein said averaging to form the averaged light distribution reduces a noise contribution to the optical retardance from the noise as compared to using a single measurement of the intensity distribution to calculate the optical retardance.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) The accompanying drawings are included to provide a further understanding, and are incorporated in and constitute a part of this specification. The drawings illustrate one or more embodiment(s), and together with the Detailed Description explain principles and operation of the various embodiments. As such, the disclosure will become more fully understood from the following Detailed Description, taken in conjunction with the accompanying Figures, in which:
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DETAILED DESCRIPTION
(18) Reference is now made in detail to various embodiments of the disclosure, examples of which are illustrated in the accompanying drawings. Whenever possible, the same or like reference numbers and symbols are used throughout the drawings to refer to the same or like parts. The drawings are not necessarily to scale, and one skilled in the art will recognize where the drawings have been simplified to illustrate the key aspects of the disclosure.
(19) The claims as set forth below are incorporated into and constitute part of this Detailed Description.
(20) Cartesian coordinates are shown in some of the Figures for the sake of reference and are not intended to be limiting as to direction or orientation.
(21) The term “strengthened” for the glass-based samples considered herein means that the original samples have undergone a process to create some stress profiles that could have a variety of shapes, typically intended to make the samples stronger and thus harder to break. Example strengthening processes include ion exchange, tempering, annealing and like thermal processes.
(22) The abbreviation “ms” stands for “millisecond.”
(23) The abbreviation “nm” stands for “nanometer.”
(24) The term “glass-based sample” as used herein includes any object made wholly or partly of glass, such as laminates of glass and non-glass materials, laminates of glass and crystalline materials, and glass-ceramics (including an amorphous phase and a crystalline phase). Thus, in an example, the glass-based sample can consist entirely of a glass material while in another example can consist entirely of a glass-ceramic material.
(25) The glass-based samples considered herein generate during a polarimetry measurement a relatively high amount of light scattering by non-stress-based mechanisms within a sample, such by scattering centers, micro-particles, inhomogeneities, crystal structure, Mie or non-selective scattering, multiple scattering, etc. Such light scattering represents noise that is not stress based and can obfuscate the stress characterization. These features generate a noise in the retardation signal in the scattered light, wherein the noise does not include stress-related information that can be used to infer a stress-based characteristic of the sample.
(26) The terms “image” and “line image” are used herein to describe a distribution of light (i.e., intensity distribution) as formed by scattered light at an image sensor of an image sensing device and do not necessarily require an imaging system to define the light distribution.
(27) In the discussion below, the polarimeter is configured to cycle between two or more polarization states (or just “polarizations” for short). In an example, there can be eight or more different polarization states per cycle that combine the linear, elliptical and circular polarizations as is known in the art.
(28) In an example, the “characterizing” of the glass-based samples considered herein includes determining an optical retardance that can be used to calculate one or more stress-based properties of the glass-based sample. In another example, the characterizing of the glass-based sample includes determining one or more stress-based properties of the glass-based sample, such as a stress profile, a surface stress, a depth of compression, a center tension, and a birefringence profile.
(29) In an example below, the minimum sample speed SS is expressed as SS=K.Math.λ/t.sub.E, where K is called the wavelength smoothing factor, λ is the wavelength of light and t.sub.E is the exposure time. This expression for the sample speed SS can be used to determine the sample speed SS to achieve a given distance of movement in terms of the wavelength λ for a given exposure time. In an example, SS≥K.Math.λ/t.sub.E. In an example, K can in the range from 0.4 to 1, while in another example K can range from 0.5 to 1, while in another example K can range from 0.6 to 1.
(30) Glass-Based Samples
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(32) Example types of samples 10 can be strengthened (e.g., chemically or thermally strengthened) and comprise either a glass, a ceramic or a glass ceramic. Example types of samples 10 include protective covers for displays and/or housings for mobile devices such as smart phones, tablets, laptop computers, GPS devices, etc. Such samples tend to be thin and planar, such as shown in
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(34) A property of the given type or types of NSR scattering feature(s) 20 present in the sample 10 is that the resulting scattered light does not include optical retardation information that can be used to determine a stress-related property of the sample, such as a stress profile, center tension (CT), depth of compression (DOC), surface stress, birefringence, etc.
(35) Thus, scattered light from NSR scattering features 20 in a given sample 10 constitutes “noise,” whereas scattered light from SR scattering features 18 of the sample constitutes what is referred to herein as the “retardation signal,” which is used to determine one or more stress-related characteristics of the sample.
(36) Light-Scattering Polarimetry System
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(38) The polarimeter 100 includes a prism 120 used to efficiently couple the light beam 112 into the sample 10. The prism 120 includes an input surface 122, a bottom surface 124 and an exit surface 126. In an example, the input light beam 112 is incident upon the input surface 112 at substantially normal incidence thereto to minimize reflections and reduce changes to the input polarization from reflection and refraction. The bottom surface 124 can be interfaced with the top surface 12 of the sample 10 using an index-matching fluid 50 to optimize optical coupling of the input light beam 112 into the body 11 of the sample 10.
(39) The polarimeter 100 also includes an image sensing device 140 having an input end 142. In an example, the image sensing device 140 comprises a digital camera. The image sensing device 140 can comprise an image sensor 144 having an array of imaging pixels 146, which in an example can have a dimension of between 1.8 microns and 10 microns. The image sensing device 140 is disposed adjacent the exit surface 126 of the prism 120.
(40) The polarimeter 100 also includes an optical compensator 150, which is shown disposed in the path of the light beam 112 between the laser source 110 and the prism 120. The optical compensator 150 is configured to continuously change the polarization of the light beam 112 between two or more different polarization states. In an example, the optical compensator 150 is operably connected to a controller 160 that controls the operation of the optical compensator. In an example, the optical compensator 150 can comprise a single liquid crystal device. In another example, the optical compensator 150 can comprise multiple elements such as polarizers, wave plates, filters, prisms (e.g., wedge prisms), etc. The compensator elements (not shown) need not all be disposed in the input light beam 112. In an example, the optical compensator 150 causes the light beam 112 to go through a full polarization cycle (i.e., change between two or more select polarizations) in anywhere from less than 1 second to 10 seconds.
(41) The controller 160 is also operably connected to the image sensing device 140.
(42) With continuing reference to
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(44) With reference now to
(45) As shown in
(46) In an example, a given measurement of the sample 10 using the polarimeter 100 can involve irradiating the sample with the input light beam 112 for a measurement time t.sub.M of between 1 second and 10 seconds. During the measurement time t.sub.M, the polarization state of the light beam 112 varies between the different polarization states, preferably making one or more cycles through the polarization states. Meantime, for each polarization state, the image sensor 144 captures an electronic image of the line image LI during exposure times t.sub.E. Prior art polarimeters typically use exposure times t.sub.E that are about the same as the image sensor frame rate FR; for example, an exposure time of t.sub.E of 50 ms, which corresponds to a frame rate FR of 20 frames per second.
(47) The electronically captured line images LI differ in their intensity distribution I(x.sub.L) depending on the polarization state of the input light beam 112 and the optical retardation incurred along the beam path. The difference is due to the difference in the destructive and constructive interference along the length of the scattered light beam 112S as a function of depth D into the sample 10 between the different polarization states.
(48) While the intensity distributions I(x.sub.L) necessarily differ between polarization states of the input light beam 112 when there is stress present in the sample 10, the different OR vs. D curves as calculated from the measured intensity distributions should ideally be the same for a given sample at the given measurement location for samples where the stress profile is (ideally) constant.
(49) However, as noted above and as shown in the close-up inset of
(50) Consequently, the measured intensity distribution I(x.sub.L) of the line image LI includes both the noise 112N and the retardation signal 112M so that the variations in intensity in the intensity distribution I(x.sub.L) are not all due to stress alone. Consequently, the different plots of the optical retardation OR versus depth D obtained from the corresponding intensity distributions I(x.sub.L) for the different polarization states will have relatively strong non-stress-related variations that can lead to an imprecise determination of one or more stress characteristics of the sample.
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(52) To address the problem of measurement noise due to the scattered light 112S including noise 112N, an aspect of the systems and methods disclosed herein include: a) moving the sample 10 relative to one of the light source 110 and the image sensing device 140 when making measurements of the sample 10 so that the intensity distribution I(x.sub.L) obtained for two different portions of the body 11 of the glass sample differ substantially (i.e., varies with time due to glass sample motion); and b) averaging two or more substantially different intensity distributions I(x.sub.L) of the line images LI for a given polarization of the input light beam 112. In examples, the averaging can be performed either by the pixels 146 of the image sensor 144 integrating over the exposure time or by averaging separately detected line images, as explained in greater detail below.
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(54) As the movable support member 214 moves in the x-direction, the engagement fixture 220 also moves in the x-direction and pushes the sample 10 in the x-direction and over the measurement face of the housing 300 of the polarimeter 100. Measurement of the sample 10 by polarimeter 100 is carried out as the sample 10 moves relative to the incident light beam 112 from the light source 110. In the example shown in
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(57) The support frame 230 can be held in place in the recess 224 of the engagement fixture 220 using one or more securing members 250, such as one or more set screws. As with the embodiment of
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(60) Note that for both plots of σ.sub.OR (nm) vs. SS (mm/s), for the no-motion data at SS=0 mm/s, the OR standard deviation σ.sub.OR is substantially constant since the noise from the sample 10 with no motion is substantially constant. With reference again to
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(62) Measurement Considerations
(63) The precise sample speed SS and exposure times t.sub.E needed to reduce the measurement noise in the polarimeter 100 to an acceptable level when measuring a sample 10 to characterize at least one stress-related characteristic depends on a number of factors. These factors include the characteristics of the image sensing device 140 (e.g., the gain, image capture rate (frames/second), pixel size, internal pixel average techniques, etc.), as well as the nature of the NSR scattering feature(s) 20, the intensity of the input light beam 112, the number of polarization states used, etc. Other factors include the measurement wavelength λ of the light beam 112 from the laser source 110 and the intensity of the scattered light beam 112S. Example measurement wavelengths λ can include 640 nm, 518 nm and 405 nm. Example exposure times can range from 0.05 millisecond to 100 milliseconds. Example frame rates FR can range between 10 and 200 frames per second. Example calculations of the optical retardation can utilize between two and two-hundred frames over a measurement time t.sub.M of between 0.1 seconds and 10 seconds.
(64) The line image LI captured by the image sensor 144 has a length L that is the same as the path length of the light beam 112 through the body 11 of the sample based on the configuration of the input end 142 of the image sensor. For an incident angle θ of the light (measured within the sample and relative to the horizontal; see
(65) Averaging the Intensity Distributions
(66) When there is no relative substrate movement (SS=0 mm/s), it has been found that the captured line images IL for a given polarization state have an intensity distribution I(x.sub.L) that is substantially constant (i.e., not time varying) but that has substantial peak-to-valley variations that result in the optical retardation OR vs. D also having large peak to valley variations, with relatively large standard deviations σ.sub.OR between different OR vs. D curves.
(67) As noted above, aspects of the systems and methods disclosed herein include moving the sample 10 relative to at least one of the light source 110 and the image sensing device 140 while averaging the now time-varying intensity distributions I(x.sub.L) from two or more line images LI. The averaging can be accomplished by integrating within the exposure time of the image sensor 144 for a given measurement polarization associated with different portions of the body 11 of the glass sample. The averaging can also be accomplished by directly averaging the intensity distributions I(x.sub.L) of separately captured (i.e., discrete) line images LI that have not undergone substantial sensor-based averaging.
(68) Averaging the intensity distributions I(x.sub.L) works best when the amount of movement between exposures is sufficient to substantially change the intensity distribution I(x.sub.L) as a function of time while keeping the measurement polarization the same. Without being bound by any particular theory, it is believed from experience and from experimentation on high-scattering samples 10 that the non-stress-based scattering features 20 are not uniformly distributed throughout the body 11 of the sample 10 so that the distribution of such features varies as a function of measurement location. Furthermore, it has been observed that movement distances on the order of the wavelength λ of the light beam 112 from the light source 110 can cause a substantial change in the intensity distribution I(x.sub.L) of a line image IL for a given polarization.
(69) For a sample speed SS of 1 mm/s and an exposure time t.sub.E of 1 ms, the sample 10 travels a distance DS=(SS)(t)=(1 mm/s)(1×10.sup.−3 s)=1 micron. This effectively averages the variation in the line image intensity distribution I(x.sub.L) by photon integration in each pixel 146 across the 1 micron of motion distance to define an averaged line image intensity distribution I.sub.A(x.sub.L). The variation in the intensity distribution I(x.sub.L) can also be averaged by first capturing a series of discrete line images and then using the discrete images to compute the average line image intensity distribution I.sub.A(x.sub.L).
(70) For a measurement time t.sub.M of 3 seconds, the total distance traveled DT=(1 mm/s)(3 s)=3 mm and the total number of exposures captured by the imaging device 140 at 20 frames per second is 60, which is the total number of line images IL captured by the image sensing device 140. The motion between frames is (1 mm/s)( 1/20 frames per second)=50 microns. So each frame is associated with a different location of the sample 10.
(71) If the optical compensator 150 is operated in a manner that causes one cycle through the select polarization states in 3 seconds, and there are 60 different polarization states in one cycle, the set of different polarization states is used to calculate the optical retardance OR as a function of depth D into the sample body 11 using relationships well known in the art. In an example, the process is repeated 8 times, each with another 3 seconds of different polarization states. With the motion continuing during the 8 repetitions, each being 3 seconds, the distance traveled between measurements is (1 mm/s)(3 seconds per measurement)=3 mm.
(72) A section of an example OR vs. D plot for eight polarization states as measured from an example sample 10 with SS=0 mm/s is shown in
(73) Since the initial data in the form of line image intensity distribution I(x.sub.L) is collected in increments of the exposure times t.sub.E, the distance DS moved during the exposure time is what causes the reduction in noise in the calculation of OR vs. D and ultimately in the improved determination of at least one stress-related characteristic from the OR vs. D data. This can be understood by noting that a cycle through the polarization states is equal to an optical phase distance of 1 wavelength λ of the light beam 112, with the various polarization states representing respective fractions of a single wavelength λ. For example, horizontal and vertical polarizations differ by half a phase distance of wavelength λ or equivalently, a phase angle ϕ of 180 degrees, where ϕ=2π(DS)/λ. For a wavelength λ of 500 nm, the distance DS of 1 micron is twice the wavelength λ and thus represents twice the total phase of 2π needed to cycle through the polarization states. In an example, the different positions (portions) of the sample 10 at which measurements are taken are spaced apart by a distance of at least half of the measurement wavelength.
(74) In an example, the sample 10 is moved such that the different portions of the sample at which the measurements are made (i.e., where scattered light 112 is captured) are spaced apart by at least one half the wavelength λ of the light beam 112, and further in an example is at least 0.6 wavelength λ or at least one wavelength λ.
(75) By averaging a relatively large number of exposures per frame NE, with each exposure corresponding to multiple line image intensity distributions I(x.sub.L), such as NE 10, the total distance DF traveled by the sample 10 for each frame can be very large compared to the wavelength λ of the light beam 112. By way of example, for a sample speed SS of 1 mm/s, a number of exposures per frame NE=10 and an exposure time t.sub.E of 2 ms, the distance traveled per frame DF=(SS).Math.(NE).Math.(t.sub.E)=(1 mm/s).Math.(10).Math.(0.002 s)=0.02 mm or 20 microns. This is also a relatively small distance as compared to a typical sample size, which for practical purposes is often at least 5 millimeters long and is usually greater than 10 mm long.
(76) It will be apparent to those skilled in the art that various modifications to the preferred embodiments of the disclosure as described herein can be made without departing from the spirit or scope of the disclosure as defined in the appended claims. Thus, the disclosure covers the modifications and variations provided they come within the scope of the appended claims and the equivalents thereto.