Apparatus and method for measuring the elasticity of microfibers at high throughput
12474245 ยท 2025-11-18
Assignee
Inventors
- Yuan LIU (Hong Kong, CN)
- Anderson Ho Cheung Shum (Hong Kong, CN)
- Janine K. NUNES (Princeton, NJ, US)
- Howard A. Stone (Princeton, NJ)
Cpc classification
G01N2203/028
PHYSICS
International classification
Abstract
The subject invention pertains to a new method for measuring the elastic properties of microfibers by rope-coiling. Rope-coiling refers to the buckling of a slender elastic fiber caused by axial compression. A continuous flow microfluidic method enables the high-throughput measurement of the elasticity of microfibers by rope-coiling, where sample loading and unloading are not needed between consecutive measurements. In certain embodiments the coiling radius can be directly proportional to the elastic modulus of the fiber, facilitating calibration to measure fiber elasticity for high-throughput applications. Throughput can be thousands of times higher than that of a tensile tester, making possible an in situ, on-line measurement in a microfluidic production line, which couples the making of microfibers and the measurement of elasticity on the same line. The new method can also measure certain fibers with local variations in elasticity.
Claims
1. A system useful for high throughput elasticity measurement of microfibers, the system comprising: a coiling device configured and adapted for operable connection to a fiber making device; a coil measurement device configured and adapted to capture a coil radius (R.sub.coil) measurement of a coil created by the coiling device; and a coil measurement calibration device configured and adapted to convert R.sub.coil to a fiber elasticity value (E).
2. The system of claim 1, wherein the coiling device is configured and adapted to receive a flow of a process fluid and a movement of a fiber from a connected fiber making device through an upstream portion to a downstream portion; the coiling device comprising a first capillary forming a small channel in the upstream portion and a second capillary forming a wide channel in the downstream portion.
3. The system of claim 2, wherein the second capillary is connected to and abruptly enlarged from the first capillary.
4. The system of claim 3, wherein the first capillary and the second capillary are each respectively configured and adapted such that together they create a condition of axial compression in the fiber sufficient to induce coiling under specified conditions and to form the fiber into a coiled fiber.
5. The system of claim 1, wherein the coil measurement device is a non-destructive measurement device.
6. The system of claim 5, wherein the coil measurement device is a non-contact measurement device.
7. The system of claim 6, wherein the coil measurement device is a microfluidics-based measurement device.
8. The system of claim 5, wherein the coil measurement device is a real time measurement device.
9. The system of claim 1, wherein the coil measurement calibration device is configured and adapted to convert R.sub.coil to E based on a linear relationship between R.sub.coil and E.
10. The system of claim 9, wherein the linear relationship comprises a slope determined according to R.sub.coil of the coiled fiber.
11. A method useful for high throughput elasticity measurement of microfibers, the method comprising: producing a microfiber having an elastic modulus (E) at a throughput greater than 1 mm per second; coiling the microfiber to create a coiled microfiber having a coil radius (R.sub.coil); recording a measurement of R.sub.coil; calculating E from R.sub.coil; and uncoiling the coiled microfiber.
12. The method of claim 11, wherein the measurement is a non-destructive, non-contact, real-time measurement.
13. The method of claim 12, wherein the measurement is an optical measurement.
14. The method of claim 13, wherein the throughput is greater than 2 mm per second.
15. The method of claim 14, wherein the throughput is greater than 10 mm per second.
16. The method of claim 12, wherein the recording a measurement of R.sub.coil and calculating E from R.sub.coil are repeated at least once per minute.
17. The method of claim 16, wherein the recording a measurement of R.sub.coil and calculating E from R.sub.coil are repeated at least once per second.
18. The method of claim 12, wherein the calculating E from R.sub.coil comprises the application of a linear relationship between E and R.sub.coil.
19. The method of claim 12, comprising the uncoiling the fiber after recording the measurement to produce a fiber that is straight and without coils.
20. A system useful for high throughput elasticity measurement of microfibers, the system comprising: a coiling device configured and adapted for operable connection to a fiber making device; a coil measurement device configured and adapted to capture a coil radius (R.sub.coil) measurement of a coil created by the coiling device; and a coil measurement calibration device configured and adapted to convert R.sub.coil to a fiber elasticity value (E); wherein the coiling device is configured and adapted to receive a flow of a process fluid and a movement of a fiber from a connected fiber making device through an upstream portion to a downstream portion, the coiling device comprising a first capillary forming a small channel in the upstream portion and a second capillary forming a wide channel in the downstream portion; wherein the second capillary is connected to and abruptly enlarged from the first capillary; wherein the first capillary is configured and adapted to approximate the flow of the process fluid and the movement of the fiber from the connected fiber making device, and the second capillary is configured and adapted to create a condition of axial compression in the fiber sufficient to induce coiling under specified conditions and to form the fiber into a coiled fiber; and wherein the coil measurement device is a non-destructive, non-contact, image based, real time measurement device; wherein the coil measurement calibration device is configured and adapted to convert R.sub.coil to E based on a linear relationship between R.sub.coil and E; and wherein the linear relationship comprises a slope determined according to R.sub.coil of the coiled fiber.
21. A system useful for high throughput elasticity measurement of a target microfiber, the system comprising: a rope-coiling device configured and adapted to induce rope-coiling in the target microfiber, thereby creating a coiled microfiber; a measurement device configured and adapted to measure one or more physical properties of the coiled microfiber within the rope-coiling device, thereby creating a coiled microfiber measurement; and a calibration device configured and adapted to convert the coiled microfiber measurement to a microfiber elasticity measurement.
22. The system of claim 21, wherein the measurement device is a microfluidic measurement device.
23. The system of claim 22, wherein the calibration device comprises a calibration curve, calibration formula, or calibration table.
24. The system of claim 23, wherein the rope-coiling device is a microfluidic device.
25. The system of claim 24, wherein the coiled microfiber measurement comprises a rope-coiling radius, diameter, or velocity and the calibration device comprises a linear relationship between the rope-coiling radius, diameter, or velocity and the microfiber elasticity measurement.
26. A method useful for high throughput elasticity measurement of a target microfiber, the method comprising: rope-coiling the target microfiber in a chamber, thereby creating a coiled microfiber; measuring one or more physical properties of the coiled microfiber within the chamber, thereby creating a coiled microfiber measurement; and converting the coiled microfiber measurement to a microfiber elasticity measurement.
27. The method of claim 26, wherein the measuring is done by a microfluidic measurement device.
28. The method of claim 27, wherein the converting is done by reference to a calibration curve, calibration formula, or calibration table.
29. The method of claim 28, wherein the chamber is a microfluidic device.
30. The method of claim 29, wherein the coiled microfiber measurement comprises a rope-coiling radius, diameter, or velocity and the reference to a calibration curve, calibration formula, or calibration table comprises a linear relationship between the rope-coiling radius, diameter, or velocity and the microfiber elasticity measurement.
31. A microfluidic method useful for high throughput elasticity measurement of a target microfiber, the method comprising: rope-coiling a solidified section of the target microfiber in a microfluidic chamber, thereby creating a coiled microfiber section; measuring, by a microfluidic sensor, a coil radius of the coiled microfiber section within the chamber, thereby creating a coiled microfiber measurement; converting the coiled microfiber measurement to a microfiber elasticity measurement; and uncoiling the coiled microfiber section.
32. A microfluidic system useful for high throughput elasticity measurement of a target microfiber, the system comprising: a microfluidic rope-coiling device configured and adapted to induce rope-coiling in a section of the target microfiber, thereby creating a coiled microfiber section; a microfluidic measurement device configured and adapted to measure a rope-coiling radius of the coiled microfiber section within the microfluidic rope-coiling device; and a calibration device configured and adapted to convert the rope-coiling radius to a microfiber elasticity measurement.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DISCLOSURE OF THE INVENTION
(10) The subject invention can be better understood by reference to certain non-limiting exemplary embodiments and related definitions, as follows. Embodiment 1. A system useful for high throughput elasticity measurement of microfibers, the system comprising: a coiling device configured and adapted for operable connection to a fiber making device; a coil measurement device configured and adapted to capture a coil radius (R.sub.coil) measurement of a coil created by the coiling device; and a coil measurement calibration device configured and adapted to convert R.sub.coil to a fiber elasticity value (E).
(11) In certain embodiments, high throughput elasticity measurement of microfibers can be advantageously applied to continuous or semi-continuous production of a fiber or fibers (e.g., between 50 m and 500 m diameter, or larger or smaller, including any fiber that can be rope-coiled) at a measurement rate greater than 1 measurement per minute (e.g., greater than 1 measurement per second, or faster or slower, including any rate at which the target fiber can be rope-coiled, measured, and optionally uncoiled in a commercially viable production process or measurement process), and at fiber throughput rate greater than 15 mm/sec, alternatively greater than 27 mm/s, alternatively greater than 40 mm/s, or faster or slower, including any rate at which the target fiber can be rope-coiled, measured, and optionally uncoiled in a commercially viable production process or measurement process.
(12) In certain embodiments a coiling device can include two channels (e.g., glass capillaries) selected to form a small channel upstream and a wide channel downstream as shown in
(13) In certain embodiments a coil measurement device can include optical and/or microfluidic measurement devices, or other devices capable of delivering measurements in the range of seconds, for example 1 measurement in less than 60 seconds, alternatively less than 45, 30, 20, 10, 5, 3, 2, or 1 second per measurement or greater than 1, 2, 3, 5, or 10 measurements per second, including increments, combinations, and ranges of any of the foregoing. A coil measurement device cannot include conventional fiber measurement devices (or techniques, methods, or procedures) requiring more than 1 minute per measurement.
(14) A coil measurement calibration device can include a physical, digital, or logical lookup table, calibration curve, or equation. Embodiment 2. The system of Embodiment 1, wherein the coiling device is configured and adapted to receive a flow of a process fluid and a movement of a fiber from a connected fiber making device through an upstream portion to a downstream portion; the coiling device comprising a first capillary forming a small channel in the upstream portion and a second capillary forming a wide channel in the downstream portion. Embodiment 3. The system of Embodiment 2, wherein the second capillary is connected to and abruptly enlarged from the first capillary. Abruptly enlarged can include the first capillary being joined at an end of, protruded inside, or connected to the second capillary, and can include a positive, negative, zero, flat, continuous, discontinuous, constant, or variable slope measured in the direction of travel of the fiber. In some embodiments the first capillary has an inner diameter about equal to a diameter of a subject fiber (with or without an allowance for a specified radius or diameter of process fluid surrounding the fiber) and an outer diameter about equal to an inner diameter of the second capillary. In other embodiments the first capillary has an outer diameter smaller than an inner diameter of the second capillary. In alternative embodiments the first capillary has an outer diameter larger than an inner diameter of the second capillary. Certain embodiments provide structures as known in the art of rope-coiling fibers, as herein disclosed, or as may be later developed, suitable to produce rope-coiling sufficient to practice the subject invention. Embodiment 4. The system of Embodiment 3, wherein the first capillary is configured and adapted to approximate the flow of the process fluid and the movement of the fiber from the connected fiber making device, and the second capillary is configured and adapted to create a condition of axial compression in the fiber sufficient to induce coiling under specified conditions as known in the art of rope-coiling fibers, as herein disclosed, or as may be later developed, and to form the fiber into a coiled fiber. Embodiment 5. The system of Embodiment 1, wherein the coil measurement device is a non-destructive measurement device. Embodiment 6. The system of Embodiment 5, wherein the coil measurement device is a non-contact measurement device. Embodiment 7. The system of Embodiment 6, wherein the coil measurement device is an image based measurement device. Embodiment 8. The system of Embodiment 5, wherein the coil measurement device is a real time measurement device. Embodiment 9. The system of Embodiment 1, wherein the coil measurement calibration device is configured and adapted to convert R.sub.coil to E based on a linear relationship between R.sub.coil and E. Embodiment 10. The system of Embodiment 9, wherein the linear relationship comprises a slope determined according to R.sub.coil of the coiled fiber. Embodiment 11. A method useful for high throughput elasticity measurement of microfibers, the method comprising the following steps: producing a microfiber having an elastic modulus (E) at a throughput greater than 1 mm/second; coiling the microfiber to create a coiled microfiber having a coil radius (R.sub.coil); recording a measurement of R.sub.coil; calculating E from R.sub.coil; and uncoiling the microfiber. Embodiment 12. The method of Embodiment 11, wherein the measurement is a non-destructive, non-contact, real-time, in-situ measurement. Embodiment 13A. The method of Embodiment 11, wherein the measurement is an optical measurement. Embodiment 13B. The method of Embodiment 11, wherein the measurement is a microfluidic measurement, or comprises a microfluidic technique. Embodiment 14. The method of Embodiment 13A or Embodiment 13B, wherein the throughput is greater than the throughput of a tensile tester. Embodiment 15. The method of Embodiment 14, wherein the throughput is greater than 1 fiber measured per minute, or optionally, greater than 1 fiber measured per second. Embodiment 16. The method of Embodiment 12, wherein the steps of recording a measurement of R.sub.coil and calculating E from R.sub.coil are repeated at least 1 time per second. Embodiment 17. The method of Embodiment 16, wherein the steps of recording a measurement of R.sub.coil and calculating E from R.sub.coil are repeated at least 2 times per second. Embodiment 18. The method of Embodiment 12, wherein the step of calculating E from R.sub.coil comprises application of a linear relationship between E and R.sub.coil. Embodiment 19. The method of Embodiment 12, comprising the step of uncoiling the fiber after recording the measurement to produce a straight fiber, the mean radius of curvature of the fiber is about 10 mm, which is much larger than the coiling radius 0.1-0.5 mm. Embodiment 20. A system useful for high throughput elasticity measurement of microfibers, the system comprising: a coiling device configured and adapted for operable connection to a fiber making device; a coil measurement device configured and adapted to capture a coil radius (R.sub.coil) measurement of a coil created by the coiling device; a coil measurement calibration device configured and adapted to convert R.sub.coil to a fiber elasticity value (E); wherein the coiling device is configured and adapted to receive a flow of a process fluid and a movement of a fiber from a connected fiber making device through an upstream portion to a downstream portion, the coiling device comprising a first capillary forming a small channel in the upstream portion and a second capillary forming a wide channel in the downstream portion; wherein the second capillary is connected to and abruptly enlarged from the first capillary; wherein the first capillary is configured and adapted to approximate the flow of the process fluid and the movement of the fiber from the connected fiber making device, and the second capillary is configured and adapted to create a condition of axial compression in the fiber sufficient to induce coiling under specified conditions and to form the fiber into a coiled fiber; wherein the coil measurement device is a non-destructive, non-contact, image based, real time measurement device; wherein the coil measurement calibration device is configured and adapted to convert R.sub.coil to E based on a linear relationship between R.sub.coil and E; and wherein the linear relationship comprises a slope determined according to R.sub.coil of the coiled fiber. Embodiment 21. A system useful for high throughput elasticity measurement of a target microfiber, the system comprising: a rope-coiling device configured and adapted to induce rope-coiling in the target microfiber, thereby creating a coiled microfiber; a measurement device configured and adapted to measure one or more physical properties of the coiled microfiber within the rope-coiling device, thereby creating a coiled microfiber measurement; and a calibration device configured and adapted to convert the coiled microfiber measurement to a microfiber elasticity measurement. Embodiment 22. The system of Embodiment 21, wherein the measurement device is a microfluidic measurement device. Embodiment 23. The system of Embodiment 22, wherein the calibration device comprises a calibration curve, calibration formula, or calibration table. Embodiment 24. The system of Embodiment 23, wherein the rope-coiling device is a microfluidic device. Embodiment 25. The system of Embodiment 24, wherein the coiled microfiber measurement comprises a rope-coiling radius, diameter, or velocity and the calibration device comprises a linear relationship between the rope-coiling radius, diameter, or velocity and the microfiber elasticity measurement. Embodiment 26. A method useful for high throughput elasticity measurement of a target microfiber, the system comprising: rope-coiling the target microfiber in a chamber, thereby creating a coiled microfiber; measuring one or more physical properties of the coiled microfiber within the chamber, thereby creating a coiled microfiber measurement; and converting the coiled microfiber measurement to a microfiber elasticity measurement. Embodiment 27. The method of Embodiment 26, wherein the measuring is done by a microfluidic measurement device. Embodiment 28. The method of Embodiment 27, wherein the converting is done by reference to a calibration curve, calibration formula, or calibration table. Embodiment 29. The method of Embodiment 28, wherein the chamber is a microfluidic device. Embodiment 30. The method of Embodiment 29, wherein the coiled microfiber measurement comprises a rope-coiling radius, diameter, or velocity and the reference to a calibration curve, calibration formula, or calibration table comprises a linear relationship between the rope-coiling radius, diameter, or velocity and the microfiber elasticity measurement. Embodiment 31. A microfluidic method useful for high throughput elasticity measurement of a target microfiber, the system comprising: rope-coiling a solidified section of the target microfiber in a microfluidic chamber, thereby creating a coiled microfiber section; measuring, by a microfluidic sensor, a coil radius of the coiled microfiber section within the chamber, thereby creating a coiled microfiber measurement; converting the coiled microfiber measurement to a microfiber elasticity measurement; and uncoiling the coiled microfiber section. Embodiment 32. A microfluidic system useful for high throughput elasticity measurement of a target microfiber, the system comprising: a microfluidic rope-coiling device configured and adapted to induce rope-coiling in a section of the target microfiber, thereby creating a coiled microfiber section; a microfluidic measurement device configured and adapted to measure a rope-coiling radius of the coiled microfiber section within the microfluidic rope-coiling device; and a calibration device configured and adapted to convert the rope-coiling radius to a microfiber elasticity measurement.
(15) One embodiment is schematically illustrated in
(16) Coiling can occur spontaneously according to an embodiment of the subject invention when microfibers enter a wide channel in a coiling device, as shown in
(17) Embodiments can analyze the relation between the elasticity and the coiling radius, as shown in
(18) Coiling methods according to embodiments of the subject invention can have several advantages over conventional pulling methods for analyzing elastic properties of fibers. For example, the throughput of certain embodiments can be up to or more than tens, hundreds, or thousands of times higher than the comparable throughput of a tensile tester. This is at least in part because in the microfluidic device it takes only one second or less than one second to measure a single microfiber. To do the same measurement on a tensile tester, using related art methods, it takes 15 minutes to complete each measurement, in part due to the skill-intensive process of loading/unloading fragile samples. One important bottleneck of the pulling method can be (e.g., for tiny and/or fragile samples) the time-consuming and skill-intensive process of sample loading and unloading. Due to the high time and labor cost, the quality of the fibers can only be assessed statistically with sampling. In contrast, for the continuous flow coiling methods provided by embodiments of the subject invention, sample loading and unloading are not needed between consecutive measurements, so certain embodiments can measure the elasticity of every microfiber in real time (e.g., taking one measurement per second, or one measurement per minute, or faster or slower, as determined according to the stability of the fiber manufacturing process) by automatic video, image, or other sensor data analysis (e.g., by optical, microscopic, or microfluidic techniques). Alternative embodiments can measure select microfibers, can measure asynchronously or in parallel, and can measure by alternate sensors utilizing methods known in the art, herein disclosed, or later developed.
(19) Additionally, the coiling method enables embodiments to achieve an in situ on-line measurement in a microfluidic production line, as demonstrated in
(20) Further, embodiments can measure the local elasticity of a segment with a spatial resolution on the order of the coiling radius rather than that of the whole fiber. This heterogeneity is demonstrated in
Materials and Methods
(21) All patents, patent applications, provisional applications, and publications referred to or cited herein are incorporated by reference in their entirety, including all figures and tables, to the extent they are not inconsistent with the explicit teachings of this specification.
(22) Following are examples that illustrate procedures for practicing the invention. These examples should not be construed as limiting. All percentages are by weight and all solvent mixture proportions are by volume unless otherwise noted.
Example 1
(23) Fabrication of Microfibers
(24) The device for making fibers is a microfluidic co-flow device with pulsed UV illumination. The co-flow device consists of two coaxially aligned inlets made by a tapered inner circular capillary in an outer square capillary, as shown in
(25) Microfibers are made of polyethylene glycol diacrylate (PEGDA) and can be cured by UV illumination.
Example 2
(26) Coiling of Microfibers
(27) The coiling device is made by connecting two glass capillaries to form a small channel upstream and a wide channel downstream as shown in
(28) Coiling occurs when the microfibers enter the wide channel downstream, as shown in
(29) We also carry out experiments for different experimental conditions (fiber elasticities, fiber velocity, fiber diameter, and channel size) and measure the resulting coiling radius, as shown in
(30) It should be understood that the examples and embodiments described herein are for illustrative purposes only and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this application and the scope of the appended claims. In addition, any elements or limitations of any invention or embodiment thereof disclosed herein can be combined with any and/or all other elements or limitations (individually or in any combination) or any other invention or embodiment thereof disclosed herein, and all such combinations are contemplated with the scope of the invention without limitation thereto.
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