Microstructured glass articles with at least 100 core elements and methods for forming the same
11643354 · 2023-05-09
Assignee
Inventors
Cpc classification
C03B37/01282
CHEMISTRY; METALLURGY
C03B37/027
CHEMISTRY; METALLURGY
C03B37/01446
CHEMISTRY; METALLURGY
G02B6/02395
PHYSICS
G02B6/0281
PHYSICS
C03B37/01214
CHEMISTRY; METALLURGY
International classification
C03B37/012
CHEMISTRY; METALLURGY
C03B37/014
CHEMISTRY; METALLURGY
C03B37/027
CHEMISTRY; METALLURGY
Abstract
According to embodiments, a method of making a microstructured glass article includes bundling M bare optical fibers in a fiber bundle, wherein M is an integer greater than 100. Thereafter, the fiber bundle may be inserted in a cavity of a soot preform. The soot preform may have a density of less than or equal to 1.5 g/cm.sup.3 and comprise silica-based glass soot. The soot preform and inserted fiber bundle may then be consolidated to form a microstructured glass article preform. The microstructured glass article preform may then be drawn into the microstructured glass article comprising M core elements embedded in a cladding matrix.
Claims
1. A method of making a microstructured glass article, the method comprising: bundling M bare optical fibers in a fiber bundle, wherein M is greater than 100; inserting the fiber bundle in a cavity of a soot preform, the soot preform having a density of less than or equal to 1.5 g/cm.sup.3 and comprising silica-based glass soot; consolidating the soot preform and inserted fiber bundle to form a microstructured glass article preform; and drawing the microstructured glass article preform into the microstructured glass article comprising M core elements embedded in a cladding matrix.
2. The method of claim 1, wherein the soot preform and inserted fiber bundle are consolidated at a temperature from about 1225° C. to about 1535° C.
3. The method of claim 1, further comprising drying the soot preform and inserted fiber bundle at a temperature from about 1000° C. to 1200° C. in flowing chlorine gas after inserting and prior to consolidating.
4. The method of claim 1, further comprising doping the soot preform with fluorine during the consolidating.
5. The method of claim 1, wherein the bare optical fibers have diameters from about 50 μm to about 500 μm.
6. The method of claim 1, wherein the bare optical fibers comprise a glassy layer comprising less than or equal to 15 wt. % TiO.sub.2.
7. The method of any of claim 1, wherein the core elements have a step index profile or a graded index profile.
8. The method of claim 1, wherein the core elements have a refractive index n.sub.C, the cladding matrix has a refractive index n.sub.C1, and n.sub.C>n.sub.C1.
9. The method of claim 1, wherein each core element has a low-index annulus surrounding the core element, the low-index annulus having an index of refraction n.sub.L such that n.sub.L<n.sub.C1<n.sub.C.
10. The method of claim 1, wherein the core elements have a refractive index n.sub.C, the cladding matrix has a refractive index n.sub.C1, and n.sub.C<n.sub.C1.
11. The method of claim 2, wherein the soot preform and inserted fiber bundle are consolidated at from about 1390° C. to about 1535° C.
12. The method of claim 8, wherein a relative refractive index percent (Δ%) of the core elements relative to the cladding matrix is greater than about 0.3%.
13. The method of claim 9, wherein the low-index annulus comprises from about 0.36 wt % to about 3.0 wt % fluorine of the low-index annulus.
14. The method of claim 1, wherein the core elements comprise silica-based glass up-doped with germania.
15. The method of claim 14, wherein the silica-based glass up-doped with germania comprises from about 5 wt % to about 16 wt % GeO.sub.2 of the core elements.
16. The method of claim 1, wherein the core elements have radii less than or equal to 5 μm.
17. The method of claim 16, wherein the radii are from 100 nm to 500 nm.
18. The method of claim 1, wherein the soot preform has a density from 0.3 g/cm.sup.3 to 1.2 g/cm.sup.3.
19. The method of claim 1, wherein the core elements are hollow.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
(16) Reference will now be made in detail to embodiments of the microstructured glass articles and methods for making the same, examples of which are illustrated in the accompanying drawings. Whenever possible, the same reference numerals will be used throughout the drawings to refer to the same or like parts. One embodiment of a microstructured glass article is schematically depicted in cross section in
(17) Ranges can be expressed herein as from “about” one particular value, and/or to “about” another particular value. When such a range is expressed, another embodiment includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent “about,” it will be understood that the particular value forms another embodiment. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
(18) Directional terms as used herein—for example up, down, right, left, front, back, top, bottom—are made only with reference to the figures as drawn and are not intended to imply absolute orientation.
(19) Unless otherwise expressly stated, it is in no way intended that any method set forth herein be construed as requiring that its steps be performed in a specific order, nor that with any apparatus specific orientations be required. Accordingly, where a method claim does not actually recite an order to be followed by its steps, or that any apparatus claim does not actually recite an order or orientation to individual components, or it is not otherwise specifically stated in the claims or description that the steps are to be limited to a specific order, or that a specific order or orientation to components of an apparatus is not recited, it is in no way intended that an order or orientation be inferred, in any respect. This holds for any possible non-express basis for interpretation, including: matters of logic with respect to arrangement of steps, operational flow, order of components, or orientation of components; plain meaning derived from grammatical organization or punctuation, and; the number or type of embodiments described in the specification.
(20) As used herein, the singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to “a” component includes aspects having two or more such components, unless the context clearly indicates otherwise.
(21) The phrase “bare optical fiber” refers to optical fiber which is devoid of any organic coatings applied to the glass portion of the optical fiber.
(22) The phrase “refractive index profile,” as used herein, refers to the relationship between refractive index or relative refractive index and the dimensions of the optical fiber.
(23) The phrase “relative refractive index,” as used herein, is defined as Δ(r)%=100×(n(r).sup.2−n.sub.REF.sup.2)/2n.sub.i.sup.2, where n.sub.i is an extrema of the refractive index in region i (i.e., the minimum or maximum of the refractive index in region i), unless otherwise specified. The relative refractive index percent is measured at 1550 nm unless otherwise specified. The term n.sub.REF is the average refractive index of the cladding matrix, which can be calculated, for example, by taking “N” index measurements (n.sub.c1, n.sub.c2, . . . n.sub.cN) of the cladding matrix (which, in some embodiments, may be undoped silica), and calculating the average refractive index by:
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(25) As used herein, the relative refractive index is represented by A and its values are given in units of “%,” unless otherwise specified. In cases where the refractive index of a region is less than the reference index n.sub.REF, the relative refractive index is negative and is referred to as having a depressed region or depressed-index, and the minimum relative refractive index is calculated at the point at which the relative refractive index is most negative, unless otherwise specified. In cases where the refractive index of a region is greater than the reference index n.sub.REF, the relative index percent is positive and the region can be said to be raised or to have a positive index.
(26) The term “α-profile” or “alpha profile” refers to a relative refractive index profile of the core elements, expressed in terms of Δ(r) which is in units of “%”, where r is the radius of the core element and which follows the equation:
Δ(r)%=Δ(r.sub.o)(1−[|r−r.sub.o|/(r.sub.1−r.sub.o)].sup.α),
where r.sub.o is the point at which Δ(r) is maximum, r.sub.1 is the point at which Δ(r)% is zero with respect to the common outer cladding, and r is in the range r.sub.i≤r≤r.sub.f, where Δ is defined as above, r.sub.i is the initial point of the α-profile, r.sub.f is the final point of the α-profile, and α is an exponent which is a real number. For a profile segment beginning at the centerline of a core element (i.e., r=0), the α-profile has the simpler form
Δ(r)%=Δ(0)(1−[|r|/(r.sub.1)].sup.α),
where Δ(0) is the refractive index delta at the centerline of the core element.
(27) Microstructured glass articles can have unique optical properties, such as refractive index, dispersion, scattering, and nonlinear effects, that conventional materials do not have. Microstructured glass articles may be used for a variety of applications including, but not limited to, optical fiber, imaging components, display components, and other optical components. For these applications, it may be desirable to have a large number (e.g., a hundred to several thousand) closely-spaced microstructure elements (e.g., core elements) having a different refractive index than that of the matrix or background material (i.e., the cladding matrix). However, making such microstructured glass articles can be challenging. The embodiments described herein relate to techniques for making microstructured glass articles with a large number of core elements and microstructured glass articles made thereby.
(28) Referring now to
(29) In the embodiments described herein, the cladding matrix 104 is formed from silica-based glass (SiO.sub.2) with an index of refraction n.sub.C1. In embodiments, the index of refraction n.sub.C1 of the cladding matrix 104 is generally less than the index of refraction n.sub.C of the core elements 102 (i.e., n.sub.C1<n.sub.C). In some embodiments the cladding matrix 104 is substantially free from dopants or contaminants which would alter the index of refraction of the cladding matrix 104 including, without limitation, up-dopants (i.e., germanium and the like) and down-dopants (i.e., boron, fluorine and the like). The term “substantially free,” as used herein, means that the cladding matrix 104 does not contain any constituent components intentionally added to the glass of the cladding matrix 104 but may contain impurities or “tramp” contaminants in an amount less than or equal to about 0.1 wt. %. In other embodiments, the cladding matrix 104 may comprise one or more up-dopants which increases the refractive index of the silica glass, or one or more down-dopants which decreases the refractive index of the silica glass.
(30) In the embodiment of the microstructured glass article 100 depicted in
(31) In the embodiments described herein, the relative refractive index Δ.sub.C of the core elements 102 relative to the cladding matrix 104 is greater than or equal to 0.3%. For example, in some embodiments, the relative refractive index Δ.sub.C of the core elements 102 relative to the cladding matrix 104 is greater than or equal to about 0.5% or even greater than or equal to about 0.75% relative to the cladding matrix 104. In some embodiments, the relative refractive index Δ.sub.C of the core elements 102 relative to the cladding matrix 104 is greater than or equal to about 1.0% or even greater than or equal to about 1.5% relative to the cladding matrix 104. In still other embodiments, the relative refractive index Δ.sub.C of the core elements 102 relative to the cladding matrix 104 is greater than or equal to about 2.0% relative to the cladding matrix 104. In these embodiments, the relative refractive index Δ.sub.C of the core elements 102 relative to the cladding matrix 104 is less than or equal to about 3.0% relative to the cladding matrix 104.
(32) In the embodiments described herein, the core elements 102 generally have radii r that are less than or equal to 5 μm or even less than or equal to 3 μm. In some embodiments, the core elements 102 generally have radii r that are less than or equal to 2 μm or even less than or equal to 1 μm. In some of these embodiments, the core elements 102 generally have radii r that are greater than or equal to 100 nm and less than or equal to 500 nm.
(33) While
(34) Referring now to
(35) In some embodiments described herein, all of the M core elements 102 may have step refractive index profiles as depicted in
(36) Referring now to
(37) In some embodiments, the low-index annulus 108 may comprise silica glass down-doped with fluorine. For example, the low-index annulus 108 may comprise from about 0.36 wt. % to about 3.0 wt. % fluorine, from about 0.72 wt. % to about 2.5 wt. % fluorine, or even from about 1.4 wt. % to about 2.0 wt. % fluorine such that the relative refractive index percent Δ.sub.L of the low-index annulus 108 relative to the cladding matrix 104 is less than the relative refractive index of the core elements 102 relative to the cladding matrix 104. For example, in some embodiments, the relative refractive index of the low-index annulus 108 relative to the cladding matrix 104 is less than or equal to about −0.2%. In some embodiments, the relative refractive index percent Δ.sub.L of the low-index annulus 108 relative to the cladding matrix 104 may be greater than or equal to about −1.0%. For example, in some embodiments, the relative refractive index percent Δ.sub.L of the low-index annulus 108 is greater than or equal to about −1.0% and less than or equal to about −0.2% relative to the cladding matrix 104. In some other embodiments, the relative refractive index percent Δ.sub.L of the low-index annulus 108 is greater than or equal to about −0.5% and less than or equal to about −0.3% relative to the cladding matrix 104.
(38) In some embodiments, the low-index annulus 108 may be positioned in direct contact with the corresponding core element 102. In other embodiments, the low-index annulus may be spaced apart from the corresponding core element 102 by an offset spacing d. The offset spacing d may generally be in the range from greater than 0 μm to less than or equal to about 1 μm. In embodiments, the offset spacing d may be in the range from greater than or equal to about 0 μm to less than or equal to about 0.5 μm. The low-index annuli 108 generally reduce the cross-talk between adjacent core elements and facilitate spacing adjacent core elements closer together than adjacent core elements which do not have low-index annuli without increasing the amount of cross-talk between the adjacent core elements. Accordingly, in some embodiments described herein, core elements with low-index annuli may be utilized to decrease the spacing between adjacent core members.
(39) While
(40) Referring to
(41) Referring now to
(42) Still referring to
(43) The microstructured glass articles 100, 200, 300 described herein may be formed in a variety of cross-sectional shapes. For example,
(44) Methods of making the microstructured glass articles 100, 200, 300 will now be described with reference to
(45) In one embodiment, the cladding matrix 104 (
(46) Referring now to
(47) The vapor phase silica-based glass precursor material and dopant precursor materials (if included) are reacted in the flame 426 to produce silica-based glass soot 428 which is deposited on the bait rod 420 as the bait rod is rotated. The flame 426 of the gas-fed burner 422 is traversed back and forth over the axial length of the bait rod 420 as indicated by arrow 424 as the bait rod 420 is rotated thereby building up the doped silica-based glass soot on the bait rod 420 and forming the soot preform 402. In the embodiments described herein, the silica-based glass soot is deposited on the bait rod 420 such that the soot preform has a density of less than 1.5 g/cm.sup.3. In embodiments, the density of the soot preform is in the range from greater than or equal to 0.3 g/cm.sup.3 to less than or equal to 1.2 g/cm.sup.3.
(48) In step 604, once sufficient silica-based glass soot 428 is built up on the bait rod 420 to achieve a soot preform 402 having the desired outer diameter, the deposition of the silica-based glass soot 428 is discontinued and the bait rod 420 is removed from the soot preform 402 such that a cavity extends through the axial length of the soot preform. The cavity may have a diameter from about 10 mm to about 10 cm. In step 606, a glass plug (not shown) may be optionally inserted in one end of the cavity to hold a fiber bundle (described in more detail herein) in the cavity of the soot preform 402. In embodiments where a glass plug is used, the glass plug may include a central port to allow gasses to flow through the glass plug and into (or out of) the cavity in the soot preform 402.
(49) Referring now to
(50) Still referring to
(51) Referring now to
(52) Referring now to
(53) Thereafter, in step 620, the soot preform 402 and the inserted fiber bundle 440 are heated to a temperature from about 1225° C. to about 1535° C. to densify (i.e., consolidate) the silica-based glass soot of the soot preform 402 into fully dense glass (i.e., glass with a density of approximately 2.2 g/cm.sup.3) and to fuse the fibers of the fiber to each other and to the densified glass of the preform. In embodiments, the soot preform 402 and the inserted fiber bundle 440 are heated to a temperature from about 1390° C. to about 1535° C. to densify the silica-based glass soot of the soot preform 402. The soot preform 402 and inserted fiber bundle 440 may be densified in an atmosphere of flowing helium. In other embodiments, such as embodiments where the cladding matrix is down-doped with fluorine, fluorine gas may be directed through the soot preform 402 during consolidation to dope the soot preform 402 with fluorine and thereby decrease the index of refraction of the cladding matrix. As the silica-based glass soot is consolidated and sintered into fully dense glass, the bare optical fibers of the fiber bundle 440 are fused to one another and to the glass of the soot preform 402 thereby forming a microstructured glass article preform having preform core elements (i.e., the bare optical fibers) embedded in a preform cladding matrix (i.e., the densified silica-based glass soot). In embodiments, a vacuum may be drawn on the microstructured glass article preform during the consolidation process to remove any residual air from the preform and thereby assist in densification.
(54) Thereafter, in step 622, the microstructured glass article preform may be further processed by conventional optical fiber manufacturing techniques to form microstructured glass articles. For example, in embodiments, the microstructured glass article preform may be drawn directly into optical fiber utilizing conventional optical fiber drawing techniques. The optical fiber includes a plurality of core elements in a cladding matrix, as described herein with respect to
(55) While
(56) Referring now to
EXAMPLES
(57) The embodiments described herein will be further clarified by the following examples.
Example 1
(58) A soot preform was formed by depositing approximately 3,000 g of silica-glass based soot on a bait rod having a diameter of 9 mm. The deposited soot was substantially free from dopants (i.e., the soot was pure silica glass). The soot preform had a density of approximately 0.45 g/cm.sup.3 following removal of the bait rod.
(59) Bare optical fiber was drawn from a multimode optical fiber preform. The optical fiber comprised a core surrounded by a cladding of pure silica glass. The core of the optical fiber had a relative refractive index of 1% relative to the cladding and a graded index profile with alpha value of about 2.1. The optical fiber had a diameter of 500 μm and a length of approximately 2 km. The optical fiber was segmented into 50 cm lengths and the 50 cm lengths were grouped into a fiber bundle having from about 150 to 200 fibers.
(60) The fiber bundle was inserted into the cavity of the soot preform formed by the bait rod. A glass plug having a small channel was inserted into one end of the soot preform to retain the fiber bundle in place. The soot preform and inserted fiber bundle was dried in a consolidation furnace with flowing chlorine gas at a temperature of about 1100° C. for 30 minutes. The soot preform and inserted fiber bundle were then consolidated in a consolidation furnace at 1450° C. in a He atmosphere for 2 hours to form a microstructured glass article preform.
(61) After consolidation a vacuum was drawn on the portion of the microstructured glass article preform corresponding to the fiber bundle as the preform was drawn to a smaller diameter to remove any residual air from the preform. The microstructured glass preform was then drawn directly into optical fiber having a diameter of about 350 μm with a plurality of core elements corresponding to the optical fibers of the fiber bundle (i.e., a microstructured glass article). An image of a cross-section of microstructured glass article is shown in
Example 2
(62) A microstructured glass article preform was made using the process of Example 1, with the exception that the microstructured glass had a relative refractive index Δ.sub.C% of 2% relative to the cladding. The microstructured glass article preform was drawn into a microstructured glass article having a diameter of 300 micrometers. An image of the cross-section of this fiber is shown in
(63) It will be apparent to those skilled in the art that various modifications and variations can be made to the embodiments described herein without departing from the spirit and scope of the claimed subject matter. Thus it is intended that the specification cover the modifications and variations of the various embodiments described herein provided such modification and variations come within the scope of the appended claims and their equivalents.