CARBON FIBER WINDOW FOR X-RAY DIFFRACTOMETER
20210080410 ยท 2021-03-18
Assignee
Inventors
- Vedran Nicholas VUKOTIC (Oldcastle, CA)
- Stanislav VEINBERG (Oldcastle, CA)
- Natan CARATASANOV (Oldcastle, CA)
Cpc classification
B32B27/12
PERFORMING OPERATIONS; TRANSPORTING
B32B5/26
PERFORMING OPERATIONS; TRANSPORTING
G01N23/207
PHYSICS
G01N23/20008
PHYSICS
B32B2262/106
PERFORMING OPERATIONS; TRANSPORTING
B32B9/007
PERFORMING OPERATIONS; TRANSPORTING
B32B15/14
PERFORMING OPERATIONS; TRANSPORTING
B32B5/12
PERFORMING OPERATIONS; TRANSPORTING
International classification
G01N23/20008
PHYSICS
B32B27/12
PERFORMING OPERATIONS; TRANSPORTING
B32B27/28
PERFORMING OPERATIONS; TRANSPORTING
B32B5/02
PERFORMING OPERATIONS; TRANSPORTING
B32B5/12
PERFORMING OPERATIONS; TRANSPORTING
B32B5/26
PERFORMING OPERATIONS; TRANSPORTING
Abstract
An X-ray window of an X-ray diffractometer diffraction chamber is provided. The X-ray window can include: a plurality of unidirectional carbon fiber sheets stacked one over another, wherein carbon fibers in adjacent carbon fiber sheets are disposed at an angle relative to one another; and a binding material that binds the plurality of unidirectional carbon fiber sheets together, the binding material being at least partially transparent to X-ray radiation. The X-ray window can also or alternatively include: at least one carbon fiber sheet, the X-ray window having a carbon fiber content of at least 50 wt % and a thickness between about 0.2 mm and about 5 mm to be adapted for use at a pressure greater than atmospheric pressure.
Claims
1. An X-ray window of an X-ray diffractometer diffraction chamber, the X-ray window comprising a plurality of unidirectional carbon fiber sheets stacked one over another and bound together, wherein carbon fibers in adjacent carbon fiber sheets are disposed at an angle relative to one another.
2. The X-ray window of claim 1, that is adapted for use at a pressure greater than atmospheric pressure.
3. The X-ray window of claim 1, that is adapted for use at atmospheric pressure or at a pressure lower than atmospheric pressure.
4. The X-ray window of claim 1, wherein the plurality of unidirectional carbon fiber sheets comprises: a first carbon fiber sheet comprising carbon fibers oriented in a first direction; and a second carbon fiber sheet stacked over the first carbon fiber sheet, the second carbon fiber sheet comprising carbon fibers oriented in a second direction at an angle .sub.1-2 between about 5 and about 175 relative to the first direction.
5. The X-ray window of claim 4, wherein the plurality of unidirectional carbon fiber sheets further comprises: a third carbon fiber sheet stacked over the second carbon fiber sheet, the third carbon fiber sheet comprising carbon fibers oriented in a third direction at an angle .sub.2-3 between about 5 and about 175 relative to the second direction.
6. The X-ray window of claim 1, wherein each of the unidirectional carbon fiber sheets is independently oriented at an angle of about 45 or about 90 relative to adjacent unidirectional carbon fiber sheets.
7. The X-ray window of claim 1, further comprising a binding material that binds the plurality of unidirectional carbon fiber sheets together, the binding material being at least partially transparent to X-ray radiation.
8. The X-ray window of claim 7, wherein the binding material comprises at least one of a thermosetting polymer and a thermoplastic polymer.
9. The X-ray window of claim 1, further comprising at least one layer of non-carbon fiber material that is at least partially transparent to X-ray radiation.
10. The X-ray window of claim 7, having a carbon fiber content between 50 wt % and 70 wt %, and a binding material content between about 50 wt % and about 30 wt %.
11. An X-ray window of an X-ray diffractometer diffraction chamber, the X-ray window comprising at least one carbon fiber sheet, the X-ray window having a carbon fiber content of at least 50 wt % and a thickness between about 0.2 mm and about 5 mm to be adapted for use at a pressure greater than atmospheric pressure.
12. The X-ray window of claim 11, wherein the pressure is of about 2 atm or greater.
13. The X-ray window of claim 11, wherein the at least one carbon fiber sheet comprises a plurality of unidirectional carbon fiber sheets stacked one over another, wherein carbon fibers in adjacent carbon fiber sheets are disposed at an angle relative to one another.
14. The X-ray window of claim 13, wherein the plurality of unidirectional carbon fiber sheets comprises: a first carbon fiber sheet comprising carbon fibers oriented in a first direction; and a second carbon fiber sheet stacked over the first carbon fiber sheet, the second carbon fiber sheet comprising carbon fibers oriented in a second direction at an angle .sub.1-2 between about 5 and about 175 relative to the first direction.
15. The X-ray window of claim 13, wherein each of the unidirectional carbon fiber sheets is independently oriented at an angle of about 45 or about 90 relative to adjacent unidirectional carbon fiber sheets.
16. The X-ray window of claim 11, further comprising at least one layer of non-carbon fiber material that is at least partially transparent to X-ray radiation.
17. The X-ray window of claim 16, wherein the non-carbon fiber material comprises at least one of beryllium, a polymer, diamond, graphene, diamond-like carbon, carbon nanotubes, and combinations thereof.
18. The X-ray window of claim 17, wherein the polymer comprises a polyimide.
19. The X-ray window of claim 16, wherein the at least one layer of non-carbon fiber material is stacked over or under the plurality of unidirectional carbon fiber sheets.
20. The X-ray window of claim 16, wherein the at least one layer of non-carbon fiber material comprises two layers of non-carbon fiber material sandwiching the plurality of unidirectional carbon fiber sheets.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
X-Ray Window
[0140] The present description provides X-ray windows including at least one carbon fiber sheet. As will be further described herein, the X-ray window can include a single carbon fiber sheet, or several carbon fiber sheets stacked one over another and bound together. In some embodiments, the carbon fiber sheets can be unidirectional carbon fiber sheets. In some embodiments, the unidirectional carbon fiber sheets can be disposed at an angle relative to one another. In other embodiments, the X-ray window can include one or more woven carbon fiber sheets, such as a carbon fiber twill weave. Several non-limiting examples and features of the X-ray windows are described herein.
[0141] The X-ray window can be adapted for use at different pressures, such as atmospheric pressure, under vacuum, at a pressure lower than atmospheric pressure, or at a pressure higher than atmospheric pressure. For example, the X-ray window can be adapted for use at pressures of about 2 atm and/or greater. For example, the thickness of the X-ray window can be adjusted depending on various parameters to be able to withstand high pressure while X-ray diffraction measurements can still be performed. The X-ray window can also be adapted by covering at least a portion of the X-ray window with a securing plate to which at least a portion of the pressure forces can be transferred. In some scenarios, the thickness of the X-ray window can be between about 0.2 mm and about 5 mm, or between about 0.2 mm and about 2 mm, or between about 0.25 mm and about 2 mm, or between about 0.25 mm and 1 mm.
[0142] As illustrated on
[0143] As illustrated on
[0144] It should be understood that the number of carbon fiber sheets that can be stacked over one another are not limited to 2 or 3, as shown in the exemplified embodiments of
[0145] In some scenarios, the angle is of about 45 or about 90. In some scenarios, the X-ray window can be provided in a quasi-isotropic configuration, wherein the carbon fibers of each carbon fiber sheet are oriented at an angle of about 45 with reference to the carbon fibers of an adjacent carbon fiber sheet upon which it is stacked. It should be understood that when the term quasi-isotropic configuration is used, with angles of about 45 between neighboring carbon fiber sheets, it is understood that the relative angle of each sheet with respect to a neighboring sheet can vary between 40 and 50 (i.e., account to an error factor on the about 45 angle). All the relative angles between the sheets of a same window are therefore not necessarily equal so long as each relative angle is of about 45.
[0146] In some scenarios, the X-ray window can be provided in a bi-directional configuration, wherein the carbon fibers of each carbon fiber sheet are oriented at an angle of about 90 with reference to the carbon fibers of an adjacent carbon fiber sheet upon which it is stacked. It should be understood that when the term bi-directional configuration is used, with angles of about 90 between neighboring carbon fiber sheets, it is understood that the relative angle of each sheet with respect to a neighboring sheet can vary between 80 and 100, or between 85 and 95 (i.e., account to an error factor on the about 90 angle). All the relative angles between the sheets of a same window are therefore not necessarily equal so long as each relative angle is of about 90.
[0147] In some embodiments the X-ray window includes at least one woven carbon fiber sheet, such as a carbon fiber twill weave. In some scenarios, the carbon fiber twill weave can be a 22 twill weave. It should be understood that at least one woven carbon fiber sheet can include a single woven carbon fiber sheet, or a plurality of woven carbon fiber sheets stacked upon one another. It should also be understood that the X-ray window can include at least one woven carbon fiber sheet and at least one unidirectional carbon fiber sheet.
[0148] The X-ray window can include a binding material that binds the carbon fiber sheets together, the binding material being at least partially transparent to X-ray radiation. In some embodiments, the binding material can include at least one of a thermosetting polymer and a thermoplastic polymer. For example, the thermosetting polymer can include an epoxy resin and the thermoplastic polymer can include a polyimide. It should be understood that certain binding materials can be classified as both a thermoplastic polymer (before curing) and a thermosetting polymer (after curing), such as certain types of polyimides. It is understood that other types of binding materials can be used to achieve desired properties of the carbon fiber window. For example, phenol resins may be used for certain applications such as high temperature applications.
[0149] In some embodiments, the X-ray window can further include at least one layer of non-carbon fiber material that is at least partially transparent to X-ray radiation. For example, the non-carbon fiber material can include at least one of beryllium, a polymer (e.g., a polyimide such as Kapton), diamond, graphene, diamond-like carbon, carbon nanotubes, and combinations thereof. In some embodiments, a layer of non-carbon fiber material can be stacked over and/or under the carbon fiber sheets. In other embodiments, a layer of non-carbon fiber material can be can be embedded in at least one of the carbon fiber sheets. In yet another embodiment, a layer of non-carbon fiber material can be stacked between two adjacent carbon fiber sheets.
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[0151] The carbon fiber content of the X-ray window can vary depending on the type of materials used in the X-ray window and/or the type of measurement performed, and/or the type of application. In some embodiments, the X-ray window can have a carbon fiber content of at least 40 wt %, or at least 50 wt %, or at least 60 wt %, or at least 70 wt %. In some embodiments, the carbon fiber content is between about 50 wt % and about 70 wt %, and the binding material content is between about 30 wt % and about 50 wt %. In some embodiments, the carbon fiber content is between 50 wt % and 70 wt %, with the remainder being the binding material. In some embodiments, the X-ray window can have a carbon fiber content of at least 40 vol %, or at least 50 vol %, or at least 60 vol %, or at least 70 vol %. In some embodiments, the carbon fiber content is between about 50 vol % and about 70 vol %, and the binding material content is between about 30 vol % and about 50 vol %. In some embodiments, the carbon fiber content is between 50 vol % and 70 vol %, with the remainder being the binding material.
[0152] By selecting appropriate X-ray panel thickness, composition, size and/or configuration of layers, the X-ray window can be adapted to attenuate a certain percentage of an X-ray radiation such as Cu, Mo and/or Ag X-ray radiation. In some scenarios, the X-ray panel can be adapted to attenuate 80% or less, or 60% or less, or 40% or less of Cu X-ray radiations. In some scenarios, the X-ray panel can be adapted to attenuate 80% or less, or 60% or less, or 40% or less, or 20% or less of Mo X-ray radiations. In some scenarios, the X-ray panel can be adapted to attenuate 80% or less, or 60% or less, or 40% or less, or 20% or less of Ag X-ray radiations.
X-Ray Diffraction Chamber
[0153] The present description also provides an X-ray diffraction chamber for an X-ray diffractometer, that can include one or more of the X-ray windows described herein. In some embodiments, the X-ray diffraction chamber can be adapted for operation at pressures higher than atmospheric pressure, such as 2 atm or greater, or for vacuum pressure applications, such as lower than 1 atm. In some embodiments, the X-ray diffraction chamber can be adapted for operation at various temperatures, humidity levels, and/or types of atmospheres (including measurements under vacuum). In some scenarios, the X-ray diffraction chamber can be used as a heating stage or to perform temperature probing. Depending on the configuration of the X-ray window (e.g., surface area, length, width of the X-ray window, configuration of the X-ray window support members, configuration of the securing plate), the X-ray diffraction chamber can be adapted to collect X-ray diffraction data at various 2 angles. In some implementations, the range of 2 angles can be between about 0.1 and 179, or between about 0.1 and about 48, or between about 10 and about 56, or between about 2 and about 70. It should be noted that the mentioned ranged are non-limiting and may vary.
[0154] Referring to
[0155] As best seen in
[0156] Still referring to
[0157] The housing 102 can also be provided with abase 112 that can be used to affix the X-ray diffraction chamber 100 to the body of the X-ray diffraction apparatus. In the embodiment shown on the Figures, the base 112 is provided with holes 114 through which a fastener can be threaded to fasten the X-ray diffraction chamber 100 to the X-ray diffraction apparatus. It should be understood that the base 112 can be affixed to the X-ray diffraction apparatus by other means.
[0158] As best seen on
[0159] The X-ray window assembly 101a, 101b includes at least an X-ray window and means of affixing the X-ray window to the housing 102. In the embodiment shown on the Figures, and as best seen on
[0160] The support surface 124 can also be provided with sealing hole 128 into which a sealing element 130 such as a gasket or an O-ring can be inserted. The sealing element 130 can allow to seal the contact area between the X-ray window 122 and the support surface 124.
[0161] In some embodiments, the securing plate 126 covers at least a certain portion of the X-ray window 101a, 101b, in order to relieve pressure force from the X-ray window and transfer at least part of the pressure forces to the securing plate 126. For example, the securing plate 126 can cover at least 20%, 30%, 40%, 50%, 60%, 70%, 80% or more of the surface area of the X-ray window 101a, 101b. Preferably, the securing plate 126 covers a portion of the X-ray window 101a, 101b starting from a periphery of the X-ray window 101a, 101b, such that a central portion of the X-ray window 101a, 101b is positioned over the aperture 111a, 111b and clear of the securing plate 126 such that X-ray radiation can pass through the first X-ray window 101a, penetrate the X-ray diffraction chamber 100 and be reflected out through the second X-ray window 101b.
[0162] Now referring to
[0163] In the embodiment shown, the support surface 224, X-ray window 222 and securing plate 226 are provided with a series of holes to allow for fasteners (e.g., screws 227 in the embodiment shown) to hold the X-ray window assembly 201 together.
[0164] The X-ray diffraction chamber 200 includes a carbon fiber window 222 that fits the outer circular shape of the X-ray diffraction chamber 200. In the embodiment shown, the X-ray window 222 is bent in a half-circle-like shape spanning from an input side of the housing 202 of the X-ray diffraction chamber 222 to an output side of the housing 202 of the X-ray diffraction chamber 222. As better shown in
[0165] It should be understood that various changes can be made to the X-ray window assembly. For example, several elements can be changed or vary, such as but not limited to the size, shape, and/or type of X-ray window, the type of fastener used to hold the X-ray window assembly together, the size, shape, thickness and/or type of securing plate. For example, the X-ray window can be a hemisphere window, that can withstand pressures above atmospheric pressure, such as up to 10 bars.
EXAMPLES
Example 1: Material Burst Pressure Test
[0166] Experiments were conducted to evaluate the burst pressure of several carbon fiber-based window films, compared to a Kapton window film. The following steps were performed to prepare for and conduct the experiments: [0167] 1. using a vessel made from an aluminum block, an oval hole (having dimensions 20 mm wide12 mm tall) was cut through the entirety of the block; this hole constituted the volume chamber. [0168] 2. A groove for a standard size O-ring (28 mm, 2 mm thickness) was made evenly around the oval hole and the O-ring placed inside it; the compression of the O-ring will form the air-tight seal required to retain pressure in the chamber. [0169] 3. An oval pattern of 12 (twelve) threaded holes was distributed evenly around the O-ring; these threaded holes will be used for securely holding the materials in place (see point 7 below). [0170] 4. A threaded hole was drilled in the aluminum block in a direction perpendicular to the oval hole, such that that two holes were connected; this second hole is used for introducing gas to the system. [0171] 5. The material to be tested was cut into two rectangles of dimensions 50 mm by 45 mm and 12 (twelve) M3 holes were drilled in a pattern matching that described in 3 above. [0172] 6. Securing plates were made out of a sheet of stainless-steel cut into a rectangle having dimensions 50 mm by 45 mm by 3 mm, having 12 (twelve) M3 holes drilled in a pattern matching that described in 3 above, and an oval hole matching that in 1. [0173] 7. The material to be tested was placed in between the aluminum block 1 and securing plates 6 and secured tightly by 12 (twelve) M3 screws. [0174] 8. The chamber was connected to an N.sub.2 gas cylinder (pressurized to ca. 2200 psi) by means of Swagelok connectors and hoses attached to the threaded hole described in 4. [0175] 9. The pressure of the system was monitored by a pressure gauge attached to the gas cylinder having pressure gradations of 100 psi. [0176] 10. The entire system (hoses from the gas cylinder and the assembled test chamber 7) was pressurized until the material failed (evidenced by tearing/breaking/cracking of the material and a subsequent release of the pressure to atmosphere).
[0177] The results are summarized in Table 1 below:
TABLE-US-00001 TABLE 1 measurement of plastic deformation pressure and burst pressure for several window films Pressure in PSI (lbs .Math. in.sup.2) Plastic Burst Window material deformation pressure Comparative: Kapton window film 150 450 (500PST, 0.15 mm thickness) 0.38 mm laminated carbon fiber sheet 150 650 (0.08 mm Polyethylene terephthalate (PET) laminating material and 0.3 mm carbon fiber panel) 0.3 mm carbon fiber sheet - 3k thread N/A 450 count - 2 2 twill weave 0.5 mm carbon fiber sheet - 6k thread N/A 650 count - 2 2 twill weave 0.8 mm carbon fiber sheet - three (3) N/A 1800 unidirectional carbon fiber layers in a quasi isotropic configuration (i.e., each layer has a 45 angle compared to adjacent(s) layer(s)) - 6k thread count
[0178] It was shown that the 0.8 mm carbon fiber sheet made of multiple unidirectional carbon fiber layers was able to withstand a far greater pressure compared to the comparative Kapton window and compared to the 0.3 mm and 0.5 mm carbon fiber sheets.
Example 2: X-Ray Attenuation Tests with Cu Source (=1.541 )
[0179] Experiments were conducted to evaluate X-ray attenuation with window films made of different materials, when using a copper source.
[0180] The cell body was aligned in an X-ray diffractometer according to standard practice (i.e., centering the sample in the beam path, adjusting beam alignment, and referencing zero position), diffraction patterns for a sample of LaB.sub.6 were obtained in Bragg-Brentano geometry in the 20 range of 1060 and using Cu radiation.
[0181] Five diffraction peaks are present for LaB.sub.6 in this 2 range. The window film materials were changed in between measurements, from no material (100% intensity reference) to Kapton, to different thicknesses and types of carbon fiber materials. The results are summarized in
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[0183] While all the CF sheets exhibited a greater attenuation than the comparative Kapton window when using a copper source, the attenuation still allowed for conducting X-ray measurements. One can simply run the X-ray diffraction experiment for a longer time period to arrive at the same signal intensity.
Example 3: X-Ray Attenuation Tests with Mo Source (=0.709 {acute over ()})
[0184] Experiments were conducted to evaluate X-ray attenuation with window films made of different materials, when using a molybdenum source.
[0185] The cell body was aligned in an X-ray diffractometer according to standard practice (i.e., centering the sample in the beam path, adjusting beam alignment, and referencing zero position), diffraction patterns for a sample of LaB.sub.6 were obtained in Bragg-Brentano geometry in the 20 range of 733 and using Mo radiation.
[0186] Eight diffraction peaks are present for LaB.sub.6 in this 20 range. Following the same procedure as for the tests using Cu radiation above, the window materials were changed in between measurements, from no material (100% intensity reference) to Kapton, to different thicknesses and types of carbon fiber materials. The results are summarized in
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[0188] All the CF sheets exhibited a slightly increased attenuation than the comparative Kapton window when using a molybdenum source. The small attenuation allowed conducting X-ray measurements with little effect on the intensity. One can simply run the X-ray diffraction experiment for a slightly longer time period to arrive at the same signal intensity.