The present application is related to x-ray windows.
X-ray windows are designed to transmit a high percent of x-rays, even low energy x-rays. X-ray windows are used in expensive systems requiring high reliability. High system requirements result in demanding characteristics of the x-ray window.
Definitions. The following definitions, including plurals of the same, apply throughout this patent application.
As used herein, the terms “on”, “located on”, “located at”, and “located over” mean located directly on or located over with some other solid material between. The terms “located directly on”, “adjoin”, “adjoins”, and “adjoining” mean direct and immediate contact.
As used herein, the terms “same as” or “equals” mean exactly the same; the same within normal manufacturing tolerances; or almost exactly the same, such that any deviation from exactly the same would have negligible effect for ordinary use of the device.
As used herein, the term “nm” means nanometer(s).
As used herein, the term “x-ray tube” is not limited to tubular/cylindrical shaped devices. The term “tube” is used because this is the standard term used for x-ray emitting devices.
Useful characteristics of x-ray windows include low gas permeability, low outgassing, high strength, low visible and infrared light transmission, high x-ray flux, made of low atomic number materials, corrosion resistance, high reliability, and low-cost. Each x-ray window design is a balance between these characteristics.
An x-ray window can combine with a housing to enclose an internal vacuum. The internal vacuum can aid device performance. For example, an internal vacuum for an x-ray detector (a) minimizes gas attenuation of incoming x-rays and (b) allows easier cooling of the x-ray detector.
Permeation of a gas through the x-ray window can degrade the internal vacuum. Thus, low gas permeability is a desirable x-ray window characteristic.
Outgassing from x-ray window materials can degrade the internal vacuum of the device. Thus, selection of materials with low outgassing is useful.
The x-ray window can face vacuum on one side and atmospheric pressure on an opposite side. Therefore, the x-ray window may need strength to withstand this differential pressure. Visible and infrared light can cause undesirable noise in the x-ray detector. The ability to block transmission of visible and infrared light is another useful characteristic of x-ray windows.
A high x-ray flux through the x-ray window allows rapid functioning of the x-ray detector. Therefore, high x-ray transmissivity through the x-ray window is useful.
Detection and analysis of low-energy x-rays is needed in some applications. High transmission of low-energy x-rays is thus another useful characteristic of x-ray windows.
X-rays can be used to analyze a sample. X-ray noise from surrounding devices, including from the x-ray window, can interfere with a signal from the sample. X-ray noise from high atomic number materials are more problematic. It is helpful, therefore, for the x-ray window to be made of low atomic number materials.
X-ray windows are used in corrosive environments, and may be exposed to corrosive chemicals during manufacturing. Thus, corrosion resistance is another useful characteristic of an x-ray window.
X-ray window failure is intolerable in many applications. For example, x-ray windows are used in analysis equipment on Mars. High reliability is a useful x-ray window characteristic.
X-ray window customers demand low-cost x-ray windows with the above characteristics. Reducing x-ray window cost is another consideration.
The x-ray windows described herein, and x-ray windows manufactured by the methods described herein, can have these useful characteristics (low gas permeability, low outgassing, high strength, low visible and infrared light transmission, high x-ray flux, low atomic number materials, corrosion resistance, high reliability, and low-cost). Each example may satisfy one, some, or all of these useful characteristics.
As illustrated in
The x-ray window 18 can include the following layers in the following order: a top strong layer 17, a stress-relief layer 16, a bottom strong layer 15, an adhesive layer 14 then a support ring 13. The support ring 13 can include a hole that is aligned with the aperture 11a. The support ring 13 can be located closer to the flange 11f than any of the other layers. The top strong layer 17 can be located farthest from the flange 11f than any of the other layers.
The top strong layer 17 and the bottom strong layer 15 can have a material composition and thickness for optimizing x-ray window strength and ability to block visible light. The top strong layer 17 and the bottom strong layer 15 are strong relative to other layers, such as the stress-relief layer 16. Although the top strong layer 17 and the bottom strong layer 15 can have the same material composition, their strength can be improved by use of these two layers instead of as a single, thicker layer with this material composition.
The top strong layer 17 and the bottom strong layer 15 can each include boron. The top strong layer 17 and/or the bottom strong layer 15 can include ≥80 mass percent boron, ≥90 mass percent boron, or ≥95 mass percent boron. The top strong layer 17 and/or the bottom strong layer 15 can include≤99.5 mass percent boron, ≤98 mass percent boron, or ≤95 mass percent boron.
The top strong layer 17 and the bottom strong layer 15 can also include hydrogen, carbon, aluminum, nitrogen, or combinations thereof.
For example, the top strong layer 17 and/or the bottom strong layer 15 can include boron and hydrogen. The top strong layer 17 and the bottom strong layer 15 can each include ≥80, ≥90, ≥95, ≥97, ≥98, or ≥99 mass percent boron. The top strong layer 17 and the bottom strong layer 15 can each include ≥0.01, ≥0.05, ≥0.1, ≥0.5, ≥0.9, ≥2, or ≥4 mass percent hydrogen.
As another example, the top strong layer 17 and/or the bottom strong layer 15 can include boron and carbon. The top strong layer 17 and the bottom strong layer 15 can each include ≥60, ≥70, or ≥76; and ≤80, ≤85, or ≤90 mass percent boron. The top strong layer 17 and the bottom strong layer 15 can each include ≥15 or ≥20; and ≤24 or ≤30 mass percent carbon.
As another example, the top strong layer 17 and/or the bottom strong layer 15 can include boron and aluminum. The top strong layer 17 and the bottom strong layer 15 can each include ≥70, ≥75, or ≥81; and ≤85, ≤90, or ≤95 mass percent boron. The top strong layer 17 and the bottom strong layer 15 can each include ≥10 or ≥15; and ≤19 or ≤25 mass percent aluminum.
As another example, the top strong layer 17 and/or the bottom strong layer 15 can include boron and nitrogen. The top strong layer 17 and the bottom strong layer 15 can each include ≥35, ≥40, or ≥42; and ≤46, ≤50, or ≤55 mass percent boron. The top strong layer 17 and the bottom strong layer 15 can each include ≥45, ≥50, or ≥54; and ≤58, ≤60, or ≤65 mass percent nitrogen.
In the above examples of different material combinations for the top strong layer 17 and the bottom strong layer 15, the total mass percent is of course 100%, and includes the elements in the mass percent ranges noted, plus other chemical elements, if any.
Example thicknesses T17 of the top strong layer 17 at the aperture 11a include ≥400 nm, ≥800 nm, or ≥1200 nm; and ≤2400 nm, ≤4000 nm, or ≤8000 nm. Example thicknesses T15 of the bottom strong layer 15 at the aperture 11a can be ≥400 nm, ≥800 nm, or ≥1200 nm; and ≤2400 nm, ≤4000 nm, or ≤8000 nm. The thickness T17 of the top strong layer 17 at the aperture 11a can equal the thickness T15 of the bottom strong layer 15 in the aperture 11a.
Placing the stress-relief layer 16 between the top strong layer 17 and the bottom strong layer 15 can reduce stress and brittleness in the top strong layer 17 and in the bottom strong layer 15. This can increase the life of, and avoid early failure of, the x-ray window 18. The material composition and thickness of the stress-relief layer 16 are selected to improve its ability to thus reduces stress and brittleness in the top strong layer 17 and in the bottom strong layer 15.
The stress-relief layer 16 can have the same or similar material composition as the adhesive layer 14. The stress-relief layer 16, the adhesive layer 14, or both can include a polymer, such as polyimide. The stress-relief layer 16 and the adhesive layer 14 can include at least 95 mass percent of the same polymer. The stress-relief layer 16, the adhesive layer 14, or both can include ≥80 mass percent, ≥90 mass percent, or ≥95 mass percent polyimide.
The stress-relief layer 16 can have a relatively larger thickness for stress relief of the top strong layer 17 and the bottom strong layer 15. The adhesive layer 14 can have a relatively smaller thickness to improve the bond between the bottom strong layer 15 and the support ring 13. For example, a thickness T16 of the stress-relief layer 16 at the aperture 11a can be ≥1.5, ≥2, or ≥2.5 times a thickness T14 of the adhesive layer 14. As another example, the thickness T16 of the stress-relief layer 16 at the aperture 11a can be ≤4, ≤6, or ≤10 times a thickness T14 of the adhesive layer 14.
Example thicknesses T16 of the stress-relief layer 16 in the aperture 11a include ≥25 nm, ≥50 nm, or ≥100 nm; and ≤400 nm, ≤800 nm, or ≤1200 nm. Example thicknesses T14 of the adhesive layer 14 include ≥10 nm, ≥20 nm, or ≥40 nm; and ≤200 nm, ≤300 nm, or ≤600 nm.
The stress-relief layer 16 does not need to be as thick as the top strong layer 17 or the bottom strong layer 15. It is useful to keep the stress-relief layer 16 no thicker than required in order to minimize x-ray attenuation. Also, the stress-relief layer 16 usually includes higher atomic number elements than the strong layers 15 and 17. Higher atomic number elements can contaminate the x-ray spectrum, so it is particularly helpful to reduce thickness of any layer with higher atomic number elements.
For example, a thickness T17 of the top strong layer 17 in the aperture 11a can be ≥2, ≥4, or ≥5; and ≤6, ≤10, or ≤15 times larger than a thickness T16 of the stress-relief layer 16. As another example, a thickness T15 of the bottom strong layer 15 in the aperture 11a can be ≥2, ≥4, or ≥5; and ≤6, ≤10, or ≤15 times larger than a thickness T16 of the stress-relief layer 16.
As illustrated in
The adhesive layer 14 also spans the aperture 11a in mounted x-ray window 10. This may be preferred for increased stress reduction of the bottom strong layer 15. Mounted x-ray window 10 can be made by the first method below.
The adhesive layer 14 does not span the aperture 11a in mounted x-ray window 20. This may be preferred for reduced x-ray attenuation. Mounted x-ray window 20 can be made by the second method below.
The support ring 13 can reduce stress in the x-ray window 18 by including a material with an intermediate coefficient of thermal expansion between the coefficient of thermal expansion of the housing 11 and coefficients of thermal expansion of layers in the x-ray window 18. The support ring 13 can include nickel, cobalt, iron, carbon, manganese, silicon, or combinations thereof. For example, the support ring 13 can include ≥24 mass percent and ≤34 mass percent nickel; ≥7 mass percent and ≤27 mass percent cobalt; and ≥43 mass percent and ≤64 mass percent iron. A sum of the above mass percentages plus mass percentages of trace elements in the support ring 13 can equal 100 mass percent. Example trace elements include carbon, manganese, and silicon.
A bonding ring 12 can be sandwiched between the support ring 13 and the flange 11f. The bonding ring 12 can seal the support ring 13 to the flange 11f. The bonding ring 12 can be a brazed metal, liquid crystal polymer, or other adhesive.
A first method of making a mounted x-ray window can include some or all of the following steps:
Step 30 (
Step 40 (
The stress-relief layer 16 can be cured at 400° C. at this stage of the method.
Step 50 (
Step 60 (
Step 70 (
Step 80 (
The adhesive layer 14 can be cured at room temperature for 24 hours at this stage of the method.
Step 90 (
A final step (
A second method of making a mounted x-ray window can include some or all of the following steps:
Step 30 (
Step 40 (
The stress-relief layer 16 can be cured at 400° C. at this stage of the method.
Step 50 (
Step 60 (
Step 100 (
Step 110 (
Step 120 (
The adhesive layer 14 can be cured at room temperature for 24 hours at this stage of the method.
Step 130 (
A final step (
This application claims priority to US Provisional Patent Application Number U.S. 63/578,781, filed on Aug. 25, 2023, which is incorporated herein by reference.
Number | Date | Country | |
---|---|---|---|
63578781 | Aug 2023 | US |