WO1996027194A1

WO1996027194A1 - High intensity, small diameter x-ray beam, capillary optic system

Info

Publication number: WO1996027194A1
Application number: PCT/US1996/002583
Authority: WO
Inventors: David M. Gibson
Original assignee: X-Ray Optical Systems, Inc.
Priority date: 1995-02-28
Filing date: 1996-02-27
Publication date: 1996-09-06
Also published as: US5570408A; CN1176707A; JPH10508947A; EP0812460A4; EP0812460A1; JP3057378B2

Abstract

A system comprising a novel combination of a multiple-channel monolithic capillary optic (44) and an x-ray source (30) with a spot size (42) of less than 300 microns to produce a high intensity small diameter x-ray beam is described. A system of this invention can be easily adapted for use in the analysis of small samples where an intense quasi-parallel, or converging x-ray beam is required.

Description

HIGH INTENSITY, SMALL DIAMETER X-RAY BEAM, CAPILLARY OPTIC SYSTEM

Statement As To Rights under Federally Sponsored Research

This invention was made with government support under Contract No. 70NANB2H1250 awarded by the Department of Commerce. Accordingly, the U.S. Government has certain rights in the invention.

Field of the Invention

This invention relates broadly to the field of x-rays. More particularly this invention relates to the field of x-ray optics. This invention provides a device and a method for improvement in the capability of capillary x-ray optic/x-ray source systems to produce high intensity, small diameter x-ray beams.

Background of the Art

When samples are analyzed by various x-ray techniques, such as x-ray diffraction, it is desirable that the dimensions of the x-ray beam hitting the sample be on the order of the sample size, or of the order of the spot on the sample to be examined. This criteria on beam size is important because it maximizes spacial resolution, while minimizing background noise produced by unwanted photons. In many cases, for example in the case of x-ray diffraction of protein crystals, sample sizes are very small, and conventional x-ray diffraction equipment does not function efficiently. When traditional laboratory x-ray sources are used to analyze such small samples, beams of appropriate size are typically obtained by collimation methods. This includes such things as passing the x-ray beam through pin holes cut into x-ray absorbing materials such as lead. Because low beam divergence is also desirable, these pin holes must be placed a significant distance away from the source. This means that the solid angle of collection from the source is quite small. This in turn results in a very low intensity beam reaching the sample, one significant disadvantage of a low intensity beam is that measurement times can be extremely long. For some samples this is merely an inconvenience. However, for samples like protein crystals which have relatively short life times, this extended period of analysis can render the analysis technique useless. In all cases, extended measurement times lead to a decrease in the signal-to-noise ratio. Also, it is important for commercial analysis operations to maximize the sample through-put by minimizing analysis time. Shorter analysis times can thus lead to substantial financial rewards.

It is known in the art that to obtain more x- rays from a source, a larger spot size on the anode is required. Thus, conventional wisdom dictates that in order to increase power transmitted to a sample, either with or without an optic, a more powerful source with a larger spot size should be used. A general rule that is followed is that the source spot size should be the size of the sample being analyzed.

It is known to the art that single hollow glass capillaries can form x-ray beams of very small dimensions see for example P.B. Hirsch and J.N. Keller, Proc. Phys. Soc. 64 369 (1951) . Tapering these single capillaries to further limit output spot size is also known to the art, see E. A. Stern et. al. Appl. Opt. 27 5135 (1988). However, both these devices only capture x rays from a very small portion of the source. Thus, their use also leads to x-ray beams of less intensity than is desired. Yet another disadvantage of the tapered devices is that the minimum x-ray spot size is located right at the tip of the device. This places strict limitations on the positioning of a sample. In addition, these single tapered capillaries can only form a small spot with considerable divergence. Often times for diffraction experiments, a parallel beam is desirable.

Also known to the art are multi-fiber polycapillary x-ray optics. These devices form a particular class of a more general type of x-ray and neutron optics known as Kumakhov optics. See for example commonly assigned U.S. patent number 5,192,869 to Kumakhov. Disclosed in this patent are optics with multiple fibers which are bent to produce high flux quasi-parallel beams. Although these optics can capture a large solid angle of x rays from diverging sources, their potential for capturing from a small spot source or for forming small dimension output beams is limited by the relatively large outer diameter of the individual polycapillary fibers. The outer diameter of the fibers is on the order of 0.5 millimeters. Because of the fiber outer diameter these multi-fiber optics have a minimum input focal length of roughly 150 millimeters. The critical angle for total external reflection at 8 KeV for glass is 4 milliradians. Effective transmission after many reflections is obtained only if the photons are at approximately one-half the critical angle. So using 0.5 mm diameter fiber geometry shows that with a source as small as 100 μm, for the outer channels to transmit effectively the source-optic distance should be at least 150 millimeters. Because of this relatively long input focal distance, to capture a large angular range of x-rays from the source the input diameter needs to be relatively large, which in turn constrains the minimum diameter and maximum intensity (photons/unit area) of the output beam. The minimum beam diameter for a multi- fiber polycapillary optic with 0.15 radian capture angle which forms a quasi-parallel beam is on the order of 30 millimeters. These optics are thus not appropriate to produce the intense small diameter x- ray beams needed for small sample diffraction experiments such as protein crystallography. For focusing optics, because of the fiber diameter, the minimum focused spot size has a diameter on the order of 0.5 millimeters.

Object of the invention

Thus it is an object of the subject invention to provide a solution to the long felt need in the art for a laboratory based, small dimension, high intensity x-ray beam. It is another object of this invention to allow the analysis sample to be placed at a position removed from the output end of the device. It is yet another object of this invention to provide a small, intense x-ray beam which is highly collimated with a minimum of divergence. Yet another object of this invention is to produce small, high intensity, focused x-ray spots. Another object of this invention is to provide these benefits in a relatively compact, and cost effective system.

Brief Summary of the invention

The subject invention accomplishes these objects with a carefully engineered x-ray source/capillary optic system comprising:

1) A monolithic multiple-channel capillary optic with scaled down input and output diameters minimized with respect to photon energy, source diameter, and channel diameter; and,

2) an x-ray source with a spot size designed to maximize optic output intensity for a desired output beam diameter.

The specially designed optic is positioned within 60 mm or less relative to the x-ray source.

Monolithic optics are an essentially integral one-piece structure in which fiber channels are closely packed and self-aligning along their entire length. At the input end of the optic the channels are oriented to aim substantially at the x-ray source. The output end of the optic can be shaped to form either a converging, or a quasi-parallel beam, depending on the intended use of the invention.

The smaller source, although less powerful, provides an increase in the areal density of x-rays. The monolithic optic enables the efficient capture of the small spot x rays, because each individual channel can be aligned more efficiently with the source spot. Surprisingly, it has been discovered that a small spot, lower power source, when combined with a monolithic capillary optic's superior x-ray collection abilities, can lead to a higher intensity of x rays at the output of the optic compared with the use of a large spot, higher power source, with or without an optic.

The basic idea behind the invention then is to continue to capture the x-rays from the source, and to squeeze these photons into a proportionally smaller output space in order to produce the desired high intensity, small diameter beam. This requires significant reenigineering of existing optic designs, and modification of the x-ray source used. The first modification is that the input diameter of the optic must be decreased from what is currently known. A critical point to the invention is that in order to keep the same amount of photons entering the input end of the optic, the optic must be moved closer to the x-ray source to maintain the same capture solid angle. Characteristic input focal lengths of the subject invention are less than half of the roughly 150 millimeters required for the best multi-fiber polycapillary optics. Moving closer and using smaller input diameters all aimed at a common point, means the optic will "see" a smaller portion of the source. Thus, another key element of the subject invention is to decrease the source spot size in order to increase the power density and therefore the x-ray production from the area of the source from the which the optic captures photons. This is done in spite of the fact that the total number of x rays emerging from the source is decreased. This invention provides for more efficient use of existing x-ray power. Brief Description of Drawings

These and other objects, advantages and features of the present invention will be more readily understood from the following detailed description of certain preferred embodiments of the invention, when considered in conjunction with the accompanying drawings in which:

Fig. 1 is a schematic diagram of an x-ray source;

Fig. 2 is a graph of power density and total power as a function of spot size diameter;

Fig. 3 depicts a multi-fiber polycapillary optic;

Fig. 4 depicts a monolithic capillary optic and source in accordance with the present invention; and

Fig. 5 depicts another embodiment of a monolithic capillary optic in accordance with the present invention.

Best Mode For Carrying Out The Invention

Referring now to Fig. 1, the basic elements of a typical x-ray source are shown. Filament 10, is heated, by applying a voltage, to a temperature such that electrons 12, are thermally emitted. These emitted electrons are accelerated by an electric potential difference to anode 14, which is covered with target material 16, where they strike within a given surface area of the anode which is called the spot size 18. X rays 20, are emitted from the anode as a result of the collision between the accelerated electrons and the atoms of the target. In order to control the spot size, electromagnetic focusing means 22 is positioned between electron emitting filament 10 and anode 14, so that the electron beam passes within its area of influence. X ray sources with spot sizes of 2 microns or less are available commercially. However, as the electron spot size decreases, so does the production of x rays.

Fig. 2 shows how x-ray power (production of x rays) , and the power density (power/spot area) of a source varies with spot diameter. Noting that the linear vertical scale on the right of the graph is used for the total power, it can be seen from the lower tail 24 of total power curve 26 that power decreases nearly linearly with spot diameter for very small spot sizes. Turning our attention now to the power density curve 28, and noting that the vertical scale on the left of the graph which applies to this curve is logarithmic, it can be seen that there is an inverse relationship between the power density and the spot diameter. The reason for this is that the total power varies linearly with spot diameter, while the area varies as the inverse of the square of the spot diameter. Thus, it can be seen that even though total x ray production is decreased, the power density increases with decreasing spot size.

Monolithic capillary optics allow unprecedented possibilities for efficient use of the increased power density of small spot x-ray sources. The combination of the smaller spot source, and properly engineered monolithic capillary optic of the subject invention can thus lead to a substantial increase in intensity of small diameter output x-ray beams.

Specific design parameters vary depending on the energy of x rays used. Two types of systems are particularly pointed out. First, a system in which a very intense small diameter quasi-parallel beam is formed and second a system in which a very small, intense converging x-ray spot is formed. In all cases, systems of the type defined by the subject invention can be easily differentiated from other prior art systems based on a much reduced source to optic distance. Fig. 3 shows an x-ray source 30, and a multi-fiber polycapillary optic 32. In order for the polycapillary fiber 33 to efficiently capture radiation from source 30, the collection angle 34 of the capillary must be less than the critical angle for total external reflection. This angle is dependent on the x-ray energy. For a typical example of an approximately 8 keV optic with polycapillary outer diameters of around 0.5 millimeters, simple geometric considerations lead to the conclusion that the optic must be placed at least 150 millimeters away from the source. The subject invention is defined by optics which are placed no more than half that distance from the source.

The first embodiment of the subject invention is shown in Fig. 4. The system 40, for producing a high intensity, small diameter x-ray beam comprises two main components; namely, a small spot x-ray source 42, and a monolithic capillary optic 44. The two components are separated by a distance f, known as the focal distance, measured along optical axis 46. The optic 44 comprises a plurality hollow glass capillaries 48 which are fused together and plastically shaped into configurations which allow efficient capture of divergent x radiation 43 emerging from x-ray source 42. In this example, the captured x ray beam is shaped by the optic into a quasi-parallel beam 50. The output beam is not completely parallel because of divergence due to the finite critical angle of total external reflection. The channel openings 52 located at the optic input end 54 are roughly pointing at the x-ray source. The ability of each individual channel to essentially point at the source is of critical importance to the subject invention for several reasons: 1) it allows the input diameter of the optic to be sufficiently decreased, which in turn leads to the possibility of smaller optic output diameters; 2) it enables efficient capture of x-rays even when the source spot is decreased; and 3) it makes efficient x-ray capture possible for short optic to source focal lengths.

The diameters of the individual channel openings 52 at the input end of the optic 54, are smaller than the channel diameters at the output end of the optic 56. The class of optics used in the subject invention are monolithic. This means that the walls of the channels themselves 70 form the support structure which holds the optic together. For this case, the maximum capture angle is given by 2ψ, where is the maximum bend angle of a curved capillary.

In a preferred embodiment, the x-ray source 42 has a spot size of roughly 30 microns and is located approximately 1.0 millimeter from the input end 54 of capillary optic 44. The collection angle ψ for this optic is around 0.2 radians. The optic produces an output beam 50 with a diameter of essentially 1.0 millimeter. The overall length of the optic is approximately 8.0 millimeters. The increase in intensity is expected to be more than roughly 2 orders of magnitude brighter than currently available laboratory sources.

Fig. 5 shows a second embodiment of the subject invention. Again the source/optic system 80 comprises a small spot x-ray source 82 and a monolithic capillary optic 84. The optic has channels formed by individual glass capillaries 89 which have been fused together. The channel openings 86 at the input end 88 are positioned to capture radiation from divergent source 82. In this particular embodiment, however, the optic output end 90 is shaped to form a very small spot converging beam. For this case, because the radiation is turned through twice the angle of the quasi-parallel output optic, so the maximum capture angle is just φ, the maximum bend angle. A preferred embodiment of this system, designed for approximately 8 keV x rays, can be specified as follows. Again referring to Fig. 5, the x-ray source 82 has an anode spot size of around 100 micrometers. The converging optic 84 is placed essentially 27 millimeters in front of the source.

The acceptance angle of the optic 85 is roughly 0.13 radians, and the optic has an output focal length 87 of nearly 2 millimeters. The overall length of the optic is about 165 millimeters. The optic input diameter 88 is approximately 7 millimeters, with input channel diameters of essentially 14 micrometers. The output diameter 90 is roughly 0.6 millimeters. The maximum channel diameter is around 10 micrometers. This invention has been specified in part by specific embodiments. It is to be understood that it will be apparent to those skilled in the art that various modifications, substitutions, additions and the like can be made without departing from the spirit of the invention, the scope of which is defined by the claims which follow and their equivalents.

Claims

1. Apparatus for producing an x-ray beam, said apparatus comprising:

an x-ray source; and

a multiple-total-external reflection monolithic capillary optic ("optic") having an input and an output and being positioned such that said input to said optic faces said x-ray source and is disposed at an optic-to-source distance of less than 60 millimeters, said optic having multiple channels each of which has an input aimed at said x-ray source, said output of said optic providing said x-ray beam.

2. The apparatus of claim 1, wherein said x-ray beam comprises a quasi-parallel x-ray beam.

3. The apparatus of claim 2, wherein said x-ray source comprises a spot source and has a spot size width of approximately 30 micrometers, and wherein the optic-to-source distance is approximately 1 millimeter such that said optic produces at its output a quasi-parallel x-ray beam with a width of 1 millimeter.

4. The apparatus of claim 1, wherein said x-ray beam comprises a focused x-ray beam, each channel of said multiple channels of said optic having an output aimed at an output focal point spaced from the output of said optic. 5. The apparatus of claim 4, wherein said x-ray source has a spot size width of 100 micrometers, the optic-to-source distance is approximately 27 millimeters, and said optic has an output focal length of approximately 2 millimeters.

6. The apparatus of claim 5, wherein said optic input has a diameter of 7 millimeters and the input of each channel of said multiple channels in said optic is 14 micrometers.

7. The apparatus of claim 1, wherein said x-ray beam comprises a divergent x-ray beam, and wherein said multiple channels of said optic have outputs divergently aimed, thereby providing said divergent x-ray beam.

AMENDED CLAIMS

[recei ved by the International Bureau on 22 July 1996 (22.07.96 ) ; new claims 8 and 9 added ; remaining claims unchanged ( 1 page ) ]

5 . The apparatus of claim 4 , wherein said x-ray source has a spot size width of 100 micrometers , the optic-to-source distance is approximately 27 millimeters , and said optic has an output focal length of approximately 2 millimeters .

6 . The apparatus of claim 5 , wherein said optic input has a diameter of 7 millimeters and the input of each channel of said multiple channels in said optic is 14 micrometers .

7 . The apparatus of claim 1 , wherein said x-ray beam comprises a divergent x-ray beam, and wherein said multiple channels of said optic have outputs divergently aimed , thereby providing said divergent x-ray beam .

8. The apparatus of claim 1, wherein said x-ray source comprises a spot source having a spot size width of less than 300 micrometers.

9. The apparatus of claim 2, wherein said quasi-parallel x-ray beam has a width 'w', and wherein said x-ray source comprises a spot source having a spot size width 'w' sufficiently small to maximize intensity of said quasi-parallel x-ray beam with width 'w' with said optic disposed at said optic-to-source distance of less than 60 millimeters. STATEMENT UNDER ARTICLE19

In substitute claim page 14, claims 5-7 remain unchanged and new claims 8 i 9 are added. The subject matter of the claims pending herein now corresponds to that which has recently been allowed by the U.S. Patent Office. Further, c . reference cited in the International Search Report is of record with the U.S. Patent Office m the corresponding application. Based upon this, issuance of a favorable Preliminary Examination Report, subsequent to filing of the Demand for Preliminary Examination, is requested.