SPECIMEN CONTROL MEANS FOR PARTICLE BEAM MICROSCOPY
20210285899 · 2021-09-16
Inventors
Cpc classification
H01J2237/162
ELECTRICITY
G01N2223/33
PHYSICS
International classification
Abstract
Specimen control means are disclosed for use with multipurpose particle beam instruments, such as with SEM, ESEM, TESEM, TEM, ETEM and ion microscopes. It provides a control stage located outside a chamber with a flexible wall that allows specimen movement inside the chamber. The same stage can open or close the bottom of the chamber base carrying a specimen stub, which is transferred to and from a conveyor belt or carousel supplied with a multitude of stubs filled with new specimens for examination. The chamber is further supplied with directed gas controls to regulate its gaseous environment. There is a supply of clean gas to maintain the instrument and specimen free of contamination, or to provide a reactant gas for microfabrication, or to enhance signal detection in a microscope. Stationary charged particle beam instruments are equipped with micro-mechanical specimen scanning for use in ultra-high resolution particle beam technologies.
Claims
1-10. (canceled)
11. An environmental charged particle beam microscope comprising an open-ended optics column for generating and focussing a charged particle beam, such as electrons or ions, comprising: (a) a charged particle beam; (b) a pressure limiting aperture separating the vacuum of the column from the gaseous environment allowed beyond the end of the column; (c) an envelope optionally surrounding and abutting the end of the said column to form a specimen chamber wall comprising flexible and/or shiftable walls; (d) a multi-directional motion stage placed at ambient (external) conditions; (e) a specimen stub coupled with the multi-directional motion stage; (f) the specimen stub configured to permit a specimen, when positioned in or on the specimen stub to be impinged by the particle beam; and (g) an environmental gas inlet configured to permit environmental gas to be admitted inside the envelope.
12. The microscope according to claim 11, wherein the envelope comprises flexible and/or shiftable walls, and wherein the specimen stub is removably coupled to the multi-directional motion stage via a sealingly locking port plate configured to be moveable and removable with respect to the specimen chamber wall.
13. The microscope according to claim 11, wherein the gas inlet comprises an annular opening around the pressure limiting aperture for the formation and delivery of a gaseous annular jet along and around the path of the particle beam all the way to the specimen.
14. The microscope according to claim 11, wherein: (a) the charged particle beam is stationary; (b) the pressure limiting aperture is marginally larger than the charged particle beam passing through; and (c) the multidirectional motion stage comprises a bidirectional micro-scanner for the control of the specimen.
15. The microscope according to claim 13, wherein the gaseous annular jet is delivered either at sufficient subsonic speed to remove overlaying loose particles from a specimen surface and to prevent contamination in the open-ended optics column, or at supersonic speed to provide pumping action on the gas from the open-ended optics column towards the specimen chamber.
16. The microscope according to claim 11, further comprising a light optical microscope using photons configured to permit the simultaneous or sequential examination and imaging of the specimen by the charged particle beam microscope together with the added light optical microscope.
17. The microscope according to claim 11, wherein the specimen chamber is evacuated by the naturally occurring gas flow (gas leak) through the pressure limiting aperture separating the open-ended optics column from the specimen chamber in order to obtain a desired pressure environment in the specimen chamber.
18. The microscope according to claim 17, wherein the leaking gas is replenished by a method selected from the group consisting of: (i) supplying the gas from ambient gas via a leak valve; (ii) supplying the gas from ambient gas through an annular opening around the pressure limiting aperture; and (iii) recirculating the gas from the open-ended optics column.
19. The microscope according to claim 14, further comprising: (a) a transmission electron microscope; (b) a specimen chamber with ambient atmosphere separated from the optics column by a set of two apertures with each having a micro-meter range opening in order to suppress the adverse effects of the supersonic air jets and depletion zones forming in the direction of the environmental gas flow through the apertures; and (c) a thin specimen section in the specimen chamber configured to be movable in order to sequentially (consecutively, or serially) survey and store information from any desired area of the specimen.
20. The microscope according to claim 14, further comprising: (a) a transmission electron microscope; (b) an insertable micro-chamber comprising a set of two apertures each having a micro-meter range opening in order to suppress the adverse effects of the supersonic air jets and depletion zones forming in the direction of the environmental gas flow through the apertures; and (c) a thin specimen section in the insertable micro-chamber configured to be movable and scanned in order to sequentially (consecutively, or serially) survey and store information from any desired area of the specimen.
21. The microscope according to claim 11, wherein the specimen is mechanically controlled with an atomic force microscope scanner.
22. The microscope according to claim 11, wherein the charged particle beam is a stationary charged particle beam, wherein the pressure limiting aperture has a diameter slightly greater than the diameter of the stationary charged particle beam, wherein the microscope further comprises: (a) a bidirectional micro-scanner configured to control the specimen stub and result in imaging of the specimen by use of the signals from beam-specimen interactions without vignetting; and (b) the bidirectional micro-scanner operating either inside a chamber with a controlled gaseous environment or operating in the absence of a chamber beyond the open-ended optics column at ambient pressure on account of the diameter of the pressure limiting aperture.
23. The microscope according to claim 22, wherein the bidirectional micro-scanner comprises piezo-electrical elements that provide deformation when an electrical signal is applied thereto.
Description
BRIEF DESCRIPTION OF DRAWINGS
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BEST MODES FOR CARRYING OUT THE INVENTION
[0029] To assist with the understanding of the invention, reference will now be made to the accompanying drawings, which embody some examples of the invention, without limiting the scope of the invention.
[0030] One embodiment of the present invention is shown in
[0031] In another embodiment of the invention, the gas 4 leaking through the pressure limiting aperture 3, is returned into the chamber via ducting 17. When a steady state of the recirculating gas is achieved, we obtain the condition that the amount of leaking gas Q(4) is equal to the amount of returning gas Q(4′), i.e. Q(4)=Q(4′), whereupon the leak valve 15 is closed, the pump 16 is turned off or isolated from the chamber and/or a flap or other valve 18 is shut sealed.
[0032] In yet a further embodiment, a clean or control gas is supplied to the chamber via an inlet 19 close to the PLA in order to provide a contamination free gaseous region immediately below the PLA by directing gas along the beam towards the specimen. In one option, the clean gas is delivered with a needle but in another preferred option the gas is delivered with an annular opening 20 surrounding the PLA 3. The gas jet formed in the vicinity of the PLA is generally at the lowest subsonic speed that is sufficient to create a clean zone without disturbing the specimen. However, when required, the subsonic speed is increased by increasing the gas supply pressure, so that the jet is used to remove loose particles from the surface of the specimen to expose the underlying material layer or to prevent dust particles entering the column via the PLA.
[0033] In yet another embodiment, the above said gas supply serves the purpose of providing a controlled reaction with the specimen surface as used in microfabrication.
[0034] In yet another embodiment, the nature of the said gas is chosen to enhance the gaseous detection device (GDD) usually employed in an ESEM.
[0035] In yet another embodiment, the said gas supply is delivered at supersonic speed inducing a pumping action of gas flowing from the electron optics column towards the chamber, as disclosed by prior art patent D1, also known as reverse flow PLA.
[0036] It is important that in all above embodiments provided with a clean or control gas supply, there must be also removal of the supplied gas via suitable means, like via the pump 16 if a hypobaric pressure level is required (i.e. below ambient pressure) or via a loose fit of plate 7 breaking the seal and letting the excess gas out of the chamber at ambient level but with a clean gas or a gas of choice for specific purposes. With a sealed chamber, it is again preferable to balance the supply of gas with the leaking gas through aperture 3, whilst pump 16 operates only during pressure level adjustment.
[0037] Depending on the industrial application, the leak valve 15 and clean gas supply at inlet 19 can be combined or substitute each other in one single inlet.
[0038] Optionally, the specimens are supplied to the said conveyor belt or carousel by a sample filling station 21 manually or automatically operated. The entire operation of described specimen exchange and chamber environment control can be computerized and automated to increase productivity and efficiency.
[0039] In a variant embodiment shown in
[0040] In a further embodiment shown in
[0041] In yet another embodiment shown in
[0042] In yet a further embodiment shown in
[0043] In all above embodiments, the movable port plate is locked sealably at the bottom of the chamber by suitable means. Sealing means may comprise O-rings, gaskets, appropriate suitable flange fittings, etc. Locking means may comprise magnetic force, spring force, flaps, clamps, pins, grooves, etc. It should be appreciated that the choice of any or all of these practical engineering details does not depart from the spirit of the invention.
[0044] It should also be appreciated that the type, size, geometry, and materials chosen in the design and construction of any flexible wall used is determined by the actual ambient conditions of pressure and atmosphere, in which any given instrument is designed to operate. Said conditions vary in terrestrial and planetary environments, such as on Mars, where the pressure is two orders of magnitude lower than on Earth, but with an abundance of dust particles. It should be appreciated that the previous embodiments are provided by way of example only and do not exhaust other combinations of material means that achieve the spirit of the invention, namely, any chamber wall that allows the transmission of specimen movement by means external to the chamber. Some of these combinations can be illustrated by the following numerical examples:
[0045] With a cylindrical shape bellows, the lateral forces due to pressure cancel out and can be supported by the mechanical strength of the bellows wall. That leaves only the force exerted on the circular base. For a base diameter of 2 cm, the atmospheric pressure (100 kPa) on Earth exerts a force of 3.2 kg, if the chamber pressure is vacuum. This maximum force can be sustained by a hexapod (six-arm) stage, so that each arm would bear only 0.53 kg at the most, because this is greatly reduced and minimized by the bellows spring force in the compressed position. The hexapod can be mounted in inverted orientation to be supported by the column of the instrument, for stability and compactness. Furthermore, life is supported at ambient pressure greater than about 20 kPa, which is ⅕ of a full atmosphere, so that the maximum force would become only 0.1 kg per arm of the hexapod. If we then reduce the chamber base diameter by ½, then the force is further reduced by ¼, which is very small with no practical problems during implementation. In this and other examples, the bellows can be replaced with a fabric material supported by or embedded with a mesh structure that allows both strength and flexibility with a variable deformation to allow all motions provided by a hexapod or by any other mechanical stage or combinations thereof. The bellows or other flexible wall principle can be highly suitable for Martian operations of a mini-ESEM instrument, since the pressure force ( 1/100 of that on Earth) becomes negligible allowing also the use of much larger size specimen chambers.
[0046] In a another drastic simplification of the chamber,
[0047] In all of the embodiments disclosed above and more to follow below, the said control stage is mechanically secured on a firm base connected solidly with the main instrument column, as for example is shown in
[0048] A special embodiment is further disclosed by
[0049] The previous embodiment is enhanced as shown in
[0050] Now, a breakthrough embodiment of the present invention is shown in
[0051] The previous embodiment is not limited to the examination of the surface of bulk specimens only, but it can be used also in TESEM mode and other transmission beam instruments for the examination of the internal material of thin specimens. This is shown by way of example in
[0052] It should be appreciated that all disclosed embodiments in this invention can be combined with any desired detection mode of the emanating signals from the beam-specimen interactions without departing from the spirit of the invention. Said detectors include, but not limited to, the detection of secondary electrons, backscattered electrons, x-rays and cathodoluminescence. Any or all of said detectors can be placed above or below the specimen, while said specimen can be presented in bulk or thin section form. The orientation of the particle beam column can be in any direction without departing from the spirit of the invention. In addition, the specimen can be observed and examined simultaneously or alternatingly with a light microscope, which also falls within the scope of the invention. By way of example of these variations and incorporations,
[0053] A further embodiment of the invention in conjunction with a stationary electron beam is provided by the drawing in
[0054] With reference to
[0055] The specimen chamber may optionally be pumped to a lower pressure to allow for applications that are not adversely affected by a hypobaric pressure, or vacuum, if needed.
[0056] The ambient gas may be replaced by another gas, inert or reactive, to further assist and expand the scope of applications.
[0057] The specimen holder may optionally incorporate additional detectors, such as an x-ray detector, or an electron detector, etc. Similar detectors may also be provided in any convenient location inside the provided specimen chamber.
[0058] A final embodiment of the invention is shown in
[0059] The general object of the embodiments in
[0060] In outlining the above description of the invention, it is assumed that the electron optics requirements are fully accounted for and are taken into consideration for the actual values of all design parameters involved. For example, the size of PLA at the exit of the transmitted beam on the side of the objective lens (to be called PLA2), should be adjusted to be consistent with a good or optimum objective diaphragm angle value in the range of 10-25 mrad. If the specimen section is located 100 micro-meters above this PLA2, then the diameter of this aperture should be in the range of 2-5 micro-meters. By lowering the distance of the specimen to PLA2, we can accordingly make the size of this aperture even smaller. The first aperture (to be called PLA1) nearest to the condenser lens can be chosen around 1 micro-meter and will define the field of view at the lowest possible magnification. Now, the distance of PLA1 from the specimen can be minimized down to several aperture diameters, where the stagnation condition of the atmospheric gas is maintained (no streaming and depletion of gas). The attainment of such very small working distance is physically allowed only by the present invention and is limited only by the engineering precision available. As a result, the total gaseous layer thickness is determined by the distance between PLA1 and PLA2 only, whilst there is practically no other gas thickness in the remaining electron optics column. By such minimal gas thickness in the specimen chamber, the electron beam loss and accompanying signal noise are minimal or negligible, which allows the contrast produced to arise predominantly from the properties of the specimen section under examination at the lowest beam accelerating voltage. Therefore, the ultimate smallest size choice for either or both PLAs depends on the engineering precision used for the location and movement of the specimen in the confined space between PLA1-PLA2. Clearly, as these apertures become ever smaller, they may take over (even replace) the function of the adjacent condenser and objective diaphragms already in operation under vacuum for a conventional TEM. These are also interdependent on the accelerating voltage used (high or ultra-high). The engineering choices are left to the manufacturer to determine for all practical purposes, including aperture materials, specimen scanning controls, etc., and manufacturing costs. These engineering choices are finally dependent on the type of gaseous atmosphere (nature and pressure of gas) that should ultimately be allowed to use with any given application, whilst none of said choices are departing from the spirit of the present invention.
INDUSTRIAL APPLICABILITY
[0061] By virtue of the simplicity, ease of operation, increased specimen examination rate and minimum bulkiness of the multipurpose specimen chamber, this invention has limitless industrial applications in conjunction with SEM, ESEM, TESEM, ETEM and ion microscopy.
[0062] The device of the present invention can also be used in conjunction with other instruments requiring vacuum, or controlled gaseous environment around specimens.
[0063] One particular industrial application is in the field of geological exploration and mining industry, especially because the entire device can be made compact, light and transportable to the field, and for in situ specimen examination.
[0064] Yet another application is with instruments of planetary exploration, such as on planet Mars having a thin atmosphere with a pressure two orders of magnitude less than Earth. Martian atmospheric conditions allow and require for transportation a miniaturized multipurpose device for the study of the surface and atmosphere of the planet. Considering the dusty conditions on Mars, the provision of a clean gas supply around the PLA and specimen would ensure a fault-free operation.
[0065] Existing scanned beam instruments can be greatly enhanced, simplified and applied to novel areas of industrial applications by use of a stationary probe in conjunction with mechanical scanning provided by the specimen control means of the present invention. This embodiment provides great advantages not only in general microscopy but also in microfabrication technologies using focussed particle beams to manufacture electronic or other devices with the finest structures in an open or controlled gaseous environments. Inspection by imaging and microfabrication can be integrated by a single machine with maximum controls and output efficiencies.
[0066] Another application is in biological research and development, since specimens can now be observed and studied at ambient or other environmental conditions with high resolution. When combined with light microscopy, it can advance the technology of molecular biology to novel ways of exploration.
[0067] The above embodiments disclosed having a mechanically scanned specimen in conjunction with a stationary particle beam constitute effectively a new technology that bridges the established prior art technologies of electron microscopy with atomic force or tunnelling microscopies. This opens a completely new frontier of industrial applications.
PATENT LITERATURE
[0068] D1: U.S. Pat. No. 6,396,064 B1 patent (Danilatos)
[0069] D2: PCT/AU2016/050757 (Danilatos)
OTHER LITERATURE
[0070] D3: Danilatos G, Kollia M, Dracopoulos V (2015) Transmission environmental scanning electron microscope with scintillation gaseous detection device. Ultramicroscopy 150, 44-53. doi:10.1016/j.ultramic.2014.11.010