This disclosure generally relates to Neutral Atom Microscopy (NAM) and, more particularly, to apparatus and methods that provide relatively high resolution imaging using non-charged atom or molecule (herein “neutral particle”) beams. This field has also been termed Atomic deBroglie Microscopy and also Scanning Helium Microscopy (SHeM).
Microscopes provide imaging in two general modes, transmission mode and reflection mode. Transmission mode relates to illumination through a sample, where reflection mode relates to illumination that returns from the surface of the sample. Various historic microscope apparatus and method enabling both modes of microscopy rely on different types of physical interactions to provide magnified imaging of a sample.
For example, conventional optical microscopes rely upon light reflecting from, or transmitting through a sample. The light is then passed through focusing lenses or mirrors to achieve high magnification. The resolution limit of conventional optical microscopes is related to the light wavelength of hundreds of nanometers. Electron and ion microscopes rely on charged particles, focused using lenses that employ electric or magnetic fields, and offer significantly higher resolution potential due to the shorter deBroglie wavelength of the relatively high-Momentum particles used, in most cases under 0.1 nm. The deBroglie wavelength of a particle can be thought of as a scale of distance over which a particle interacts, similarly to the wavelength of light. This wavelength is, λ=h/m0V, where h is Planck's constant, m0 is the particle mass and V the particle velocity.
The Scanning Electron Microscope and Helium Ion Microscope rely upon a charged particle beam generally of 1,000 to 50,000 eV energy directed at the sample, as compared to 2 to 3 eV for visible light. Albeit the imaging resolution is extremely good, but the high kinetic energy and the charge of the particles directed at the sample can be destructive to and/or reactive with the sample. In addition, the resulting electrical charging of insulating samples can interfere with successful imaging. At such energies, the beam particles also penetrate many atomic layers through the sample and therefore do not exclusively image the surface atomic layer of the sample, but may instead produce images from some greater depth range through the sample, as is the case for conventional optical microscopes for wavelength reasons.
For over two decades scientists have pursued imaging surfaces using a focused beam of neutrally charged atoms or molecules. Imaging without high energy beams while achieving high resolution is theoretically possible this way, because the high mass of atoms compared to electrons produces a short deBroglie wavelength, under 0.1 nm even at less than 0.1 eV energy. Molecular beam experiments show that certain neutral atoms and molecules at this energy scatter from the top atomic layer of samples, and imaging with this method could result in new information about materials and objects that cannot be readily obtained using previous forms of microscopy.
However, previous attempts at a neutral particle microscope have produced poor image signal to noise ratio and/or poor resolution due to a combination of problems. One problem is the difficulty of finding a suitable focusing element able to produce a high intensity, sharply focused beam spot of neutral particles. Neutral atoms and molecules are not strongly affected by electric or magnetic fields, and for the most part, scatter randomly off of mirror surfaces, making it difficult to focus, control, and direct the beam for imaging purposes. A second problem is the poor sensitivity of available neutral atom or neutral molecule detectors, which can only detect a very small fraction of the particles entering them. Probably the first images published from a neutral atom microscope were published in 2008, and were obtained in transmission mode.1 They were of poor signal to noise ratio and had somewhat better than 2 μm resolution. Prior to the disclosed invention, no published images improved significantly on these and none were obtained in reflection mode. 1 Imaging with neutral atoms—a new matter-wave microscope, M. Koch, S. Rehbein, G. Schmahl, T. Reisinger, G. Bracco, W. E. Ernst, and B. Hoist., Journal of Microscopy 229: 1 (2008).
Accordingly a need exists for a microscope apparatus and method which provides reflective mode and transmission mode non-destructive imaging using neutral particles.
This disclosure generally relates to neutral particle microscope methods and systems, including such systems and methods that utilize a “pinhole”aperture to form a neutral particle beam without a focusing element, and detector nozzle technology that increases neutral particle detector performance. The terms neutral atom and neutral molecule are used synonymously herein as neutral particles, as the inventive apparatus may use either or combinations of the same, specifically excepting neutrons. The term “neutral particle” will be used herein to reference both neutral atoms and neutral molecules with the stated exclusion of neutrons.
In accordance with one embodiment of the invention, a stream of neutrally charged particles such as Helium atoms, are first emitted by a source nozzle and then formed into a beam by a very small aperture proximally located to the sample. “Proximal” means the aperture is not more than 100 μm away from the sample in order to maintain the relative small spot size of the beam required for high resolution imaging. The aperture's mechanism for beam formation is the blocking of all particles of the neutral particle stream, except those traveling in the desired direction that pass through the aperture as a narrowed beam of neutral particles.
The neutral particle beam reaches the sample and some of the reflected or transmitted particles are detected by a gas particle detector. A scanner controllably changes the relative position of the sample and aperture allowing for a mapping of particle detections over the sample surface, thereby providing information that is converted into sample images by a processor. The sample is easier to maneuver for scanning purposes, but changing position of the aperture or the source nozzle can be performed to accomplish the same objective of altering the relative position of the sample to the beam.
Detection by the gas particle detector is enhanced through the use of a detector nozzle having an input end located close to the sample, positioned to receive a favorable cross-section of neutral particles coming from the sample after impact or transmission. In accordance with one embodiment, the detector nozzle has an inlet that is placeable close to the sample, requiring the inlet end to be relatively small and shaped to accommodate the aperture holder. The detector nozzle outlet may be much larger, matching the volume enclosing the detector for connection. Detected pressure is enhanced by the relatively small inlet area being located close to the sample where the reflected or transmitted pressure (neutral particle density) is higher. The enclosing volume of the detector nozzle and surrounding the detector prevents escape of the neutral particles that enter the detector nozzle, except for that portion of neutral particles that escape backwards out the inlet.
Further aspects of the invention will be described herein in the following portions of the specification wherein the detailed description is for fully disclosing preferred embodiments without placing limitations thereon.
The following description is provided to enable any person having ordinary skill in the art to make the disclosed neutral particle microscope, and is provided in the context of microscopy. Various modifications to the embodiments will be readily apparent to those skilled in the art, and the principles and configurations defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the invention. Thus, applicant's invention is not intended to be limited to the preferred and other embodiments described herein, but is to be accorded the widest scope consistent with the principles, features and teachings disclosed herein.
As shown in
As the beam 80 passes into the sample chamber 300, it will diverge in spot size the further it travels from the aperture 30. As a small spot size is desired, the sample 40 is positioned in close proximity to the aperture 30 such that the neutral particle beam 80 reaches the sample while the beam's spot size is still relatively small. The adequately small spot size impacting the sample is achieved through a combination of an aperture of less than 1 μm in diameter and a working distance between the sample surface and the aperture of less than 100 μm as depicted in
In the preferred embodiment in reflection mode as shown configured in
In other embodiments in transmission mode as shown configured in
The sample 40 and aperture 30 are mechanically scanned relative to each other, meaning either the sample 40 or the aperture 30 may be moved, or both as shown in
As illustrated in
On the source side, vacuum 200 is needed to ensure free molecular flow conditions between the source 110 and aperture 30. On the sample side 300 of the aperture, the gas pressure must be low enough to ensure free molecular flow between the aperture 30 and sample 40, and between the sample 40 and the detector inlet 15.
In addition, the background partial pressure of the chosen beam gas in the sample chamber 300 must be sufficiently low that the background level of this gas in the detector(s) 60 does not interfere with image quality. If it were too high, it would produce an excessive noise level in the images. For this reason the source system must be separated from the sample chamber 300. These evacuated chambers communicate through the beam-forming aperture hole 30.
As illustrated in
Valve 603 is opened when venting to atmosphere or rough pumping the system from atmospheric pressure to prevent a large pressure difference from occurring across the aperture 30. Not shown are various valves and components that are not necessary to the function of the microscope but which are common place in vacuum apparatus, such as a vent valve and foreline isolation valves to allow shutoff without venting.
As used in the preferred embodiment and depicted in
The source 110 may incorporate provisions to aid in alignment of the source 110 and aperture 30 relative positions, such as fingers or other areas that contact the interior of the aperture holder 20.
D2 is the “quitting surface” diameter if a free jet nozzle 111 is used as the source. “Quitting surface” refers to the area surrounding a free jet nozzle 111 within which gas to gas scattering is still common due to the gas density, before the gas has expanded into free molecular flow at a lower density. This approximate sphere is the area from which all downstream source gas particles appear to originate. D2 may also be the inside diameter of the final aperture of the source system if it is not a simple free jet nozzle 111.
From this calculation it can be seen that a short Working Distance (WD) produces a smaller beam spot size.
A certain minimum beam intensity (flow rate) is needed to take images of good signal to noise ratio in a reasonable period of time. Beam flow rate (nbeam, in particles/sec) can be estimated with the following formula.
I0 is the source intensity (in particles/s×sr). From this it can be seen that increasing the aperture 30 diameter or moving the source closer will increase beam intensity. This is a compromise with resolution, since to improve resolution, the aperture diameter (D3) must be reduced, and/or the source distance Lsep must be increased.
Shortening WD also allows the source 110 to aperture 30 distance Lsep and the aperture diameter D3 to be reduced, with an increase in resolution resulting. For best performance, WD is reduced as far as practical without risk of contacting the sample 40. In the preferred embodiment, the aperture diameter D3 is under 1 μm and WD is under 100 μm. To achieve this short working distance, the Z position of the sample 40 (position along the beam axis) can be manually adjusted for close proximity to the aperture 30. The position of the sample 40 can be monitored optically by microscope or camera observing the gap between the aperture 30 and sample 40. To achieve a closer WD, Z approach may be monitored by another means, such as capacitance, or electrical conduction, or conduction of vibration between the aperture holder 20 and sample 40, and Z approach may thus be controlled electronically.
As illustrated in
This shape also must not have too narrow a point angle or it would concentrate reflected source gas on the interior side to an excessive degree, which could scatter the beam. In the preferred embodiment, the angle measured at the aperture point across the exterior face is nominally 120 degrees, and could range from 90 degrees to just under 180 degrees. There is no requirement that this shape is a body of rotation or that it have symmetry, hence many shapes would function.
In the preferred embodiment, the material at the end of the aperture holder 20 has a thickness of less than the aperture-hole diameter, as illustrated in
In one embodiment, the aperture holder 20 is made of three pieces. The main body is machined from metal with a large hole on the end of its cone shape. A separate cone stamped from metal sheet, about 1 cm diameter, has a small hole drilled in its tip, for instance with a number 80 drill bit. On this cone is glued (using epoxy) a flake of graphite paper pealed (“exfoliated”) from Highly Oriented Pyrolytic Graphite, forming a thin membrane. Ideally the graphite flake is stamped into a cone shape before gluing but may be glued on flat, as in
The result of a FIB drilling the aperture is shown in
In other embodiments, materials other than graphite may form the thin membrane at the end of the aperture holder 20, such as a polymer film formed by dipping a mechanically drilled hole in a polymer solution and allowing it to dry. This would then be FIB drilled to produce the aperture 30. Part or all of the aperture holder 20 and aperture may 30 be formed by micromachining techniques in silicon or other materials.
In one embodiment, the aperture holder is replaceable by removing it from the source chamber side after disassembling the source vacuum chamber 200. This is accomplished by mounting the aperture holder 20 in a machined, cylindrical port at the junction of the source 200 and sample 300 chambers depicted in
The aperture holder 20 may incorporate provisions to aid in alignment of the source 110 to the aperture 30, such as by providing an area in its interior for the source 110 to contact for alignment. This could include going so far as to integrate the source 110 and aperture holder 20 together, such as by providing a ferrule and threaded clamp for holding a source nozzle tube 110 in place.
No focus or astigmatism adjustments are required, which is a speed advantage over potential focused NAM designs since making adjustments would require a number of additional scans.
As depicted in
A more effective but more expensive embodiment would have more than one detector 60, collecting from different angles relative to the sample 40. Two can be used for differential mode to improve signal to noise ratio. Two or more could be used to produce a pseudo-color image, or simply to provide post-scan choice of sample “illumination” direction.
He and D2 are good source gas choices due to the low typical background partial pressure at mass 4, but any gas could be used simply by changing the gas supplied to the source, and selecting the corresponding mass for filtering by the detector (RGA or other mass spectrometer). Scanning a sample 40 with two or more different gasses may provide contrast information that is useful in identifying the nature of the surface material. In one embodiment, multiple gasses could be mixed for the source gas and detected nearly simultaneously by the spectrometer in one scan, for this purpose.
In reflection mode as shown in
In transmission mode as shown in
As shown in
As shown diagrammatically in
In the preferred embodiment, the sample 40 is raster-scanned (controllably positioned) in two dimensions using an electro-mechanical scanner and the aperture 30 is fixed. In one embodiment the scanner is a 2-D electromagnetic actuator based on the lens focus and tracking actuator from a CD-ROM drive. This uses a moving coil assembly suspended in a permanent magnet field by four flexure wires. It is driven through two D to A converter channels and an electronic driver circuit. In another embodiment, a piezoelectric scanner with drive electronics is used or any other type of mechanical scanner that can be controlled by the computer, or which the computer can synchronize to.
In the preferred embodiment, approach of the sample 40 to the aperture 30 along the Z axis (beam axis) and large-scale positioning in X and Y are done by an electromechanical positioner 50 controlled through the computer 500. This positioner controls the base location of a separate 2D raster scanning positioner 50. The three axis of angular positioning (tilt and rotation) are similarly controlled.
The sample 40 surface angle and XY scan plane angle may be adjusted to optimize the image illumination angle so as to increase specular reflection of the beam from the surface towards a detector, as depicted in
In another embodiment, large-scale positioning is manually controlled by a screw positioner having at least control of movement on the Z axis, but more ideally three to six axis of control, as in a typical electron microscope goniometer.
In one embodiment, the sample rate is from 1 to 60 samples per second and the images are typically of between 20*20 and 800*800 pixel size.
If the partial pressure of gas sensed by the detector 60 can be increased, the Signal/Noise ratio will improve due to the improved counting statistics within a sample period. By the same factor, the sample rate can be increased to speed up scans or the beam flow rate can be reduced to improve resolution.
A detector “nozzle” 10 has been constructed as depicted in
Since this inlet area 15 is also the only area through which the gas can exit back into the sample vacuum chamber 300 from the detector volume 400, the pressure within the detector volume 400 is raised in inverse proportion to the inlet area 15. This is a free molecular flow vacuum conductance situation, where the probability of the gas particles passing out of the detector volume 400 reaches equilibrium with the incoming particles at a higher pressure as the inlet area 15 is made smaller. Another equivalent way of understanding this is that the pressure equalizes internally at roughly the same pressure produced by the gas particles incoming from the sample 40. That pressure is higher up closer to the beam landing spot since they are radiating from there and have a higher density closer in. Thus if the detector nozzle inlet 15 is made smaller, it can be moved closer to measure the pressure where it is higher.
In addition, the roughly conical shape of the nozzle 10, expanding away from the inlet 15, adds some additional boost to the internal pressure. Due to the fact that the incoming particles are radiating in straight lines from the beam landing spot on the sample 40, some of them pass straight into the nozzle inlet 15 while those passing out of the nozzle 10 must do so through random, thermal motion. Particles passing straight into the expanding area of the nozzle 10 have a decreased probability of hitting the internal walls of the nozzle 10 and thus an increased probability of traveling deep into the detector volume 400. Conversely, particles leaving, travelling outward toward the inlet area 15 face a normal chance of randomly scattering from the nozzle 10 walls and thus see the normal conductance restriction of a narrowing conical tube.
The detector has a response time constant τ due to the pressure response of the enclosed detector volume behind the opening area to the sample chamber. The response of the pressure roughly follows a first order response similar to a resistor-capacitor low pass filter. As a result of adding the nozzle 10, the pressure response time constant z will increase, proportional to
v/a, where v is the enclosed detector volume 400 and a is the inlet area 15 plus any other area open to the vacuum. The result is a higher pressure and a slower tau, a compromise which can be optimized in relation to the image pixel sample time by adjusting the inlet area 15. In one embodiment, the detector volume 400 is approximately 0.23 liters, the inlet area 6 mm2, and τ is roughly 0.2 seconds for helium. This is used with a detector sampling rate of four to eight per second.
For reflection mode, the inlet area 15 is also optimized in position and shape to produce the desired image illumination qualities. This is because in order to be brightly illuminated in the image, the sample area 40 should have a direct path to the detector 60 in the direction of its strongest reflection. [
In embodiments with more than one detector 60 as depicted in
In one embodiment, the detector nozzle(s) 10 and aperture holder 20 are integrated together by bonding or machining in one piece. In another embodiment, the nozzle(s) 10 and aperture holder 20 have provisions for common alignment to the sample 40. This is useful since the most ideal detector nozzle inlet areas 15 are usually up close to the aperture holder surface 20 and close to the sample 40.
In another embodiment, the source, aperture holder 20, and detector nozzle 10 are all integrated into one assembly.
By substituting a charge particle source for the neutral gas source, and a charged particle detector such as an Everhart-Thornly secondary electron detector instead of the neutral particle detector and nozzle, the proximate aperture concept could be used to construct a particularly simple and small charged particle microscope. This would dispense with much of the focusing lens system and the scan coils of an SEM of FIB, and substitute the “pinhole” aperture and electromechanical scanning.
The foregoing description of the illustrated embodiments of the present invention is by way of exemplary depiction only, and other variations and modifications of the described embodiments and methods are possible in light of the foregoing teaching. Further, individual components of this invention may be implemented using one or more programmed general purpose computers, using application specific software and integrated circuits. Signal and for power connections may be hardwired, wireless, modem, etc. The embodiments described herein are not intended to be exhaustive or limiting as this invention is limited only by the following claims.
This application claims priority under 35 U.S.C. §119(e)(1) to U.S. Ser. No. 61/571,521, filed Jun. 29, 2011, which is hereby incorporated by reference in its entirety.
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20130001413 A1 | Jan 2013 | US |
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61571521 | Jun 2011 | US |