The invention relates to an Electron Microscope comprising:
The invention also relates to a method of using such an Electron Microscope.
Electron microscopy is a well-known and increasingly important technique for imaging microscopic objects. Historically, the basic genus of electron microscope has undergone evolution into a number of well-known apparatus species, such as the Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), and Scanning Transmission Electron Microscope (STEM), and also into various sub-species, such as so-called “dual-beam” apparatus (e.g. a FIB-SEM), which additionally employ a “machining” Focused Ion Beam (FIB), allowing supportive activities such as ion-beam milling or Ion-Beam-Induced Deposition (IBID), for example. More specifically:
In all cases, an Electron Microscope (EM) will comprise at least the following components:
In the case of a transmission-type microscope (such as a (S)TEM or TSEM, for example), an EM will additionally comprise:
Although there is a constant desire—from within various technological fields—to further improve the imaging resolution that can be obtained with EMs, this task is far from trivial. State-of-the-art EMs already employ aberration correctors (typically comprising groups of multipole (e.g. quadrupole, hexapole and/or octupole) lens elements) to mitigate imaging aberrations such as astigmatism, chromatic aberration and spherical aberration, which can contribute significantly to image degradation. However, despite such elaborate measures, EM imaging quality is still generally adversely affected by a variety of physical effects, including higher-order aberrations, Coulomb interactions, vacuum level fluctuations, and stray fields, for example. One such impediment that was recently discovered is electron beam disturbance due to “parasitic” thermal magnetic field noise along the beam path, as described by S. Uhlemann et al. in Physical Review Letters [PRL] 111, pp. 046101-046105, Jul. 26, 2013 (American Physical Society), in which the authors demonstrate a thermodynamic character of the observed magnetic field noise in a TEM, and take measures to cool “conductive parts of the instrument” to cryogenic temperatures (e.g. ˜77 K) in an attempt to curtail this phenomenon. Because the magnitude of the phenomenon scales with temperature, the intimation is that cooling to liquid helium temperatures will be required in order to achieve ultimate minimization of these noise effects.
It is an object of the disclosure to address these issues in an alternative way. More specifically, it is an object of the disclosure to provide an EM design in which such magnetic field noise effects are addressed without having to rely on the abovementioned elaborate cooling measures.
The invention will now be elucidated in more detail on the basis of exemplary embodiments and the accompanying schematic drawings (not to scale), in which:
In the Figures, where pertinent, corresponding parts are indicated using corresponding reference symbols.
In a first approach, these and other objects are achieved in an Electron Microscope as set forth in the opening paragraph above, characterized in that at least a longitudinal portion of said beam conduit extends at least through said aberration corrector and has a composite structure comprising:
A solution that requires cryogenic cooling of “conductive parts of” an EM (such as the iron cores/yokes in magnetic lenses, the beam conduit, etc.) is considered to be highly burdensome. The particle-optical column of an EM is already a tightly packed space in which relatively bulky, ultra-high-precision sub-components are positioned in close proximity to one another within tight tolerances, leaving very little room to spare. It would be an onerous undertaking to try to make additional space in such a set-up for the relatively cumbrous cooling elements/coils/supply lines that would be required to cool large parts of the microscope to cryogenic temperatures. The present disclosure therefore provides a different approach. Realizing the parasitic magnetic fields referred to above to be largely attributable to Johnson-Nyquist currents in the walls of the beam conduit—which traditionally consists of a metallic (e.g. stainless steel or titanium) pipe—the inventors decided to replace conventional beam conduit designs by an electrically insulating tube, e.g. comprising a durable ceramic such as Zirconia (ZrO2) or Alumina (Al2O3). To prevent space charging of such a tube, its inner surface is covered by a (grounded) skin of electrically conductive material, such as a metallic film—which should be relatively thin/resistive, so that it itself does not become a significant harbor/source for parasitic currents. A construction such as this seems to be disqualified by the abovementioned PRL journal article, which makes an argument that, by reducing conductivity and metallic wall thickness, the noise spectrum may be shifted somewhat from lower to higher frequencies, but the total noise power remains essentially the same, resulting in a negligible/marginal net effect on image spread. However, it is shown in the present disclosure that this argument is flawed: if the abovementioned spectral shift is large enough, then peak spectral power can be diverted into a frequency domain where Johnson-Nyquist fields no longer significantly affect the electron beam. More specifically, frequencies higher than the microwave cut-off frequency of the disclosed beam conduit do not make a substantial contribution to image spread/blurring.
On the basis of the discussion above, the skilled artisan will understand that the inner skin of the disclosed composite beam conduit should (simultaneously) be:
In this regard, the product at of skin (electrical) conductivity σ and skin thickness t can play an indicative role, and there tends to be a general preference for relatively small values of σt. For example, and to offer some guidance, in a (S)TEM operating at 300 kV, it has been found that a value of σt<0.1 Ω−1 yields satisfactory results, with better results obtained for σt<0.01 Ω−1, and a further improvement for σt<0.001 Ω−1. A given value of σt can be realized by choosing a variety of different (but complementary) values of σ and t individually; however, in practice, the skilled artisan will understand that some practical constraints need to be taken into account. For example:
To offer some guidance, acceptable results have been achieved using tin a range of about 5-20 μm, corresponding to a σ value that can be achieved using various relatively common conductive materials. It should be noted that:
As regards suitable materials for use in the disclosed composite beam conduit, the following non-limiting examples are given for guidance purposes:
It should be noted that, as referred to in the context of the current disclosure, the term “electrically insulating material” can also include materials that might traditionally be considered as being semiconductors. For example, SiC is a ceramic material that is conventionally labelled as being a semiconductor; however, its electrical resistivity is ˜106 Ω/cm—which makes it about 1016 times less conductive than aluminum, which has a resistivity of ˜10−10 Ω/cm. By comparison, the electrical resistivities of Quartz, Alumina and Zirconia are ˜1016, 1014 and 109 Ω/cm, respectively. The skilled person will understand that an electrical insulator is a material in which there is (basically) no free transport of (conduction) electrons, usually due to the presence of a relatively large band gap in such materials.
In an alternative solution, the Electron Microscope as defined herein is characterized in that at least a longitudinal portion of said beam conduit extends at least through said aberration corrector and is comprised of an aggregate composite material comprising:
In this second, related approach, the beam conduit is comprised of an aggregate composite material comprising intermixed electrically insulating material and electrically conductive material. Such an approach builds upon similar insights to those set forth above, but it does so using a beam conduit architecture in which the “laminate structure” of separate electrically insulating outer tube and electrically insulating inner skin described above are effectively “morphed” into a single “monolithic” aggregate composite structure. The electrical conductivity of this morphed structure is intermediate between that of regular conductive materials and insulating materials, and it can be functionally referred to as a “high-volume-resistivity” material. It is concurrently:
If one considers:
With regard to the constitution of an aggregate composite structure as set forth in the previous paragraph, suitable examples of component materials include:
One way of achieving such a composite is to intermix conductive material (e.g. in the form of particles or fibers) in a matrix of insulating material (e.g. in the form of green ceramic material); alternatively, one can start with a conductive material and “temper” its conductivity by intermixing an insulating material therein. The additive in question may, for example, be included in the receptive bulk material using a process such as diffusion or ion implantation, or by physical mixing of granulates, for instance. The skilled artisan will be able to determine the relative quantities of different materials to be mixed in order to achieve an aggregate composite with a given bulk resistivity, and/or he can purchase pre-made products. For example, aggregate composite materials as referred to herein are commercially available from firms such as Poco Graphite, Inc., in Decatur, Tex., USA. They are sometimes referred to as “ESD” materials, because of their suitability to mitigate electrostatic discharge issues. Other terms that are sometimes used for such materials include “electro-ceramics” and “granular metals”.
The disclosed composite beam tube construction set forth above (in either approach) does not necessarily have to be employed over the entire length of the (primary) beam path in the microscope (though such full-length deployment is, of course, possible). In practice, it has been found that:
Examples of an aberration corrector as referred to herein include a spherical aberration (Cs) corrector, a chromatic aberration (Cc) corrector, and a combined spherical-chromatic (Cs-Cc) corrector—which may be employed in SEMs and/or TEMs. For instance:
When an aberration corrector as referred to above is employed, another relatively sensitive portion of the beam path in which the present disclosed techniques can be exploited is a trajectory extending between the specimen plane (specimen holder) and the aberration corrector. By this is meant either or both of:
Moreover, application of the disclosed techniques at portions of the beam path that are located in/near electrostatic deflection modules can be advantageous. The skilled artisan will be able to decide which portions of the beam path (most) merit application of the disclosed composite beam conduit, and may decide to deploy it along (substantially) the entire primary beam path. This latter scenario is of merit inter alia in that it avoids having to make a joint between two different types of beam conduit—bearing in mind that the entire beam conduit must reliably sustain a high vacuum (at least) during operation of the microscope.
Using the present invention, one can achieve excellent STEM image resolution values of, for example, 30 pm at a beam voltage of 300 kV, and 60 pm at a beam voltage of 60 kV, in both cases for a beam half opening angle of 50 mrad, and without having to resort to cumbersome cryogenic cooling as set forth in the abovementioned PRL journal article. With respect to a conventional stainless steel beam conduit, the invention typically allows image spread caused by Johnson-Nyquist noise to be reduced by a factor of the order of about 10-15.
Supplemental to the disclosed techniques described herein, there are additional measures that can be taken to further reduce the detrimental imaging effects of Johnson-Nyquist noise, without necessarily having to resort to the cryogenic cooling described in the aforementioned PRL journal article. One such measure is to widen the bore in one or more magnetic (e.g. iron) yokes used to conduct field lines into the direct vicinity of the beam. Nominally, such bores hug/contact the outer surface of the beam conduit, so as to get as close as possible to the beam axis. However, it has been noted that, for a cylindrical bore of (inner) radius r, the yoke contributes to Johnson-Nyquist blurring according to a 1/r dependency; consequently, widening the bore will reduce the effect of such blurring. Increasing the bore size in this manner will cause an empty gap to be created between the inner surface of the bore and the outer surface of the beam conduit, but such a gap does not necessarily have significant (overriding) negative aspects.
For sake of completeness, it is referred to the following prior art documents.
U.S. Pat. No. 3,787,696 A and DE 30 10 376 A1 disclose liner tubes for use in scanning and/or focusing coils. U.S. Pat. No. 3,634,684 A also uses a liner tube for a scanning coil. Here, the liner tubes are used to counter Eddy currents originating from the high-frequency magnetic flux originating from the scanning. These documents do not suggest the use of these liner tubes to counter Johnson noise in a multi-pole lens assembly as an aberration corrector.
JP H03 22339 A discloses an aberration corrector with an electrically conductive inner skin and an electrically isolating outer tube. Here, the electrically conductive inner skin is required to apply a desired voltage to the liner tube and to keep the specimen grounded.
The specimen S is held on a specimen holder H that can be positioned in multiple degrees of freedom by a positioning device/stage A, which moves a cradle A′ into which holder H is (removably) affixed; for example, the specimen holder H may comprise a finger that can be moved (inter alia) in the XY plane (see the depicted Cartesian coordinate system), with motion parallel to Z and tilt about X/Y also typically being possible. Such movement allows different parts of the specimen S to be illuminated/imaged/inspected by the electron beam B traveling along axis B′ (in the Z direction), and/or allows scanning motion to be performed as an alternative to beam scanning. If (as is often the case) the specimen S is a cryogenic specimen, then the specimen holder H can be maintained at a cryogenic temperature using a (schematically depicted) temperature control assembly T; this may, for example, comprise a thermally conductive (e.g. metallic) wick that is thermally connected to the holder H and is immersed in a bath of cryogen, or a pipe system carrying a circulating cryogen, for example.
The electron beam B will interact with the specimen S in such a manner as to cause various types of “stimulated” radiation to emanate from the specimen S, including (for example) secondary electrons, backscattered electrons, X-rays and optical radiation (cathodoluminescence). If desired, one or more of these radiation types can be nominally detected with the aid of analysis device 22, which might be a combined scintillator/photomultiplier or EDX (Energy-Dispersive X-Ray Spectroscopy) module, for instance; in such a case, an image could be constructed using basically the same principle as in a SEM. However, alternatively or supplementally, one can study electrons that traverse (pass through) the specimen S, exit/emanate from it and continue to propagate (substantially, though generally with some deflection/scattering) along axis B′. Such a transmitted electron flux enters an imaging system (projection lens) 24, which will generally comprise a variety of electrostatic/magnetic lenses, deflectors, correctors (such as stigmators), etc. In normal (non-scanning) TEM mode, this imaging system 24 can focus the transmitted electron flux onto a fluorescent screen 26, which, if desired, can be retracted/withdrawn (as schematically indicated by arrows 26′) so as to get it out of the way of axis B′. An image or diffractogram of (part of) the specimen S will be formed by imaging system 24 on screen 26, and this may be viewed through viewing ports 28a, 28b located in suitable parts of the walls of enclosure V/cabinet 2. The retraction mechanism for screen 26 may, for example, be mechanical and/or electrical in nature, and is not depicted here.
As an alternative to viewing an image/diffractogram on screen 26, one can instead make use of the fact that the depth of focus of the electron flux leaving imaging system 24 is generally quite large (e.g. of the order of 1 meter). Consequently, various other types of analysis apparatus can be used downstream of screen 26, such as:
Note that controller (computer processor) 20 is connected to various illustrated components via control lines (buses) 20′. This controller 20 can provide a variety of functions, such as synchronizing actions, providing setpoints, processing signals, performing calculations, and displaying messages/information on a display device (not depicted). Needless to say, the (schematically depicted) controller 20 may be (partially) inside or outside the cabinet 2, and may have a unitary or composite structure, as desired.
The skilled artisan will understand that the interior of the enclosure V does not have to be kept at a strict vacuum; for example, in a so-called “Environmental TEM/STEM”, a background atmosphere of a given gas is deliberately introduced/maintained within the enclosure V.
The microscope M can comprise one or more aberration correctors 40, each of which comprises a multipole lens assembly that is configured to mitigate spherical (Cs) and/or chromatic (Cc) aberration. For example, the depicted corrector 40 in the illumination system 6 might be a Cs corrector, whereas the corrector 40 in the imaging system 24 might be a combined Cs-Cc corrector.
Traditionally, beam conduit B″ comprises a metallic pipe. However, in the context of the present disclosure, this basic structure has been modified over at least part of the length (along the Z axis) of the beam conduit B″. With reference to
Note that the skin 52 in both of
A composite beam conduit structure according to the disclosure and such as that illustrated in
In an alternative approach, tube 50 is pre-formed (e.g. cast or rolled) in a cylindrical shape, and skin 52 is then deposited on its inside surface.
A condensed mathematical treatise will now be given of certain aspects of the invention. Electrical conductors (both magnetic and non-magnetic) produce a substantial fluctuating magnetic field at low frequencies, via the same thermal currents that cause the well-known Johnson-Nyquist noise in resistors. Consider a non-magnetic tube with inner radius α, wall thickness t«α, and electrical conductivity σ. One threshold frequency is related to the skin effect, and is given by:
νskin=(πμ0σt2)−1 (3:1)
Here, μ0 is the permeability of vacuum. Consider now a loop current in a large plate of thickness t, with average radius α»t and DC resistance R0=2π/(σt), whereby the fluctuating magnetic field is measured at a distance α from the plate. A reasonable approximation for the frequency-dependent resistance R in this case is:
Current fluctuations are given by:
in which self-inductance Lind≈μ0α, k is the Boltzmann constant and T is temperature. Hence there is a second threshold frequency νind, which satisfies:
R(νind)=2πμ0ανind
with:
νind=(μ0ασt)−1, (3.5)
for t«α.
Equations for the low frequency variation of the magnetic field are of the form:
with geometric factor Cgeo<≈0.2. For a tube, α=tube radius. This can be extended to the spectral density:
Because t«α, equation (3.7) can be approximated by:
which integrates to:
Hence, wall thickness t and conductivity σ drop out of the equation. If σt is reduced, the spectral density at low frequencies is reduced, but all the noise power is transferred to higher frequencies.
In order to calculate deflection angles induced by fluctuating magnetic fields, one needs to know the so-called correlation distance ξ (along the tube axis) of the lateral magnetic field. One can use ξ=3α/2 for fields that are generated via Johnson-Nyquist currents. In a so-called ‘frozen dipole’ scenario, assuming frequencies well below v/2ξ, where v is the electron speed, one obtains:
for a tube of length L, where:
A
n(z)=e−2|z|/ξ (3.11)
and
A
n(z)=e−πz
The latter equation will be assumed hereunder.
For frequencies larger than the aforementioned ‘frozen dipole’ threshold v/2ξ, electrons wiggle a number of periods while traversing the correlation distance ξ. This strongly reduces the net deflection angle as compared to the ‘frozen dipole’ case, which (partly) explains why black body radiation does not contribute significantly to image spread in a TEM. In order to include these frequencies for Johnson-Nyquist currents, use is made of a simple model with an arbitrarily large set of discrete frequencies for the lateral magnetic field on the optical axis, without any mutual correlation between the different frequencies. An axial electron is still assumed to be governed by the Lorentz force, via:
Here, γr=1+U e/mc2. The correlation function for the magnetic field is allowed to vary with frequency, i.e. An(z) and ξ are assumed to be frequency-dependent. One can then show for deflection angle θ that:
in which η=(e/2m)1/2, and the exponent factor accounts for the wiggling of the electron. Equation (3.12) then leads to:
This equation suggests that:
in which the upper limit roughly equals the ‘frozen dipole’ threshold:
in terms of the cut-off frequency:
and speed of light c in vacuum. Using equation (3.8) this leads to:
from which it follows that a large reduction of thermal magnetic field noise can be achieved if:
in which case equation (3.1.6) simplifies to:
i.e. image spread simply scales according to (σt)1/2 in the regime given by equation (3.1.7). For example, in the specific case of an electron microscope with Umax=300 kV, one obtains:
σt<<4/(μ0c)=0.011 Ω−1. (3.1.9)
Δ=θ(σt)inv/θ(σt)ref
where the subscripts “dis” and “ref” respectively refer to “disclosure” and “reference”. A conventional stainless steel beam conduit is the reference used for the vertical axis.
Points below the horizontal dashed line (Δ=1) represent an improvement with respect to the conventional beam conduit. Note that improvement is already manifest at Σ=−1 (corresponding to σt=0.1), but that there is stronger improvement Σ=−2 (corresponding to σt=0.01), and even greater improvement at Σ=−3 (corresponding to σt=0.001).
Number | Date | Country | Kind |
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18182145.5 | Jul 2018 | EP | regional |
This application is a Divisional, under 35 U.S.C. § 120, of co-pending and co-assigned U.S. patent application Ser. No. 16/453,699, titled “Electron Microscope with Improved Imaging Resolution, which was filed on Jun. 26, 2019 and which claims foreign priority, to European Patent Office (EPO) application No. 18182145.5, which was filed on Jul. 6, 2018.
Number | Date | Country | |
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Parent | 16453699 | Jun 2019 | US |
Child | 18171750 | US |