The present invention relates to charged particle beam-induced deposition and more specifically to deposition processes in which beam is not orthogonal to the work piece surface.
Monitoring nanometer scale processes, such as the photolithography processes used in the fabrication of integrated circuits, is challenging. To fabricate integrated circuits, a semiconductor substrate, such as silicon wafer, on which circuits are being formed is coated with a material, such as a photoresist, that changes solubility when exposed to radiation. A lithography tool, such as a mask or reticle, positioned between the radiation source and the semiconductor substrate casts a shadow to control which areas of the substrate are exposed to the radiation. After the exposure, the photoresist is removed from either the exposed or the unexposed areas, leaving a patterned layer of photoresist on the wafer that protects parts of the wafer during a subsequent etching or diffusion process.
During the manufacturing process, variations in exposure and focus require that the patterns developed by lithographic processes be continually monitored or measured to determine if the dimensions of the patterns are within acceptable ranges. The importance of such monitoring, often referred to as process control, increases considerably as pattern sizes become smaller, especially as minimum feature sizes approach the limits of resolution available by the lithographic process. In order to achieve ever-higher device density, smaller and smaller feature sizes are required. This may include the width and spacing of interconnecting lines, spacing and diameter of contact holes, and the surface geometry such as corners and edges of various features. Features on the wafer are three-dimensional structures and a complete characterization must describe not just a surface dimension, such as the top width of a line or trench, but a complete three-dimensional profile of the feature. Process engineers must be able to accurately measure the critical dimensions (CD) of such surface features to fine tune the fabrication process and assure a desired device geometry is obtained.
Typically, CD measurements are made using instruments such as a scanning electron microscope (SEM). In a scanning electron microscope (SEM), a primary electron beam is focused to a fine spot that scans the surface to be observed. Secondary electrons are emitted from the surface as it is impacted by the primary beam. The secondary electrons are detected, and an image is formed, with the brightness at each point of the image being determined by the number of secondary electrons detected when the beam impacts a corresponding spot on the surface. As features continue to get smaller and smaller, however, there comes a point where the features to be measured are too small for the resolution provided by an ordinary SEM.
Transmission electron microscopes (TEMs) allow observers to see extremely small features, on the order of nanometers. In contrast to SEMs, which only image the surface of a material, TEMs also allow analysis of the internal structure of a sample. In a TEM, a broad beam impacts the sample and electrons that are transmitted through the sample are focused to form an image of the sample. The sample must be sufficiently thin to allow many of the electrons in the primary beam to travel though the sample and exit on the opposite site. Samples, also referred to as lamellae, are typically less than 100 nm thick.
In a scanning transmission electron microscope (STEM), a primary electron beam is focused to a fine spot, and the spot is scanned across the sample surface. Electrons that are transmitted through the sample are collected by an electron detector on the far side of the sample, and the intensity of each point on the image corresponds to the number of electrons collected as the primary beam impacts a corresponding point on the surface.
Because a sample must be very thin for viewing with transmission electron microscopy (whether TEM or STEM), preparation of the sample can be delicate, time-consuming work. The term “TEM” as used herein refers to a TEM or an STEM and references to preparing a sample for a TEM are to be understood to also include preparing a sample for viewing on an STEM. The term “S/TEM” as used herein also refers to both TEM and STEM.
A focused ion beam (FIB) system can be used to form lamellae for observation on a TEM. One process for preparing lamellae is described in U.S. Pat. Pub. 2013/319,849 A1 for “Preparation of Lamellae for TEM Viewing,” which is assigned to the application of the present invention and which is hereby incorporated by reference. FIB systems are widely used in microscopic-scale manufacturing operations because of their ability to image, etch, mill, deposit, and analyze very small structures with great precision. FIB systems produce a narrow, focused beam of ions that is typically scanned across the surface of a sample in a raster fashion. In many commercial FIB systems, positively charged gallium ions (Ga+) are extracted from a liquid metal ion source. In some systems, other ion species, such as argon or xenon, are extracted from a plasma ion source. The extracted ions are accelerated, collimated, and focused onto a sample by a series of apertures and electrostatic lenses. The ion beam can be used to remove material from the sample surface or to deposit material onto the surface. When used to remove material, often referred to as etching or milling, the ions in the focused ion beam physically eject atoms or molecules from the surface by sputtering, that is, by a transfer of momentum from the incoming ions to the atoms at the surface.
When used to deposit material with a FIB, a precursor gas, such as tungsten hexacarbonyl or styrene gas, is directed onto the sample surface, usually via a fine needle inserted near the position of the ion beam. The gas is broken down into volatile and non-volatile components when the ion beam strikes the surface. The non-volatile component is deposited onto the surface, while the volatile component is pumped away.
Because FIB milling can cause significant damage to small structures, the work piece surface is often coated with a protective layer of tungsten or carbon before milling begins. The protective layer can be deposited using ion beam-induced deposition. To reduce artifacts on the lamella that interfere with TEM imaging, the protective layer should be symmetrical.
As used here, the term “angle of incidence” or “incidence angle” refers to the tilt of the beam axis relative to a normal to the surface to which the beam is directed. That is, the angle of incidence of a beam perpendicular to the surface is zero. In some systems, FIB column axes are oriented at a small angle, such as +/−3 degrees, from a normal to the sample surface. Such systems can apply a relatively symmetrical deposition. Other FIBs uses an FIB column axis oriented at 45 degree to the sample surface. Applicants have found that when the ion beam is not oriented normal to the work piece surface, the deposition tends to be asymmetrical.
SEM deposition of the protective layer can be used to protect sensitive surfaces from FIB damage, but this can lead to lamella placement issues unless a recognizable mark is visible to the FIB after the feature if interest has been covered with SEM deposition.
Applicants investigated, researched, and discovered a method that improves the FIB induced deposition using specific operating conditions that produce symmetrical growth using a non-orthogonal beam, which technique is particularly useful for depositing a protective layer or cap during lamella formation.
It is an object of the invention, therefore, to provide symmetrical charged particle beam-induced deposition when using a charged particle beam that is incident at a non-normal angle to the work piece surface.
The invention provides a method and apparatus for producing symmetric beam-induced deposition with an incident beam that is not orthogonal to the work piece surface. In one embodiment, the system and methods can be used to form a protective layer as part of a process of forming a lamella for viewing on a transmission electron microscope. A set of operational parameters, including, for example, beam energy and scan direction, is set to provide the symmetrical deposition.
In accordance with some embodiments, a FIB column is oriented at a non-orthogonal angle, such as 45 degrees, to the sample surface and the deposition parameters are set so that the FIB-deposited material is symmetrical.
The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter. It should be appreciated by those skilled in the art that the conception and specific embodiments disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims.
For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
The accompanying drawings are not intended to be drawn to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures is represented by a like numeral. For purposes of clarity, not every component may be labeled in every drawing.
Preferred embodiments of the present invention are directed toward methods and apparatuses for improved beam-induced deposition with a beam that is not orthogonal to the work piece surface. Embodiments are particularly useful to provide improved control of the deposition of protective layers for lamella manufacture.
When a beam inducing a deposition is incident at a non-orthogonal angle to the work piece surface, the deposition tends to grow in the direction of the beam source instead of normal to the work piece surface, resulting in an asymmetrical deposit. This asymmetrical deposition adversely affects the quality of the subsequent milling steps through the deposited layer because regions with a thicker protective layer will etch more slowly. The asymmetrical deposition is thought to be caused by the mechanics of the beam-induced deposition process. During a focused ion beam deposition process, there is competition between deposition and sputtering, and the sputtering rate depends on the angle between the beam and the surface on which the beam in incident. Sputter rates increase as the angle of incidence increases. The deposition tends to grow faster at angles having lower sputtering rate. The larger the deviation of the beam incident angle from normality, the greater the tendency for the deposit to grow towards the beam source. The magnitude of this effect varies with the incident angle and with the deposition precursor. For example, applicants have found that when using with a carbon precursor for deposition, the asymmetry is significant at the incident angles greater than about 35 to 40 degrees.
Embodiments of the invention deposit material use a FIB at a non-orthogonal incident angle. In one dual beam system commercially available from FEI Company, the present applicant, a FIB column axis is oriented at 45 degrees from the vertical and an SEM is also typically at about 45 degree angle +/−3 degrees from the vertical. In one system that has proven to be valuable for manufacturing sub ˜50 nm thick lamellae, the SEM and FIB are spaced about 90 degrees azimuthally from each other, with each column axis oriented about 45 degrees from the vertical and from the sample surface.
Carbon, deposited by beam-induced deposition, can be used as a protective layer to protect the region of interest during ion beam processing. Carbon is a hard material that can withstand the intensive ion beam irradiation and has a high deposition rate. These properties make carbon an ideal material for use as a protective layer during lamella fabrication. However, when deposited with a beam having a large incidence angle, the carbon deposit is asymmetric, which results in inconsistent milling below the non-uniform layer and therefore artifacts in the lamella. Organometallic precursors used to deposit metals contain carbon, and the material deposited by beam-induced decomposition of the precursor gas typically contains a large amount of carbon as well as the desired metal. By “carbon deposition” or “carbon precursor” is meant a deposition or precursor, such as styrene, that is used to deposit carbon, and not a metallic precursor that inadvertently deposits carbon.
The deposition of material and the sputtering of the deposited material are always competing with each other, as ions both decompose the precursor and knock materials form the surface. The balance between deposition and sputtering can be optimized toward deposition by selecting process parameters, such as gas pressure, beam current, beam energy, and ion species. Even with the beam parameters optimized to favor deposition over milling, the deposition is asymmetrical, which is detrimental for lamella TEM preparation. In the prior art, skilled persons have adjusted the operating parameters to maximize the deposition rate. Applicants have found that setting that do not maximize the deposition rate may be preferred, with the preferred parameters providing smoother or more symmetric depositions. The arrangement of this SEM 302 and FIB column 306 with a XY movable stage 310 that allows movement in the X-Y plane and rotation about an axis orthogonal to the X-Y plane is well suited for smooth and nanoscaled lamella production when used with a carbon based lamella protection layer. The FIB column 306 can include, for example, a liquid metal ion source, such as a source of gallium ions, a plasma ion source, such as an inductively coupled plasma ion source or an electron cyclotron resonance ion source, or any other source of ions that can be sufficiently directed to form a deposit of the desired resolution. The problem is that the asymmetric deposit formed by the angled beam adversely affects any lamella formed by milling through the asymmetric protective layer. The term “focused ion beam” as used herein includes a shaped beam, such as a beam that projects the shape of an aperture onto the work piece surface.
Table 1 shows TRIM simulation results of carbon sputter rate from Ga+ beams having different energies at different incidence angles.
Table 1 shows that sputter rates increase with angle of incidence and with beam energy. Applicants found that deposits at angles of 30 degrees or less were relatively smooth at all beam energies. Deposit at 45 degrees and beam energies of 30 kV and 16 kV showed substantial asymmetry. At 45 degrees and 8 kV, the deposit was less rough, but still not entirely smooth. At 5 kV and 45 degrees, the deposit was smooth. So in accordance with one embodiment of the invention, the FIB column can be fixed to a 45 degree angle from the sample surface and by reducing the ions landing energy to 5 kV, the reduction in the actual sputtering compared to higher beam energies increases throughput of the protective layer deposition process from about 2.5 minutes to 35 seconds. Furthermore, there is less damage to the sample surface at lower beam energies. Materials sputter rate increases with the angle of incidence but the sputter rate of 5 kV landing energy is low enough to reduce material sputtering even at higher angles of incidence.
As can be seen in Table 1, as the incidence angle of the Ga+ beam approaches 45 degrees at 30 kV and 16 kV landing energy, respective, the high sputter rates are 4.6 and 4.1 atoms per ion which produce non-uniform lamella protection layers that are unusable for TEM preparation and use.
Embodiments of the current invention provide deposition solutions wherein the deposition growth is symmetric. This is done by using a low landing energy, such as less than 10 keV, less than 8 keV, less than 6 keV, or preferably about 5 keV for an incidence angle of preferably greater than 30 degrees or greater than 40 degrees.
The preferred process parameters depend on the application and skilled persons can determine optimum beam energy for any incident angle and ion species. For an angle of 45 degrees, the preferred beam energy for a gallium ion beam is between 1 keV and 20 keV, more preferably between 2 keV and 10 keV, even more preferably between 3 keV and 8 keV, and most preferably between 4 keV and 6 keV. The preferred beam current any of these energies is between 200 pA and 600 pA. Any deposition precursor, such as a metallo-organic precursor or a carbon precursor such as styrene, can be used. The preferred vacuum chamber pressure when the deposition gas is present depends on the gas, but is typically between 10−5 Torr and 3×10−5 Torr.
After the lamella is prepared, it is mounted in a TEM sample grid for viewing. The removal of the lamella from the sample can be performed “ex-situ,” that is, outside of the vacuum chamber or the lamella can be removed inside the vacuum chamber and mounted to a grid using ion beam deposition. For ex-situ removal, many lamellae can be prepared on a single sample, which is then removed from the vacuum chamber. The lamella can be removed from the sample and placed onto TEM sample grids. The process described above can be automated to prepare in the vacuum chamber multiple lamellae at various designated locations for ex-situ removal.
While an example of suitable hardware is provided above, the invention is not limited to being implemented in any particular type of hardware.
Preferred embodiments of the present invention also make use of a particle beam apparatus, such as an FIB or SEM, in order to image a sample using a beam of particles. Such particles used to image a sample inherently interact with the sample resulting in some degree of physical transformation. Further, throughout the present specification, discussions utilizing terms such as “calculating,” “determining,” “measuring,” “generating,” “detecting,” “forming,” or the like, also refer to the action and processes of a computer system, or similar electronic device, that manipulates and transforms data represented as physical quantities within the computer system into other data similarly represented as physical quantities within the computer system or other information storage, transmission or display devices.
The invention has broad applicability and can provide many benefits as described and shown in the examples above. While the examples provided described providing a protective layer for lamella formation, the invention is useful for any application of beam-induced deposition with a non-orthogonal beam. The embodiments will vary greatly depending upon the specific application, and not every embodiment will provide all of the benefits and meet all of the objectives that are achievable by the invention. Particle beam systems suitable for carrying out the present invention are commercially available, for example, from FEI Company, the assignee of the present application.
Although much of the previous description is directed at semiconductor wafers, the invention could be applied to any suitable substrate or surface. Further, whenever the terms “automatic,” “automated,” or similar terms are used herein, those terms will be understood to include manual initiation of the automatic or automated process or step. Whenever a scan or image is being processed automatically using computer processing, it should be understood that the raw image data can be processed without ever generating an actual viewable image. The term “image” is used in a broad sense to include not only a displayed image showing the appearance of the surface, but also to include any collection of information characterizing the multiple points on or below a surface. For example, a collection of data corresponding to the secondary electrons collected when a particle beam is at different point on a surface is a type of “image,” even if the data is not displayed. Collecting information about points on the sample or sample is “imaging.”
In the following discussion and in the claims, the terms “including” and “comprising” are used in an open-ended fashion, and thus should be interpreted to mean “including, but not limited to . . . . ” The term “integrated circuit” refers to a set of electronic components and their interconnections (internal electrical circuit elements, collectively) that are patterned on the surface of a microchip. The term “semiconductor device” refers generically to an integrated circuit (IC), which may be integral to a semiconductor wafer, separated from a wafer, or packaged for use on a circuit board. The term “FIB” or “focused ion beam” is used herein to refer to any collimated ion beam, including a beam focused by ion optics and shaped ion beams.
To the extent that any term is not specially defined in this specification, the intent is that the term is to be given its plain and ordinary meaning. The accompanying drawings are intended to aid in understanding the present invention and, unless otherwise indicated, are not drawn to scale.
Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions, and alterations can be made to the embodiments described herein without departing from the spirit and scope of the invention as defined by the appended claims. Moreover, the scope of the present application is not intended to be limited to the particular embodiments of the process, machine, manufacture, composition of matter, means, methods, and steps described in the specification. As one of ordinary skill in the art will readily appreciate from the disclosure of the present invention, processes, machines, manufacture, compositions of matter, means, methods, or steps, presently existing or later to be developed that perform substantially the same function or achieve substantially the same result as the corresponding embodiments described herein may be utilized according to the present invention. Accordingly, the appended claims are intended to include within their scope such processes, machines, manufacture, compositions of matter, means, methods, or steps.
In a preferred embodiment, a method of charged particle beam induced deposition is used, comprising:
directing a charged particle beam toward a work piece surface at an angle of greater than 30 degrees from a surface normal, the charged particles having a landing energy of 10 keV or less; and
providing a precursor gas at the impact point of the charged particle beam, the precursor gas decomposing in the presence of the charged particle beam to deposit material onto the work piece.
In some embodiments, directing a charged particle beam toward a work piece surface comprises scanning the charged particle beam in a direction along a normal projection of the beam onto the work piece.
In some embodiments, providing a precursor gas at the impact point of the charged particle beam comprises providing a precursor gas that does not contain metal and that deposits carbon onto the work piece surface in the presence of the charged particle beam.
In some embodiments, providing a precursor gas at the impact point of the charged particle beam comprises providing a metallo-organic compound.
In some embodiments, directing a charged particle beam toward a work piece surface comprises directing a charged particle beam toward the work piece surface at an incident angle of greater than 40 degrees from a surface normal, the charged particles having a landing energy of 8 keV or less.
In some embodiments, directing a charged particle beam toward a work piece surface comprises directing a charged particle beam toward the work piece surface at an incident angle of 45 degrees+/−5 degrees from a surface normal, the charged particles having a landing energy of between 3 keV and 7 keV.
In an embodiment of the invention, a TEM lamella may be prepared having a uniform deposition using a focused ion beam comprising:
directing a focused ion beam toward a work piece surface at an angle of greater than 30 degrees from a surface normal, the charged particles having a landing energy of 10 keV or less;
providing a precursor gas at the impact point of the charged particle beam, the precursor gas decomposing in the presence of the ion beam to deposit material onto the work piece; and
directing a focused ion beam toward the deposited material on the work piece to remove material from both sides of a region of interest to leave a thin lamella containing the region of interest, the deposited material protecting the thin lamella during formation.
In some embodiments, directing a charged particle beam toward a work piece comprises scanning the charged particle beam in a direction along a normal projection of the beam onto the work piece.
In some embodiments, providing a precursor gas at the impact point of the charged particle beam comprises providing a precursor gas that does not contain metal and that deposits carbon onto the work piece surface in the presence of the charged particle beam.
In some embodiments, providing a precursor gas at the impact point of the charged particle beam comprises providing a metallo-organic compound.
In some embodiments, directing a charged particle beam toward a work piece surface comprises directing a charged particle beam toward the work piece surface at an incident angle of greater than 40 degrees from a surface normal, the charged particles having a landing energy of 8 keV or less.
In some embodiments, directing a charged particle beam toward a work piece surface comprises directing a charged particle beam toward the work piece surface at an incident angle of 45 degrees+/−5 degrees from a surface normal, the charged particles having a landing energy of between 3 keV and 7 keV.
In an embodiment of the invention, a charged particle beam system for processing a work piece is provided, said charged particle beam system comprising:
an ion beam column oriented at least 30 degrees from the vertical;
an electron beam column oriented at least 30 degrees from the vertical;
a gas injection system for directing a precursor gas to be decomposed by the ion beam or the electron beam;
a sample stage, the sample stage capable of moving in at least two dimensions and of rotating about a vertical axis, but not capable of tilting;
a controller for controlling the operation of the charged particle beam system in accordance with stored instructions; and
a memory for storing computer instructions for performing the methods described above.
In some embodiments, the ion beam column is oriented at least 45 degrees plus or minus 10% from the vertical.
In some embodiments, the ion beam column includes a liquid metal ion source.
In some embodiments, the ion beam column includes a plasma ion source.
This application claims priority from U.S. Prov. Pat. App. No. 62/016,464, filed Jun. 24, 2014, which is hereby incorporated by reference.
Number | Date | Country | |
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62016464 | Jun 2014 | US |