The present invention relates to a transmission electron microscope and a sample observation method.
There is a transmission electron microscope that has an annular aperture, a lens and a pinhole, which are located between a sample and an electron detector, and causes the annular aperture to remove unnecessary electrons scattered from the sample, causes the lens to focus necessary scattered electrons that have passed through the annular aperture on the pinhole and detects the necessary scattered electrons (refer to Patent Document 1).
Patent Document 1: JP-2008-270056-A
In general, a focusing lens that focuses an electron beam has a spherical aberration. For the technique described in Patent Document 1, in order to focus the scattered electrons that have passed through the annular aperture on the pinhole, an expensive spherical aberration corrector needs to be arranged. A microscope of this type is capable of measuring compositional contrast as a high angle annular dark field (HAADF) image by detecting electrons scattered at a scattering angle of 80 mrad or higher and has an advantage of improving a depth resolution by detecting the electrons scattered at the high angle. However, Scattering angles of electrons that can be corrected by the spherical aberration corrector are limited.
An object of the present invention is to provide a transmission electron microscope and a sample observation method, which enable electrons scattered at high angles to be detected without a limitation caused by a spherical aberration of an electron lens and enable a depth resolution to be improved.
The present invention relates to a technique for causing a plurality of annular apertures to limit electrons scattered by irradiating a sample with an electron beam and detecting scattered electrons that have passed through the plurality of annular apertures.
In addition, the present invention relates to a technique for causing a single annular aperture to limit electrons scattered by irradiating a sample with an electron beam and causing an electron detector with a light receiving surface to detect scattered electrons that have passed through the single annular aperture.
According to the present invention, it is possible to detect electrons scattered at high angles without a limitation caused by a spherical aberration of an electron lens and improve a depth resolution.
Embodiments of the present invention are described below with reference to the accompanying drawings.
First, a comparative example is described below.
In recent years, an application of a technique for an optical confocal microscope to an electron microscope has started to be considered. However, many interactions of an electron beam with a sample occur, and a spherical aberration largely affects the electron microscope. Thus, it is difficult to simply use the technique (for the optical microscope) for the electron microscope.
As illustrated as the comparative example in
In the comparative example, the electron beam 2′, with which the sample 5′ is irradiated and which has passed through a part (located near the center of the focusing lens 4′) of the focusing lens 4′, passes through the sample 5′. Thus, when the sample 5′ is a crystalline sample, a strong channeling effect occurs depending on a crystal orientation. In this case, when a target region 6′ to be observed is located in the sample 5′ or a specific region included in the sample 5′ and located in a thickness direction (optical axis direction), an electron 7′ is scattered from the side of the electron gun 1′ or an electron 9′ is scattered from a layer located on the opposite side of the electron gun 1′, and the scattered electron 7′ and the scattered electron 8′ become noise so that a desired depth resolution cannot be ensured. Thus, it is desirable to suppress the occurrence of the scattered electrons 7′ and 8′ and efficiently obtain the target electron 8′ scattered from the target region 6′.
In the comparative example illustrated in
When a technique for an optical confocal microscope is used for a scattered electron detection system according to the comparative example, a configuration in which a pinhole 12′ is arranged in front of an electron detector 13′ can be considered as illustrated in
In this case, an annular aperture 10′ is arranged between the sample 5′ and the lens 11′. If the annular aperture 10′ is not arranged, electrons that are scattered from a region other than the target region 6′ pass through the pinhole 13′ and reach the electron detector 13′ due to a spherical aberration of the lens 11′, and the pinhole 12′ does not effectively function. When the annular aperture 10 is arranged and a spherical aberration corrector (not illustrated) is arranged between the lens 11 and the pinhole 12, it is necessary to suppress incidence of the electrons scattered from the region other than the target region 6′ on the electron detector 13′.
There are, however, problems that the spherical aberration corrector that corrects the spherical aberration of the lens 11 is an expensive part and scattering angles of the electrons that can be corrected are limited. The confocal microscope is capable of measuring compositional contrast as a high angle annular dark field (HAADF) image by detecting electrons scattered at angles of 80 mrad or higher and has an improved depth resolution. Thus, there is a demand for a scattered electron detection system that is capable of detecting electrons scattered at high angles without being affected by a spherical aberration of an electron lens.
First Embodiment
The transmission electron microscope illustrated in
The irradiation-side annular aperture 14 has a ring-shaped slit formed between a circular hole portion 14a and a concentric circular shielding plate 14b located on the inner side of the hole portion 14a. The shielding plate 14b is held by a plurality of thin holding portions (not illustrated) on the inner side of the hole portion 14. The hole portion 14a and the shielding plate 14b are arranged so that an optical axis of the electron beam 2 extends substantially through the center of the hole portion 14a and the center of the shielding plate 14b. An inner diameter of the hole portion 14a is smaller than the diameter of the electron beam at the position of the irradiation-side annular aperture 14. A part of the electron beam 2 emitted by the electron gun 1 propagates near the optical axis and is shielded by the shielding plate 14b. The inner and outer diameters of the electron beam 2 are limited by the hole portion 14a and the shielding plate 14b so that the electron beam 2 is formed in a hollow shape. The electron beam 2 that passes through the irradiation-side annular aperture 14 is focused on a target region 6 of the sample 5 by the focusing lens 4 so that the electron beam 2 formed in a hollow cone shape is incident on the target region 6 at an irradiation angle α(0°<α<90°) and the target region 6 is irradiated with the electron beam 2. For example, when a plurality of focusing lenses 4 are arranged by combining a dual stage lens system with an objective lens as generally applied to a TEM, the focusing of the electron beam 2 is improved. In addition, the irradiation angle α of the electron beam 2 can be changed by moving up and down the irradiation-side annular aperture 14.
The first detection-side annular aperture 15 has a ring-shaped slit in a similar manner to the irradiation-side annular aperture 14 and limits inner and outer diameters of a transmission region of electrons scattered from the sample 5. The diameter of the slit of the first detection-side annular aperture 15 and the position of the first detection-side annular aperture 15 in the optical axis direction are adjusted so that the slit of the first detection-side annular aperture 15 matches a path of target electrons 8 scattered from the target region 6.
The second detection-side annular aperture 16 has a ring-shaped slit in a similar manner to the annular apertures 14 and 15 and limits inner and outer diameters of a transmission region of scattered electrons that have passed through the first detection-side annular aperture 15. The diameter of the slit of the second detection-side annular aperture 16 and the position of the second detection-side annular aperture 16 in the optical axis direction are adjusted so that the slit of the second detection-side annular aperture 16 matches a path of the target electrons scattered from the target region 6. Thus, the diameter of the slit of the second detection-side annular aperture 16 is larger than the slit of the first detection-side annular aperture 15.
The micromotion mechanisms 17 to 19 are driving systems that each use at least one of a motor and a piezoelectric element. The micromotion mechanisms 17 to 19 move the annular apertures 14 to 16 in the optical axis direction (Z direction) and planar directions (X and Y directions) that are perpendicular to the optical axis direction. The sample 5 can be moved in the planar directions and the optical axis direction by a sample stage (not illustrated) that uses at least one of a motor and a piezoelectric element. In order to acquire an image to be observed, the sample 5 is moved (scanned) relative to the focal point region of the electron beam 2 in the planar directions and the optical axis direction. Then, the image to be observed is acquired, while information of the position of the sample stage is linked with information of detected scattered electrons. The linking is controlled by the control device 20.
In order to actually acquire the image to be observed, it is preferable to match a target point of an irradiation system for the electron beam or the position of the focal point with a target point of a detection system for scattered electrons on an atomic size level. Thus, it is necessary to adjust in detail a current to be applied to the focusing lens 4 and the positions of the annular apertures 14 to 16. A resolution of the transmission electron microscope according to the present embodiment is determined on the basis of an initial setting of the current to be applied to the focusing lens 4 and initial settings of the positions of the annular apertures 14 to 16.
In the present embodiment, a standard sample that is used to appropriately set those conditions is prepared. Examples of the configuration of the standard sample are illustrated in
A standard sample 50a illustrated in
A standard sample 50b illustrated in
A standard sample 50c illustrated in
Next, the initial adjustments of the positions of the annular apertures 14 to 16 and the initial adjustment of the current to be applied to the focusing lens 4 are described.
The adjustment of the position of the irradiation-side annular aperture 14 is described with reference to
In order to adjust the position of the irradiation-side annular aperture 14, the electron beam 2 that is emitted by the electron gun 1 is focused by the focusing lens 4 so that a crossover (focal point) is formed, while the sample and the detection-side annular apertures 15 and 16 are not arranged as illustrated in
When the adjustment of the position of the irradiation-side annular aperture 14 is completed, the focusing lens 4 is adjusted. When the focusing lens 4 has astigmatism, and the slit of the irradiation-side annular aperture 14 is actually a true circle, the slit image 28 that exists on the detected electron image 26 is not a true circle. In this case, the astigmatism of the focusing lens 4 is corrected by an astigmatism adjusting mechanism (not illustrated) so that the slit image 28 becomes a true circle, while the detected electron image 26 is viewed.
Next, the adjustment of the position of the first detection-side annular aperture 15 is described with reference to
In order to adjust the position of the first detection-side annular aperture 15, the sample stage (not illustrated) is driven so that the focal point of the focusing lens 4 is located on the scattered wave generating portion 25 of the standard sample 50. Then, the scattered wave generating portion 25 is irradiated with the electron beam 2 so that a large amount of scattered waves are generated. Thus, the detected electron image 26 is wholly light. In this state, the micromotion mechanism 18 is driven so that the first detection-side annular aperture 15 is inserted between the standard sample 50 and the electron detector 13 (refer to
After that, the sample stage (not illustrated) is driven so that the target 21 of the standard sample 50 matches the crossover or the focal point of the focusing lens 4. In this procedure, the standard sample 50 is scanned on the sample stage and an electron beam that is scattered from the standard sample 50 at a high scattering angle passes through the slit of the detection-side annular aperture 15 and is detected by the electron detector 13. In this manner, a scanning transmission electron microscope image is acquired. The target 21 is matched with the focal point while the electron microscope image is viewed. First, during the adjustment of the vertical position of the sample, when the vertical position of the target 21 matches the focal point, the sharpest two-dimensional image can be acquired. Thus, the sample 50 is moved and the vertical position of the target 21 is adjusted so that the two-dimensional image is sharpest. The target 21 is made up of the atom that is heavier than each of the atoms that form the holding portion 22. Next, the position of the sample in the horizontal direction is adjusted. When the target 21 matches the focal point during the adjustment of the position of the sample in the horizontal direction, the intensity of a detected signal of a scattered electron is highest. Thus, while the scattered electron signal that is detected by the electron detector 13 is monitored, the standard sample 50 is moved to a position so that the intensity of the detected signal is highest. Thus, the target 21 matches the focal point.
Lastly, the adjustment of the position of the second detection-side annular aperture 16 is described with reference to
In order to adjust the position of the second detection-side annular aperture 16, the micromotion mechanism 19 is driven so that the second detection-side annular aperture 16 is inserted between the first detection-side annular aperture 15 and the electron detector 13 as illustrated in
The adjustments are completely performed for the observation through the aforementioned procedures. Information of the setting of the current to be applied to the focusing lens 4 and the settings of the positions of the annular apertures 14 to 16 is stored in a storage unit of the control device 20 or an external memory. In order to perform the next adjustments, fine adjustments are performed on the basis of the stored setting information. Thus, operations of preparing an observation can be efficiently performed.
As illustrated in
The procedures for controlling the device can be manually performed. It is considered that the procedures for controlling the device are automatically performed by the control device 20. Control procedures of the control device 20 when the device is automatically controlled are described below.
<Positioning 34 of Irradiation-Side Annular Aperture 14>
In the procedures, the control device 20 controls the micromotion mechanism 17 in accordance with stored information (or separately set positional information) of a previously set position of the irradiation-side annular aperture 14 so as to insert the irradiation-side annular aperture 14 between the electron gun 1 and the focusing lens 4, causes the micromotion mechanism 17 to move up and down the irradiation-side annular aperture 14, and determines a vertical position of the irradiation-side annular aperture 14 so that the slit image 28 is sharpest. In this case, the vertical position that causes the contrast of the slit image 28 to be highest is selected, for example. Next, the control device 20 drives the micromotion mechanism 17 and causes the micromotion mechanism 17 to move the irradiation-side annular aperture 14 in the horizontal direction on the basis of the acquired detected electron image 26 so that the center of the slit image 28 matches the original point of the guide lines 27.
<Astigmatism Correction 35 of Focusing Lens 4>
In the procedure of correcting the astigmatism, the control device 20 instructs the astigmatism adjusting mechanism (not illustrated) to correct the astigmatism of the focusing lens 4 so that the slit image 28 that exists on the detected electron image 26 becomes a true circle.
<Positioning 36 of First Detection-Side Annular Aperture 15>
In order to adjust the position of the first detection-side annular aperture 15, the control device 20 drives the sample stage (not illustrated) in accordance with stored information (or separately set positional information) of a previously set position of the standard sample 50 so as to position the focal point of the focusing lens 4 on the scattered wave generating portion 25 of the standard sample 50, and causes the scattered wave generating portion 25 to be irradiated with the electron beam 2 so that a large amount of scattered waves are generated. In addition, the control device 20 drives the micromotion mechanism 18 and causes the micromotion mechanism 18 to insert the first detection-side annular aperture 15 between the standard sample 50 and the electron detector 13 in accordance with stored information (or separately set positional information) of a previously set position of the first detection-side annular aperture 15. After that, the control device 20 adjusts a vertical position of the first detection-side annular aperture 15 on the basis of the detected electron image 26 so that the slit image 30 is sharpest. Then, the control device 20 drives the micromotion mechanism 18 and causes the micromotion mechanism 18 to move the first detection-side annular aperture 15 in the horizontal direction so that the center of the slit image 28 matches the original point of the guide lines 27.
<Positioning 37 of Standard Sample 50>
In order to adjust the position of the standard sample 50, the control device 20 causes, on the basis of a two-dimensional or three-dimensional scanning transmission electron microscope image obtained by scanning the sample stage, the standard sample 50 to move to a position from which a signal of a scattered electron with the highest intensity is detected so that the standard sample 50 is located at a vertical position that causes the contrast of the slit image included in the microscope image to be highest.
<Positioning 38 of Second Detection-Side Annular Aperture 16>
In order to adjust the position of the second detection-side annular aperture 16, the control device 20 drives the micromotion mechanism 19 and causes the micromotion mechanism 19 to insert the second detection-side annular aperture 16 between the first detection-side annular aperture 15 and the electron detector 13 in accordance with stored information (or information of a position geometrically calculated on the basis of information of the position of the first detection-side annular aperture 15 and information of the position of the standard sample 50) of a previously set position of the second detection-side annular aperture 16. Then, the control device 20 causes the micromotion mechanism 19 to slightly move the second detection-side annular aperture 16 from the position between the first detection-side annular aperture 15 and the electron detector 13 to a position from which a scattered electron with the highest intensity is detected.
When the aforementioned procedures are programmed and stored in the storage unit of the control device 20, the control device 20 can automatically control the device.
Next, operations and effects of the transmission electron microscope that has the aforementioned configuration are described.
For example, referring to
According to the present embodiment, since the two detection-side annular apertures 15 and 16 are arranged in the detection system, an electron (noise) that is scattered from a region other than the target region 6 of the sample 5 can be blocked by any of the detection-side annular apertures 15 and 16, and only the target scattered electrons 8 can reach the electron detector 13. In the present embodiment, only the detection-side annular apertures 15 and 16 are arranged between the sample 5 and the electron detector 13. Thus, an electron lens for the detection system can be omitted by simply arranging the two detection-side annular apertures 15 and 16. A spherical aberration corrector for correcting a spherical aberration of the electron lens is not necessary. In addition, an electron that is scattered at any scattering angle can be detected by arbitrarily designing the inner diameters R1 and R2 of the detection-side annular apertures 15 and 16, the distances Z1 and Z2 between the sample 5 and the detection-side annular apertures 15 and 16, and the area of the electron detector 13. Thus, an electron that is scattered at a high scattering angle of, for example, 80 mrad or higher can be easily detected, and a high depth resolution can be ensured.
According to the present embodiment, it is possible to detect electrons scattered at high angles and improve the depth resolution without a limitation caused by the spherical aberration of the electron lens.
In the present embodiment, the irradiation-side annular aperture 14 is arranged in the irradiation system and the sample is irradiated with the electron beam 2 formed in the hollow cone shape. Thus, an unnecessary electron beam that is located at a central part of the electron beam 2 can be blocked. The focused electron beam that contributes to the depth resolution is incident on the sample 5 at the high irradiation angle so that the sample 5 can be irradiated only with the focused electron beam. Since the unnecessary electron beam is blocked, and the focused electron beam is incident on the sample at the high irradiation angle so that the sample can be efficiently irradiated with the focused electron beam, the focal depth can be small and the depth resolution can be improved. In this manner, the single point can be irradiated only with an electron at a specific high irradiation angle. While the detection system efficiently detects only the target scattered electrons 8, the depth resolution can be improved.
The electron lens is arranged as the focusing lens 4 in the irradiation system. Thus, the focal depth is large due to an influence of the spherical aberration, or a focal point of an electron beam that passes through a central portion of the lens is shifted from a focal point of an electron beam that passes through an outer circumferential portion of the lens. This causes a reduction in the depth resolution. In the present embodiment, however, the influence of the spherical aberration of the focusing lens 4 can be suppressed by blocking the unnecessary electron beam located at the central part of the electron beam 2 and focusing only the electron beam that has passed through the outer circumferential portion of the lens. This contributes to the increase in the depth resolution. In addition, damage of the sample 5 due to the electron beam can be reduced by blocking the unnecessary electron beam located at the central part of the electron beam 2.
In a general tomography observation in which a three-dimensional electron microscope is used to observe a thin film sample, the sample is largely inclined. Thus, a visually estimated thickness of the sample is large and it is difficult for an electron beam to pass through the sample. It is, therefore, difficult to accurately, three-dimensionally observe the sample. Thus, in order for an electron beam to be incident on the sample at an irradiation angle that is as large as possible, to irradiate the sample with the electron beam, and to cause the electron beam pass through the sample, the sample is formed in a needle shape, has a diameter of approximately 200 nm, and is observed while being rotated. In this case, however, a region that can be three-dimensionally observed is physically limited to a range of approximately 200 nm. On the other hand, the thin film sample can be applied to the present embodiment. Thus, a wide range can be three-dimensionally observed in the present embodiment, compared with the conventional technique.
The present embodiment describes the case in which the two detection-side annular apertures 15 and 16 are arranged in the detection system. In the present embodiment, however, three or more detection-side annular apertures may be arranged when necessary.
Second Embodiment
A second embodiment of the present invention is described with reference to
The present embodiment is an example in which the second detection-side annular aperture 16 described in the first embodiment is omitted and an electron detector 39 that has an annular light receiving surface corresponding to the slit of the second detection-side annular aperture 16 is used instead of the electron detector 13.
A transmission electron microscope according to the present embodiment includes the electron gun 1, the irradiation-side annular aperture 14, the focusing lens 4, the electron detector 39 and the detection-side annular aperture 15. The electron gun 1 irradiates the sample 5 with the electron beam 2. The irradiation-side annular aperture 14 is located between the electron gun 1 and the sample 5. The focusing lens 4 is located between the irradiation-side annular aperture 14 and the sample 5. The electron detector 39 detects electrons that have passed through the sample 5 and have been scattered. The detection-side annular aperture 15 is located between the electron detector 39 and the sample 5 and has a ring-shaped slit that limits inner and outer diameters of a transmission region of electrons scattered from the sample. In addition, the transmission electron microscope according to the present embodiment also includes the control device 20 and the micromotion mechanisms (micromotion mechanisms 17 to 19 described in the first embodiment) that move the irradiation-side annular aperture 14, the detection-side annular aperture 15 and the electron detector 39 in the optical axis direction (Z direction) of the electron gun 1 and the planar directions (X and Y directions) that are perpendicular to the optical axis direction, although the micromotion mechanisms and the control device 20 are not illustrated in
In the present embodiment, only the single detection-side annular aperture 15 is arranged in a detection system. Thus, if the electron detector 13 that has a large light receiving surface were used in the present embodiment, scattered electrons other than the target scattered electrons 8 would be easily detected as noise. In the present embodiment, however, the electron detector 39 that has the annular light receiving surface is used instead of the electron detector 13. Thus, even when a scattered electron other than the target scattered electrons 8 passes through the detection-side annular aperture 15, the light receiving surface does not exist on a path of the interested scattered electron and noise is not detected. Thus, effects that are the same as or similar to the effects described in the first embodiment can be obtained.
Number | Date | Country | Kind |
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2009-277305 | Dec 2009 | JP | national |
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/JP2010/071810 | 12/6/2010 | WO | 00 | 5/15/2012 |
Publishing Document | Publishing Date | Country | Kind |
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WO2011/071008 | 6/16/2011 | WO | A |
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Number | Date | Country | |
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20120235035 A1 | Sep 2012 | US |