SCANNING ELECTRON MICROSCOPE AND IMAGE PROCESSING APPARATUS
20190035597 ยท 2019-01-31
Inventors
- Thantip KRASIENAPIBAL (Tokyo, JP)
- Yasuhiro Shirasaki (Tokyo, JP)
- Momoyo ENYAMA (Tokyo, JP)
- Sayaka KURATA (Tokyo, JP)
Cpc classification
H01J37/244
ELECTRICITY
G06V10/25
PHYSICS
H01J37/20
ELECTRICITY
International classification
H01J37/22
ELECTRICITY
H01J37/244
ELECTRICITY
H01J37/20
ELECTRICITY
Abstract
In this invention, information of material composition, process conditions and candidates of crystal structure either known or imported from material database is used to determine sample stage tilt angle and working distance (WD). Under these determined tilt angle and WD, the intensity of the electrons emitted at different angles and with different energies is measured using a scanning electron microscope (SEM) system comprising: a use of materials database containing materials composition, formation process, crystal structure and its electron yield; a sample stage that is able to move, rotate and tilt; an processing section for calculating optimum working distance for an observation from material database and measurement condition; means for acquiring an image of crystal information of a desired area of a sample based on an image obtained from SEM observation.
Claims
1. A scanning electron microscope (SEM) comprising: a sample stage for mounting a sample; a detector for detecting an electron emitted from the sample; an SEM control section for controlling a distance between the sample stage and the detector; a memory, which stores: a material database storing a plurality of datasets comprising information associated with a material, information of a crystal structure of the material, and information of an electron emitted from the material; and first relationship between the information of electron emitted from the material, the distance, and a signal detected by the detector.
2. The system of claim 1, wherein the SEM control section calculates the distance between the sample stage and the detector based on the first relationship and the material database.
3. The system of claim 2, wherein the SEM control section calculates the distance having maximum length that provides the signal greater than a predetermined threshold value.
4. The system of claim 2, wherein the information associated with the material includes at least material composition information and formation process information, and, the crystal structure information includes phase information.
5. The system of claim 4, wherein the information of the crystal structure includes phase information and orientation information.
6. The system of claim 5, wherein the information of the electron emitted from the material is an electron yield which is defined as a number of electrons emitted from the material per incident electron.
7. The system of claim 6, wherein the first relationship includes a condition parameter of the SEM comprising at least one of probe current of the SEM measurement and gain of the detector.
8. The system of claim 1, further comprising: a user terminal to receive input specifying a desired resolution for crystal orientation discrimination, wherein the SEM control section controls an angle between the sample stage and the detector, wherein the SEM control section comprises means to continuously acquire SEM images, and wherein the memory contains a second relationship which defines a relationship between the resolution and the angle, to calculate the angles at which the measurements are made.
9. The system of claim 8, wherein the SEM control section comprises means for image processing with overlaying of more than one image; and for determining a region of interest (ROI).
10. The system of claim 8, wherein the SEM control section comprises means for optimizing the distance between the sample stage and the detector using the first relationship, the materials database, and the angle between the sample stage and the detector.
11. The system of claim 8, wherein the acquiring means is configured to perform at least one of tilting and rotating a stage for more than three conditions of tilt.
12. An image processing apparatus comprising: an operation interface; a processing section for processing an-image data obtained from the operation interface; and a data storage section which stores a material database and a plurality of signal values according to the first relationship, wherein the material database comprises a plurality of datasets, each said dataset comprising information associated with a material, information of a crystal structure of the material, and information of an electron emitted from the material, the first relationship indicates a relationship between the information of electron emitted from the material, and a signal detected by a detector, the processing section selects one dataset among the material database based on input data received from the operation interface, the processing section calculates brightness information of the crystal structure of the material based on the selected dataset and the first relationship, the processing section recognizes a region of interest (ROI) in the image data, and the processing section determines the crystal structure of the ROI based on the image data and the brightness information.
13. The apparatus of claim 12, wherein the information of the crystal structure includes at least two phases, and the information of the electron emitted from the material includes an electron yield of each phase.
14. The apparatus of claim 12, wherein the information associated with the material includes at least one of material composition information and formation process information, and wherein the processing section is configured to accept the input data including at least one of a known material composition information and a known formation process information.
15. The apparatus of claim 12, wherein the operation interface displays the image data and a crystal phase map with colored or filling patterned for each ROI based on the determined crystal structure.
Description
BRIEF DESCRIPTION OF DRAWINGS
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DESCRIPTION OF EMBODIMENTS
[0033] Hereinafter, an embodiment of this invention is described with reference to the accompanying drawings. It should be noted that this embodiment is merely an example to realize this invention and is not to limit the technical scope of this invention.
[0034] In the following embodiments, SEM measurement conditions such as acceleration voltage and information of material composition, process conditions, and candidates of crystal structure either known or imported from material database are used to determine the optimal sample stage tilt angle and working distance (WD). Under these determined tilt angle and WD, crystal phase and orientation of a sample can be analyzed, resulting in fast acquisition of crystal phase and orientation maps.
[0035] One embodiment explained below is a scanning electron microscope (SEM) system comprising: a use of materials database containing materials composition, formation process, crystal structure and its electron yield; a sample stage that is able to move, rotate and tilt; a processing section for calculating optimum working distance for an observation from material database and measurement condition; means for acquiring an image of crystal information of a desired area of a sample based on an image obtained from SEM observation.
First Embodiment
[0036] The first embodiment is explained using
[0037]
[0038] Firstly, configuration of an SEM in
[0039] An acquisition method of an SEM image or SEM observation for this embodiment will be explained with reference to
[0040] Although it is not shown, there are components other than the control system and the circuit system such as that arranged in vacuum chamber and operation section of vacuum evacuation. In addition, in the present embodiment, the detector 105 is placed between electron gun 101 and scanning coils 103, but the position arrangement could be changed.
[0041] From here, the present embodiment describing crystal phase discrimination of a sample that is known to have two different phases, one phase with single orientation and one phase with multi orientation, is explained. We define crystal phase discrimination to mean the ability to distinguish one crystal phase from another.
[0042]
[0043]
[0044]
[0045]
[0046] The amount of electron that is detected by the detector 106 can be calculated from equation (1) where signal is the amount of emission electron 113 detected at detector 106, Ip is probe current of primary electron 102, yield is the electron yield defined as the average number of electrons the sample 107 emits per incident primary electron 102, f.sub.1(WD) is a function of WD and f.sub.2(G) is a function of detector gain.
signal=Ipyieldf.sub.1(WD)f.sub.2(G) (1)
[0047]
[0048]
[0049]
[0050] The procedure to perform crystal phase discrimination is explained using a flow chart in
[0051] In step S1, the user input material composition and material process such as percentage of elements in the sample 107, formation temperature, formation pressure and quenching condition in the window 501 and window 502 in GUI 500. In general, the user has above basic information about the sample. In step S2, by using operation button 503 on GUI 500, the information such as crystal structure and secondary electron yield will be imported from material database.
[0052]
[0053] In step S3, candidates of crystal structure in the sample 107 according to the information input in S1 and information in S2 are suggested using processing section 111 and the result of candidates is shown in window 506 on GUI 500. If there are same conditions inputted by user in the material database 600, the processing section 111 selects the structure corresponding to the condition. If there is not same condition inputted by user in the material database 600, the processing section 111 suggests structure corresponding to the most similar condition. In this embodiment, the candidates are body center cubic (BCC) and face cubic center (FCC).
[0054] If the result of candidates is not preferred by the user, step S4 is performed. In step S4, the user can define the crystal structure using operation button 504. The defined structure will be listed in window 506. In window 505, the user can see the basic crystal information of each crystal structure listed in window 506. In this example, BCC is selected in window 506 and the basic crystal information of BCC appears in window 505 on GUI 500.
[0055] In step S5, the user uses the information in window 505 to finalize the crystal structures to be analyzed which is shown as a list in window 507. In this example, BCC and FCC are assumed to be present in the sample and, therefore, selected. After deciding the crystal structures to be analyzed, clicking the operation button 508 will lead to the next step GUI for analysis.
[0056]
[0057] The suggested measurement conditions which are shown when window 701 is popped-up are considered from most frequently used conditions to analyze SEM images for the subject materials which is generally known. For example, for a sample with SEY<1, the suggested probe current Ip is 10 nA for crystal analysis; for a sample with SEY>1, the suggested probe current Ip is 1 nA for crystal analysis. Other conditions such as acceleration voltage, type of detector are suggested in same way. These conditions should be prior installed in the data storage section 110. The default condition of lens current, which is related to focusing condition, is auto. Under the auto setting, the SEM control section 109 will calculate the lens current to focus primary electron beam onto the sample. The user also can input conditions in window 701 by themselves.
[0058] In step S6, the user determines measurement condition for SEM observation such as acceleration voltage of primary electron (V.sub.acc), type of detector, lens current and probe current using window 701 then uses operation button 706 to scan SEM image. The scanned SEM image shows in window 702. At this stage applied WD can be predetermined as a fixed value (for example medium length).
[0059] In step S7, the user determines field of view (FOV) for the analysis by observing window 702 and moving sample stage 108. When the FOV is determined, the analysis to determine the crystal phase of selected area starts by using operation button 707. Estimated WD is not applied at this step 7 because it is not necessary as long as SEM image can be scanned in order to determine FOV. If predetermined WD is needed, it shall be fixed with a value of a distance between sample surface and objective lens such as 15 mm, when detector 106 is inserted or 5 mm when detector 106 is not inserted.
[0060] In step S8, the processing section 111 calculate the optimum WD from equation (1) for the analysis and SEM system control section 109 control the position of sample stage 108 according to the optimum WD. The optimum WD which provides the signal greater than the minimum analyzable signal such as a signal with signal-to-noise ratio greater than 3, is calculated by using minimum yield among crystal phases that are being analyzed. For the calculation, Ip is obtained from user settings according to window 701. Yield is obtained by material database 600. f2(G) depends on the detector itself so it is prior installed in the data storage section 110.
[0061] The yield that will be used for calculation depends on type of detector and acceleration voltage (V.sub.acc) listed in window 701. In the case of
[0062] SEM observation is performed in step S9 with calculated WD. The obtained SEM image 702 is processed and analyzed in step S10.
[0063]
[0064] As explained above, the image brightness is estimated based on the value of signal calculated by equation (1) since the brightness is in proportion to the signal. For calculating signal of each phase, Ip, f1, and f2 in equation (1) are fixed based on the optical condition determined in window 701 by step S6. Yield for calculating brightness of each phase are selected from the data of material database 601 based on the crystal structures determined in step S5.
[0065] For example, when the user determined analyze crystal based on input data Fe 100%, T=950, P=2*10.sup.5, R.sub.quenc=30, Additive=Al in window 501 and 502, the material on second line of
[0066] In the example explained by
[0067]
[0068] In step S1002B, image brightness of the obtained SEM image 702 is measured resulting in the histogram of pixel brightness in window 704. In order to perform binary image method, brightness measurement of the average brightness of the pixels constituting each ROI in SEM image is performed. Image processing with binary image method is applied to a set of average brightness of the pixels constituting each ROI in SEM image by using binary threshold as average of image brightness of each crystal phase estimated using equation (1) by processing section 111 according to material database 600. The binary threshold is not limited to the method described here.
[0069] In step S1003B, crystal phase map is constructed. Using an operation button 708, information of crystal phase map such as average domain size and area of each crystal phase in SEM image 703 is analyzed and displayed in window 704. According to user's knowledge, the user can also adjust the binary threshold level that is the intensity level at which binary segregation is performed, manually using window 704 and re-analyzed the information in window 704 by using operation button 709.
[0070] With the embodiment described, fast crystal phase discrimination was performed. In this embodiment, detection of different electron emission angle was performed but it is not limited to detector 106 and emission electron 113. The detector 106 and emission electron 113 might be replaced by any emission electron detection system. In addition, the present embodiment mentioned changing WD by moving samples stage 108, but it is not limited. Changing WD also includes moving of detector 106 and others.
Second Embodiment
[0071] The present embodiment describing crystal orientation discrimination for extracting an average grain size of a sample that is known to have single crystal phase with multiple crystal orientations is explained. We define crystal orientation discrimination to mean the ability to distinguish one crystal orientation from another with the same phase. The second embodiment is described referring to
[0072] In contrast to the first embodiment, a crystal orientation dependent contrast within a phase is desired for crystal orientation discrimination. Since shorter WD generates a large contrast within a phase as a result of channeling contrast, according to measurement condition such as type of materials, electron yield and probe current the WD is prior determined. Since the signal is known to decrease when WD becomes too short as shown in f.sub.1(WD) 301, the shortest WD that gives signal greater than the minimum analyzable signal is calculated by using equation (1). For example, the minimum analyzable signal is determined as a signal that gives signal-to-noise ratio greater than 3.
[0073]
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[0075]
[0076] The amount of electron that is detected by the detector 106 depends on angle between primary electron beam and sample tilt angle. A change of relative image brightness of the ROIs shown in
[0077]
[0078] With the WD that is prior determined, a range of possible tilt angle might be less than 20 degree considered from the geometry of SEM at which none of crashing between physical bodies occurs during tilting. In this case, new WD that 20 degree range of possible tilt angle is satisfied is calculated and used for crystal orientation discrimination. Tilt condition is determined by range of possible tilt angle and acceptable angle of mis-orientation which is an angle between two different orientations to be analyzed as same orientation as shown in equation (2) where (n) tilt angle for a tilt condition is n.sup.th, .sub.range is a range of possible tilt angle and is acceptable angle of mis-orientation. The measurement of SEM images is performed for n conditions of at least one tilt and/or rotation axis according to the calculated tilt angle.
[0079]
[0080] In step S12, after determine FOV in step S7, user inputs acceptable mis-orientation in window 1206 on GUI 1200 and click an operation button 707. In step S13, the processing section 111 calculates the minimum WD according to equation (1) that yields SN greater than 3. Then, the processing section 111 calculate tilt conditions according to equation (2) and re-calculate or determine WD that satisfied the tilt conditions by considering the geometry such as sample size, sample height and position of physical bodies in SEM. The analysis and SEM system control section 109 controls the position of sample stage 108 according to the calculated WD and tilt conditions. In step 14, SEM observation is performed for all tilt conditions determined in step S13. Since the crystal orientation can exist in a sample with 3-dimensional rotation, SEM images of at least 3 tilt conditions such as 3 tilt conditions of zero tilt angle and a tilt angle at two different tilt axis, are observed.
[0081] After click an operation button 1201, the obtained SEM images are processed and analyzed in step S15 with the details showing
Third Embodiment
[0082] The present embodiment describes crystal analysis of a sample that only its composition and material process are known. The third embodiment is described referring to
[0083] The crystal analysis in the present embodiment contains both crystal phase discrimination and crystal orientation discrimination for extracting an average grain size of a sample. For crystal analysis of a sample that only its composition and material process are known, material database 600 which is used in step S2 is important to match crystal candidates and information input in step S1. The finalized crystal structure to be analyzed which is shown as a list in window 507 may contains only one or more than one crystal phases. If there is only one crystal structure to be analyzed, the process will follow the steps in
[0084]
Fourth Embodiment
[0085] The present embodiment describes a method for extracting distribution of orientations that exists in a sample. With a sample that is known to have single crystal phase with multi-orientations, a fast screening of how a sample is oriented can be performed. A scanning electron microscope (SEM) and method to acquire SEM image referring to
[0086] The processes of crystal orientation discrimination will be the same as described in the second embodiment. Here, the ROI is defined as a grain domain according to the result of analysis described in the second embodiment. The distribution of orientations that exists in a sample can be extracted by using an operation button 1205. After using operation button 1205, brightness measurement of the average brightness of each ROIs at all tilt conditions is performed by analyzing section 111. The dependence of the average brightness of each ROIs on tilt conditions such as that shown in
BRIEF DESCRIPTION OF SYMBOLS
[0087] 101 electron gun
[0088] 102 primary electron
[0089] 103 scanning coil
[0090] 104 objective
[0091] 105 detector
[0092] 106 detector
[0093] 107, 107A, 107B sample
[0094] 108, 108A, 108B sample stage
[0095] 109 SEM system control section
[0096] 110 data storage section
[0097] 111 processing section
[0098] 112 emitted electron
[0099] 113 emitted electron
[0100] 114 operation interface
[0101] 500 GUI window
[0102] 501 window
[0103] 502 window
[0104] 503 operation button
[0105] 504 operation button
[0106] 505 window
[0107] 506 window
[0108] 507 window
[0109] 508 operation button
[0110] 509 operation button
[0111] 511 operation button
[0112] 600 database
[0113] 700 window
[0114] 701 window
[0115] 702 window
[0116] 703 window
[0117] 704 window
[0118] 705 operation button
[0119] 706 operation button
[0120] 707 operation button
[0121] 708 operation button
[0122] 709 operation button
[0123] 1200 window
[0124] 1201 operation button
[0125] 1202 window
[0126] 1203 window
[0127] 1204 window
[0128] 1205 operation button
[0129] 1206 window