JP5135941B2 - Elemental analysis apparatus and method - Google Patents

Description

  The present invention relates to an element analyzer for measuring the position and time of flight of an element by applying an electric field to a sample which is a three-dimensional structure and utilizing the phenomenon of element detachment from the sample due to the electric field. It relates to the elemental analysis method.

  A field ion microscope (FIM) introduces an inert gas such as helium or neon into a lens body and applies a high electric field to a sample whose tip is processed into a needle shape having a length of about 100 nm. The inert gas is ionized on the sample surface, and this inert gas ion is detected by a microchannel plate and a fluorescent plate, whereby the surface of the needle-like sample can be observed.

  The atom probe device (Atom Probe) is a FIM equipped with a time-of-flight mass analyzer. By applying a high electric field to a needle-shaped sample and evaporating atoms, the elements that make up the sample can be determined. It is a local analyzer that can be identified. Recently, a three-dimensional atom probe device (hereinafter abbreviated as 3DAP) has been developed that uses a position-sensitive mass analyzer as a mass analyzer to specify the position along with the mass of an atom. .

  In order to perform elemental analysis by 3DAP, a high electric field sufficient to evaporate atoms from a needle-shaped sample is applied between the sample and the extraction electrode, and atoms are evaporated one by one from the sample surface. The position and flight time of atoms (ions) detached from the sample are measured by a position sensitive detector and a timer. As a result, the type of the detached element is identified from the electric field applied to the sample and the flight time of the atoms. By continuously executing this and accumulating measurement data, the constituent elements on the outermost surface of the sample can be two-dimensionally mapped with atomic level resolution. By giving coordinates in the depth direction to this two-dimensional mapping and reconstructing it in three dimensions, the composition and structure of the sample can be observed three-dimensionally.

    At the time of preparing a sample for performing elemental analysis by 3DAP, preliminary observation of the sample is performed using an electron microscope such as a transmission electron microscope. Such preliminary observation is also performed to confirm the state of the sample before or during elemental analysis by 3DAP, and is used to correct the scale during 3D reconstruction and to compensate for the lack of detection efficiency. Is done. Preliminary observation involves attaching and detaching the sample to and from the transmission electron microscope. Particularly, attaching and detaching the sample during elemental analysis by 3DAP is an obstacle to high-precision elemental analysis. . For this reason, an elemental analyzer that does not require these operations has been proposed by the same applicant as the present invention (Japanese Patent Application No. 2006-77482).

  Japanese Patent Application No. 2006-77482 is unpublished at the time of the filing of the application and is not a literature-known invention, but forms the basis of the present invention. In Japanese Patent Application No. 2006-77482, an element analysis mechanism that applies an electric field to a sample that is a three-dimensional structure and measures the position and time of flight of the detached element by utilizing the phenomenon of element detachment from the sample by the electric field, There has been proposed a complex elemental analysis device mounted on an electron microscope mechanism for observing a sample. With this configuration, it is possible to perform preliminary observation and elemental analysis of the sample without requiring the operation of attaching and removing the sample from the electron microscope.

  On the other hand, Non-Patent Document 1 discloses a sample holder capable of rotating a sample 360 degrees in a transmission electron microscope. It is possible to evaluate a three-dimensional shape from a two-dimensional transmission electron microscope image by extracting and fixing a small sample of about 10 μm square including the analysis part and observing the sample prepared in a columnar shape from various angles. It is described that it is possible.

FIB microsampling | DRAM observation example ", [online], Hitachi High-Technologies Corporation, [searched on March 12, 1999], Internet <URL: http://www.hitachi-hitec.com/em/fib /fibmicro.html>

The composite elemental analyzer of Japanese Patent Application No. 2006-77482 can perform sample observation with an electron microscope and elemental analysis with 3DAP without requiring sample mounting and removal operations.
In order to accurately grasp the state of a sample from an electron microscope image that is two-dimensional information photographed before or during elemental analysis by 3DAP, the electron microscope image and 3DAP three-dimensional information must be accurately associated with each other. Don't be. As shown in Japanese Patent Application No. 2006-77482, when the function of 3DAP is completely fixed in the electron microscope, the optimal positions for both the electron microscope mechanism and the 3DAP mechanism (the three axes of X axis, Y axis, and Z axis) (Direction) and angle (around three axes of X, Y, and Z axes) must be adjusted by the sample holder. Even in the prior art, it is possible to provide a two-axis tilted sample holder having five degrees of freedom. However, since the space around the sample is limited in the electron microscope, it is difficult to provide a sample holder having six degrees of freedom of position (three-axis direction) and angle (around three axes). In the complex elemental analyzer of 2006-77482, it is impossible to adjust the sample to the optimum position and angle for both the electron microscope mechanism and the 3DAP mechanism.

  The present invention has been made in view of the above problems, and in a complex elemental analysis apparatus in which an elemental analysis mechanism of a sample is mounted on a microscope mechanism for observing the sample, the sample is divided into a microscope mechanism and an elemental analysis mechanism. Easy and accurate adjustment to the optimal position and angle for both of them, and the microscopic image and the 3D information of the elemental analysis mechanism correspond to each other accurately to easily correct the lack of scale and detection efficiency during 3D reconstruction. It is an object of the present invention to provide an elemental analysis apparatus and method that enable highly accurate elemental analysis.

The elemental analysis apparatus of the present invention is installed so as to face the sample, a sample installation part where the sample is installed, a power source for applying an electric field to the sample installed in the sample installation part, An element analysis mechanism having an element detection unit for detecting an element detached from the sample, and a microscope mechanism for observing the sample installed in the sample installation unit, wherein the sample installation unit has an X-axis direction, Y The first moving unit that performs each parallel movement in the axial direction and the Z-axis direction, and each rotational movement about the X-axis and the Y-axis, and the light of the microscope mechanism that coincides with the Z-axis of the element detection unit And a second moving unit that performs rotational movement about the axis .

  The elemental analysis method of the present invention includes an element detection mechanism that applies an electric field to a sample installed in a sample installation unit and detects an element separated from the sample by an element detection unit, and the sample installed in the sample installation unit An elemental analysis method using an elemental analysis apparatus comprising: a microscope mechanism for observing the light source, wherein the sample has an optical axis based on observation by a scanning transmission electron microscope (or scanning electron microscope) by the microscope mechanism. A step of calculating a displacement angle between the sample and the element detection unit in a state adjusted to be in a plane perpendicular to the coincident Z axis, and rotating the element detection unit by the calculated displacement angle; Moving the element detection unit so that the direction of the element detection unit coincides with the direction of the sample.

  The program of the present invention is equipped with an element detection mechanism that applies an electric field to a sample installed in a sample installation unit and detects an element separated from the sample by an element detection unit, and the element detection mechanism. When performing an elemental analysis using an elemental analysis apparatus comprising a microscope mechanism for observing the sample installed in the installation unit, based on the observation by the microscope mechanism, the sample has a Z-axis that matches the optical axis. A step of calculating a displacement angle between the sample and the element detection unit in a state adjusted so as to be positioned in a vertical plane; and rotating the element detection unit by the calculated displacement angle, and And causing the computer to execute a step of causing the direction of the detection unit to coincide with the direction of the sample.

  According to the present invention, in a complex elemental analysis apparatus in which the elemental analysis mechanism of a sample is mounted on a microscope mechanism for observing the sample, the sample can be easily placed at an optimum position and angle for both the microscope mechanism and the elemental analysis mechanism. In addition, it is possible to accurately adjust, make the microscopic image and the three-dimensional information of the elemental analysis mechanism correspond exactly, and easily correct the lack of scale and detection efficiency at the time of three-dimensional reconstruction, and perform high-precision elemental analysis. Is possible.

-Basic outline of the present invention-
In the present invention, the function of performing each parallel movement in the X-axis direction, Y-axis direction, and Z-axis direction, and each rotational movement around the X-axis and the Y-axis on the sample-installing portion where the sample is installed (first In addition to adding a moving part), a function (second moving part) that rotates around the Z-axis that matches the optical axis in the microscope mechanism is added to the element detection part that detects the elements detached from the sample. To do. With this configuration, the first moving unit can adjust the sample (sample setting unit) to be positioned in a plane perpendicular to the optical axis of the microscope mechanism, and the second moving unit can adjust the sample (sample). Independently of the installation unit), the element detection unit is rotated in a plane perpendicular to the optical axis, and the direction of the element detection unit (for example, the normal direction with respect to the center of the element detection unit) is set to the direction of the sample ( For example, it can coincide with the longitudinal direction with reference to the needle-like tip of the sample. As a result, the sample is easily and accurately adjusted to the optimum position and angle for both the microscope mechanism and the elemental analysis mechanism, and the microscopic image and the three-dimensional information of the elemental analysis mechanism are accurately associated with each other during the three-dimensional reconstruction. It is possible to easily correct the lack of scale and detection efficiency, and to perform highly accurate elemental analysis.

  Further, an angle calculation unit that calculates a displacement angle between the sample and the element detection unit in a plane perpendicular to the Z-axis direction, and an element detection unit that rotates and moves the element detection unit by the displacement angle calculated by the angle calculation unit. And a movement control unit for driving the second moving unit so as to match the direction of the sample with the direction of the sample. With this configuration, position adjustment in the plane perpendicular to the optical axis by the second moving unit can be automatically performed, and highly accurate elemental analysis can be performed very easily and quickly.

-Preferred embodiment to which the present invention is applied-
DESCRIPTION OF EMBODIMENTS Hereinafter, preferred embodiments to which the present invention is applied will be described in detail with reference to the drawings.

(Configuration of elemental analyzer)
First, the configuration of the elemental analyzer according to the present embodiment will be described.
FIG. 1 is a schematic diagram showing a basic configuration of a 3DAP mechanism employed by the present invention.

  The 3DAP mechanism is installed so as to face the sample 11 in the chamber 1, the power source 2 for applying an electric field to the sample 11, the chamber 1 in which the needle-shaped sample 11 is disposed, A high DC bias voltage is applied between the position sensitive detector 3 which is an element detecting means for detecting an element detached from the sample 11 and the sample 11 in the chamber 1 to position sensitively remove atoms (ions) from the sample 11. A lead electrode 4 for sending to the mold detector 3, a gas introduction mechanism 5 for introducing a predetermined gas into the chamber 1 at a predetermined flow rate, a vacuum pump for bringing the chamber 1 into a desired vacuum state, and the like are included. An exhaust mechanism 6 and a timer 7 connected to the power source 2 and the position sensitive detector 3 are provided.

The power source 2 includes a high voltage power source unit 2a that applies a DC bias voltage between the sample 11 and the extraction electrode 4, and a pulse generator that applies a pulse voltage to the sample 11 in a state in which the DC bias voltage is applied by the high voltage power source unit 2a. 2b.
The power source 2 applies a high DC bias voltage between the sample 11 and the extraction electrode 4 using the high-voltage power source 2a when the element measuring device is in operation, and uses the pulse generator 2b when the timer 7 is started. A pulse voltage is applied to the sample 11 so as to cause field evaporation of the element. It is ideal that the field evaporation of one atom is caused by the application of a single pulse voltage. However, in order to avoid the unexpected situation in which a plurality of atoms are simultaneously evaporated by the application of a single pulse voltage, Then, the pulse voltage is adjusted so that field evaporation of one atom occurs by applying the pulse voltage 10 to 100 times. Note that field evaporation may be induced by a laser instead of a pulse voltage.

The position sensitive detector 3 has a planar element detection surface, and the position coordinates ((x ₁ , y ₁ ) to (x _n , y _n )) of atoms (ions) evaporated from the sample 11 by electric field evaporation. It has a function of displaying as a two-dimensional map. By using the field evaporation phenomenon, the two-dimensional map can be expanded in the depth direction of the sample 11 by performing field evaporation for each atomic layer from the surface of the sample 11 for each atomic layer. By storing the data of the two-dimensional map in a computer (not shown) and performing a predetermined calculation process, the atomic distribution of the sample 11 can be reconstructed three-dimensionally.

  The extraction electrode 4 is a hollow ring-shaped electrode, and is disposed in the vicinity of the sample 11 between the sample 11 and the position sensitive detector 3, and a DC bias voltage between the sample 11 and the power source 2. Is applied. When a pulse voltage is applied to the sample 11 by being superposed on a DC bias voltage by the power source 2, the field-evaporated atoms (ions) fly through the cavity of the extraction electrode 4 toward the position sensitive detector 3. .

  The timer 7 has a function of starting a pulse voltage applied to the sample 11 of the power source 2. The timer 7 further measures the time from when an element is released from the tip of the sample 11 by applying a pulse voltage until the atom (ion) reaches the position sensitive detector 3, that is, the flight time of the atom (ion). It also has a function to do.

  FIG. 2 is a schematic diagram showing a schematic configuration of the elemental analysis apparatus according to the present embodiment in which the 3DAP mechanism having the basic configuration of FIG. 1 is mounted on a transmission electron microscope (TEM). FIG. 3 is a schematic diagram showing an enlarged portion of the 3DAP mechanism mounted on the elemental analyzer of FIG. 2, and shows a state in a plane perpendicular to the optical axis of FIG.

  As shown in FIG. 2, this elemental analyzer is configured such that a 3DAP mechanism is mounted on an electron microscope mechanism. The electron microscope mechanism includes an electron gun 21 provided at the top, an acceleration tube 22 for accelerating an electron beam irradiated from the electron gun 21 in the irradiation direction (optical axis direction), an electron beam converging lens 23, 1, a sample chamber 24 in which the sample 11 to be analyzed by the electron microscope mechanism and the analysis target by the 3DAP mechanism is installed, an objective lens 25, and an intermediate lens. A lens 26, a projection lens 27, an STEM detector 28 for detecting an electron beam transmitted through the sample 11 and obtaining a scanning transmission electron microscope image (STEM image), and a transmission electron microscope image (TEM image) are observed. The CCD camera 29 is provided.

  The sample chamber 24 has the functions of the chamber 1 and the exhaust mechanism 6, and as shown in FIG. 3, a sample holder 31 having a sample setting portion 31a on which the needle-like sample 11 is placed and fixed, and a lead electrode And an extraction electrode holder 32 in which 4 is installed. Furthermore, the power source 2 connected to the sample holder 31 and the extraction electrode holder 32, the position sensitive detector 3 provided to face the sample 11 through the extraction electrode 4, and the position sensitive detector 3 are supported. The detector support 33 and the timer 7 are configured.

The sample holder 31 is supported by a holder stage 34. With respect to the sample placement portion 31a, each parallel movement in the X axis direction, the Y axis direction, and the Z axis direction, and each rotational movement around the X axis and the Y axis, The first moving unit 35 that can freely perform the above is provided. Here, “around the X axis” is when the axis P _X in the longitudinal direction of the sample 11 in the sample setting portion 31 a is the rotation axis, and “around the Y axis” is the axis P _Y in the longitudinal direction of the sample holder 31 is the rotation axis. It corresponds to the case. In the first moving unit 35, for example, it is rotatable about 360 ° around the X axis and ± 5 ° to 10 ° around the Y axis.

  By using the first moving unit 35, the sample setting unit 31a can be adjusted to be positioned at an optimum height in a plane perpendicular to the optical axis of the electron microscope mechanism. In addition, although the 1st moving part 35 is typically shown in the example of illustration, as the 1st moving part 35, bearing mechanisms, such as a guide mechanism and a bearing for performing said parallel movement and rotational movement, etc. are shown. Is provided.

The detector support unit 33 includes a second moving unit 36 that can freely rotate the position sensitive detector 3 around the Z axis that coincides with the optical axis P _Z in the electron microscope mechanism. In addition, although the 2nd moving part 36 is shown typically in the example of illustration, as the 2nd moving part 36, the rail mechanism etc. for performing said rotational movement are provided. The position-sensitive detector 3 is rotated and moved in a plane perpendicular to the optical axis P _Z by the second moving unit 36 independently of the sample 11 (sample setting unit 31a). (For example, the normal direction with respect to the center of the position sensitive detector 3) can be made to coincide with the direction of the sample 11 (for example, the longitudinal direction with reference to the needle tip of the sample 11).
The second moving unit 36 has, for example, a stepping motor built in the detector support unit 33, and the position sensitive detector 3 moves, for example, on the arc-shaped rail centered on the optical axis _PZ to the maximum. 14 cm (value when the flight distance of the atom (ion) (distance from the sample 11 to the position sensitive detector 3) is 40 cm) is moved by ± 10 ° in a plane perpendicular to the optical axis P _Z. It is installed so that it can rotate in range.

  Further, the detector support 33 is calculated by an angle calculator 37 for calculating a displacement angle between the sample 11 and the position sensitive detector 3 in a plane perpendicular to the optical axis direction, and the angle calculator 37. A controller 38 is provided for driving the second moving unit 36 so that the position sensitive detector 3 is rotated and moved by the displacement angle so that the direction of the position sensitive detector coincides with the direction of the sample 11. The control unit 38 also controls driving of a synchronization circuit 42 described later and operations of the power source 2, the gas introduction mechanism 5, the exhaust mechanism 6, the timer 7, and the like in the 3DAP mechanism. In FIG. 3, the power supply 2, the gas introduction mechanism 5, the exhaust mechanism 6, and the timer 7 are not shown.

  The angle calculation unit 37 is, for example, the direction of the basic position (0 degree) of the position sensitive detector 3 in the STEM image (the positional relationship between the scanning direction of the STEM image and the basic position is measured in advance). As a reference, the amount of angular deviation between the direction and the direction of the sample 11 is measured as a displacement angle. For example, it is configured as a program in a control computer of an electron microscope mechanism.

The extraction electrode holder 32 is supported by a holder stage 39, and the extraction electrode 4 can be freely rotated around the Z axis that coincides with the optical axis P _Z in the electron microscope mechanism. It has.
The third moving unit 41 further translates the extraction electrode 4 of the extraction electrode holder 32 in the X-axis direction, the Y-axis direction, and the Z-axis direction (X _E direction, Y _E direction, and Z _E direction). have. This mechanism finely adjusts the position of the extraction electrode 4 with respect to the sample 11 and the position sensitive detector 3. In the illustrated example, the third moving unit 41 is schematically shown. However, the third moving unit 41 includes, for example, a guide mechanism or a bearing mechanism such as a bearing for performing the above-described parallel movement and rotational movement. Is provided

Furthermore, a synchronizing circuit 42 connected to the second moving part 36 and the third moving part 41 is provided in the extraction electrode holder 32, for example.
The synchronizing circuit 42 synchronizes the rotational movement of the position sensitive detector 3 around the optical axis and the rotational movement of the extraction electrode 4 around the optical axis. By using this synchronization circuit 42, the movement control unit 38 is driven to simultaneously rotate and move the extraction electrode 4 together with the position sensitive detector 3 by the displacement angle calculated by the angle calculation unit 37, thereby detecting the position sensitive detector 3. And the direction of the extraction electrode 4 (for example, the normal direction with respect to the center of the annular shape of the extraction electrode 4) can coincide with the direction of the sample 11.

  When the control unit 38 rotates the extraction electrode 4, the synchronization circuit 42 causes the stepping motor of the second moving unit 36 to make the rotation angle of the extraction electrode 4 coincide with the rotation angle of the position sensitive detector 3. A pulse current is output, whereby the detector support 33 and the position sensitive detector move on a rail (not shown).

(Elemental analysis method)
Hereinafter, an elemental analysis method using the above-described elemental analysis apparatus will be described.
FIG. 4 is a flowchart showing the elemental analysis method according to this embodiment in the order of steps.

  The needle-like sample 11 immediately after being fixed to the sample setting part 31a of the sample holder 31 and being inserted into the sample chamber 24 has an electron microscope mechanism and a difference due to variations that occur when the sample 11 is produced or attached to the sample setting part 31a. There is no proper positional relationship with any of the 3DAP mechanisms. Therefore, using the first moving unit 35, each parallel movement of the sample holder 31 in the X-axis direction, the Y-axis direction, and the Z-axis direction and each rotational movement around the X-axis and the Y-axis are executed. The position and angle of the sample 11 are adjusted so that the structure of the analysis region of the sample 11 is clearly observed by the electron microscope mechanism, and the inclination of the sample 11 is located in a plane perpendicular to the electron beam irradiation direction. To do.

Specifically, first, the sample holder 31 is placed on the sample 11, and the state of the sample 11 is observed by the electron microscope mechanism (step S1).
Subsequently, it is confirmed whether or not the structure of the analysis region of the sample 11 is clearly observed by the electron microscope mechanism (step S2). If the structure of the analysis region of the sample 11 is clearly observed in step S2, the process proceeds to step S4. On the other hand, when it is not clearly observed, the first moving unit 35 is used to make the structure of the analysis region of the sample 11 clear so that the X-axis direction, the Y-axis direction, and the Z-axis of the sample holder 31 are clear. Each parallel movement in the axial direction and each rotational movement around the X axis and the Y axis are executed (step S3). Thereafter, step S1 is executed again.

  In step S4, it is confirmed whether the inclination of the sample 11 is located in a plane perpendicular to the electron beam irradiation direction. In step S4, when it is confirmed that the inclination of the sample 11 is located in a plane perpendicular to the electron beam irradiation direction, the process proceeds to step S5. On the other hand, if it is not confirmed that the sample holder 31 is located in a vertical plane, the process proceeds to step S3, where the sample holder 31 is placed so that the inclination of the sample 11 is located in a plane perpendicular to the electron beam irradiation direction. Each parallel movement in the X axis direction, the Y axis direction, and the Z axis direction, and each rotational movement around the X axis and the Y axis are executed.

After the STEM (scanning transmission electron microscope) observation of the sample 11 by the electron microscope mechanism in Step S5, based on the observation, the sample 11 is in a plane perpendicular to the Z axis that coincides with the optical axis P _Z in the electron microscope mechanism. In the state adjusted to be positioned, the angle calculation unit 37 calculates a displacement angle between the direction of the sample 11 and the direction of the position sensitive detector 3 (step S6).

  Subsequently, the control unit 38 drives the second moving unit 36 and the synchronizing circuit 42 to simultaneously rotate the position sensitive detector 3 and the extraction electrode 4 around the optical axis by the displacement angle calculated in step S5. Then, the directions of the position sensitive detector 3 and the extraction electrode 4 are made to coincide with the direction of the sample 11 (step S7). By this step S7, the sample 11 is easily and accurately adjusted to the optimum position and angle for both the electron microscope mechanism (the optical system thereof) and the 3DAP mechanism.

Subsequently, the sample 11 is observed using the 3DAP mechanism as the FIM (step S8).
Subsequently, based on step S8, the control unit 38 operates the gas introduction mechanism 5 to introduce an inert gas such as Ar or He into the sample chamber 24, and whether or not the intensity of the FIM image is maximum. Is confirmed (step S9). When the intensity of the FIM image is maximum, for example, as described above with reference to FIG. 1, the control unit 38 operates the power source 2, the timer 7, the exhaust mechanism 6, and the like to perform elemental analysis of the sample 11 by the 3DAP mechanism. Execute (Step S11). In step S11, the control unit 38 operates the power source 2, the gas introduction mechanism 5, the exhaust mechanism 6, the timer 7 and the like as described above to appropriately operate the 3DAP mechanism based on the structure analysis (length measurement) data by the electron microscope mechanism. The result of elemental analysis of the sample 11 is composed and output as final analysis data as appropriate.

On the other hand, when the intensity of the FIM image is not the maximum, the extraction electrode 4 of the extraction electrode holder 32 is moved in the X _E direction, the Y _E direction, and the third moving unit 41 so that the intensity of the FIM image is maximized. performing fine adjustment to translate appropriately to Z _E direction (step S10). Then, step S8 is performed again.

  As described above, according to the present embodiment, in the complex elemental analysis apparatus in which the 3DAP mechanism of the sample 11 is mounted on the electron microscope mechanism for observing the sample 11, the sample 11 is moved to the electron microscope mechanism and the 3DAP mechanism. Easy and accurate adjustment to the optimal position and angle for both of them, the electron microscope image and the 3D information of the 3DAP mechanism are accurately matched, and the lack of scale and detection efficiency during 3D reconstruction is easily corrected In addition, highly accurate elemental analysis can be performed.

(Other embodiments to which the present invention is applied)
Among the components constituting the elemental analysis apparatus according to the present embodiment described above, the functions of the angle calculation unit 37 and the control unit 38 shown in FIG. 3 are stored in the RAM or ROM of a computer that controls the electron microscope mechanism. This can be realized by operating the stored program. Similarly, among the steps of the elemental analysis method shown in FIG. 4, steps S6 and S7 can be realized by operating a program stored in a RAM or ROM of a computer. This program and a computer-readable storage medium storing the program are included in the present invention.

  Specifically, the program is recorded on a recording medium such as a CD-ROM or provided to a computer via various transmission media. As a recording medium for recording the program, besides a CD-ROM, a flexible disk, a hard disk, a magnetic tape, a magneto-optical disk, a nonvolatile memory card, or the like can be used. On the other hand, as the program transmission medium, a communication medium in a computer network system for propagating and supplying program information as a carrier wave can be used. Here, the computer network is a WAN such as a LAN or the Internet, a wireless communication network, or the like, and the communication medium is a wired line such as an optical fiber or a wireless line.

  Further, the program included in the present invention is not limited to the one in which the functions of the above-described embodiments are realized by the computer executing the supplied program. For example, such a program is also included in the present invention when the function of the above-described embodiment is realized in cooperation with an OS (operating system) or other application software running on the computer. Further, when all or part of the processing of the supplied program is performed by the function expansion board or function expansion unit of the computer and the functions of the above-described embodiment are realized, the program is also included in the present invention.

  For example, FIG. 5 is a schematic diagram illustrating an internal configuration of a personal user terminal device. In FIG. 5, reference numeral 1200 denotes a personal computer (PC) provided with a CPU 1201. The PC 1200 executes device control software stored in the ROM 1202 or the hard disk (HD) 1211 or supplied from the flexible disk drive (FD) 1212. The PC 1200 generally controls each device connected to the system bus 1204.

  The functions stored in the CPU 1201 of the PC 1200, the ROM 1202, or the hard disk (HD) 1211 realize the functions of the angle calculation unit 37 and the control unit 38 in FIG. 3 of this embodiment, the procedures of steps S6 and S7 in FIG. Is done.

  Reference numeral 1203 denotes a RAM which functions as a main memory, work area, and the like for the CPU 1201. A keyboard controller (KBC) 1205 controls instruction input from a keyboard (KB) 1209, a device (not shown), or the like.

  Reference numeral 1206 denotes a CRT controller (CRTC), which controls display on a CRT display (CRT) 1210. Reference numeral 1207 denotes a disk controller (DKC). The DKC 1207 controls access to a hard disk (HD) 1211 and a flexible disk (FD) 1212 that store a boot program, a plurality of applications, an editing file, a user file, a network management program, and the like. Here, the boot program is a startup program: a program for starting execution (operation) of hardware and software of a personal computer.

  Reference numeral 1208 denotes a network interface card (NIC) that exchanges data bidirectionally with a network printer, another network device, or another PC via the LAN 1220.

  Hereinafter, various aspects of the present invention will be collectively described as supplementary notes.

(Supplementary note 1) a sample installation part in which a sample is installed;
A power source for applying an electric field to the sample installed in the sample installation unit;
An element analysis mechanism that is disposed so as to face the sample and has an element detection unit that detects an element detached from the sample;
A microscope mechanism for observing the sample installed in the sample installation unit,
A first moving unit that performs each parallel movement of the sample placement unit in the X-axis direction, the Y-axis direction, and the Z-axis direction, and each rotational movement around the X-axis and the Y-axis;
An element analyzer comprising: a second moving unit that rotates the element detecting unit around the Z axis that coincides with an optical axis in the microscope mechanism.

(Supplementary Note 2) An angle calculation unit that calculates a displacement angle between the sample and the element detection unit in a plane perpendicular to the Z-axis direction;
A movement control unit for driving the second moving unit so as to rotate the element detecting unit by the displacement angle calculated by the angle calculating unit and to match the direction of the element detecting unit with the direction of the sample; The elemental analyzer according to appendix 1, further comprising:

(Additional remark 3) The said element analysis mechanism is further provided between the said sample installation part and the said element detection part, and also has the extraction electrode which sends out the element detach | leaved from the said sample by voltage application to the said element detection part And
The apparatus further includes a third moving unit that performs parallel movement of the extraction electrode in the X-axis direction, the Y-axis direction, and the Z-axis direction and rotational movement about the Z-axis that coincides with the optical axis. The elemental analyzer according to 1 or 2.

  (Additional remark 4) It is connected to the 2nd moving part and the 3rd moving part, The rotation movement about the Z axis of the element detection part by the 2nd moving part and the 3rd moving part and the above-mentioned The elemental analyzer according to appendix 3, further comprising a rotation synchronization unit that synchronizes the rotational movement of the extraction electrode around the Z axis.

  (Additional remark 5) The said microscope mechanism is a transmission electron microscope apparatus, The elemental analyzer of any one of Additional remarks 1-4 characterized by the above-mentioned.

(Appendix 6) An element detection mechanism for applying an electric field to a sample installed in the sample installation unit and detecting an element detached from the sample by an element detection unit, and a microscope for observing the sample installed in the sample installation unit An elemental analysis method using an elemental analysis device comprising a mechanism,
A step of calculating a displacement angle between the sample and the element detection unit in a state in which the sample is adjusted to be positioned in a plane perpendicular to the Z axis that coincides with the optical axis based on observation by the microscope mechanism. When,
And rotating the element detection unit by the calculated displacement angle so that the direction of the element detection unit coincides with the direction of the sample.

  (Supplementary note 7) The elemental analysis method according to supplementary note 6, wherein the microscope mechanism is an electron microscope apparatus.

(Supplementary Note 8) An element detection mechanism for applying an electric field to the sample installed in the sample installation unit and detecting an element separated from the sample by the element detection unit, and the element detection mechanism are mounted, and the sample installation unit When performing an elemental analysis using an elemental analyzer equipped with a microscope mechanism for observing the sample installed in
A step of calculating a displacement angle between the sample and the element detection unit in a state in which the sample is adjusted to be positioned in a plane perpendicular to the Z axis that coincides with the optical axis based on observation by the microscope mechanism. When,
A program for causing a computer to execute the step of rotating the element detection unit by the calculated displacement angle and causing the direction of the element detection unit to coincide with the direction of the sample.

It is a schematic diagram which shows the basic composition of 3DAP mechanism which this invention employ | adopts. It is a schematic diagram which shows schematic structure of the elemental analyzer by this embodiment by which 3DAP mechanism which has the basic composition of FIG. 1 is mounted in TEM. It is a schematic diagram which expands and shows the part of 3DAP mechanism mounted in the elemental analyzer of FIG. It is a flowchart which shows the elemental analysis method by this embodiment in order of a step. It is a schematic diagram which shows the internal structure of a personal user terminal device.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Chamber 2 Power supply 2a High voltage power supply part 2b Pulse generator 3 Position sensitive detector 4 Extraction electrode 5 Exhaust mechanism 6 Timer 11 Sample 21 Electron gun 22 Acceleration tube 23 Converging lens 24 Sample chamber 25 Objective lens 26 Intermediate lens 27 Projection lens 28 STEM Detector 29 CCD camera 31 Sample holder 31a Sample installation unit 32 Extraction electrode holder 33 Detector support unit 34 Holder stage 35 First moving unit 36 Second moving unit 37 Angle calculating unit 38 Control unit 41 Third moving unit 42 Synchronous circuit

Claims (7)

A sample placement section where the sample is placed;
A power source for applying an electric field to the sample installed in the sample installation unit;
An element analysis mechanism that is disposed so as to face the sample and has an element detection unit that detects an element detached from the sample;
A microscope mechanism for observing the sample installed in the sample installation unit,
A first moving unit that performs each parallel movement of the sample placement unit in the X-axis direction, the Y-axis direction, and the Z-axis direction, and each rotational movement around the X-axis and the Y-axis;
An element analyzer comprising: a second moving unit that rotates the element detecting unit around the optical axis of the microscope mechanism that coincides with the Z axis . An angle calculation unit that calculates a displacement angle between the sample and the element detection unit in a plane perpendicular to the Z-axis direction;
A movement control unit for driving the second moving unit so as to rotate the element detecting unit by the displacement angle calculated by the angle calculating unit and to match the direction of the element detecting unit with the direction of the sample; The elemental analysis apparatus according to claim 1, further comprising: The element analysis mechanism is further provided between the sample setting unit and the element detection unit, and further includes a lead electrode for sending an element detached from the sample by voltage application to the element detection unit,
The apparatus further comprises a third moving unit that performs parallel movement of the extraction electrode in the X-axis direction, Y-axis direction, and Z-axis direction, and rotational movement about the Z-axis that coincides with the optical axis. Item 3. The elemental analyzer according to Item 1 or 2.   The second moving unit and the third moving unit are connected to the second moving unit and the third moving unit, and the element detecting unit is rotated around the Z axis by the second moving unit and the third moving unit. The elemental analysis apparatus according to claim 3, further comprising a rotation synchronization unit that synchronizes rotational movement about the axis.   The element analysis apparatus according to claim 1, wherein the microscope mechanism is an electron microscope apparatus. An element detection mechanism that applies an electric field to a sample installed in the sample installation unit and detects an element separated from the sample by an element detection unit, and a microscope mechanism that observes the sample installed in the sample installation unit An elemental analysis method using an elemental analysis apparatus comprising:
A step of calculating a displacement angle between the sample and the element detection unit in a state in which the sample is adjusted to be positioned in a plane perpendicular to the Z axis that coincides with the optical axis based on observation by the microscope mechanism. When,
And rotating the element detection unit by the calculated displacement angle so that the direction of the element detection unit coincides with the direction of the sample. An element detection mechanism for applying an electric field to the sample installed in the sample installation unit and detecting the element detached from the sample by the element detection unit, and the element detection mechanism are installed, and installed in the sample installation unit When performing an elemental analysis using an elemental analyzer comprising a microscope mechanism for observing the sample,
A step of calculating a displacement angle between the sample and the element detection unit in a state in which the sample is adjusted to be positioned in a plane perpendicular to the Z axis that coincides with the optical axis based on observation by the microscope mechanism. When,
A program for causing a computer to execute the step of rotating the element detection unit by the calculated displacement angle and causing the direction of the element detection unit to coincide with the direction of the sample.

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