JP4534273B2 - Sample preparation device - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a sample preparation device for extracting a desired micro sample from a sample piece using an ion beam and a transfer means, fixing the sample to a sample holder, and processing the sample into a shape suitable for analysis and observation, and a sample using the sample preparation device Regarding the creation method.
[0002]
[Prior art]
As semiconductor devices are highly integrated, the objects of analysis and observation handled in the manufacturing or inspection process are becoming increasingly smaller. Scanning electron microscopes (hereinafter referred to as SEM) are used as means for analyzing and observing them. Instead, a transmission electron microscope (hereinafter referred to as TEM) having a higher observation resolution has become an effective means.
[0003]
As a conventional method for preparing a TEM sample, a method using polishing or ion thinning is well known. However, recently, a method using a focused ion beam (hereinafter referred to as FIB) processing has been established. In this method, a strip-shaped pellet having a size of about 3 × 0.1 × 0.5 mm (0.5 mm is the thickness of the wafer) including an area to be observed is first removed from a sample such as a wafer using a dicing apparatus. The observation area of the strip-shaped pellet is cut out and further FIB-processed into a thin wall shape having a thickness of about 0.1 μm to obtain a TEM sample. This TEM sample is transferred to a TEM sample holder, further mounted on a TEM stage, introduced into a TEM apparatus, and observed by irradiating a thin wall surface with an electron beam.
[0004]
This technique is described in, for example, the paper “Microscopy of Semiconducting Materials”, 1989, Institute of Physics Series No.100, p.501-506.
[0005]
Recently, a sample stage that can be used both as an FIB apparatus and a TEM apparatus has been used. FIG. 13 shows a schematic shape of a conventional side entry type sample stage. An outer tube portion 9 is attached to the tip of a gripping portion 13, and a FIB-processed TEM sample 48 is fixed to a tip thereof by a fixing jig 49. ing.
[0006]
As shown in FIG. 14, this sample stage is introduced into the FIB apparatus 24, and the position of the sample is adjusted by the sample stage fine movement mechanism 37. The FIB is irradiated parallel to the thin wall part of the sample during FIB processing, and the electron beam is irradiated perpendicularly to the thin wall surface during TEM observation. Therefore, the sample stage is rotated by 90 degrees between FIB processing and TEM observation. Use. With such a sample stage, it is possible to immediately bring the sample processed in the FIB apparatus 24 into the TEM apparatus and observe it, but even if the FIB processing is used, the processing time of one sample is 3 to 5 hours. Is needed.
[0007]
The above-mentioned FIB and TEM combined stage is described in JP-A-6-103947. Japanese Patent Publication No. 2774884 discloses a method of extracting a specific minute sample created in a wafer using an ion beam with a probe.
[0008]
In addition, a method in which only a thin film for TEM observation is formed in a wafer using a focused ion beam, and only this thin film is transported on a TEM mesh using a glass needle to form a TEM sample, for example, Material Research Society Symposium Ding (Material Research Society Symposium Proceeding), 1997, vol. 480. , P19-27.
[0009]
[Problems to be solved by the invention]
Conventionally, when preparing a sample suitable for analysis, observation, and measurement, particularly a TEM sample, the following problems have been encountered.
[0010]
In order to prepare a TEM sample, a plurality of devices such as an ion thinning, polishing machine, dicing device, and FIB device are required. In addition, the sample preparation requires skilled time and skill. Necessitates complicated manual work. In addition, in the method of extracting a micro sample with a probe and the method of transporting the prepared TEM sample onto a TEM mesh, since the prepared TEM sample is held by the probe, it is very difficult to introduce it into the TEM apparatus. In addition, there is a risk of accidents such as dropping or loss. In addition, there is a similar risk when replacing with another sample after TEM observation.
[0011]
In view of the above-described problems, the object of the present invention is to provide a sample preparation device that allows simple work from sample preparation to analysis, observation, and measurement, enables sample preparation with a single device, and facilitates delivery of the prepared sample to the analyzer. And to provide a method. Furthermore, it is providing the sample preparation apparatus and method which can shorten the time from sample preparation to analysis, observation, and measurement, and can improve the efficiency of analysis and observation.
[0012]
[Means for Solving the Problems]
An object of the present invention is to provide an irradiation optical system of either a focused ion beam or a projection ion beam, secondary particle detection means for detecting secondary particles generated by the irradiation of the ion beam, and an irradiation region of the ion beam. A deposition gas supply source for supplying a source gas for forming a deposition film on the substrate, a transfer means for transferring an extracted sample separated from a sample piece to a sample holder, and a side entry type for placing the sample piece In a sample preparation device comprising a sample stage and a sample stage fine moving means for mounting and finely moving the side entry type sample stage, the sample setting portion of the side entry type sample stage can be moved in a direction including the axial component of the sample stage. And the sample mounting portion can be rotated with a rotation axis including a component perpendicular to the axial direction of the sample stage. It is accomplished by providing a stage.
[0013]
In particular, the purpose is to allow the sample setting part to be separated from the side entry type sample stage, the sample setting part has a degree of freedom of rotation about the vertical line of the sample setting surface, and further to the side entry type sample stage axis center. Therefore, this can be easily achieved by adopting a configuration having a degree of freedom of straight movement that moves straightly in parallel.
[0014]
Sample preparation using this method is performed according to the following procedure. First, the operator attaches a sample piece to the side entry type sample stage having the above-described degree of freedom. The sample piece can be fixed without worrying about the direction of the cross section of the sample piece or the positional deviation during bonding because the sample setting portion has a degree of freedom of rotation. Further, since the side entry type sample stage also has a degree of freedom of straight advancement, it is easy to FIB process a sample piece with a side on the order of several millimeters from any direction and position. As a result, anyone can perform the cutting and fixing of the sample piece, which has been dependent on experience and intuition in the past, regardless of the operator. Therefore, processing from a sample having a desired observation site to a micro sample in a state suitable for TEM observation, for example, can be reliably performed in a short time.
[0015]
After fixing the sample piece, the sample setting part is coupled to the side entry type sample stage, loaded into the sample stage fine movement means, and introduced into the vacuum vessel. The sample stage fine movement means can be inserted into and removed from the vacuum container of the side entry type sample stage without exposing the inside of the vacuum container to the atmosphere.
[0016]
After this, the region including the desired observation site of the sample piece is FIB-processed to a desired size and extracted, and once held by the transfer means, the side entry type sample stage is pulled out and another side on which the TEM holder is mounted. An entry type sample stage is introduced. After exchanging the side entry type sample stage, the minute sample piece held by the transfer means is fixed to the TEM holder by forming a deposition film. After the fixation, the TEM observation can be performed by pulling it out from the vacuum container and loading it into the TEM apparatus.
[0017]
Such a side entry type sample stage that brings various effects to the production of a small sample piece represented by the production of a TEM sample can be realized by adopting the following configuration.
[0018]
The end of the single drive shaft on the vacuum side is formed into a screw shape, and an arm that constrains the degree of freedom of rotation about the central axis of the drive shaft is coupled via the drive shaft and a rotatable member. The first pulley around which a rotational motion transmission medium such as a wire is wound is rotatable with respect to the arm so that a sample setting part for placing the sample piece is placed at a predetermined position of the arm. It couple | bonds through a rotation member. A second pulley around which the rotary motion transmission medium is wound is coupled to a position that makes a pair with this pulley via a rotating member so as to be rotatable with respect to the arm. A second arm that fixes one end and one end of a rotation transmission medium wound between the first pulley and the second pulley is disposed.
[0019]
The other end of the second arm is in the shape of a screw that fits into the screw of the drive shaft, and meshes with the screw of the drive shaft. Similar to the arm, the second arm restrains the degree of freedom of rotation about the center axis of the drive shaft. The drive shaft is rotatable and rectilinear through a vacuum seal, and the arm is covered with an outer cylinder portion that is held linearly.
[0020]
The above is the very basic configuration of the side entry type sample stage having two degrees of freedom of rotation and straight travel. Such a side entry type sample stage having two degrees of freedom can be used in various ways. For example, by installing a plurality of sample placement units, a plurality of sample pieces can be FIB processed at a time. In another example, it is possible to further improve the usability by configuring the sample setting portion with a first stage on which a sample piece is placed on one side and a second stage on which the TEM holder is placed on the other.
[0021]
Another configuration includes a side entry type sample stage having the following structure. The configurations of the arm, the drive shaft, and the outer cylinder portion are the same as those described above, and only the changes are described. The circumference of the sample installation part is made into a gear shape, for example, a bevel gear shape. The shape of the end of the drive shaft on the vacuum side is the second bevel gear shape that meshes with the aforementioned bevel gear.
[0022]
Another configuration includes a side entry type sample stage having the following structure. The configurations of the arm, the drive shaft, and the outer cylinder portion are the same as those described above, and only the changes are described. The configuration is the same as that described above until the first pulley and the second pulley of the sample setting section are coupled by a rotational motion transmission medium such as a belt. The circumference of the second pulley has a gear shape, for example, a bevel gear shape. The shape of the end of the drive shaft on the vacuum side is the second bevel gear shape that meshes with the aforementioned bevel gear.
[0023]
As another configuration, there is a side entry type sample stage having the following structure. The configurations of the arm, the drive shaft, and the outer cylinder portion are the same as those described above, and only the changes are described. A projecting portion is provided on the end surface on the drive shaft side of the sample installing portion. The shape of the protrusion is not limited. On the vacuum side end face of the drive shaft, a rotary shaft whose free end comes into contact with the surface of the protrusion described above in a posture parallel to the central axis of the drive shaft is disposed at a position eccentric from the rotation center axis of the drive shaft. The configuration having the rotation shaft eccentric with respect to the rotation center axis of the drive shaft can easily cope with the rotation direction of the sample installation portion by changing a part of the structure. In other words, when the rotation center of the sample mounting part is arranged in parallel with a perpendicular line that runs horizontally to the rotation center axis of the drive shaft, the sample installation part rotates in the pitching direction as viewed from the center axis of the drive shaft. Can be moved. Further, in the configuration in which the rotation center is arranged in parallel to the central axis of the drive shaft, it can be rotated and moved in the yawing direction.
[0024]
The side entry type sample stage described above includes a focused ion beam, a transmission electron microscope, a scanning electron microscope, a scanning probe microscope, an Auger electron spectroscopic analyzer, an electron probe X-ray microanalyzer, an electron energy defect analyzer, two Sample surface analysis and observation is easy by using a secondary ion mass spectrometer, a secondary neutron ionization mass spectrometer, an X-ray photoelectron spectrometer, or an electrical measurement device using a probe. And you will be able to do it quickly.
[0025]
DETAILED DESCRIPTION OF THE INVENTION
Example 1
FIG. 1A is a longitudinal sectional view of a side entry type sample stage in the sample preparation apparatus of one embodiment of the present invention, and FIG. 1B is a top view thereof. FIG. 2 is a bird's eye view showing the basic parts constituting the side entry type sample stage of the first embodiment for each layer. In addition, in the code | symbol shown to this specification below, it shows that the member using the same code | symbol is a member which has an equivalent function.
[0026]
The configuration of the first embodiment will be described with reference to FIG. Note that FIG. 2 is mainly intended to explain the configuration, and the scale ratio of each component is not accurate.
[0027]
A sample setting portion 1 for setting a sample piece (not shown) is held by the first pulley 2 so that it can be easily separated. In the present embodiment, the sample mounting portion 1 is structured to be screw-coupled to the pulley 2. The first pulley 2 is held by a first arm 4 that moves straight through a rotatable member (a bearing 3 a having self-lubricating property in this embodiment). A rotational motion transmission medium (wire 6 in this embodiment) is wound around the outer circumferences of the first pulley 2 and the second pulley 5. The second pulley 5 is also rotatably held via a member (self-lubricating bearing 3b in this embodiment) that is rotatable on the first arm 4 that moves straight.
[0028]
A part of the wire 6 is coupled to the second arm 7 whose end is processed with a screw (7a). The drive shaft 8 is processed with a screw portion 8a that fits with a screw portion 7a provided at the end of the second arm 7, and the drive shaft 8 and the second arm 7 are connected to the screw portions 7a and 8a. Connect with.
[0029]
At this time, the first arm 4 and the drive shaft 8 are pressed through a rotatable member (not shown). These first and second arms 4 and 7 are inserted into the outer cylinder 9 while restricting the degree of freedom in the rotational direction, and the drive shaft 8 is interposed with a bearing 14 and a vacuum seal (not shown) that can rotate and go straight. And inserted into the outer cylinder 9.
[0030]
The end of the drive shaft 8 protrudes from the outer cylinder 9. A gear 10 a is fixed to the protruding drive shaft 8, and a minute feed mechanism 11, which is a linearly moving actuator, is pressed on the end surface of the drive shaft 8. Another gear 10b that meshes with the gear 10a is disposed in parallel with the drive shaft 8, and a knob 12 for rotational movement is fixed to the gear 10b). Although not shown, it goes without saying that these gears 10a and 10b are held via rotatable members.
[0031]
The above is the basic configuration of the side entry type sample stage having two degrees of freedom of rotation and straight travel. The operation will be described below with reference to FIG.
[0032]
The drive shaft 8 is linearly moved using the minute feed mechanism 11. The straight movement of the drive shaft 8 is transmitted to the first and second arms 4 and 7, so that the sample placement unit 1 installed on the first arm 4 moves straight without rotating.
[0033]
The sample holder 1 is rotated by rotating the knob 12 and rotating the drive shaft 8 through the gears 10a and 10b. The rotational motion of the drive shaft 8 is converted into the straight motion of the second arm 7 whose rotational direction is regulated by the screw 7a meshed with the screw 8a of the drive shaft 8. The straight movement of the second arm 7 acts to pull the wire 6 wound around the pulley 2 because one end of the second arm 7 is coupled to the wire 6. The pulled wire 6 rotates the pulley 2 by friction, thereby enabling the sample placement unit 1 to rotate with a rotation axis including a component perpendicular to the axial direction of the sample stage.
[0034]
As described above, the sample placement unit 1 can be moved straight and rotated by a simple operation of the straight drive and the rotary motion of the single drive shaft 8.
[0035]
(Example 2)
FIG. 3 shows a side entry type sample stage of another embodiment. FIG. 4A is a longitudinal sectional view, and FIG. In this embodiment, since the drive unit 20 is the same as that of the first embodiment, the drive unit 20 is omitted in the drawing. The configuration of the arm 4, the drive shaft 8, and the outer cylinder 9 is the same as that of the first embodiment, and only the changes are described.
[0036]
Let the circumference of the sample installation part 1 be a gear shape (for example, bevel gear 25b) shape. The shape of the end of the drive shaft 8 on the vacuum side is a second bevel gear 25a shape that meshes with the aforementioned bevel gear 25b. Thus, by rotating the drive shaft 8, the direction of rotation of the drive shaft 8 is changed by the bevel gears 25a and 25b meshing with each other, and the sample placement unit 1 rotates. The straight movement can be performed by the method of the first embodiment.
[0037]
(Example 3)
FIG. 4 shows a side entry type sample stage of another embodiment. FIG. 4A is a longitudinal sectional view, and FIG. 4B is a top view. Since the drive unit is the same as that of the first embodiment, the drive unit is also omitted from the drawing. The configuration of the arm 4, the drive shaft 8 and the outer cylinder 9, and the embodiment until the first pulley 2 and the second pulley 5 of the sample installation unit 1 are coupled by a rotational motion transmission medium such as a belt. 1 and only the changes will be described below.
[0038]
In this embodiment, the circumference of the second pulley 5 is a gear shape, for example, a bevel gear 26a. Further, the shape of the end of the drive shaft 8 on the vacuum side is a second bevel gear 26b shape that meshes with the bevel gear 26a formed on the second pulley. Thus, by rotating the drive shaft 8, the direction of rotation of the drive shaft 8 is changed by the bevel gears 26 a and 26 b meshing with each other, the second pulley 5 is rotated, and the sample is placed via the wire 6 by friction. Part 1 rotates. The straight movement can be performed by the same method as in the first embodiment.
[0039]
Example 4
The side entry type sample stage having two degrees of freedom as in the first to third embodiments can be used in various applications. Like the side entry type sample stage shown in FIG. 5, by installing a plurality (two in this embodiment) of the sample setting sections 1, a plurality of sample pieces can be FIB processed at a time. Since the time required for inserting / removing the entry type stage, evacuating the vacuum, leaking, and exchanging the sample piece 15 is only once, the required time can be greatly reduced.
[0040]
(Example 5)
6A, one is a first stage 1a on which a sample piece is placed, and the other is, for example, a sample setting unit 1 that is a second stage 1b on which a TEM holder 21 is placed. As a result, the usability can be further improved. Here, FIG. 4B is a top view.
[0041]
FIG. 6 shows a state in which the sample setting unit 1 is retracted into the outer cylinder 9 by driving the microfeed mechanism 11. In this side entry type sample stage, the shape of the observation position of the outer cylinder 9 is made a shape capable of FIB processing and TEM observation, and the pulley 2 is arranged directly below the first stage 1a for the sample piece, and is in a cantilever shape. The second stage 1b on which the TEM holder 21 is loaded is arranged on the other end of the sample placement unit 1. Here, the pulley 2 is not limited to the position immediately below the first stage 1a, and it is natural that there is no problem at any position.
[0042]
At the time of FIB processing, the micro feed mechanism 11 is driven, and the first stage 1a to which the sample piece is fixed is moved straight to the observation position. At this time, the pulley 2 protrudes from the thin outer tube 9 together with the arm 4, but there is no inconvenience for FIB processing when extracting a small sample piece (not shown).
[0043]
After the FIB processing is completed, while the minute sample piece 22 is held by the transfer means (not shown), the drive shaft 8 is moved straight forward by a predetermined amount to the atmosphere side, that is, the sample setting unit 1 is retracted. After moving to a predetermined position, the drive shaft 8 is rotated until the pulley 2 rotates 180 degrees, and the second stage 1b loaded with the TEM holder 21 is rotated to the observation position.
[0044]
Since the opening 23 is provided on the side surface of the outer cylinder 9 so as not to interfere with the rotation trajectory of the TEM holder 21, it can be rotated. After the rotational movement to a predetermined position, the micro sample is transferred to the desired position of the TEM holder 21 by the transfer means 18 by moving it straight if necessary. In TEM observation, more stable observation can be performed by moving the second stage 1b loaded with the TEM holder 21 straightly and pressing the second stage 1b against the outer cylinder 9 part.
[0045]
As described above, by adopting the present embodiment in which the first stage 1a for the sample piece and the second stage 1b for the TEM holder 21 are provided, the side entry type sample stage is not required to be inserted and removed, and the sample piece is surely obtained. 15 can be extracted, transferred to the TEM holder 21, and fixed. Further, by making the shape of the outer cylinder 9 part a shape that can be shared by the FIB apparatus and the TEM apparatus, the micro sample piece 22 transferred to the TEM holder 21 can be subjected to FIB processing, for example, on the TEM sample as it is. Simplification of creation and shortening of creation time can be realized.
[0046]
Furthermore, by loading the side entry type sample stage as it is into the TEM device 19, the operator can only work directly on the bonding of the sample piece. After the side entry type sample stage is introduced into the vacuum vessel 17, , Extraction of the micro sample piece 22 and transfer to the TEM holder 21, FIB processing, and preparation of the TEM sample can be performed consistently in the same apparatus, and the operator can perform the TEM only by inserting and removing the side entry type sample stage. Can observe. According to the present embodiment, a process that conventionally requires a skilled operator for several days until TEM observation can be performed safely and reliably without significantly selecting the operator.
[0047]
(Example 6)
FIG. 7 shows a side entry type sample stage of another embodiment. FIG. 4A is a longitudinal sectional view, and FIG. Also in this embodiment, since the drive unit is the same as that of the first embodiment, the drive unit is not shown in the figure. The configurations of the arm 4, the drive shaft 8, and the outer cylinder 9 are the same as the configurations of the previous embodiments, and only the changes are described.
[0048]
In the present embodiment, the projecting portion 27 is provided on the end surface of the sample installing portion 1 on the drive shaft 8 side. The shape of the protrusion 27 is not limited. Further, the free end contacts the vacuum end surface of the drive shaft 8 at a position eccentric from the rotation center axis of the drive shaft 8 in a posture parallel to the surface of the protrusion 27 and the center axis of the drive shaft 8. A rotating shaft 28 is disposed.
[0049]
In the rotational movement of the sample setting unit 1, the rotation shaft 28 is eccentrically rotated by rotating the drive shaft 8, and the protrusion 27 where the free end of the rotation shaft 28 is in contact with the eccentric amount and the rotation amount of the rotation shaft 28. Rotate and move accordingly. That is, the sample placement unit 1 rotates.
[0050]
Although the side entry type sample stage shown in the present embodiment has a limitation in the rotational movement amount of the sample setting unit 1, the point that the rotation direction of the sample setting unit 1 can be easily handled by changing a part of the structure so far. There is a characteristic that the embodiment does not have.
[0051]
(Example 7)
FIG. 8 shows a side entry type sample stage of the embodiment in which the rotation direction of the sample setting unit 1 is changed by 90 degrees. FIG. 4A is a longitudinal sectional view, and FIG. 4B is a top view.
[0052]
As in this embodiment, when the rotation center 29 of the sample placement unit 1 is arranged in parallel with a perpendicular line that is drawn horizontally with respect to the rotation center axis of the drive shaft 8, the sample placement unit 1 has the drive shaft 8. It can be rotated in the direction of pitching as viewed from the central axis of the. Although not shown in the figure, the configuration in which the rotation center is arranged in parallel with the central axis of the drive shaft 8 can be rotated in the yawing direction.
[0053]
In the embodiment described above, the configuration is made with the automation of the drive unit 20 in mind. Therefore, as shown in FIG. 1, a knob in which the rotational motion is arranged in parallel with the microfeed mechanism 11 via the gears 10a and 10b. 12 is used. Automation can be realized without changing any dimensions by replacing the micro feed mechanism 11 and the knob 12 with a drive source (not shown) such as a motor.
[0054]
(Example 8)
Needless to say, it is easier to handle if the grip portion 13 is narrowed when complete manual driving is acceptable. At that time, the object of the present invention is also achieved by the configuration shown in FIG. FIG. 9 shows a longitudinal sectional view of a side entry type sample stage in which only the driving unit of the first embodiment is changed.
[0055]
The present embodiment is different from the previous embodiments in that the rotary drive knob 12 and the minute feed mechanism 11 are arranged in series in order to reduce the diameter of the drive unit 20. The rotary knob 12 is coupled to the drive shaft 8 via a straight bearing 31 that restricts the degree of freedom of rotation so that the degree of freedom of straight movement is limited. Further, the rotary knob 12 is pressed through the outer cylinder 9 and a rotatable bearing 14. The minute feed mechanism 11 is coupled to the end of the rotary knob 12, and the linearly moving portion of the minute feed mechanism 11 is pressed against the end of the drive shaft 8.
[0056]
The linear movement of the drive shaft 8 is performed by driving the minute feed mechanism 11 in the same manner as in the previous embodiments, so that only the drive shaft 8 moves linearly without rotating the rotary knob 12. The rotational movement of the drive shaft 8 is transmitted by rotating the rotary knob 12 and rotating the drive shaft 8 for each minute feed mechanism 11. By adopting the configuration of the present embodiment, the diameter of the grip portion 13 can be reduced to about 30 mm, and the apparatus can be easily handled.
[0057]
Although the example in which the drive unit 20 of the first embodiment is changed has been described above, the configuration of the present embodiment can be applied to any of the second to sixth embodiments. It should be noted that in various side entry type sample stages described so far, by placing a mark on the grip 13 so that the relationship between the rotation direction of the rotary knob 12 and the rotation direction of the sample placement unit 1 can be understood. Further ease of use can be achieved.
[0058]
Example 9
FIG. 10 is a bird's-eye view of a sample preparation apparatus according to an embodiment of the present invention. The side entry type sample stage described in the above embodiment is used in the sample preparation apparatus shown in FIG.
[0059]
The apparatus 38 includes an irradiation optical system 32 for an ion beam 33 of either a focused ion beam or a projection ion beam, a secondary particle detector 34 for detecting secondary particles generated by the irradiation of the ion beam 33, and the above-described device. A deposition gas supply source 35 for supplying a source gas for forming a deposition film in the irradiation region of the ion beam 33, and a transfer means 18 for transferring a micro sample piece 22 from which a part of the sample piece 15 has been extracted to a sample holder 36. And a sample stage fine moving means 37 for mounting and finely moving the side entry type sample stage.
[0060]
The sample preparation device 38 further includes an ion beam control unit 39 that controls the irradiation optical system 32 of the ion beam 33, a secondary particle detector control unit 40 that adjusts the voltage applied to the secondary particle detector 34, and the like. For driving the gas supply source control means 41 for the deposition gas for controlling the temperature adjustment of the position gas supply source 35 and the opening / closing of the valve, the stage control section 42 for controlling the sample stage fine movement means 37, and the transfer means 18. The image display unit 44 for displaying an image of the sample transfer unit 43, the sample piece 15, the transfer unit 18 and the like are controlled by a calculation processing unit 45.
[0061]
Sample preparation using the side entry type sample stage of the present invention is performed in accordance with the following procedure. First, the operator attaches the sample piece 15 to the sample setting portion 1 of the side entry type sample stage having the above-described degree of freedom. At this time, a reference line (not shown) is carved on the sample setting surface so that the sample setting unit 1 may be separated from the side entry type sample stage. It becomes a standard. Further, by fixing a plurality of sample pieces 15 in advance to the plurality of sample setting sections 1, work efficiency can be increased, and as a result, work time can be shortened.
[0062]
The sample piece 15 can be fixed without worrying about the direction of the cross section of the sample piece 15 or the positional deviation at the time of bonding since the sample setting portion 1 has a degree of freedom of rotation. Further, since it also has a degree of freedom of straight advancement, FIB processing can be easily performed in any direction and position of the sample piece 15 whose side is on the order of several millimeters.
[0063]
As a result, anyone can cut out the sample piece 15 and fix the sample piece 15 depending on experience and intuition, regardless of the operator. Thereby, for example, a TEM sample of a desired observation site can be reliably created in a short time.
[0064]
After fixing the sample piece 15, the sample setting unit 1 is coupled to the side entry type sample stage, loaded into the sample stage fine movement means, and introduced into the vacuum container 17.
[0065]
The sample stage fine moving means can be taken in and out of the vacuum vessel 17 of the side entry type sample stage without exposing the inside of the vacuum vessel 17 to the atmosphere.
[0066]
Thereafter, the region including the desired observation site of the sample piece 15 is extracted by FIB processing to a desired size, temporarily held by the transfer means 18, the side entry type sample stage is pulled out, and the TEM holder 21 is mounted. Another side entry type sample stage is introduced. After exchanging the side entry type sample stage, the minute sample piece 15 held by the transfer means 18 is fixed to the TEM holder 21 by forming a deposition film.
[0067]
After the micro sample piece is fixed, the side entry type sample stage is pulled out from the vacuum vessel 17 and loaded into a TEM device 19 (not shown), whereby TEM observation can be performed. At this time, if the side entry type sample stage of the embodiment of FIG. 6 is used, the exchange operation of the side entry type sample stage becomes unnecessary, and only the operation of rotating the sample setting unit 1 is sufficient.
[0068]
In the embodiments described above, the preparation and observation of a TEM sample has been described as an example for the sake of explanation. However, the embodiment is not limited to a TEM, and is not limited to a TEM, but a focused ion beam, a transmission electron microscope, a scanning electron microscope, a scanning probe. Electricity using a microscope, an Auger electron spectrometer, an electron probe X-ray microanalyzer, an electron energy defect analyzer, a secondary ion mass spectrometer, a secondary neutron ionization mass spectrometer, an X-ray photoelectron spectrometer, or a probe It goes without saying that sample plane analysis and observation can be facilitated by adopting a configuration that can be loaded into any of the measuring devices.
[0069]
(Example 10)
A storage 46 for storing the side entry type sample stage described above may be provided. FIG. 11 is a bird's-eye view showing the state of the side entry type sample stage inserted into the storage 46. As described above, when the sample pieces 15 are fixed to the sample setting unit 1 together, the sample pieces 15 are stored in a storage room having a vacuum atmosphere in order to prevent physical or chemical contamination of the sample pieces 15. Since the upper surface of the storage 46 is configured with a transparent lid 47 so that the inside can be seen, the state of the stored side entry type sample stage can be confirmed at any time. By preparing the storage 46, a plurality of side entry type sample stages can be stored in a clean atmosphere without taking a storage place.
[0070]
(Example 11)
Further, when the FIB device 24 and the above-described various analysis devices and measurement devices are in a remote location, the embodiment of the portable storage shown in FIG. 12 may be used. The portable storage 50 includes a side entry type sample stage on which the sample piece 15 subjected to FIB processing into a shape suitable for a desired analysis means, observation means, or measurement means by the ion beam 33 is placed on the above-described various analyzers and measurement devices. When transporting to the apparatus, it has a function of sealing only the vicinity of the sample installation part 1 in a vacuum atmosphere, and is lightweight and easy to transport.
[0071]
The portable storage 50 is made of a transparent member, so that the state of the sample placement unit 1 can be grasped, and attention is urged in handling during transportation. A typical usage of the portable storage 50 is to pull out the side entry type sample stage from the FIB device 24 and then quickly insert the tip including the sample setting unit 1 into the portable storage 50.
[0072]
A vacuum seal 16 member is arranged on the outer cylinder 9 of the side entry type sample stage, and the inside of the portable storage 50 is kept airtight by using the vacuum seal 16 member. After the insertion, the valve 52 connected to the exhaust device 51 is operated to exhaust the interior of the portable storage 50 for an appropriate time.
[0073]
After evacuation, the valve 52 is operated to seal the inside of the portable storage 50, the valve 52 and the exhaust device 51 are separated, and the portable storage 50 is transported together with the valve 52 to, for example, the analyzer described above. After transportation, the valve 52 is operated, and the inside of the portable storage 50 is brought to atmospheric pressure, and then quickly loaded into the analyzer. In this case, it goes without saying that it is safer to carry out the process while being fixed to the stage 53 holding the side entry type sample stage.
[0074]
By using this portable storage 50, precious samples can be prevented from being contaminated, accidents such as dropping or breaking can be prevented in advance, and they can be easily carried because they are lightweight.
[0075]
The insides of the storage 46 and the portable storage 50 described above are not limited to a vacuum atmosphere, and may be in a clean dry atmosphere, for example. Further, there is no problem even if the storage 46 itself is a thermostatic layer and the internal temperature is constantly controlled to be constant.
[0076]
【The invention's effect】
A sample piece is loaded and the sample installation part of the side entry type sample stage to be loaded into the FIB apparatus has two degrees of freedom of straight advancement and rotation. Extraction of a minute sample and FIB processing become possible.
[0077]
In addition, by providing a sample installation part for the sample piece and the TEM holder, the side entry type sample stage is not required to be inserted or removed, and the micro sample is reliably extracted from the sample piece, transferred to the TEM holder, fixed, and FIB processing. Sample preparation work can be performed consistently, and sample preparation and preparation time can be further shortened.
[Brief description of the drawings]
FIG. 1 is a longitudinal sectional view and a top view showing a first embodiment of the present invention.
FIG. 2 is a bird's-eye view showing the basic configuration of the side entry type sample stage of the first embodiment of the present invention.
FIG. 3 is a longitudinal sectional view and a top view showing a second embodiment of the present invention.
FIG. 4 is a longitudinal sectional view and a top view showing a third embodiment of the present invention.
FIG. 5 is a bird's eye view of a fourth embodiment of the present invention.
FIG. 6 is a longitudinal sectional view and a top view showing a fifth embodiment of the present invention.
7 is a longitudinal sectional view and a top view showing a sixth embodiment of the present invention. FIG.
FIG. 8 is a longitudinal sectional view and a top view showing a seventh embodiment of the present invention.
FIG. 9 is a longitudinal sectional view showing an eighth embodiment of the present invention.
FIG. 10 is a bird's-eye view of a sample preparation apparatus equipped with the side entry type sample stage of the present invention.
FIG. 11 is a bird's-eye view of a storage room storing the side entry type sample stage of the present invention.
FIG. 12 is a longitudinal sectional view showing another embodiment of the storage of the present invention.
FIG. 13 is an external view showing a conventional side entry type sample stage.
FIG. 14 is a bird's-eye view showing a conventional FIB apparatus.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Sample installation part, 1a ... 1st stage, 1b ... 2nd stage, 2 ... Pulley, 3 ... Bearing, 4 ... Arm, 5 ... 2nd pulley, 6 ... Wire, 7 ... 2nd arm, 8 ... Drive shaft, 8a ... screw, 9 ... outer cylinder, 10a ... gear, 10b ... gear, 11 ... micro feed mechanism, 12 ... knob, 13 ... grip part, 14 ... bearing, 15 ... sample piece, 16 ... vacuum seal, 17 DESCRIPTION OF SYMBOLS ... Vacuum container, 18 ... Transfer means, 19 ... TEM apparatus, 20 ... Drive part, 21 ... TEM holder, 22 ... Minute sample piece, 23 ... Opening part, 24 ... FIB apparatus, 25a ... Gear, 25b ... Gear, 26a ... Bevel gear, 26b ... Bevel gear, 27 ... Projection, 28 ... Rotating shaft, 29 ... Center of rotation, 30 ... Drive source, 31 ... Linear bearing, 32 ... Irradiation optical system, 33 ... Ion beam, 34 ... Secondary particle detection 35 ... deposition gas supply source, 36 ... sample 37 ... Sample stage fine movement means, 38 ... Sample preparation device, 39 ... Ion beam control unit, 40 ... Secondary particle detector control unit, 41 ... Deposition gas supply source control unit, 42 ... Stage control unit, 43 DESCRIPTION OF SYMBOLS ... Transfer means control part, 44 ... Image display part, 45 ... Calculation processing part, 46 ... Storage, 47 ... Cover, 48 ... TEM sample, 49 ... Fixing jig, 50 ... Portable storage, 51 ... Exhaust device, 52 ... valve, 53 ... stand.

Claims (6)

An ion beam irradiation optical system for irradiating a specimen with a focused ion beam;
Secondary particle detecting means for detecting secondary particles generated by irradiation of the focused ion beam;
A deposition gas supply source for supplying a source gas for forming a deposition film in the focused ion beam irradiation region;
A transfer means for transferring the extracted sample from which a part of the sample piece is separated;
And the side entry type sample stage, the sample preparation apparatus having,
The side entry type sample stage is provided with a sample setting part including a first stage on which the sample piece is placed and a second stage on which the extracted sample is placed,
A sample preparation comprising: means for moving the sample setting portion straightly in parallel with the central axis of the side entry type sample stage; and means for rotating the sample setting portion with a direction perpendicular to the central axis as a rotation axis apparatus. In the sample preparation device according to claim 1 ,
The side entry type sample stage has a configuration in which a rotation moving member of the sample setting part is loaded on a straight movement member of the sample setting part, and the straight movement and rotation movement of the sample setting part are introduced from the atmosphere side to the vacuum side. And a single drive shaft capable of rotating and moving in a straight line. In the sample preparation device according to claim 1 or 2 ,
The above-mentioned side entry type sample stage is a focused ion beam device, a projection ion beam device, a transmission electron microscope, a scanning electron microscope, a scanning probe microscope, an Auger electron spectrometer, an electron probe X-ray microanalyzer, an electron energy defect analysis A sample preparation device characterized in that the sample preparation device can be loaded into at least one of an apparatus, a secondary ion mass spectrometer, a secondary neutron ionization mass spectrometer, an X-ray photoelectron spectrometer, or an electric measurement device using a probe. In the sample preparation device according to any one of claims 1 to 3 ,
It has a depot storing the side entry type sample stage, a sample in which the vault, characterized in that it is a or under dry 燥雰囲気vacuum atmosphere, and or depot Store under isothermal atmosphere Production device. In the sample preparation device according to any one of claims 1 to 4 ,
A part of the side entry type sample stage including the sample setting part is removable. In the sample preparation device according to claim 4 ,
The sample preparation apparatus, wherein the storage is a storage for sealing a part of the side entry type sample stage including the sample setting section.

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