JP2010204118A - Sample holder - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample preparing method and device for sampling (extracting) only a sample piece including a desired specific region from a semiconductor wafer or a device chip and mounting it on a sample stage of an analyzing/measuring device without going through a manual sample preparing process which requires experience, skill and time. <P>SOLUTION: Techniques for FIB machining, transfer of an extracted sample and fixing of the extracted sample to a sample holder are used. Experience and skill in preparation of a sample for analysis and measurement are eliminated, and time from determination of a sampling part to loading to various devices can be shortened to improve overall efficiency in analysis and measurement. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

The present invention relates to a sample holder .

  In semiconductor element manufacturing, it is required to continue producing good products without stagnation. Since the number of production is large, the occurrence of defects in a certain process leads to a decrease in product yield and production line stoppage, which greatly affects profitability. For this reason, at the manufacturing site of semiconductor elements, careful inspection is performed after a specific process or after the device is completed, and efforts are made to eliminate defective products and to investigate the causes. Actually, in the manufacturing process, wafers and devices are extracted regularly or at a fixed number, and the presence or absence of defective portions is inspected. In the case of wafers, the inspection location and inspection items are determined in advance, and each wafer is constantly monitored to detect abnormalities in the manufacturing process. If there is an abnormal part such as a pattern defect or a foreign object, the device is discarded or a countermeasure is taken to investigate the cause of the abnormality.

  As an example of the inspection method, there is an inspection method for detecting adhesion of foreign matters or defects in a circuit pattern formed on the entire surface of a wafer or a partial area of the wafer. There are a wafer inspection device), a wafer inspection electron microscope (hereinafter abbreviated as inspection SEM), and a prober device for detecting an electrical failure such as a circuit disconnection or short circuit.

More detailed the sample external observation of high-resolution scanning electron microscope (hereinafter, SEM hereinafter) although Ru is used, with high integration of the semiconductor, as ultrafine those objects can not be observed at a resolution of SEM Need to be analyzed. In this case, a transmission electron microscope (hereinafter abbreviated as TEM) having a high observation resolution instead of SEM is a promising apparatus.

Here, a method for preparing a sample for TEM will be described. FIG. 2 is a diagram for explaining one of the conventional methods for producing a TEM sample. FIG. 2A shows a semiconductor wafer (hereinafter referred to as a wafer 30 for short) on which an LSI is formed, and includes an upper layer portion 32 and a substrate portion 31 . Assume that a TEM sample is produced for a specific region of the wafer 30. First, an area to be observed is marked, and the wafer 30 is scratched and cleaved with a diamond pen or the like so as not to destroy the observation area, or is divided along a cutting line 33 with a dicing saw, for example. 2 pieces of strip-shaped pellets 34 as shown in FIG. 2 (b), in order to make the central portion of the TEM sample to be an observation region, the observation regions are bonded with an adhesive 35 so as to face each other, A bonded sample 36 is made (FIG. 2 (c)). Next, the bonded sample 36 is sliced with a diamond cutter, and a slice sample 37 is cut out (FIG. 2 (d)). The size of the slice sample 37 is about 3 × 3 × 0.5 mm. Further, the slice sample 37 is thinly polished on a polishing board using an abrasive to produce a polished sample 38 having a thickness of about 20 μm, and this is fixed to a single-hole TEM holder 39 mounted on the TEM stage (see FIG. 2 (e)). Then the ion beam 40 irradiated on both surfaces of the polishing sample 38 (FIG. 2 (f)), by ion thinning (FIG. 2 (g)), the ion beam 40 irradiated the opened hole in the center portion It stops and it is set as the TEM sample 41 (FIG.2 (h)). Thus, the thin piece portion 42 thinned to about 100 nm or less was used as a TEM observation region (in the circle in the figure). Because of this method, positioning is very difficult when the location to be observed is specified at the micron level.

  In addition, there is an example in which focused ion beam (hereinafter abbreviated as FIB) processing is used as another conventional method relating to TEM sample fabrication. This will be described with reference to FIG. First, the wafer 30 is diced in the vicinity of the region to be observed as shown in FIG. 3A (reference numeral 33 is a cutting line) to cut out the strip-shaped pellet 34 (FIG. 3B). The size of the pellet is approximately 3 × 0.05 × 0.5 mm (wafer thickness). This strip-shaped pellet 34 is fixed to a TEM sample holder 37 made of a slightly semicircular thin metal piece (FIG. 3 (c)). The observation area in the strip-shaped pellet 34 is irradiated with the FIB 24 so as to leave a thin piece portion (hereinafter referred to as a wall portion) 43 having a thickness of about 0.1 microns (FIG. 3 (d)) to form a thin wall portion. (Hereinafter referred to as wall processing. FIG. 3 (e)). Using this as a TEM sample 41, a TEM holder is mounted on a TEM stage, introduced into a TEM apparatus, and the wall portion 43 is observed. By this method, the observation part can be positioned at a micron level. This technique is described in, for example, E.C.G.Kirk et al. In the collection of papers Microscopy of Semiconducting Materials 1989, Institute of Physics Series No.100., P.501-506 (Prior Art 1).

  As described above, TEM can be expected to provide high-resolution observation, but has the aspect of requiring a great deal of effort for sample preparation.

Microscopy of Semiconducting Materials 1989, Institute of Physics Series No.100., P.501-506

  As described above, the conventional sample analysis method and sample preparation method have the following problems. (1) Coordinate problem: When analyzing a defective part such as a foreign substance or a defect found by inspection of the entire surface or a part of the wafer, the coordinates of the defective part are clarified in an inspection apparatus such as a wafer inspection apparatus or inspection SEM. However, it must be divided into dimensions that can fit into the analyzer, observation device, and measurement device (hereinafter referred to as the “analyzer” for short), and processed into an analytical sample piece. There is a problem that the position is not known and the desired analysis cannot be performed.

(2) Problem of sample preparation: Even if a defective part is detected at a certain position as a result of inspection of the whole or part of the wafer by a wafer inspection apparatus or inspection SEM, In some cases, the minute foreign matter disappears or deteriorates, or another damage is caused and superimposed, and the cause of the original defective portion cannot be investigated. This is because the conventional sample preparation method relied on mechanical and chemical methods such as cutting, polishing, and cleaving of the sample, and the yield of obtaining accurate analysis results by introducing the original defective part into the analyzer as it was. Was not expensive. In addition, since such an accurate analysis takes a long time, defective products may occur in succession in the final product, resulting in a great deal of damage.

(3) wafer breakage problem: in order to that monitor the finish in some of course the manufacturing process, in a continuous inspection of a particular portion of the wafer only periodically every quantitation number, only a few points examined The wafer is divided into locations, and everything except the inspection location is discarded. Recently, the wafer diameter has become 200 mm, and the diameter tends to increase to 300 mm and beyond, so wafers with many high-value-added devices can be separated by cutting or cleaving for several inspections. Disposing of it was very uneconomical.

Here, a TEM sample will be described as an example related to any of the problems (1) to (3). TEM has a high resolution as described above, so it is a powerful tool for analysis of minute parts, but it takes a very long time from the identification of a defective area to the result of analysis. It is not as widespread as SEM with immediate results. One of the causes of the long time required for analysis results is the sample preparation process before TEM observation. Since the thickness of the TEM observation region must be reduced to about 100 nm, the conventional method is accompanied by manual operations that require the skill of the sample creator, such as polishing and machining. Moreover, if the observation region is specified at the micron level, sample preparation becomes extremely difficult. In addition, the position of a defective area, which has been specified in a micron order in advance by a microscope, is often lost or mistaken during sample preparation. In addition, since a desired sample piece is produced from a wafer by mechanical processing such as wafer cleavage or cutting, new damage to the sample may occur, making it impossible to distinguish the original defective area. Furthermore, the sample chamber of the TEM is very small, and the sample piece must be subdivided into a size on the order of millimeters, and the wafer must be divided. Once analysis or observation is performed , if another analysis or observation is required at an adjacent location, the subsequent analysis area may be damaged or damaged due to the division of the previous sample preparation. This causes a problem that the accurate positional relationship is not known and continuous analysis and observation information cannot be obtained.

With respect to such a conventional technique, with respect to a defective portion obtained by various inspection methods, while maintaining the wafer shape, without overlapping mechanical or chemical damage only on a desired portion on the wafer, There has been a demand for a sample analysis method and a sample analysis apparatus that can be processed and analyzed into sample pieces that can be introduced into various analysis apparatuses .

An object of the present invention relates to shortening the time required for observation with a transmission electron microscope.

In the present invention, by finishing subjected to thin-wall processability by further focused ion beam irradiating the specimen pieces were fixed to the sample holder to the sample for transmission electron microscope observation, a time required for transmission electron microscopy Can be greatly reduced.

By using the present invention, it is possible to prepare a sample for other analysis, measurement, and observation starting from TEM observation without manual operation from the wafer, and shorten the time until obtaining the analysis result. .

The block diagram which shows one Embodiment of the sample analyzer by this invention. The figure for demonstrating the preparation procedure of the conventional TEM sample. The figure for demonstrating another preparation procedure of the conventional TEM sample. The block diagram for demonstrating one Embodiment of the sample preparation part among the sample analyzers by this invention. The figure for demonstrating especially a sample holder by embodiment of the sample analyzer by this invention. The figure for demonstrating the conventional TEM holder. The figure for demonstrating one Embodiment of especially a transfer means among the sample preparation parts in embodiment of the sample analyzer by this invention. The block diagram which shows another embodiment of the sample analyzer by this invention. The figure for demonstrating the sample preparation process in the sample analysis method by this invention. It is a figure for demonstrating the conventional sample holder for TEM.

An embodiment of a sample preparation apparatus according to the present invention includes a wafer inspection unit that inspects a wafer and stores coordinate information of a desired location such as a foreign substance or a defect, and a focused ion with respect to a sample substrate based on the coordinate information of the desired location. A sample piece that includes the desired portion is extracted using a beam, fixed to a sample holder suitable for at least one of an analysis device, an observation device, and a measurement device, and processed into a shape corresponding to these devices The wafer inspection unit and the sample preparation unit are connected by a vacuum transfer path for moving the wafer.
Below, the concrete example of embodiment is shown.

<Embodiment 1>
FIG. 1 is a schematic configuration diagram showing an embodiment of a sample analyzing apparatus for realizing a sample analyzing method according to the present invention.
In the sample analyzer 100, a wafer inspection unit 101 and a sample preparation unit 102 are mechanically connected. The wafer inspection unit 101 corresponds to a wafer appearance inspection apparatus, an inspection SEM, and a prober apparatus. When it is necessary to detect and analyze a defective portion by wafer inspection, the valve 106 installed between the wafer inspection unit 101 and the sample preparation unit 102 can be opened to transfer the wafer 12 to the sample preparation unit 102. The sample piece processed and prepared by the sample preparation unit 102 is carried into another observation device such as TEM or SEM, an analysis device, a measurement device, or the like, and the defective portion is analyzed. On the contrary, if there is no abnormality as a result of the wafer inspection, the wafer 12 does not need to be sent to the sample preparation unit 102 and is transferred to the apparatus for the next manufacturing process.

  As an example of the wafer inspection unit 101, an inspection SEM is shown here. A sample stage on which the wafer 12 is placed and moved in the electron beam irradiation optical system 103, the secondary electron detector 104, and the sample chamber 107. 105 or the like. The secondary electron signal flowing into the secondary electron detector 104 and the beam deflection of the electron beam irradiation optical system 103 can be synchronized so that the wafer surface shape can be displayed on the display means 13 ′, and the control of the entire wafer inspection unit 101 can be controlled by a calculation processing device. 17 '. The wafer inspection includes a method of comparing a plurality of devices formed on the wafer and a method of comparing cells in the devices, but is not limited here. The coordinate information of the desired portion detected by the wafer inspection unit 100 can be temporarily stored in the calculation processing device 17 ′ and transmitted to the calculation processing unit 17 of the sample preparation unit 102 by the information transmission unit 110. Also, the wafer appearance and coordinate information during inspection can be displayed on the display means 13 '.

The sample preparation unit 102 includes an FIB irradiation optical system 2 that processes and observes the sample substrate 12 and the extracted sample, a secondary particle detector 3 that detects secondary electrons and secondary ions emitted from the sample by this FIB irradiation, and an FIB. A deposition gas source 4 for supplying a source material gas for forming a deposition film in an irradiation region, a sample stage 5 for mounting a sample substrate 12 such as a semiconductor wafer or a semiconductor chip, and a transfer means 8 for transferring an extracted sample to a sample holder An optical microscope 9 for observing the sample substrate 12, display means 13 for displaying an image by the optical microscope 9 and an image by the secondary particle detector 3, a calculation processing device 17 for controlling the entire sample preparation unit 102, and a sample stage 5 It is the structure provided with at least the sample chamber 18 etc. which installs. Further details will be described with reference to FIG.

4 shows, in addition to the components shown in FIG. 1, a sample holder 6 for fixing a minute extracted sample obtained by extracting a part of the sample substrate 12, and a holding means 7 for holding the sample holder (hereinafter also referred to as a holder cassette). ), A stage control apparatus 10 for controlling the position of the sample stage 5, a transfer means control apparatus 11 for driving the transfer means 8 independently of the sample stage 5, a sample holder 6, the sample substrate 12, the transfer means 8, and the like. It consists of image display means 13 for imaging with secondary electrons or secondary ions generated by ion beam irradiation, FIB control device 14 of FIB irradiation optical system 2, etc. In addition, deposition gas source control device 15, secondary particle detection The control device 16, the image display means 13, the transfer means control device 11 and the like are controlled by the calculation processing device 17.

The FIB irradiation optical system 2 forms the FIB 24 having a diameter of about 10 nm to about 1 micron by passing the ions emitted from the liquid metal ion source 20 through the beam limiting aperture 21, the focusing lens 22, and the objective lens 23. By scanning the sample substrate 12 with the FIB 24 using the deflector 25, the sample substrate 12 can be processed in the scanning shape from the micron to the submicron level. The processing here refers to a concave portion formed by sputtering, a convex portion formed by FIB assist deposition, or an operation for changing the shape of the sample substrate by combining these. The deposition film formed by FIB irradiation is used to connect the contact portion at the tip of the transfer means 8 and the sample substrate 12 or to fix the extracted sample to the sample holder. In addition, the processing region and the like can be observed by detecting secondary electrons and secondary ions generated during the FIB irradiation with the secondary particle detector 3 and imaging them.

  The sample stage 5 is installed in the sample chamber 18, and the FIB irradiation optical system 2 and the like are also arranged in the vacuum container. A holding means (sample holder cassette) 7 on which the sample holder 6 is mounted can be attached to and detached from the sample stage 5, and movement, tilt, and rotation in the three-dimensional (X, Y, Z) direction are controlled by the stage controller 10. The The sample substrate 12 enters and exits using the sample substrate transport path 19 as necessary.

  The sample holder 6 is a strip-shaped silicon piece 27 having a convex cross section as shown in FIG. The strip-shaped silicon piece 27 was formed by cleaving from a silicon wafer or using a dicing saw. The sample holder used in this example has a length of 2.5 mm, an upper width of 50 microns, a lower width of 200 microns, a height of 0.5 mm (silicon wafer thickness), and the fixed surface of the extracted sample is a silicon wafer surface or a cleavage surface. Thus, even if the extracted sample 70 is fixed to the fixed surface and observed by TEM, the unevenness of the fixed surface does not hinder the electron beam irradiation. Further, the shape of the sample holder is not limited to the dimensions shown here, but it is necessary to make the fixed surface a wafer surface or a cleaved surface and to make the width as thin as possible in order to facilitate TEM observation. FIG. 5 shows an example in which three extracted samples 70 are mounted on one sample holder 6. On the other hand, the conventional sample holder for TEM is the single hole type of FIG. 6 (a) or the mesh type of (b). The single hole type has a single hole 75 having a diameter of about 1 mm in the center and a diameter of about 3 mm. Although it is a thin metal disc 76, if it is as small as 10 to 20 microns like the extracted sample 70 obtained by the sample preparation method according to the present invention, it is very difficult to attach the extracted sample 70 to the side wall of the single hole 75 accurately. . In the case of the mesh type, the mesh 77 is attached to the thin metal disk 76, and if the mesh 77 having an interval according to the size of the sample is used, the attachment position can be arbitrarily selected. There was a very high risk that the line path would be behind the mesh 77 and TEM observation would not be possible.

  The holder cassette (holding means) 7 is a jig that supports the sample holder 6 and is mounted on the sample stage 5. The sample stage 5 refers to a general-purpose large stage on which a wafer can be placed or a small stage to which a device chip can be mounted. One or more sample holders 6 may be mounted on one holder cassette 7. The number of holder cassettes 7 that can be installed on the sample stage 5 may be one or more.

As the optical microscope 9, a laser scanning microscope which can be expected to have a higher resolution than a conventional optical microscope was used. The laser scanning microscope focuses the laser beam emitted from the oscillator 28 by the objective lens and irradiates the sample, and the fluorescence from the focal point excited by the minute laser spot passes through the dichroic mirror and is confocal with the focal point of the sample. An image is formed only by the fluorescence from the focal point of the sample after reaching the CCD 29 through the aperture set at the position of. Very little stray light compared to a method of uniformly exciting the field, even in the event the fluorescence focus except or al Assuming clear statue not reach is obtained in CCD29 hampered in the aperture. By installing two mirrors between the sample substrate 12 and the dichroic mirror and scanning in the X and Y directions, a sample surface image can be obtained and displayed on the display means 13. The optical microscope 9 uses mark (not shown) coordinates previously set on the sample substrate 12 and coordinate information obtained by the inspection unit 101 .
An apparatus provided with a laser microscope in a focused ion beam apparatus is disclosed in Japanese Patent Application Laid-Open No. 9-134699 “Focused Ion Beam Apparatus” (Known Example 3), and a specific region portion of the sample substrate 12 is extracted. The presence of the transfer means 8 is not described at all.

Even if the sample substrate is a large-diameter wafer, the transfer means 8 has a coarse moving part 60 having a high moving speed and a large stroke, and a moving resolution of the coarse moving part in order to realize quick sampling from an arbitrary position. And the fine moving part 61 having a high movement resolution with the same stroke as the above, and the entire transfer means is installed independently of the sample stage, and the large movement of the sampling position is shared by the movement of the sample stage. The coarse moving part is driven in the XYZ directions by motors, gears, piezoelectric elements, etc., and has a moving resolution of several microns with a stroke of about several millimeters. Since the fine movement portion is required to be as compact as possible and to move precisely, a sub-micron moving resolution is obtained using a bimorph piezoelectric element. FIG. 7 shows a configuration example of the coarse movement part 60 and the fine movement part 61 of the transfer means 8. In the coarse movement part 60, the support 63 can be moved in the XYZ axis direction by three encoders 64X, 64Z, 64Y (not shown) with the narrowed part 62 as a fulcrum. The drive system of the coarse movement unit 60 is on the atmosphere side through the lateral port of the sample chamber wall 66, and the vacuum is blocked by the bellows 65. The tip of the bimorph piezoelectric element 67 was connected with a thinly sharpened tungsten probe 68 having a diameter of about 50 microns, and connected with the coarse movement portion 60 by an extension rod 69. By applying a voltage to the bimorph piezoelectric element 67, the tip of the probe 68 finely moves. Thus the transfer means 8, the configuration, size, must be sufficiently taken into account the installation position, the sample preparation apparatus according to the present invention solves all of these.

As a conventional technique similar to the transfer means 8, there is JP-A-5-52721 “Sample separation method and analysis method of a separated sample obtained by this separation method” (known example 2).
According to this prior art, the transport means for transporting the separated sample is constituted by three bimorph piezoelectric elements corresponding to the XYZ axes. However, the installation position of the transport means is unknown, and only from FIG. Can be read if installed on stage. Thus, when the transfer means is installed on the sample stage, when the target sample is at the center of a wafer having a diameter of 300 mm, for example, the movement stroke at the tip of the transfer means is from the position of the transfer means to the desired location of the sample. Since it is far smaller than the distance, it has a fatal problem that it cannot be reached by the transfer means installed on the sample stage. Further, in the configuration of the bimorph piezoelectric element with these three axes, the bimorph piezoelectric element moves with the other end deflecting with one end as a fulcrum, so the other end draws an arc according to the applied voltage. That is, in the movement in the XY plane, the probe at the tip of the transport means does not move linearly in one axial direction only by the operation of one bimorph piezoelectric element. Therefore, in order to configure the fine movement portion with three bimorph piezoelectric elements and move the probe tip to a desired position, the three bimorph piezoelectric elements must be controlled very complicatedly. .

<Embodiment 2>
In the first embodiment, the example in which the wafer inspection unit 101 and the sample preparation unit 102 are mechanically coupled to carry the wafer as the sample substrate 12 between both apparatuses has been described. The second embodiment is an example in which the wafer inspection unit 101 and the sample preparation unit 102 are mechanically independent as shown in FIG. 8, and the coordinate information of the defective portion travels between the calculation processing devices 17 and 17 ′. . The wafer 12 which is a sample substrate is transported by being enclosed in a transport container 107 which is small and can be evacuated. Coordinate information and the like in the wafer inspection unit 101 can be transmitted from the calculation processing device 17 ′ to the calculation processing device 17 of the sample preparation unit 102 through the information transmission unit 110. With such a configuration, the defective portion of the wafer 12 detected by the wafer inspection unit 101 is processed and manufactured in the sample preparation unit 102 into a shape that can be easily analyzed by various analysis apparatuses.

<Embodiment 3>
Next, an embodiment of a sample analysis method according to the present invention will be described. Here, a sample piece manufacturing method to be observed by TEM will be taken as an example of the sample, and a specific description of the sample analysis method from wafer observation to sample piece processing and TEM observation will be given. Further, in order to clarify the procedure, it will be described below with reference to the drawings divided into several steps.

(1) Appearance inspection process:
First, the entire surface of the wafer to be inspected or a part thereof is inspected for abnormalities. The inspection contents include a visual inspection such as a wafer inspection device using light (laser) and an inspection SEM using an electron beam, and an electric circuit inspection using a probe device. By this inspection, it is possible to know the position of a defective part such as a foreign object, a defect, or a wiring abnormality. At this time, the calculation processing apparatus stores the corresponding device coordinates of the defective portion on the basis of a mark (wafer mark) previously set on the wafer and coordinate information based on the mark previously set on the corresponding device.

(2) Sample preparation process
(a) Marking process:
The wafer is introduced into the sample preparation unit, and first, a mark (device mark) of the corresponding device is searched. Here, the device mark is searched for with a laser microscope installed in the sample preparation section. The above-mentioned defective part is found by a more detailed search. At this time, when searching by a secondary electron image by FIB irradiation, the sample surface is sputtered by FIB, so the surface is damaged, and in the worst case, a defective object to be analyzed is desired. Will be lost. Therefore, the coordinates of the defective part in the sample preparation apparatus were derived by calculation based on the coordinates of the wafer mark, device mark and defective part at the time of wafer inspection, and the coordinates of the wafer mark and device mark in the sample preparation part. After that, FIB is marked in multiple places so that the defective part can be confirmed.

  In this example, as shown in FIG. 9a, two + marks 80 are provided at intervals of 10 microns across the observation region. The sample stage is rotationally adjusted in advance so that the straight line connecting the two marks is parallel to the tilt axis of the sample stage.

(b) Large rectangular hole machining process:
Two rectangular holes 82 were provided by FIB 81 on both sides of the two marks on a straight line connecting the two marks 80. The opening size is, for example, 10 × 7 microns, the depth is about 15 microns, and the interval between both rectangular holes is 30 microns. Both were processed with a large current FIB with a diameter of about 0.15 microns and a current of about 10 nA in order to complete in a short time. Processing time was approximately 5 minutes.

(c) Vertical grooving process:
Next, as shown in FIG. 9b, the width is about 2 microns apart from the straight line connecting the marks 80 and about 2 microns wide so that it intersects with one rectangular hole 82 and does not intersect with the other rectangular hole. An elongated vertical groove 83 having a depth of about 30 microns and a depth of about 10 microns is formed. The beam scanning direction is set so as not to fill vertical grooves and large rectangular holes formed by sputtered particles generated when the sample is irradiated by the FIB. A small region that does not intersect with one rectangular hole 82 becomes a support portion 84 that supports a sample to be extracted later.

(d) Inclined groove machining process:
After the steps (b) and (c), the sample surface is inclined slightly (20 ° in this embodiment). Here, the straight line connecting the two marks 80 is set parallel to the tilt axis of the sample stage. Therefore, as shown in FIG. 9c, the width is about 2 microns and the length is about 2 microns apart from the straight line connecting the marks 80, and the rectangular holes 82 are connected to the opposite side of the elongated vertical groove 83. A groove having a depth of about 32 microns and a depth of about 15 microns is formed. The rectangular hole 82 formed by the sputtered particles by FIB irradiation is not filled. An elongated inclined groove 85 is formed by FIB 81 incident obliquely with respect to the sample substrate surface, and intersects with the previously formed elongated vertical groove 83. By the steps (b) to (d), the wedge-shaped extracted sample having a right triangle cross section with the apex angle of 70 ° is held in the state of a cantilever, leaving the support portion 84. .

(e) Probe fixing depot process:
Next, the sample stage is returned to the horizontal position as shown in FIG. 9d, and the probe 87 at the tip of the transfer means is brought into contact with the end opposite to the support portion 84 of the sample 86 to be extracted. The contact can be sensed by conduction between the sample and the probe or a change in capacitance between the two. In addition, in order to avoid damaging the sample 86 and the probe 87 to be extracted by careless pressing of the probe 87, it has a function of stopping driving in the + Z direction when the probe contacts the sample. Next, in order to fix the probe 87 to the sample 86 to be extracted, the FIB is scanned while allowing the deposition gas to flow out into an area of about 2 microns including the probe tip. In this way, the deposition film 88 is formed in the FIB irradiation region, and the probe 87 and the sample 86 to be extracted are connected.

(f) Extracted sample extraction process:
In order to extract the extracted sample from the sample substrate, the supporting portion 84 is released from the supporting state by FIB irradiation and sputter processing. Since the support portion 84 is 2 microns square and about 10 microns deep when viewed from above the sample surface, it can be removed by FIB scanning for 2 to 3 minutes. (Fig. 9e, f)

(g) Extracted sample transport (sample stage movement) process:
Although the extracted sample 89 connected to the tip of the probe 87 is moved to the sample holder, the sample stage is actually moved to move the sample holder 90 into the FIB scanning region. At this time, in order to avoid an unexpected accident, the probe may be retracted in the + Z direction . ( Figure 9g)

(h) Extracted sample fixing process:
When the sample holder 90 enters the FIB scanning region, the movement of the sample stage is stopped, and the probe is moved in the −Z direction so as to approach the sample holder 90. When the extracted sample 89 comes into contact with the sample holder 90, FIB is irradiated to the extracted sample 89, the sample holder 90, and the contact portion while introducing deposition gas. By this operation, the extracted sample can be connected to the sample holder. In this embodiment, the deposition film 92 is formed on the end surface of the extracted sample 89 in the longitudinal direction.
The FIB irradiation area is about 3 microns square, part of the deposition film 92 is attached to the sample holder 90, and part is attached to the side of the extracted sample, and both are connected. (Fig. 9h)

(i) Probe cutting process:
Next, after stopping the introduction of the deposition gas, the probe 87 can be separated from the extracted sample 89 by irradiating the deposited film connecting the probe 87 and the extracted sample 89 by irradiating with FIB 81 and removing the sputter. The sample 89 stands on the sample holder 90. (Fig. 9i)

(j) Sample piece processing step (wall processing):
Finally, FIB irradiation is performed, and finally the observation region is thinly processed so as to become a wall 93 having a thickness of about 100 nm or less to obtain a TEM sample. At this time, since one of the longitudinal side surfaces of the extracted sample is a vertical surface, when determining the FIB irradiation region for wall processing, a wall substantially perpendicular to the surface of the sample substrate 89 is obtained by using this vertical surface as a reference. 93 can be formed. Prior to FIB irradiation, an FIB deposit film may be formed on the upper surface including the wall formation region in order to process the wall surface more planarly. This method is already well known. As a result of the above processing, a wall having a width of about 15 microns and a depth of about 10 microns can be formed, and a TEM observation region is completed. As described above, the time from marking to completion of wall processing was about 1 hour and 30 minutes, and the time could be reduced to a fraction of that of the conventional TEM sample preparation method. (Fig. 9 j)

(3) Analysis process (TEM observation):
After wall processing, the sample holder is introduced into the TEM sample chamber. At this time, the TEM stage is rotated and inserted so that the electron beam path and the wall surface intersect perpendicularly. Since subsequent TEM observation techniques are well known, they are omitted here.

In the sample analysis method, there is a known example 2 as a conventional technique similar to the sample preparation process. In order to show that this sample preparation process is completely different from the conventional method, the conventional method will be described with reference to FIG. First, the posture of the sample 50 is maintained so that the FIB 24 irradiates at right angles to the surface of the sample 50, and the FIB 24 is scanned in a rectangular shape on the sample to form a square hole 51 having a required depth on the sample surface (FIG. 10). (a)). Next, the sample is tilted so that the FIB axis with respect to the sample surface is tilted by about 70 ° to form the bottom hole 52. The tilt angle of the sample is changed by a sample stage (not shown) (FIG. 10 (b)). The orientation of the sample is changed, the sample is placed so that the surface of the sample becomes perpendicular to the FIB again, and a notch groove 53 is formed (FIG. 10 (c)). A manipulator (not shown) is driven, and the tip of the probe 54 at the tip of the manipulator is brought into contact with a portion where the sample 50 is separated (FIG. 10 (d)). A deposition gas 56 is supplied from a gas nozzle 55, and FIB is locally irradiated to a region including the tip of the probe to form an ion beam assisted deposition film (hereinafter abbreviated as a deposition film 57). The separation portion of the sample in contact with the tip of the probe 54 is connected by a deposition film 57 (FIG. 10 (e)). The remaining part is cut and processed with the FIB 24 (FIG. 10 (f)), and the separated sample 58 is cut out from the sample 50. The cut out separated sample 58 is supported by the connected probe 54 (FIG. 10 (g)). When this separated sample 58 is processed by FIB in the same manner as the second conventional method and the region to be observed is wall processed, a TEM sample (not shown) is obtained.

  In order to extract a minute sample from a sample substrate, it is essential to separate the minute sample from the substrate, which involves a separation step (hereinafter referred to as a bottom edge) between the surface to be the bottom surface of the extracted sample and the substrate. In the bottoming method using FIB shown in the known example 2, since the FIB is incident on the substrate surface from an oblique direction and processed, the ion beam incident angle and processing aspect at the time of bottoming are placed on the bottom surface of the extracted sample piece. There is a slope of ratio. Also, the square hole 51 for realizing FIB irradiation from an oblique direction shown in FIG. 10b must be very large. This indicates that a great deal of time is required when forming the square hole 51. In this known example, the sample is tilted by about 70 ° in order to perform oblique FIB irradiation. Considering the distance between the objective lens and the sample required from the FIB focusing property, such a large inclination deteriorates the FIB performance, and it is expected that satisfactory processing cannot be performed. In order to maintain the performance of the FIB device that is normally used, the limit is about 60 °. In addition, it is very difficult mechanically to tilt a large-diameter wafer sample stage having a diameter of 300 mm by as much as 70 °. Even if a large inclination of 70 ° is possible, the bottom surface of the extracted sample has an inclination of 70 °, and when placed on a horizontal sample holder, the original sample surface is inclined by 20 ° with respect to the sample holder surface. However, it becomes difficult to form a cross section or wall substantially perpendicular to the wall. In order to form a cross section or wall that is almost perpendicular to the surface of the sample substrate, it is essential to reduce the inclination of the bottom surface and make the bottom surface parallel to the surface. Rather, this becomes more difficult due to the device limitations described above. Therefore, in order to install the extracted sample as intended by the present invention in another member (sample holder) and introduce it to another observation apparatus or analysis apparatus, another method for forming a vertical section can be studied. Must. (However, in the known example 2, since the separated sample is not placed in the sample holder but is observed while attached to the probe of the transport means, the shape of the bottom surface does not affect.)

  As described above, the sample preparation process according to the present invention and the sample separation method according to the known example 2 are significantly different from each other in that (1) the beam irradiation method at the time of sample extraction (separation) is completely different, so The side surface in the longitudinal direction (parallel to the TEM observation surface) is inclined to simplify the separation of the bottom surface and to make the inclination of the sample stage as small as possible. (2) The extracted sample is separate from the transfer means. A sample preparation device and a sample preparation method are provided that can be removed from a wafer by fixing to a sample holder which is a member of the above.

<Embodiment example 4>
The sample analysis process of the above embodiment is not limited to TEM analysis, and can be used for other observation techniques, analysis techniques, and observation techniques.

For example, the present invention can also be applied when the analysis device is an in-lens type high resolution SEM.
In-lens type SEM is a method that puts the observation sample in the objective lens and is a powerful tool for surface observation because the resolution is very good compared to the out lens, but for the convenience of putting the sample in the lens, it is about several millimeters Must be small. Therefore, even if a defective part is discovered by a wafer inspection apparatus or the like and the part is further observed, it cannot be introduced into the in-lens scanning electron microscope as it is, but the wafer is divided and subdivided. I had to. According to the sample analysis method according to the present invention, a sample piece in a desired region can be extracted from a wafer, so that high-resolution observation can be performed with an in-lens SEM. Since the observation region can observe not only the wafer surface but also the cross section that can be formed at the time of extraction, if the FIB irradiation direction at the time of sample piece extraction is appropriately performed, the cross section of the defective portion can also be observed. By such a method, sample analysis can be performed by solving the problem of coordinates, the problem of sample preparation, and the problem of wafer division. In addition, sample analysis for performing elemental analysis such as Auger electron spectroscopy or secondary ion mass spectrometry can be performed in the same manner.

  DESCRIPTION OF SYMBOLS 2 ... FIB irradiation optical system, 3 ... Secondary particle detector, 4 ... Depo gas source, 5 ... Sample stage, 6 ... Sample holder, 7 ... Holding means (holder cassette), 8 ... Transfer means, 9 ... Optical microscope, 100 DESCRIPTION OF SYMBOLS ... Sample analyzer, 101 ... Wafer inspection part, 102 ... Sample preparation part, 103 ... Electron beam irradiation system, 104 ... Secondary electron detector, 105 ... Sample stage, 107 ... Container for conveyance, 110 ... Information transmission means.

Claims (1)

A sample stage on which the sample is placed;
A sample chamber in which the sample stage is installed;
An irradiation optical system for irradiating the sample with an ion beam;
A sample holder provided in the sample chamber for placing a sample piece extracted from the sample;
Transfer means for extracting the sample piece from the sample;
Means for moving the sample holder to a predetermined position in the sample chamber,
The sample preparation apparatus, wherein the transfer means is separated from the sample when the sample holder moves.