JP4675701B2 - Ion milling apparatus and ion milling method - Google Patents

Description

  The present invention relates to an ion milling apparatus and an ion milling method for producing a sample observed with a scanning microscope (SEM), a transmission microscope (TEM), or the like.

  An ion milling device is a device for polishing the surface or cross section of metal, glass, ceramic, etc. by irradiating an argon ion beam, etc., and a pretreatment device for observing the surface or cross section of a sample with an electron microscope It is suitable as.

  In the cross-sectional observation of a sample with an electron microscope, conventionally, the vicinity of the part to be observed is cut using, for example, a diamond cutter, a thread saw, etc., and then the cut surface is mechanically polished and attached to a sample stage for an electron microscope. I was observing.

  In the case of mechanical polishing, for example, a soft sample such as a polymer material or aluminum has a problem that the observation surface is crushed or deep scratches remain due to abrasive particles. In addition, for example, a hard sample such as glass or ceramic is difficult to polish, and a composite material in which a soft material and a hard material are laminated has a problem that cross-sectional processing is extremely difficult.

  In contrast, ion milling enables polishing of hard samples and composite materials that can be processed without damaging the surface morphology even with soft samples. There is an effect that a mirror-shaped cross section can be easily obtained.

  Patent Document 1 describes a sample holder and a holder fixture of an ion milling apparatus.

  In Patent Document 2, an ion beam irradiation means for irradiating a sample with an ion beam disposed in a vacuum chamber and an inclination having an inclination axis disposed in the vacuum chamber and in a direction substantially perpendicular to the ion beam. A sample preparation apparatus comprising a stage, a sample holder disposed on the inclined stage and holding the sample, and a shielding material positioned on the inclined stage and blocking a part of an ion beam that irradiates the sample There is described a sample preparation apparatus in which a sample processing by the ion beam is performed while changing an inclination angle of the inclination stage, and an optical microscope for adjusting the position of the sample is attached to an upper end portion of the sample stage drawing mechanism. ing.

JP-A-9-293475 JP 2005-91094 A

  In a conventional ion milling apparatus in which an optical microscope for adjusting the position of the sample is attached to the upper end of the sample stage extraction mechanism, the adjustment of the shielding position between the sample and the mask is in the vicinity of the vacuum chamber and directly above the sample stage extraction mechanism. Work in a limited space must be performed, and it takes time to make adjustments with high accuracy. Whether the optical microscope is in a position almost perpendicular to the sample and whether the sample and mask are in close contact with each other. There is a problem that confirmation cannot be made, and the state of polishing cannot be confirmed unless the sample holder to which the sample is fixed is removed.

  In view of this point, the present invention can confirm whether the sample and the mask are in close contact with each other when the shielding position adjustment between the sample and the mask can be performed with high accuracy and can be easily performed without taking time and effort. Another object of the present invention is to provide an ion milling apparatus and an ion milling method capable of observing a polished state with a mask and a sample in close contact with each other.

  The present invention includes an ion beam source that irradiates a sample with an ion beam, a sample holder fixture that fixes a sample holder that fixes the sample, the sample holder, and a sample fixed to the sample holder. A sample mask unit comprising a mask that partially shields, a sample rotation mechanism that rotates the sample holder, and a mask position adjustment unit that adjusts a shielding position relationship between the mask and the sample, and a vertical direction of the ion beam In an ion milling apparatus provided with a sample mask unit fine movement mechanism capable of XY driving the sample mask unit and an optical microscope for observing a shielding positional relationship between the mask and the sample, the optical microscope is configured separately from the vacuum chamber, The sample mask unit fine movement mechanism can be attached and removed at a fixed position with reproducibility by the positioning shaft and hole. A fixed base to be attached, and at the time of adjusting the shielding positional relationship between the mask and the sample, the sample mask unit fine movement mechanism on which the sample mask unit is installed is removed, and the mask is attached to the fixed base of the optical microscope. Provided is an ion milling apparatus characterized in that a shielding positional relationship with respect to a sample is adjusted by the mask position adjusting unit, returned to a sample fine movement base, and mounted.

  The present invention also includes another fixing base to which the sample mask unit fine movement mechanism is detachably attached at a fixed position with reproducibility by a positioning shaft and a hole, and the sample mask unit fine movement mechanism includes a sample fine movement base. The sample mask has a detachable portion from the sample fine movement base and is detachable at a fixed position with reproducibility by a positioning shaft and a hole, and when adjusting the shielding positional relationship between the mask and the sample, the sample mask The unit fine movement mechanism is detached from the sample fine movement base and mounted on another fixed base of the optical microscope, and the mask has a shielding position relationship with respect to the sample adjusted by the mask position adjusting unit, and a shielding position with respect to the sample during ion milling. The sample mask unit fine movement mechanism having the mask whose relationship is adjusted is returned to the sample fine movement base and mounted. A method of ion milling, which is a shall.

  According to the present invention, when the shielding positional relationship between the sample and the mask is accurately performed, it can be easily performed without taking time for adjustment, and it can be confirmed whether the sample and the mask are closely attached and fixed, and the polished state. It is possible to provide an ion milling apparatus and an ion milling method capable of observing a mask and a sample in close contact with each other.

  Embodiments of the present invention will be described below with reference to the drawings.

  FIG. 1 shows a configuration of an ion milling apparatus according to the present invention, and shows a state in which a sample mask unit and a sample holder fixture are installed inside a vacuum chamber. Below, the case where an argon ion beam is irradiated from an ion source is demonstrated. Therefore, hereinafter, the ion beam means an argon ion beam, but the present embodiment is not limited to the argon ion beam.

  The current density of argon ions in the ion source 1 of argon ions is controlled by the ion source controller 7. The vacuum chamber 15 can be in a vacuum or atmospheric state by controlling the vacuum exhaust system 6 by the vacuum exhaust system controller 9 and can maintain the state.

  The sample fine movement base 5 is configured to fix the sample holder 23 for fixing the sample 3 and to be able to rotate and tilt at an arbitrary angle with respect to the optical axis of the ion beam. It is controlled by the fine movement control unit 8. By rotating and tilting the sample fine movement base 5, the sample 3 fixed to the sample holder 23 can be set at a predetermined angle with respect to the optical axis of the ion beam. Further, the sample mask unit fine movement mechanism 4 is configured to be movable in the front and rear, right and left directions in the direction perpendicular to the optical axis of the ion beam, that is, in the X and Y directions.

  The sample fine movement base 5 is disposed on a flange 10 that also serves as a part of the container wall of the vacuum chamber 15 via a rotation mechanism, and the flange 10 is pulled out along the linear guide 11 to open the vacuum chamber 15 to the atmospheric state. Sometimes, the sample fine movement base 5 is configured to be pulled out of the vacuum chamber. In this way, the sample stage drawing mechanism is configured.

  The configuration of the sample mask unit main body will be described with reference to FIG. 2A is a plan view, and FIG. 2B is a side view. In the embodiment, a configuration in which at least the sample holder 23 and its rotation mechanism, and the mask 2 and its fine adjustment mechanism are integrally formed is referred to as a sample mask unit (main body) 21. In FIG. 2, a sample holder rotating ring 22 and a sample holder rotating screw 28 are provided as a rotating mechanism of the sample holder 23 so that the sample holder can be rotated perpendicularly to the optical axis of the ion beam. The sample holder rotating ring 22 is configured to rotate by turning the sample holder rotating screw 28, and the reverse rotation is returned by the spring pressure of the spring 29.

  The sample mask unit 21 has a mechanism capable of finely adjusting the position and rotation angle of the mask, and can be attached to and detached from the sample mask unit fine movement mechanism 4.

  The mask 2 is fixed to the mask holder 25 by a mask fixing screw 27. The mask holder 25 moves along the linear guide 24 by operating a mask fine adjustment mechanism (that is, a mask position adjustment unit) 26, thereby finely adjusting the positions of the sample 3 and the mask 2. The sample holder 23 is inserted and fixed to the sample holder rotating ring 22 from the lower side. The sample 3 is bonded and fixed to the sample holder 23. The position of the sample holder 23 in the height direction is adjusted by the sample holder position control mechanism 30, and the sample holder 23 is brought into close contact with the mask 2.

  FIG. 3 shows another example of the sample mask unit 21. In this example, the sample holder fixing bracket 35 is used, and the other configuration is basically the same as the example shown in FIG. FIG. 3A shows a state in which the sample holder 23 to which the sample 3 is fixed is mounted in the sample mask unit 21, and FIG. 3B shows that the sample holder 23 to which the sample 3 is fixed is removed from the sample mask unit 21. Indicates the state.

FIG. 4 is an explanatory view showing a method of making the cross section of the sample parallel to the mask.
The sample holder rotating screw 28 is rotated to adjust the position in the X1 direction, and fine adjustment is performed under the microscope as described later so that the cross section of the sample 3 and the ridge line of the mask 2 are parallel. At this time, the fine adjustment mechanism 26 is set so that the cross section of the sample 3 slightly protrudes from the mask, for example, approximately 50 μm.

FIG. 5 shows the configuration of the sample stage drawing mechanism 30. The sample stage extraction mechanism 30 includes a linear guide 11 and a flange 10 fixed to the linear guide 11, and the sample fine movement base 5 fixed to the flange 10 is extracted from the vacuum chamber 15 along the linear guide 11 . Along with this operation, the sample mask unit fine movement mechanism 4 in which the sample mask unit 21 is installed on the sample fine movement base 5 is installed, that is, the mask 2, the sample holder 23, and the sample 3 are drawn out from the vacuum chamber 15.

  In this embodiment, the sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 has a configuration that is detachably fixed to the sample fine movement base 5. Accordingly, when the sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 is pulled out of the vacuum chamber 15, the sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 is made detachable from the sample fine movement base 5. The (Removal standby of sample mask unit 21)

  FIG. 5 shows a state in which the sample mask unit fine movement mechanism 4 in which the sample mask unit 21 is installed is detached from such a detachable state. This attachment / detachment is performed manually or with an appropriate instrument.

  On the other hand, as shown in FIG. 6, the optical microscope 40 for observing the shielding positional relationship between the mask 2 and the sample 3 is configured separately from the vacuum chamber 15 and can be arranged at an arbitrary location. The optical microscope 40 includes a known loupe 12 and loupe fine movement mechanism 13. Further, the optical microscope 40 is provided with a fixed base 42 for installing the sample mask unit fine movement mechanism 4 on which the sample mask unit 21 removed from the observation table 41 is installed. The optical microscope 40 is reproducible by a positioning shaft and a hole. The sample mask unit fine movement mechanism 4 in which the sample mask unit 21 is installed at a predetermined position is installed on the fixed base 42.

  FIG. 7 shows a state in which the sample mask unit fine movement mechanism 4 on which the sample mask unit 21 is installed is fixed on the fixed base 42.

  FIG. 8 is an explanatory diagram showing a method for aligning the portion of the sample 3 whose cross section is to be polished with the center of the ion beam. A photosensitive paper or the like is attached to the sample holder 23, and the trace formed by irradiating the ion beam, that is, the center of the beam and the center of the loupe are driven by the loupe fine movement mechanism 13 to drive X2, Y2. The sample mask unit fine movement mechanism 4 on which the sample mask unit main body 21 after the sample 3 is installed in FIG. By adjusting the position of the fixing base 42 in the X3 and Y3 directions to match the center of the loupe, it is possible to match the center of the ion beam and the part to be cross-polished.

  Thus, when adjusting the shielding positional relationship between the mask 2 and the sample 3, the sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 is detached from the sample fine movement base 5 and mounted on the fixed base 42 of the optical microscope 40. Then, the mask 2 has its shielding position relative to the sample 3 adjusted by a mask position adjustment unit (mask fine adjustment mechanism).

  FIG. 9 is an explanatory diagram showing a method of mirror polishing the cross section of the sample 3 with an ion beam. When the argon ion beam is irradiated, the sample 3 not covered with the mask 2 can be removed along the mask 2 in the depth direction, and the surface of the cross section of the sample 3 can be mirror-polished.

  In this way, the sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 including the mask 2 in which the shielding positional relationship with respect to the sample is adjusted during ion milling is returned to the sample fine movement base 5 and attached.

  As described above, when adjusting the shielding positional relationship between the mask 2 and the sample 3, the sample mask unit fine movement mechanism 4 on which the sample mask unit 21 is installed is detached from the sample fine movement base 5 and mounted on the fixed base 42 of the optical microscope 40. The sample mask unit fine movement mechanism 4 provided with the sample mask unit 21 having the mask 2 with the mask 2 adjusted in the shield position relationship with respect to the sample is adjusted in the vacuum chamber 15 during ion milling. The ion milling method is configured to return and attach to the sample fine movement base 5.

Further, as shown in FIG. 10, the optical microscope 40 is also provided with another fixing base 42 that can be installed in a state where the sample mask unit fine movement mechanism 4 is inclined (for example, 30 degrees ) with respect to the optical axis. Then, after adjusting the positions of the sample 3 and the mask 2, the sample mask unit fine movement mechanism 4 is installed in an inclined state under the optical microscope, and it is confirmed that the sample 3 and the mask 2 are in close contact with each other without any gap. A method that can be confirmed at 40 is also configured.

  In recent years, particularly in the semiconductor field, it has become important to observe a cross-section of a composite material with an electron microscope, and the importance of mirror-polishing the cross-section of the composite material has increased. According to the present embodiment, it becomes possible to set the mask accurately and easily at the site where the cross section of the sample is desired to be observed. In the present embodiment, if a plurality of mask sample units 21 are provided, it is possible to prepare a large number of samples in a state where the mask position is finely adjusted in advance, which is very efficient.

It is a schematic block diagram of the ion milling apparatus by one Example of this invention. It is a schematic block diagram of a sample mask unit. It is a figure which shows the other example of a sample mask unit. It is explanatory drawing which showed the method of making the cross section of a sample and a mask into parallel. It is a figure which shows the state which pulled out the sample fine movement base and attached / detached the sample mask unit fine movement mechanism which installed the sample mask unit. It is a figure which shows the state which mounts | wears with the sample mask unit fine movement mechanism which installed the sample mask unit in the optical microscope provided separately. It is a figure which shows the state which mounted | wore the optical microscope with the sample mask unit fine movement mechanism which installed the sample mask unit. It is explanatory drawing which showed the method to match | combine the argon ion beam center and the site | part which wants to grind | polish the cross section of a sample. It is explanatory drawing which showed the sample cross-section grinding | polishing method by ion milling. It is a figure which shows the other apparatus state of the example shown in FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Ion source, 2 ... Mask, 3 ... Sample, 4 ... Sample mask unit fine movement mechanism, 5 ... Sample fine movement base, 6 ... Vacuum exhaust system, 7 ... Ion source control part, 8 ... Sample fine movement control part, 9 ... Vacuum Exhaust system control unit, 10 ... flange, 11 ... linear guide, 12 ... loupe, 13 ... loupe fine movement mechanism, 15 ... vacuum chamber, 21 ... sample mask unit, 22 ... sample holder rotating ring, 23 ... sample holder, 24 ... linear Guide, 25 ... Mask holder, 26 ... Mask fine adjustment mechanism, 27 ... Mask fixing screw, 28 ... Sample holder rotating screw, 30 ... Sample holder position control mechanism, 35 ... Sample holder fixing bracket, 40 ... Optical microscope, 41 ... Observation Stand, 42 ... Fixed stand.

Claims (3)

An ion beam source that is attached to a vacuum chamber and irradiates a sample with an ion beam, a sample holder that fixes the sample, a mask that shields a part of the sample fixed to the sample holder, and a sample rotation mechanism that rotates the sample holder And a sample mask unit comprising a mask position adjustment unit for adjusting the shielding position relationship between the mask and the sample, a sample mask unit fine movement mechanism capable of XY-driving the sample mask unit with respect to the vertical direction of the ion beam , and the sample mask unit It includes a sample fine movement base capable established the fine movement mechanism, and the ion milling apparatus provided with an optical microscope to observe the shielding positional relationship between the mask and the sample,
The optical microscope is configured separately from the vacuum chamber , and is detachably attached at a reproducible position in attaching the loupe, the fine movement mechanism for adjusting the loupe center of the loupe, and the sample mask unit fine movement mechanism. and a fixed base,
The sample holder can be moved to a position where the center of the loupe and the center of the ion beam are combined by the fine movement mechanism,
The sample mask unit fine movement mechanism is detachable from the sample fine movement base at a reproducible position,
When moving the sample to a position where the ion beam is desired to be irradiated, the sample mask unit fine movement mechanism is attached to a fixed base of the optical microscope, and the position of the sample holder is adjusted by the fine movement mechanism to adjust the loupe center and the ion beam center The mask is provided with the mask in which the shielding position relationship with respect to the sample is adjusted by the mask position adjustment unit and the shielding position relationship with respect to the sample is adjusted during ion milling after the sample is moved to a target position. An ion milling apparatus, wherein a sample mask unit fine movement mechanism to which a sample mask unit is attached is returned to and mounted on the sample fine movement base. An ion beam source that is attached to a vacuum chamber and irradiates a sample with an ion beam, a sample holder that fixes the sample, a mask that shields a part of the sample fixed to the sample holder, and a sample rotation mechanism that rotates the sample holder And a sample mask unit comprising a mask position adjustment unit for adjusting the shielding position relationship between the mask and the sample, a sample mask unit fine movement mechanism capable of XY-driving the sample mask unit with respect to the vertical direction of the ion beam, and the sample mask unit In an ion milling apparatus comprising a sample fine movement base on which a fine movement mechanism can be installed, and an optical microscope for observing the shielding positional relationship between the mask and the sample,
The optical microscope includes a fixing base that is configured separately from the vacuum chamber and is detachably attached at a reproducible position in attaching the sample mask unit fine movement mechanism.
The sample mask unit fine movement mechanism is detachable from the sample fine movement base at a reproducible position, and when the sample is moved to a position to be irradiated with an ion beam, the sample mask unit fine movement mechanism is placed on the fixed base of the optical microscope. After the mechanism is attached and the sample is moved to the target position, the mask is provided with the mask in which the shielding positional relationship with respect to the sample is adjusted by the mask position adjustment unit, and the shielding positional relationship with respect to the sample is adjusted during ion milling. The sample mask unit fine movement mechanism attached with the sample mask unit is returned to the sample fine movement base,
The optical microscope is also provided with a fixing base that can be installed in a state where the sample mask unit is inclined (for example, 30 °) with respect to the optical axis, and after adjusting the position of the sample and the mask, the sample mask An ion milling apparatus, characterized in that the unit is installed under an optical microscope in an inclined state, and the optical microscope can confirm that the sample and the mask are in close contact with each other without a gap . 3. The position of the sample and the mask is adjusted according to claim 1, and after polishing the sample by ion beam irradiation, the sample mask unit is removed from the sample mask unit fine movement mechanism, and the relationship between the sample and the mask is left as it is. Confirm the condition of the polished surface of the sample with an optical microscope or SEM. If the polishing is insufficient, attach the sample mask unit to the fine movement mechanism while maintaining the relationship between the sample and the mask. An ion milling apparatus characterized in that polishing by irradiation can be continued .

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