JPH06297304A - Polishing device, cutting/grinding device, and cutting device for solid material - Google Patents

Abstract

PURPOSE:To polish a sample without fixing it by means of an adhesive or the like by providing a device with two ultrasonic drivers that are opposite to each other and function as driving sources for polishing the surfaces of a solid body, and by constituting the device in such a way that the upper and lower surfaces of the solid body can be simultaneously or separately polished by these ultrasonic drivers. CONSTITUTION:A device is provided with ultrasonic drivers 21, 22 in which nickel vibrators have been used, and thereto ultrasonic vibrators 23, 24 which are arranged in the vertical direction so as to be opposite to each other are provided respectively. The surface of the upper ultrasonic vibrator 23 is formed in a curved shape, for example, of a radius of curvature of 5mm, and the surface of the lower ultrasonic vibrator 24 is formed in a plane shape. When a sample 27 is polished, carborundum aqueous solution is used as an abrasive, and polishing is carried out by operating only the ultrasonic vibrator 23. To mirror-polishing the upper and lower surfaces, the upper and lower ultrasonic vibrators 23, 24 are changed to another ultrasonic vibrators each of which has the same shape and whose surface has been covered with buff cloth, and also the abrasive is changed to alumina aqueous solution. In this condition, the upper and lower vibrators 23, 24 are driven, and the upper and lower surfaces of the sample 27 are simultaneously polished.

Description

Detailed Description of the Invention

[0001]

[Industrial applications]

(First Invention) The present invention relates to a polishing apparatus,
In particular, it relates to a polishing apparatus used for preparing a sample for electron microscope observation.

(Second invention) The present invention relates to a solid cutting and grinding apparatus by a so-called ultrasonic machining method, and in particular, cutting out a disk from a solid sample used for preparing a sample for observation with a transmission electron microscope. Also, the present invention relates to a cutting and grinding device capable of performing dimples in a single operation.

(Third Invention) The present invention relates to a solid material cutting apparatus, and more particularly to a solid material cutting apparatus used for preparing a sample for electron microscope observation.

[0004]

[Prior art]

(First Invention) In order to observe the structure of a solid sample using a transmission electron microscope, it is necessary to prepare the sample thin so that incident electrons can pass through the sample. As one of the sample thinning methods, generally, mechanical polishing is first performed to reduce the thickness of the sample to about several tens of μm. After that, ion irradiation, chemical etching, or the like is used to finally make the observation region have a thickness of 1 μm or less. The mechanical polishing step is usually performed as shown below. 1) One side a of the sample is bonded with a soluble adhesive and fixed to the sample table. 2) The other exposed surface b is mirror-polished. 3) Melt the adhesive to remove the sample from the sample table, and then fix the mirror-polished surface b to the sample table with the adhesive. 4) Polish from the exposed surface a side so that the center of the sample is 1
It is thinned to less than 00 μm. 5) Polish the surface a. 6) Melt the adhesive and remove the sample from the sample table. The polishing is performed by friction caused by relative movement (translation, rotation) between a sample and a polishing table coated with an abrasive (alumina abrasive grains, diamond abrasive grains, etc.).

(Second Invention) When observing a solid sample using a transmission electron microscope, first, the diameter is 3 mm or 2. so that the sample can be mounted on the sample holder.
It is necessary to cut the sample into a disk shape of 3 mm, and at the same time, it is necessary to make the sample extremely thin so that incident electrons can pass through the sample. On the other hand, the mechanical strength of the entire disk must be maintained to a certain extent or more. Therefore, by forming dimples, the outer peripheral portion of the disk remains thick and only the inner peripheral portion is thinned. Conventionally, when a disk having such dimples is manufactured from a solid sample, a method has been adopted in which the disk is first cut out from the solid sample and then mechanically ground to form dimples.

(Third invention) In evaluating the structure of a thin film, observation from a cross-sectional direction by a transmission electron microscope (cross-sectional TEM) is an effective means. In order to perform cross-sectional TEM observation, it is necessary to thin the thin-film sample in the cross-sectional direction so that incident electrons can be transmitted. The conventional standard cross-section thinning process is as follows. 1) Cutting process: Two strips of ˜1 × 2 mm are cut out from a sample in which a thin film is formed on a substrate. 2) Adhesion step: The surfaces of the two cut sample pieces are faced to each other and bonded with an adhesive. 3) Mechanical polishing step: 100 μm of the bonded sample in the cross-sectional direction
It is polished to a thickness of m, and both sides are mirror finished. 4) The observation area is reduced to 1 μm or less by ion irradiation. The cutting method in the cutting step of the above conventional method,
It is performed by rotating a blade (diamond slicer) on a disk containing diamond abrasive grains.

[0007]

[Problems to be Solved by the Invention]

(First Invention) The above-mentioned conventional method has some problems as a method for preparing a sample for observation with a transmission electron microscope. First of all, the series of steps is complicated and takes time and labor.
Furthermore, the risk of failure such as breakage of the sample increases accordingly. The second problem is that there is an adhesive layer between the sample and the sample stand, so the height from the sample stand may not accurately reflect the thickness of the sample. Is difficult to measure accurately, and it cannot be polished to a sufficient thickness with good reproducibility. Therefore, an object of the present invention is to solve the above-mentioned problems of the prior art, to simplify the process, to perform polishing quickly and without fear of sample damage, and to control the thickness of the sample with high precision. To provide a device.

(Second Invention) However, in the above-mentioned conventional manufacturing method, the cutting of the disk and the dimpling must be performed by using different devices,
There was a problem that work efficiency was not good. Further, the cutting out of the disc and the dimpling have to be performed by using different sample stands, and there is a problem that the transfer takes a considerable amount of time and labor and is complicated. Therefore, an object of the present invention is to solve the above-mentioned problems of the prior art and to provide a novel cutting and grinding apparatus capable of producing a disk-shaped sample having dimples in one working step.

(3rd invention) Further, in the above-mentioned step of thinning a sample for forming a sample used for observation with a transmission electron microscope, when the observation sample is cut in 1),
A particularly important point is to cut out a sample with reproducible and accurate dimensions. This is because, in the above-mentioned bonding step 2), when sample pieces having poor dimensional accuracy and different lengths and heights are bonded, it is difficult to perform uniform polishing in the subsequent polishing step 3). Uneven thickness, or
This is because the probability of damaging the sample also increases. In this respect, the conventional method using the diamond slicer has a problem that sufficient dimensional accuracy and reproducibility cannot be obtained due to an error associated with the vibration mechanism of the sample and the rotational movement of the disk. Therefore, the object of the present invention is to solve the above-mentioned problems of the prior art, and to quickly and easily cut a plurality of accurately sized sample pieces, resulting in the problem of sample damage in the polishing process. An object of the present invention is to provide an excellent solid material cutting device which does not cause

[0010]

[Means for Solving the Problems]

(First Invention) The above object is achieved by the present invention described below. That is, the first invention of the present invention is provided with two ultrasonic vibrating bodies facing each other as a driving force for polishing the solid surface, and the upper surface and the lower surface of the solid are simultaneously or individually provided by the ultrasonic vibrating body. The polishing apparatus is characterized in that it is polished to.

(Second Invention) The above object is achieved by the present invention described below. That is, the second invention of the present invention is
In a cutting / grinding device that grinds and grinds abrasive grains mixed with a solution on a tool surface that vibrates ultrasonically in the vertical direction, the tool surface has a cylindrical shape and a radius of curvature of 3 to 50.
A cutting and grinding apparatus having an upper surface formed of a curved surface of mm.

(Third Invention) The above object can be achieved by the present invention described below. That is, the third invention of the present invention is
A width of 0.1 mm to 1 mm and a depth of 1 on the surface of the ultrasonic vibrating body in contact with the surface to be cut with ultrasonic vibration as the driving force for cutting
A cutting device for a solid material, characterized in that a plurality of protrusions having a size of 5 mm to 5 mm are provided.

[0013]

[Action]

(First invention) The operating principle of the polishing apparatus of the present invention is to place a sample between two ultrasonic vibrating bodies facing each other and polish the upper surface and the lower surface of the sample simultaneously or individually using ultrasonic vibration as a driving force. It is a thing. In the cutting device of the present invention, the following points can be mentioned as advantages of using ultrasonic vibration as a driving force instead of the translational / rotary motion used in the conventional method. 1) The sample can be polished without being fixed to the sample table with an adhesive or the like. 2) According to the surface shape of the ultrasonic vibrating body, it can be ground into a free curved surface other than a flat surface. 3) It is possible to easily and freely adjust the polishing rate and the state of the finished surface by arbitrarily selecting the pressure, frequency, amplitude and abrasive of the ultrasonic vibrator. In the cutting device of the present invention, as described in 1), the sample can be polished without being fixed to the sample table with an adhesive or the like. It is characterized in that and can be polished simultaneously or individually. Further, since there is no adhesive layer, the thickness of the sample can be accurately obtained by measuring the distance between the sample table and the surface of the sample. Therefore, polishing can be performed with good reproducibility even at a thickness of 10 μm or less. . Further, according to the surface shape of the ultrasonic vibrator mentioned in 2), by utilizing the property that it can be ground to a free curved surface other than a flat surface, if a convex curved surface is used for at least one surface shape of the ultrasonic vibrator. , It is also easy to selectively thin only the vicinity of the center of the sample necessary for observation, and it is possible to prevent the sample from being damaged. As a result, in the pretreatment of sample preparation for electron microscope observation,
It is possible to polish a sample with high accuracy and without damage.

(Second invention) The cutting and grinding apparatus of the present invention comprises:
A disk having a dimple having the same curvature as the tool surface can be cut out at the cylindrical portion of the tool surface and at the same time dimpled at the curved surface portion having a radius of curvature of 3 to 50 mm of the tool surface. Can be easily manufactured in a single operation, and work efficiency can be improved.

(Third invention) One of the advantages of using ultrasonic vibration as a driving force for cutting is that it does not involve any relative motion other than ultrasonic waves between the ultrasonic vibrator and the object to be cut. The object is to be able to accurately follow the shape of the sonic vibrator and cut it. The solid material cutting device of the present invention utilizes this property,
By forming 2 to 20 protrusions on the surface of the ultrasonic vibrator, a plurality of sample pieces with uniform dimensions are cut out at the same time. As a result, polishing when preparing a sample for a transmission electron microscope. The sample is less damaged in the process and the cutting time is shortened.

[0016]

The present invention will be described in more detail with reference to the following examples. (First Invention) First Embodiment FIG. 1 shows a first embodiment of a polishing apparatus of the present invention. In the figure, reference numerals 21 and 22 denote ultrasonic oscillators using a nickel oscillator, and ultrasonic oscillators 23 at the upper and lower portions, respectively.
And 24. The surface of the upper ultrasonic vibrator 23 has a curved surface shape with a radius of curvature of 5 mm, and the lower ultrasonic vibrator 24 has a planar shape. 25 is a film thickness gauge, 2
Reference numeral 6 is a pressure adjusting mechanism utilizing hydraulic pressure. The polishing apparatus of this example was applied to the sample 27 that had been cut into 3 mmφ in advance. First, an aqueous solution of carborundum was used as an abrasive, and only the ultrasonic vibrator 23 was operated to polish the sample 27 to a center film thickness of 15 μm. Next, in order to mirror-polish the upper and lower surfaces, the upper and lower ultrasonic vibrators 23 and 24 are changed to ultrasonic vibrators having the same shape and the surfaces thereof are covered with a buff cloth. It was changed to an aqueous solution of alumina. In this state, the upper and lower ultrasonic vibrators 23 and 24 were operated, and the upper surface and the lower surface of the sample 27 were simultaneously polished. As a result, a good mirror surface condition was promptly obtained on both the upper surface and the lower surface.

Example 2 The ultrasonic vibrator 23 on the upper side of the polishing apparatus of Example 1 shown in FIG. 1 has a curved surface shape with a radius of curvature of 5 mm and a surface shape with a flat center portion. Instead of the sonic vibrating body 28. The cutting device of this example was applied to a sample 27 that had been cut into 3 mmφ in advance. First, an aqueous solution of carborundum was used as an abrasive, and only the ultrasonic vibration body 28 was operated to polish to a center film thickness of 15 μm. Next, in order to polish the upper surface and the lower surface to the mirror surface, the upper and lower ultrasonic vibrators 2
Each of 8 and 24 was changed to an ultrasonic vibrating body having the same shape and the surface of which was covered with a buff cloth, and the abrasive was changed to an aqueous solution of alumina. In this state, the upper and lower ultrasonic vibrators 28
As a result of operating Nos. 24 and 24, both the upper surface and the lower surface of the sample 27 were in a good mirror surface state. When the sample 27 obtained as described above was irradiated with argon ions, a thin region where a transmission electron microscope observation was possible was formed over a wide area because the center was flat.

(Second Invention) Third Embodiment A cutting and grinding apparatus of the present invention will be described with reference to FIG. In the figure, reference numeral 1 denotes an ultrasonic oscillator using a Ni oscillator, which is connected to an ultrasonic oscillator 2 below. A tool surface 3 is attached to the tip of the ultrasonic vibrating body 2 and vibrates ultrasonically in the vertical direction. The tool surface 3 is formed of a cylindrical shape having an inner diameter of 3 mm and a curved upper surface having a radius of curvature of 20 mm. Reference numeral 4 is a sample table, 5 is a film thickness gauge, and 6 is a pressure adjusting mechanism utilizing hydraulic pressure. The cutting and grinding apparatus of this example was applied to a Si wafer sample 7 having a thickness of 1.5 mm, and the ultrasonic vibrator 2 was operated using the carborundum aqueous solution 8. The diameter was 3 mm and the radius of curvature was 20 m.
A disk having m dimples was formed. It was also confirmed that a disc having dimples can be easily obtained by appropriately selecting the frequency, amplitude, pressure, polishing abrasive grains, etc. of the ultrasonic vibrator 2.

Embodiment 4 In the case of the second embodiment of the present invention, as in Embodiment 3,
Reference numeral 1 denotes an ultrasonic oscillator using a Ni oscillator, which is connected to the ultrasonic vibrator 2 below. Further, the tool surface 3 is attached to the tip of the ultrasonic vibrating body 2.
Is a cylindrical shape with an inner diameter of 2.3 mm and a radius of curvature of 10 mm
And an upper surface formed of a curved surface. 4 is the sample table,
Reference numeral 5 is a film thickness gauge, and 6 is a pressure adjusting mechanism utilizing hydraulic pressure. The cutting and grinding machine of this example was applied to a Si wafer sample 7 having a thickness of 1 mm. When the ultrasonic vibrator 2 was operated using the carborundum aqueous solution 8, the diameter was 2.
A disk having dimples with a radius of curvature of 3 mm and a radius of 10 mm was formed. It was also confirmed that a disc having dimples can be easily obtained by appropriately selecting the frequency, amplitude, pressure, polishing abrasive grains, etc. of the ultrasonic vibrator 2.

(Third Invention) Fifth Embodiment FIG. 3 is a schematic view of a solid material cutting device according to an embodiment of the present invention. Reference numeral 11 denotes an ultrasonic oscillator using a nickel oscillator, which is connected to the ultrasonic oscillator 12. Reference numeral 13 is a film thickness gauge, and 14 is a pressure adjusting mechanism using hydraulic pressure. 4 is a partially enlarged view of the ultrasonic vibrating body 12 of the cutting apparatus of FIG. 3, the ultrasonic vibrating body 12 has a width of 0.2 mm and a length of 2 mm.
Five stainless steel blades 5 having a depth of 1 mm are arranged at intervals of 1 mm, and the periphery is surrounded by blades 16 having a height difference of 1.2 mm. The cutting apparatus of the embodiment of the present invention as described above was applied to a Si wafer sample having a thickness of 0.4 mm shown in 17 of FIG. When an ultrasonic wave amplitude conductor 12 was operated using an aqueous solution of carborundum as an abrasive, it was quickly cut into four sample pieces having the same shape. or,
It was confirmed that a cut surface with less damage can be easily obtained by appropriately selecting the pressure of the ultrasonic amplitude conductor 12, the amplitude, or the abrasive.

[0021]

【The invention's effect】

(First invention) As described above, according to the polishing apparatus of the present invention, it is used as a sample for transmission electron microscope observation.
It is possible to rapidly and reproducibly prepare a sample having a wide observation region.

(Second Invention) As described above, according to the cutting and grinding apparatus of the present invention, cutting and dimpling of a disk can be performed at the same time, so a disk having a dimple having a curvature similar to that of the tool surface. Can be manufactured in a single operation, and work efficiency can be improved.

(Third Invention) As described above, according to the cutting apparatus of the present invention, it is possible to easily and quickly cut out a plurality of sample pieces having uniform dimensions, and to observe them with a transmission electron microscope. The efficiency of sample preparation is greatly improved.

[Brief description of drawings]

FIG. 1 is a schematic view of an example showing an embodiment of a polishing apparatus of the first invention of the present invention.

FIG. 2 is a schematic view of an example of a cutting and grinding apparatus of a second invention of the present invention.

FIG. 3 is a schematic view of an example of a solid material cutting device of a third invention of the present invention.

4 is a partially enlarged view of the ultrasonic vibration body 12 in FIG.

[Explanation of symbols]

 1: Ultrasonic oscillator 2: Ultrasonic oscillator 3: Tool surface 4: Sample stage 5: Pressure adjusting mechanism 6: Thickness gauge 7: Sample 8: Abrasive grains mixed with solution 11: Nickel vibrator 12: Ultrasonic wave Vibrator 13: Film thickness gauge 14: Hydraulic pressure adjusting mechanism 17: Sample 15: Blade 16: Blade 21: Upper nickel vibrator 22: Lower nickel vibrator 23: Upper ultrasonic vibrator 24: Lower ultrasonic vibrator 25 : Thickness gauge 26: Hydraulic pressure adjusting mechanism 27: Sample 28: Upper ultrasonic vibrator

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Claims (3)

[Claims] 1. Two ultrasonic vibrating bodies facing each other as a driving force for polishing a solid surface are provided, and the upper surface and the lower surface of the solid are simultaneously or individually polished by the ultrasonic vibrating body. Characteristic polishing device. 2. In a cutting and grinding apparatus for grinding abrasives mixed with a solution on a tool surface which is ultrasonically vibrated in the vertical direction by rubbing it against a workpiece, the tool surface has a cylindrical shape and a radius of curvature of 3 A cutting and grinding machine having an upper surface having a curved surface of ˜50 mm. 3. An ultrasonic vibration is used as a driving force for cutting, and a width of 0.1 mm to the surface of the ultrasonic vibrator which is in contact with the surface to be cut.
A cutting device for a solid material, which is provided with a plurality of protrusions having a depth of 1 mm and a depth of 1 mm to 5 mm.