JP5473772B2 - SAMPLE INSTALLATION METHOD AND SAMPLE INSTALLATION DEVICE FOR SAMPLE SURFACE CUTTING DEVICE - Google Patents

Description

  The present invention relates to a sample setting method and a sample setting device in a sample surface layer cutting apparatus, and more specifically, a sample capable of cutting a certain depth from the surface of a sample even when there is a gradient of μm level in the thickness of the sample. The present invention relates to a sample setting method and a sample setting device in a surface layer cutting device.

  2. Description of the Related Art Conventionally, a coating film adhesion strength / shear strength measuring apparatus that evaluates mechanical characteristics of a surface layer material by cutting the surface layer of a sample fixed to a sample holder with a cutting blade is known (see, for example, Patent Document 1). ).

JP 2003-254894 A

If you want to cut a certain depth from the surface of the sample in the conventional coating strength / shear strength measuring device, adjust the surface of the sample holder horizontally and fix the sample of a certain thickness on the surface of the sample holder. The cutting depth of the cutting edge (= the vertical position of the cutting edge tip during cutting relative to the vertical position where the cutting edge tip contacts the sample surface at the cutting start point) is kept constant. The surface layer was cut. In this case, if the surface of the sample was truly horizontal, a certain depth could be cut from the surface of the sample.
However, at the μm level, the surface of the sample is often not horizontal. For example, when the surface layer is a coating film, the thickness of the coating film often has a gradient of μm level, so even if the back surface of the sample is held horizontally by the sample holder, the surface of the sample has a gradient. Yes. Therefore, even if it is intended to cut a certain depth from the surface of the sample, the depth of cut actually varies. Then, when the depth of cut is in the μm level, there is a problem that the measurement cannot be ignored.
Therefore, an object of the present invention is to provide a sample placement method and a sample placement device in a sample surface layer cutting device capable of cutting a certain depth from the surface of the sample even if the sample thickness has a gradient of μm level. There is.

In a first aspect, the present invention provides a sample holding means for holding a sample so that the inclination of the sample surface can be adjusted, a cutting blade holding means for holding a cutting edge, and a surface layer of the sample held by the sample holding means. Relative moving means for moving the cutting blade holding means relative to the sample holding means for cutting with the cutting blade held by the cutting blade holding means, and measurement for measuring the vertical position and vertical load of the cutting blade And a vertical position when the tip of the indenter is pressed against the surface of the sample held by the sample holding means instead of the cutting edge. In the sample surface layer cutting apparatus, the inclination of the sample holding means is adjusted so that the change amplitude of the vertical load is minimized by reciprocating or turning the indenter by the relative moving means while maintaining To provide a fee installation method.
When the indenter sinks shallowly in the sample, the repulsive force from the sample is small, so the vertical load is small. Therefore, in the sample setting method in the sample surface layer cutting apparatus according to the first aspect, when the indenter is moved while maintaining the vertical position, if the vertical position of the sample surface has a gradient, the indenter sinks deeply and deeply. The vertical load changes with a large amplitude. Therefore, if the inclination of the sample holding means is adjusted so that the change amplitude of the vertical load becomes small, as a result, the indenter has moved a certain depth from the surface of the sample. And it can detect cheaply rather than detecting the inclination of the sample surface of the micrometer level directly. Thus, after adjusting the inclination of the sample holding means, if the indenter is cut back to the cutting edge and cut, a certain depth can be cut from the surface of the sample even if there is a gradient of μm level in the thickness of the sample. .
If there is no effect on the physical properties of the sample surface at the portion rubbed with the indenter, the same portion may be cut. However, if there is a possibility of influence, it is preferable to cut not the same portion but the neighboring portion.

In a second aspect, the present invention provides a sample holding means for holding the sample so that the inclination of the sample surface can be adjusted, an indenter holding means for holding an indenter, and the indenter on the surface of the sample held by the sample holding means. A relative moving means for moving the indenter holding means relative to the sample holding means by pressing the indenter held by the holding means; a measuring means for measuring a vertical position and a vertical load of the indenter; and the sample holding means. While maintaining the vertical position when the tip of the indenter is pressed against the surface of the held sample, the sample is reciprocated or swung by the relative movement means so that the change amplitude of the vertical load is minimized. Provided is a sample placement device comprising an adjustment means for adjusting the inclination of the holding means.
When the indenter sinks shallowly in the sample, the repulsive force from the sample is small, so the vertical load is small. Therefore, in the sample placement apparatus according to the second aspect, when the indenter is moved while maintaining the vertical position, if there is a gradient in the vertical position of the sample surface, the indenter repeatedly passes through the shallowly sinking portion and the deeply sinking portion. As a result, the vertical load changes with a large amplitude. Therefore, if the inclination of the sample holding means is adjusted so that the change amplitude of the vertical load becomes small, as a result, the indenter has moved a certain depth from the surface of the sample. And it can detect cheaply rather than detecting the inclination of the sample surface of the micrometer level directly. Thus, after adjusting the inclination of the sample holding means, the vertical position of the sample surface can be made constant.

In a third aspect, the present invention provides a sample holding means for holding a sample so that the inclination of the sample surface can be adjusted, a cutting blade holding means for holding a cutting blade, and a surface layer of the sample held by the sample holding means. Relative moving means for moving the cutting blade holding means relative to the sample holding means for cutting with the cutting blade held by the cutting blade holding means, and measurement for measuring the vertical position and vertical load of the cutting blade A vertical load when the indenter is held by the cutting blade holding means instead of the cutting blade and the tip of the indenter is pressed against the surface of the sample held by the sample holding means In the sample surface layer cutting apparatus, wherein the indenter is reciprocally moved or swiveled by the relative moving means while maintaining the inclination, and the inclination of the sample holding means is adjusted so that the change amplitude of the vertical position is minimized. To provide a fee installation method.
When the indenter is pressed against the sample with a constant vertical load, the indenter sinks into the sample to a certain depth according to the vertical load. Therefore, in the sample setting method in the sample surface cutting apparatus according to the third aspect, when the indenter is moved while maintaining the vertical load, if the vertical position of the sample surface has a gradient, the vertical position of the indenter also has a gradient. As a result, the vertical position changes with a large amplitude. Therefore, if the inclination of the sample holding means is adjusted so that the change amplitude of the vertical position becomes small, the indenter moves as a result from the sample surface at a certain depth. And it can detect cheaply rather than detecting the inclination of the sample surface of the micrometer level directly. Thus, after adjusting the inclination of the sample holding means, if the indenter is cut back to the cutting blade and cut, a certain depth can be cut from the surface of the sample even if there is a gradient of μm level in the thickness of the sample. .
If there is no effect on the physical properties of the sample surface at the portion rubbed with the indenter, the same portion may be cut. However, if there is a possibility of influence, it is preferable to cut not the same portion but the neighboring portion.

In a fourth aspect, the present invention provides a sample holding means for holding a sample so that the inclination of the sample surface can be adjusted, an indenter holding means for holding an indenter, and the indenter on the surface of the sample held by the sample holding means. A relative moving means for moving the indenter holding means relative to the sample holding means by pressing the indenter held by the holding means; a measuring means for measuring a vertical position and a vertical load of the indenter; and the sample holding means. While maintaining the vertical load when the tip of the indenter is pressed against the surface of the held sample, the sample is reciprocated or swung by the relative moving means so that the change amplitude of the vertical position is minimized. Provided is a sample placement device comprising an adjustment means for adjusting the inclination of the holding means.
When the indenter is pressed against the sample with a constant vertical load, the indenter sinks into the sample to a certain depth according to the vertical load. Therefore, in the sample placement apparatus according to the fourth aspect, when the indenter is moved while maintaining the vertical load, if there is a gradient in the vertical position of the sample surface, the gradient also occurs in the vertical position of the indenter. The vertical position changes with a large amplitude. Therefore, if the inclination of the sample holding means is adjusted so that the change amplitude of the vertical position becomes small, the indenter moves as a result from the sample surface at a certain depth. And it can detect cheaply rather than detecting the inclination of the sample surface of the micrometer level directly. Thus, after adjusting the inclination of the sample holding means, the vertical position of the sample surface can be made constant.

According to the sample setting method in the sample surface layer cutting apparatus of the present invention, it is possible to cut a certain depth from the surface of the sample even if there is a gradient of μm level in the thickness of the sample.
Further, according to the sample placement device of the present invention, the vertical position of the sample surface can be made constant even if the sample thickness has a gradient of μm level.
Further, for example, it can be detected at a lower cost than directly detecting the inclination of the μm level of the sample surface using a spectral interference laser displacement meter (resolution: 1 nm).

1 is a configuration explanatory view showing a sample surface layer cutting apparatus according to Embodiment 1. FIG. It is explanatory drawing which shows the state which changed the cutting blade into the indenter. It is a flowchart which shows the sample installation process concerning Example 1. FIG. It is explanatory drawing which shows the sinking depth of the sample surface when an indenter is pressed by an initial stage vertical load. It is explanatory drawing which shows the sinking depth of the sample surface at the time of moving maintaining the vertical position of an indenter. It is explanatory drawing which shows the change of the vertical load at the time of moving maintaining the vertical position of an indenter. It is explanatory drawing which shows the holding state of the sample after completion of a sample installation process. It is explanatory drawing which shows the state which cuts a sample surface layer after completion of a sample installation process. FIG. 6 is a flowchart showing a sample installation process according to Example 2; It is explanatory drawing which shows the change of the sinking depth of the sample surface at the time of moving maintaining the vertical load of an indenter. It is explanatory drawing which shows the change of the vertical position at the time of moving while maintaining the vertical load of an indenter. It is explanatory drawing which shows the change of the vertical position at the time of moving while maintaining the vertical load of an indenter.

  Hereinafter, the present invention will be described in more detail with reference to embodiments shown in the drawings. Note that the present invention is not limited thereby.

Example 1
FIG. 1 is an explanatory front view of a sample surface layer cutting apparatus 100 according to the first embodiment.
In the sample surface layer cutting apparatus 100, a piezoelectric element driving fine movement stage 30 h is fixed to the support member 1.
The piezoelectric element driving fine movement stage 30h is an apparatus (trade name Nanostage; Nano Control Co., Ltd.) in which the stage 36h moves relative to the frame 35h in one direction by driving the piezoelectric element.
The frame 35h of the piezoelectric element driving fine movement stage 30h is fixed to the support member 1 so that the stage 36h moves in the horizontal direction. The horizontal movement range of the stage 36h is, for example, 300 μm.

The lower end side of the connecting rod 32 is fixed to the stage 36h of the piezoelectric element driving fine movement stage 30h.
A piezoelectric element driving fine movement stage 30v is fixed to the other end side of the connecting rod 32.
The piezoelectric element driving fine movement stage 30v is an apparatus (trade name Nanostage; Nano Control Co., Ltd.) in which the stage 36v moves relative to the frame 35v in one direction by driving the piezoelectric element.
The stage 36v of the piezoelectric element driving fine movement stage 30v is fixed to the connecting rod 32 so that the frame 35v moves in the vertical direction. The vertical movement range of the frame 35v is, for example, 100 μm.

One end of the vertical load detector 15 is fixed to the frame 35v of the piezoelectric element driving fine movement stage 30v.
The vertical load detector 15 is a load cell for scale (trade name CB17; Minebea Co., Ltd.), and detects a vertical load applied to the other end.

A first end of a horizontal load detector 17 is fixed to the other end of the vertical load detector 15 via a connector 16.
The horizontal load detector 17 is a load cell for scale (trade name CB17; Minebea Co., Ltd.), and detects a horizontal load applied to the second end.

  A cutting edge 18 is fixed to the second end of the horizontal load detector 17.

  A sample holder 23 for fixing the sample S to the upper surface is shown in the figure because actuators 24a, 24b, 24c, and 24d for adjusting the inclinations of the upper surface in the x and y directions (24d is behind 24b). It is supported by the support member 1 through the

The piezoelectric element driving fine movement stages 30h and 30v and the actuators 24a to 24d are connected to the personal computer 28 via the output interface 38a.
The vertical load detector 15 and the horizontal load detector 17 are connected to the personal computer 28 via the input interface 28b.

  The personal computer 28 drives the piezoelectric element driving fine movement stages 30h and 30v in accordance with an instruction from the operator to cut the surface layer of the sample S. Then, the vertical load Fv is detected from the output of the vertical load detector 15 at that time, the horizontal load Fh is detected from the output of the horizontal load detector 17, and the horizontal movement amount is determined from the movement amount of the stage 36h of the piezoelectric element driving fine movement stage 30h. And the vertical movement amount is detected from the movement amount of the frame 35v of the piezoelectric element driving fine movement stage 30v. Further, the detected vertical load Fv, horizontal load Fh, horizontal movement amount and vertical movement amount are graphed and displayed on a display or printed by a printer.

As shown in FIG. 2, the cutting blade 18 can be replaced with an indenter 22. The indenter 22 is a diamond spherical indenter (r = 0.2) used in, for example, a Rockwell hardness tester.
After the operator replaces the cutting blade 18 with the indenter 22, the operator activates the sample setting process shown in FIG.

FIG. 3 is a flowchart showing the operation of the sample setting process by the sample surface layer cutting apparatus 100.
In step P1, the operator sets the initial vertical load Fvo, the x-axis period Tx, the x-axis amplitude Lx, the y-axis period Ty, and the y-axis amplitude Ly in the personal computer 28.
Appropriate values for these parameters can be determined by trial. That is, trials are repeatedly performed with various parameter values for various samples in advance, and a value such that the indenter 22 sinks to an appropriate depth (for example, 5 μm) is obtained, and a sample of the same type as the sample S to be evaluated is obtained. You just need to set the parameter value.
For example, when the sample S is a PCV plate (Takiron S604 (press molding) ESS8800A), Fvo = 10 mN, and when moving linearly in the x direction, Tx = 30 seconds, Lx = 100 μm, Ty = 0 seconds, Ly = 0 μm (a parameter value of 0 means no movement in that direction).

In step P2, the personal computer 28 presses the indenter 22 against the sample S with the set initial vertical load Fvo.
As shown in FIG. 4, the indenter 22 sinks from the surface of the sample S to a depth D corresponding to the initial vertical load Fvo.
In step P3, the personal computer 28 measures and stores the vertical position H1 of the indenter 22.

  In step P4, the personal computer 28 moves the indenter 22 by x = Lx · sin (2 · π · t / Tx) in the x direction while performing feedback control so as to maintain the stored vertical position H1 of the indenter 22. In the y direction, y = Ly · cos (2 · π · t / Ty).

  As shown in FIG. 5, although the bottom surface of the sample S is held horizontally by the sample holder 23, the surface of the sample S is inclined downward in the x direction (thickness is reduced). Then, when the indenter 22 is moved in the x direction while maintaining the vertical position H1 of the indenter 22, the depth at which the indenter 22 sinks from the surface of the sample S becomes shallow. Therefore, the vertical load Fv becomes small. Therefore, when the linear movement is repeated, the vertical load Fv varies with a cosine wave as shown in FIG.

  In Step P5, as shown in FIG. 6B, the operator or the personal computer 28 extends and contracts the actuators 24a, 24b, 24c, and 24d so that the fluctuation amplitude of the vertical load Fv is minimized. Adjust the tilt. Then, the process ends.

  As shown in FIG. 7, after completion of the sample setting process, the sample holder 23 is tilted and the bottom surface of the sample S is held so that the surface of the sample S is horizontal in the x direction.

Therefore, as shown in FIG. 8, if the indenter 22 is returned to the cutting edge 18 and cut horizontally in the x direction, a certain depth d can be cut from the surface of the sample S.
Note that the same portion may be cut if there is no effect on the surface physical properties of the sample S in the portion rubbed with the indenter 22, but if there is a possibility of influence, it is preferable to cut the neighboring portion instead of the same portion. For example, when the width of the cutting edge 18 is 100 μm, it is preferable to cut a portion about 100 μm away from the portion rubbed with the indenter 22.

  According to the sample surface layer cutting apparatus 100 of Example 1, it is possible to cut a certain depth d from the surface of the sample S even if the thickness of the sample S has a gradient of μm level. Further, it can be detected at a lower cost than directly detecting the slope of the μm level on the surface of the sample S.

-Example 2-
The hardware configuration of the sample surface layer cutting apparatus according to the second embodiment is the same as that of the first embodiment.

FIG. 9 is a flowchart illustrating the operation of the sample setting process performed by the sample surface layer cutting apparatus according to the second embodiment.
In step P1, the operator sets the initial vertical load Fvo, the x-axis period Tx, the x-axis amplitude Lx, the y-axis period Ty, and the y-axis amplitude Ly in the personal computer 28.

In step P2, the personal computer 28 presses the indenter 22 against the sample S with the set initial vertical load Fvo.
As shown in FIG. 10, the indenter 22 sinks from the surface of the sample S to a depth D corresponding to the initial vertical load Fvo.

  In Step P4 ′, the personal computer 28 controls the indenter 22 at x = Lx · sin (2 · π · t / Tx) in the x direction while performing feedback control so as to maintain the vertical load Fv at the initial vertical load Fvo. In the y direction, y = Ly · cos (2 · π · t / Ty).

  As shown in FIG. 11, although the bottom surface of the sample S is held horizontally by the sample holder 23, the surface of the sample S is inclined downward in the x direction (thickness is reduced). Then, when the indenter 22 is moved in the x direction while maintaining the vertical load Fv of the indenter 22 at the initial vertical load Fvo, the depth at which the indenter 22 sinks from the surface of the sample S is a depth corresponding to the initial vertical load Fvo. It becomes constant at D. Therefore, the vertical position H decreases from H1 in FIG. 10 to H2 in FIG. Therefore, when the linear movement is repeated, the vertical position H varies with a cosine wave as shown in FIG.

  In step P5 ′, the operator or the personal computer 28 extends and contracts the actuators 24a, 24b, 24c, and 24d so that the fluctuation amplitude of the vertical position H is minimized as shown in FIG. 23 is adjusted. Then, the process ends.

  As shown in FIG. 7, after completion of the sample setting process, the sample holder 23 is tilted and the bottom surface of the sample S is held so that the surface of the sample S is horizontal in the x direction.

Therefore, as shown in FIG. 8, if the indenter 22 is returned to the cutting edge 18 and cut horizontally in the x direction, a certain depth d can be cut from the surface of the sample S.
Note that the same portion may be cut if there is no effect on the surface physical properties of the sample S in the portion rubbed with the indenter 22, but if there is a possibility of influence, it is preferable to cut the neighboring portion instead of the same portion. For example, when the width of the cutting edge 18 is 100 μm, it is preferable to cut a portion about 100 μm away from the portion rubbed with the indenter 22.

  According to the sample surface layer cutting apparatus of Example 2, it is possible to cut a certain depth d from the surface of the sample S even if the thickness of the sample S has a gradient of μm level. Further, it can be detected at a lower cost than directly detecting the slope of the μm level on the surface of the sample S.

-Other examples-
In the first and second embodiments, the cutting blade 18 and the indenter 22 are replaced, but the cutting blade 18 and the indenter 22 may be held at the same time.

  The sample setting method and sample setting apparatus in the sample surface layer cutting apparatus of the present invention can be used, for example, to examine the mechanical properties of the surface material.

18 Cutting blade 22 Indenter 23 Sample holder 24a to 24d Actuator 28 Personal computer 100 Sample surface layer cutting device S Sample

Claims (4)

  A sample holding means for holding the sample so that the inclination of the sample surface can be adjusted, a cutting edge holding means for holding the cutting edge, and a cutting layer held by the cutting edge holding means for the surface layer of the sample held by the sample holding means. In a sample cutting apparatus comprising a relative moving means for moving the cutting blade holding means relative to the sample holding means for cutting with a blade, and a measuring means for measuring a vertical position and a vertical load of the cutting blade, In place of the cutting blade, the indenter is held by the cutting blade holding means, and the relative movement means maintains the vertical position when the tip of the indenter is pressed against the surface of the sample held by the sample holding means. A sample placement method in a sample surface layer cutting apparatus, wherein the indenter is reciprocated or swung to adjust the inclination of the sample holding means so that the change amplitude of the vertical load is minimized.   A sample holding means for holding the sample so that the inclination of the sample surface can be adjusted, an indenter holding means for holding the indenter, and an indenter held by the indenter holding means against the surface of the sample held by the sample holding means. A relative moving means for moving the indenter holding means relative to the sample holding means; a measuring means for measuring a vertical position and a vertical load of the indenter; and a surface of the sample held by the sample holding means. Adjusting means for adjusting the inclination of the sample holding means so that the change amplitude of the vertical load is minimized by moving the indenter back and forth by the relative moving means while maintaining the vertical position when the tip is pressed. A sample placement device characterized by comprising:   A sample holding means for holding the sample so that the inclination of the sample surface can be adjusted, a cutting edge holding means for holding the cutting edge, and a cutting layer held by the cutting edge holding means for the surface layer of the sample held by the sample holding means. In a sample cutting apparatus comprising a relative moving means for moving the cutting blade holding means relative to the sample holding means for cutting with a blade, and a measuring means for measuring a vertical position and a vertical load of the cutting blade, In place of the cutting blade, the indenter is held by the cutting blade holding means, and the relative movement means maintains the vertical load when the tip of the indenter is pressed against the surface of the sample held by the sample holding means. A sample placement method in a sample surface layer cutting apparatus, wherein the indenter is reciprocated or swung to adjust the inclination of the sample holding means so that the change amplitude of the vertical position is minimized.   A sample holding means for holding the sample so that the inclination of the sample surface can be adjusted, an indenter holding means for holding the indenter, and an indenter held by the indenter holding means against the surface of the sample held by the sample holding means. A relative moving means for moving the indenter holding means relative to the sample holding means; a measuring means for measuring a vertical position and a vertical load of the indenter; and a surface of the sample held by the sample holding means. Adjusting means for adjusting the inclination of the sample holding means so that the amplitude of change in the vertical position is minimized by reciprocating or turning the indenter by the relative moving means while maintaining a vertical load when the tip is pressed. A sample placement device characterized by comprising:

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