JPH08327635A - Cantilever, heater employing it, and heating/shape measuring apparatus employing it - Google Patents

Abstract

PURPOSE: To heat a micro area of a sample locally at a desired temperature by providing a heating element for heating the forward end part of a probe and a thermocouple. CONSTITUTION: The cantilever comprises a support 1, a flexible plate 2 being supported by the support 1 at one end thereof, a probe 3 disposed at the tip thereof, and a heating element 4 for heating the forward end part thereof. A thermocouple constituting part 8 extends to the peripheral part of the probe 3 and a thermocouple constituting part 10 extends to the lower surfaces of the plate 2 and the support 1. The heating element 4 is formed in hair pin shape on an electric insulation layer 11 formed on the constituting part 8 in order to heat the forward end part of probe 3. Since the probe 3 is pointed sharply, when the forward end part thereof is brought into contact with the surface of sample or brought extremely close thereto, a micro area on the order of atomic of molecular dimensions on the surface can be heated locally through the forward end part. When the temperature is detected and controlled by means of the thermocouple, temperature of the probe can be set at a desired level and the active state of organism can be observed in detail.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a heating device for heating a sample surface, a cantilever used for the heating device, and a heating device capable of not only heating the sample surface but also measuring the shape of the sample surface. The present invention relates to a shape measuring device.

[0002]

2. Description of the Related Art When locally heating a sample,
For example, it is conceivable to irradiate a laser beam to heat the sample.

However, even if the size of the laser beam spot is reduced to the diffraction limit, it is very large from the viewpoint of the atoms and molecules of the sample. Therefore, the atoms and molecules of the sample are heated locally. It is not possible.

As described above, conventionally, there has been no means for locally heating the sample.

Conventionally, a scanning atomic force microscope (Atomic Force Microscop) has been used as a device for measuring the surface shape of a sample (substance) with a resolution of the order of atoms and molecules.
e) is provided. In a scanning atomic force microscope, a cantilever provided with a support, a flexible plate whose one end is supported by the support, and a probe provided in a tip side region of the flexible plate is a probe. Is used as. However, although the conventional scanning atomic force microscope can measure the shape of the sample surface, the sample cannot be locally heated.

[0006]

As described above, in the past, it was not possible to locally heat the minute region of the sample on the atomic or molecular order. It was not possible to elucidate the changes in properties due to.

Further, it is more effective if the minute region can be heated not only locally but also to a desired temperature.

The present invention has been made in view of the above circumstances, and a heating device that can locally heat a minute region of the sample in the order of atoms and molecules to a desired temperature and a cantilever used in the heating device. The purpose is to provide.

Further, according to the present invention, it is possible to locally heat a minute region of the sample in the order of atoms or molecules to a desired temperature and measure the shape of the sample surface with a resolution in the order of atoms or molecules. It is an object of the present invention to provide a heating / shape measuring device that can perform heating.

[0010]

In order to solve the above problems, a cantilever according to a first aspect of the present invention comprises a support, a flexible plate having one end supported by the support, and a flexible plate. In a cantilever having a probe provided in the tip side region of the plate, a heating element for heating the tip of the probe is provided, and a thermocouple is provided at the probe.

The cantilever according to the second aspect of the present invention is the cantilever according to the first aspect, wherein at least a part of the metal material forming the thermocouple is interposed between the heating element and the probe. It is also used as a high thermal conductor.

According to a third aspect of the present invention, there is provided a heating device in which the cantilever according to the first or second aspect, a heat generating driving means for causing the heat generating element to generate heat, and a direction substantially parallel to the surface of the sample. First moving means for moving the probe relative to the sample, and second moving means for moving the probe relative to the sample in a direction substantially perpendicular to the sample surface.
Based on the moving means and the thermoelectromotive force from the thermocouple,
In order that the temperature of the probe becomes a desired temperature, a temperature control unit that controls the heat generation driving unit and a state where the probe is pressed against the sample surface by bending the cantilever, Control means for controlling the heat generation driving means and the first and second moving means so that only desired points are heated or respective points in desired areas of the sample surface are heated sequentially. Be prepared.

A heating device according to a fourth aspect of the present invention is a cantilever according to the first or second aspect, a heat generating drive means for causing the heating element to generate heat, and a deflection detecting means for detecting deflection of the cantilever. First moving means for moving the probe relative to the sample in a direction substantially parallel to the sample surface; and the probe relative to the sample in a direction substantially perpendicular to the sample surface. The second moving means for relatively moving the second cantilever and the second so that the bending of the cantilever becomes constant based on a detection signal from the bending detecting means.
While controlling the moving means, the first moving means is controlled so that the probe faces a desired point on the sample surface or sequentially scans each point in a desired area on the sample surface. Means for controlling only the desired points on the sample surface, or means for controlling the heating driving means so that each point on the desired area of the sample surface is sequentially heated; Temperature control means for controlling the heat generation driving means so that the temperature of the probe becomes a desired temperature based on the thermoelectromotive force.

A heating device according to a fifth aspect of the present invention is a cantilever according to the first or second aspect, a heating drive means for heating the heating element, a vibrating means for vibrating the cantilever, and a cantilever for the cantilever. Vibration detecting means for detecting a vibration state, first moving means for moving the probe relative to the sample in a direction of a plane substantially parallel to the sample surface, and a direction substantially perpendicular to the sample surface. Second moving means for moving the probe relative to the sample, and atoms acting between the probe of the cantilever and the sample surface based on a detection signal from the vibration detecting means. While the second moving means is controlled so that the inter-force becomes constant, the probe faces a desired point on the sample surface or sequentially scans each point on a desired area of the sample surface. To the above Means for controlling the moving means, and means for controlling the heat generation driving means so that only a desired point on the sample surface is heated or each point in a desired region on the sample surface is sequentially heated. And a temperature control unit that controls the heat generation drive unit so that the temperature of the probe becomes a desired temperature based on the thermoelectromotive force from the thermocouple.

A heating / shape measuring apparatus according to a sixth aspect of the present invention is the heating apparatus according to the fourth or fifth aspect, and the probe with respect to the sample surface in a direction substantially parallel to the sample surface. Means for obtaining information on the relative position of the probe with respect to the sample surface in a direction substantially perpendicular to the sample surface, according to the relative position.

According to the cantilevers according to the first and second aspects, the tip of the probe is heated by the heating element.
Therefore, the sample surface can be heated via the tip part of the probe by bringing the tip part of the probe into contact with the sample surface or bringing them closer to each other at a minute interval. At this time, the tip of the probe can be configured to be extremely sharp like a cantilever used in a scanning atomic force microscope, so atoms and molecules on the sample surface can be inserted through the tip of the probe. A small area of the order can be locally heated.
Moreover, according to the cantilevers according to the first and second aspects, since the probe is provided with the thermocouple, it is possible to control the temperature of the probe to a desired temperature based on the thermoelectromotive force from the thermocouple. You can For this reason, it is possible to locally heat the atomic and molecular order minute regions on the sample surface to the desired temperature via the tip of the probe.

Since the cantilever according to the first and second aspects employs the cantilever structure, the flexible plate can be flexed flexibly as in the third to fifth aspects. By utilizing it, the tip portion of the probe can be brought into contact with the sample surface or can be brought close to each other at a minute interval.

In the cantilever according to the second aspect, since at least a part of the metal material forming the thermocouple is also used as a high thermal conductor interposed between the heating element and the probe, for example, Even when the heating element is provided at a position relatively far from the probe, as in the case where the heating element is provided around the probe on the flexible plate, the heat from the heating element is efficiently generated. Conducted to the tip of the probe. Therefore, the sample surface can be efficiently heated.

In the heating device according to the third aspect, only a desired point on the sample surface is heated or a desired region on the sample surface is heated in a state where the cantilever is bent and the probe is pressed against the sample surface. The heating means and the first and second moving means are controlled by the control means so that each point is heated sequentially. In this case, since the probe is pressed against the sample surface by the bending of the cantilever, the probe surely contacts the sample surface, and the heat conduction from the tip of the probe to the sample surface is effectively performed. Further, even when the probe is scanned with respect to the sample surface to heat a desired area of the sample surface, the probe can follow the unevenness of the sample surface due to the bending of the cantilever, so the probe can reliably And the heat is effectively conducted from the tip of the probe to the sample surface. Since the temperature of the probe is controlled to the desired temperature based on the thermoelectromotive force from the thermocouple, the sample can be heated to the desired temperature.

In the heating device according to the fourth aspect, the probe moves toward the desired point on the sample surface or the sample surface while the second moving means is controlled so that the deflection of the cantilever becomes constant. The first moving means is controlled so as to sequentially scan each point of the desired area. Further, the heat generation driving means is controlled so that only a desired point on the sample surface is heated or each point in a desired region on the sample surface is sequentially heated. Therefore, while realizing the movement control of the probe similar to the so-called contact mode in the atomic force microscope,
Only the desired points on the sample surface are heated, or each point on the desired area of the sample surface is heated sequentially. Therefore, since the contact state between the probe and the sample surface can be kept constant by following the unevenness of the sample surface, the heating efficiency of the sample surface can be made constant regardless of the unevenness of the sample surface. Also,
Since the movement control of the probe similar to that in the contact mode is realized, as in the heating / shape measuring device according to the sixth aspect, by obtaining the information on the relative position, simultaneously with the heating of the sample surface and before the heating. Alternatively, it becomes possible to obtain the shape data of the unevenness of the sample surface after heating, which is preferable in determining the heating location on the sample surface and observing the sample. Since the temperature of the probe is controlled to the desired temperature based on the thermoelectromotive force from the thermocouple, the sample can be heated to the desired temperature.

In the heating device according to the fifth aspect, the cantilever is vibrated by the vibrating means, and the interatomic force acting between the probe of the cantilever and the sample surface is detected based on the detection signal of the vibration state of the cantilever. While the second moving means is controlled so that the force is constant, the first probe is arranged so as to face the desired point on the sample surface or sequentially scan each point on the desired region of the sample surface. Means of movement are controlled. Further, the heat generation driving means is controlled so that only a desired point on the sample surface is heated or each point in a desired region on the sample surface is sequentially heated. Therefore, while the movement control of the probe similar to the predetermined mode in the atomic force microscope is realized, only a desired point on the sample surface is heated or each point in a desired region on the sample surface is sequentially heated.
Therefore, the distance between the center of vibration of the probe and the sample surface can be kept constant by following the unevenness of the sample surface, so that the heating efficiency of the sample surface can be made constant regardless of the unevenness of the sample surface. it can. Further, since the movement control of the probe similar to the predetermined mode in the atomic force microscope is realized, the information on the relative position is obtained by obtaining the information on the relative position as in the heating / shape measuring device according to the sixth aspect. At the same time as the heating, before or after the heating, it becomes possible to obtain the shape data of the unevenness of the sample surface, which is preferable in determining the heating point on the sample surface and observing the sample. And
Since the temperature of the probe is controlled to the desired temperature based on the thermoelectromotive force from the thermocouple, the sample can be heated to the desired temperature.

[0022]

BEST MODE FOR CARRYING OUT THE INVENTION A cantilever, a heating device and a heating / shape measuring device according to the present invention will be described below with reference to the drawings.

First, a cantilever according to an embodiment of the present invention will be described with reference to FIGS.

FIG. 1 is a schematic plan view showing a cantilever according to an embodiment of the present invention. FIG. 2 shows I in FIG.
It is an I-II line schematic sectional drawing.

As shown in FIGS. 1 and 2, the cantilever is provided in a support 1, a flexible plate 2 having one end supported by the support 1, and a distal end region of the flexible plate 2. The probe 3 having a thermocouple and the heating element 4 for heating the tip of the probe 3 are provided.

In the present embodiment, the support 1 is composed of the silicon nitride film 5, the silicon layer 6 and the silicon nitride film 7. The flexible plate 2 is composed of a silicon nitride film 5. However, the configurations of the support 1 and the flexible plate 2 are not limited to such a configuration.

In the present embodiment, the probe 3 includes a first thermocouple forming section 8 made of a metal material forming the thermocouple.
The silicon oxide film 9 surrounding the protruding portion of the first thermocouple forming portion 8 and the tip of the first thermocouple forming portion 8 slightly protruding from the apex portion of the silicon oxide film 9 are joined to the thermocouple. And a film-shaped second thermocouple constituting section 10 (the second thermocouple constituting section 10 and the first thermocouple constituting section 8 are made of different kinds of metal materials). However, the configuration of the probe 3 is not limited to such a configuration.

The first thermocouple forming portion 8 extends around the probe 3 on the flexible plate 2 and is used for electrical connection with the wiring pattern 8a for the thermocouple and the outside. The electrode pattern 8b of No. 1 extends on the support 1. Further, the second thermocouple component 10 extends over the entire lower surface of the flexible plate 2 and the lower surface of the support 1.

Further, in the present embodiment, the electric insulating layer 11 is formed on the first thermocouple forming portion 8, and the heating element 4 is formed in a hairpin shape on the electric insulating layer 11. The heat from the heating element 4 is transferred to the tip of the probe 3 due to the heat conduction phenomenon,
Will heat the tip of the probe 3. In the present embodiment, since the first thermocouple component 8 is also used as the high thermal conductor interposed between the heating element 4 and the probe 3, the heat from the heating element 4 is efficiently transferred to the probe 3. Is transmitted to the tip of the.

The heating element 4 may extend not only to the peripheral portion of the probe 3 but also to the inner portion of the probe 3, and the entire inner portion of the probe 3 is not formed into a hairpin shape. Alternatively, it may be formed in a rectangular shape around it. As a material of the heating element 4, for example, a metal film having a high volume resistivity such as chromel, alumel, or nichrome can be used. Further, when the heat generation amount of the heating element 4 may be relatively small, even if the material used for the wiring pattern is aluminum or the like, the line width can be sufficiently narrowed to increase the resistance per unit length. For example, it can be used as a material for the heating element 4.

On the flexible plate 2, a heating element 4 is placed.
A wiring pattern 12 electrically connected to is formed. The wiring pattern 12 extends on the support 1 and is connected to an electrode pattern 13 formed on the support 1 for electrical connection with the outside.

Next, an example of a method for manufacturing the cantilever shown in FIGS. 1 and 2 will be described with reference to FIG. FIG. 3 is a schematic cross-sectional view showing an example of a manufacturing process of the cantilever shown in FIGS. 1 and 2. In addition, in FIG.
The elements corresponding to the respective elements are given the same reference numerals.

First, dichlorocyan and ammonia gas are used as raw materials by low pressure vapor phase epitaxy on both surfaces of an n-type silicon substrate 6 having a thickness of 250 μm and a (100) plane orientation covered with a natural oxide film. 70 for the silicon nitride films 5 and 7
A film of 0 nm is formed. Further, the silicon nitride film 5 on the upper surface of the substrate 6
Is patterned by a photolithography method and a dry etching method to form a rectangular opening 5a exposing the surface of the substrate 6 at a predetermined position of the silicon nitride film 5 on the upper surface of the substrate 6. Then, the substrate 6 is immersed in a silicon etching solution such as potassium hydroxide solution or tetramethylammonium hydroxide, and the substrate 6 exposed through the opening 5a using the silicon nitride films 5 and 7 as a mask.
This portion is anisotropically etched into a quadrangular pyramid shape to form a quadrangular pyramid-shaped trench 6a continuous with the opening 6a of the silicon nitride film 5 (FIG. 3A). Since the substrate 6 having the (100) plane orientation is used, as is well known, the etching automatically stops at the (111) plane of silicon. Therefore, the surface of the trench 6a has an angle of 54.7 °. It becomes the taper surface of.

Then, the substrate in the state shown in FIG. 3A is placed in an electric furnace and heated to expose the trench 6a of the substrate 6.
A silicon oxide film 9 is grown by thermal oxidation on the portion. As is well known, since the growth rate of a silicon oxide film is high in a flat portion and slow in a corner portion, the cross-sectional shape of the silicon oxide film 9 grown in the trench 6a is shown in FIG. As shown in (b), the thickness of the bottom portion is extremely thin compared to other portions. After that, a metal such as silver, copper, or aluminum is formed on the substrate in this state, and the film is patterned by a photolithography method and a wet etching method to form a portion of the trench 6a of the silicon oxide film 9 and its periphery. The first thermocouple forming portion 8 is formed in a rectangular shape in the portion, and the wiring pattern 8a and the electrode pattern 8b continuous to this are formed. Furthermore, by depositing silicon oxide, silicon nitride, or the like on the upper surface of the substrate in this state, and then patterning this by photolithography and dry etching,
An insulating layer 11 is formed on the first thermocouple component 8 (see FIG. 3).
(B)). The insulating layer 11 can also be formed by a lift-off method or the like.

Next, a film of chromel, alumel, nichrome, etc. is formed on the upper surface of the substrate in the state shown in FIG. 3B, and this is patterned by photolithography and dry etching to form a film on the insulating layer 11. The heating element 4 is formed in a hairpin shape. The heating element 4 can also be formed by a lift-off method or the like. Further, by patterning a metal layer of gold, platinum, aluminum or the like on the upper surface of the silicon nitride film 5 by a lift-off method or the like,
The wiring pattern 12 and the electrode pattern 13 are formed. Although not shown in the drawing, the bending of the flexible plate 2 irradiated toward the flexible plate 2 by devising the shape of the wiring pattern 12 (for example, making a predetermined portion thick) It can also be used as a reflection layer for reflecting a light beam for detection or the like. However, a reflective layer may be formed on the flexible plate 2 separately from the wiring pattern 12, and when the flexure of the flexible plate 2 is detected without using the optical lever method, or when the flexible plate 1 is used. When it is not necessary to detect bending, it is not necessary to form the reflective layer. Thereafter, the silicon nitride films 5 and 7 on both surfaces of the substrate 6 are patterned by photolithography and dry etching in accordance with the desired shape of the flexible plate 2 and the desired shape of the support 1. FIG. 3C).

Then, the substrate in the state shown in FIG. 3C is immersed in a heated silicon etching solution such as tetramethylammonium hydroxide solution to elute only the unnecessary silicon portion exposed by the patterning. Furthermore, this substrate is a potassium hydroxide aqueous solution (this aqueous solution is
The silicon oxide film 9 is dipped in the silicon oxide film at a low speed, and the silicon oxide film 9 is isotropically and slightly etched away, and the apex portion of the silicon oxide film 9 after the etching removal (the thickness is the thinnest before etching) (Corresponding to the portion), the tip of the first thermocouple forming part 8 is slightly projected (FIG. 3 (d)).

Finally, a second thermocouple forming section 10 is formed by depositing a metal material of a different type from the first thermocouple forming section 8 on the lower surface side of this substrate. This allows
The cantilever shown in FIGS. 1 and 2 is completed.

The tip of the probe 3 is preferably sharp in order to heat the sample and measure the shape of the sample surface with high resolution.

In the cantilever shown in FIGS. 1 and 2 described above, the heating element 4 heats the tip of the probe 3. Therefore, by bringing the tip of the probe 3 into contact with the sample surface or bringing them into close proximity with each other at a minute interval,
The sample surface can be heated via the tip of the. At this time, since the tip of the probe 3 can be made extremely sharp like a cantilever adopted in the scanning atomic force microscope, atoms on the sample surface can be inserted through the tip of the probe 3. It is possible to locally heat a minute region of molecular order. Moreover, according to the cantilever shown in FIGS. 1 and 2, since the probe 3 is provided with the thermocouple, the temperature of the probe can be controlled to a desired temperature based on the thermoelectromotive force from the thermocouple. it can. For this reason, it is possible to locally and atomically heat a minute region on the sample surface to a desired temperature via the tip portion of the probe 3. And
According to the cantilever shown in FIG. 1 and FIG. 2, since the cantilever structure is adopted, the tip portion of the probe 3 can be sampled by skillfully utilizing the bending of the flexible plate 2 as described later. It can be in contact with the surface or in close proximity with a small spacing.

Next, a heating / shape measuring apparatus according to an embodiment of the present invention using the above-described cantilever will be described with reference to FIG. FIG. 4 is a schematic configuration diagram of this heating / shape measuring device.

This heating / shape measuring device is shown in FIGS.
8, a cantilever holder 22 that supports the cantilever 21, and the cantilever holder 22 in X, Y, and Z directions (X direction is a direction perpendicular to the plane of FIG. 8 and Y direction is in FIG. 8). The left and right directions and the Z direction are the up and down directions in FIG. 8, and the cantilever moving device 23 for moving the XY plane is a surface substantially parallel to the surface of the sample 50, and a drive circuit for driving the moving device 23. 24
And a moving device 2 for roughly moving the sample 50 in the X, Y, and Z directions.
5, a drive circuit 26 for driving the moving device 25, a moving device 27 for finely moving the sample 50 in the X, Y, and Z directions, a driving circuit 28 for driving the moving device 27, and an electrode pattern 13 of the cantilever 21. And a heating drive circuit 29 that energizes the heating element 4 via the wiring pattern 12 to drive the heating element 4 of the cantilever 21 to generate heat, and a bending detection unit 30 that detects bending of the flexible plate 2 of the cantilever 21. A thermoelectromotive force detection circuit 60 that performs signal processing such as amplification and compensation on thermoelectromotive force obtained through the electrode pattern 8b of the cantilever 21 and the second thermocouple component 10, and drive circuits 24, 26, 28. , 29, control the heat generation drive circuit 29 by taking in the thermoelectromotive force obtained through the thermoelectromotive force detection circuit 60, and take in the detection signal from the deflection detection section 30 to obtain a predetermined value. A calculation / control unit 31 including a computer for performing calculations, an input device 32 such as a keyboard and a mouse for giving a command to the calculation / control unit by a user, a CRT for displaying the obtained results, etc. Display device 33 of FIG. The moving device 27 is used for the sample 50.
Also serves as a sample stand. Further, in FIG. 8, 34 is a base.

In the present embodiment, the deflection detecting section 30
Is configured to detect the bending of the flexible plate 2 of the cantilever 21 according to a known optical lever method, and specifically, for example, a He-Ne laser that irradiates the flexible plate 2 with laser light. And a two-divided photodetector for detecting the laser light reflected by the flexible plate 2. However, the configuration of the deflection detection unit 30 is not limited to such a configuration, and may not be based on the optical lever method.

The configuration of the heating / shape measuring apparatus as described above is almost the same as that of the conventional scanning atomic force microscope, but the cantilever 21 has the heating element 4 and the thermocouple, and the heating driving is performed. It is completely different from the conventional scanning atomic force microscope in that it has a circuit 29, heating control and temperature control which will be described later by the arithmetic / control unit 31.

Next, an example of the operation of the heating / shape measuring device will be described.

In the first heating operation of the heating / shape measuring device, in response to a predetermined command input by the user via the input device 32, the arithmetic / control unit 31 causes the cantilever 21 to bend and search. The driving circuit is configured so that only the desired points on the surface of the sample 50 are heated or the respective points on the desired region of the surface of the sample 50 are sequentially heated while the needle 3 is pressed against the surface of the sample 50. 24, 26, 28, 29 are controlled. Further, the calculation / control unit 31 controls the thermoelectromotive force from the thermocouple (the electrode pattern 8 of the cantilever 21 during heating).
The heating drive circuit 29 is controlled so that the temperature of the probe 3 becomes the temperature set by the user with the input device 32, based on the voltage between b and the second thermocouple component 10.
When heating a desired region of the surface of the sample 50, for example, the user may set a different temperature for each point of the region, and in that case, the calculation / control unit 31 does not change the temperature. The heat generation drive circuit 29 is controlled so that the probe 3 is set to each set temperature when scanning each point according to the setting.

Specifically, in the case of heating only a desired point of the sample 50, the probe 3 is operated by operating the moving devices 25 and 27 via the drive circuits 26 and 28, for example.
X, Y whose tip corresponds to a desired point on the surface of the sample 50
Direction, the sample 50 is moved in the X and Y directions, and then the sample 50 is moved in the Z direction so that the cantilever 21 bends and the tip of the probe 3 is pressed against the surface of the sample 50. To do. After that, the heating element 4 of the cantilever 21 is made to generate heat via the drive circuit 29, or the heating element 4 is made to generate heat in advance.

When heating a desired region of the sample 50, the tip of the probe 3 is moved to the surface of the sample 50 by operating the moving devices 25 and 27 via the drive circuits 26 and 28, for example. The sample 50 in the X and Y directions until it reaches a position in the X and Y directions corresponding to the desired area of
After that, the sample 50 is moved in the Z direction and the cantilever 21 is moved.
Is bent and the tip portion of the probe 3 is pressed against the surface of the sample 50. After that, while maintaining the position of the sample 50 in the Z direction, the moving device 25,
By operating 27, the sample 50 is moved in the X and Y directions so that the tip of the probe 3 scans a desired area on the surface of the sample 50. During the scanning, the drive circuit 29
The heating element 4 of the cantilever 21 is caused to generate heat via.

In the first heating operation described above, since the probe 3 is pressed against the surface of the sample 50 by the bending of the cantilever 21, the probe 3 surely comes into contact with the surface of the sample 50, and the tip of the probe 3 comes into contact. Heat is effectively conducted from the part to the surface of the sample 50. Further, even when the probe 3 is scanned with respect to the surface of the sample 50 in order to heat a desired region of the surface of the sample 50, the probe 3 follows the unevenness of the surface of the sample 50 due to the bending of the cantilever 21. The probe 3 surely contacts the surface of the sample 50, and the heat conduction from the tip portion of the probe 3 to the surface of the sample 50 is effectively performed.

Since it is not always necessary to detect the bending of the cantilever 21 in the first heating operation, the bending detection section 30 may be removed when only the first heating operation is performed.

In the second heating operation of the heating / shape measuring device, in response to a predetermined command input by the user via the input device 32, the arithmetic / control unit 31 causes the deflection detecting unit 3 to operate.
Based on the detection signal from 0, the position of the sample 50 in the Z direction is adjusted so that the deflection of the cantilever 21 becomes constant.
6, 28 and moving devices 25, 27 while controlling
The positions of the sample 50 in the X and Y directions are set to drive circuits 26, 28 so that the probe 3 faces a desired point on the surface of the sample 50 or sequentially scans each point in a desired region on the surface of the sample 50.
And the moving device 25, 27 to control the sample 5
The heat generation drive circuit 29 is controlled so that only the desired points on the surface of 0 are heated or the respective points on the desired region of the sample surface are sequentially heated. Further, as in the case of the first heating operation, the calculation / control unit 31 also causes the thermoelectromotive force from the thermocouple (the electrode pattern 8b of the cantilever 21 and the second
Voltage between the thermocouple forming part 10 and the
The heat generation drive circuit 29 is controlled so that the temperature of is the temperature set by the user with the input device 32.

Specifically, in the second heating operation, first,
The position of the cantilever 21 is adjusted using the moving device 23. This position adjustment is to irradiate a predetermined position of the cantilever 21 with laser light from a laser light source that constitutes the deflection detection unit 30, and to cause the reflected light reflected by the cantilever 21 to enter a predetermined position of the two-divided photodetector. , To adjust the position of the cantilever 21. Next, by operating the moving devices 25 and 27 via the drive circuits 26 and 28, the tip of the probe 3 is positioned in the X and Y directions corresponding to a desired point or a desired region on the surface of the sample 50. The sample 50 is moved in the X and Y directions until it reaches. After that, the moving devices 25 and 27 are used to move the sample 50 in the Z direction until the probe 3 of the cantilever 21 and the sample 50 come into contact with each other. At this time, the contact between the probe 3 of the cantilever 21 and the sample 50 can be achieved by detecting the bending of the cantilever 21 by the bending detection unit 30. In the case of heating only a desired point on the surface of the sample 50, in this contact state, the cantilever 2 is driven through the drive circuit 29.
The heating element 4 of No. 1 is caused to generate heat, and the heating is finished. on the other hand,
When heating a desired region of the surface of the sample 50, after the contact between the sample 50 and the probe 3 is achieved, the moving device 27 is used.
The cantilever 21 measured by the deflection detection unit 30 using
The sample 50 is moved in the X and Y directions so that the tip of the probe 3 scans a desired region on the surface of the sample 50 while moving the sample 50 up and down in the Z direction so as to keep the deflection of the sample constant.
During the scanning, the cantilever 21 is driven through the drive circuit 29.
The heating element 4 is heated.

In the second heating operation described above, while the movement control of the probe 3 similar to the so-called contact mode in the atomic force microscope is realized, only a desired point on the surface of the sample 50 is heated or Each point in the desired area on the surface of the sample 50 will be heated sequentially. Therefore, since the contact state between the probe 3 and the surface of the sample 50 can be kept constant by following the unevenness of the surface of the sample 50, the heating efficiency of the surface of the sample 50 regardless of the unevenness of the surface of the sample 50. Can be constant.

For example, when so-called raster scanning is performed by the probe 3, if the heating element 4 is made to generate heat in a pulsed manner in accordance with the scanning order, it is possible to heat an area of arbitrary shape on the surface of the sample 50. .

In the shape measuring operation of the heating / shape measuring apparatus, in response to a predetermined command input by the user via the input device 32, the calculation / control unit 31 causes the calculation / control section 31 to perform the second heating operation described above. Similarly to the case, the position of the sample 50 in the Z direction is controlled via the drive circuits 26 and 28 and the moving devices 25 and 27 so that the bending of the cantilever 21 becomes constant based on the detection signal from the bending detection unit 30. While the probe 3 is the sample 5
The position of the sample 50 in the X and Y directions is controlled via the drive circuits 26 and 28 and the moving devices 25 and 27 so as to sequentially scan each point of the desired area on the surface of 0 and the X and Y directions. The information about the relative position of the probe 3 with respect to the surface of the sample 50, that is, the shape data of the surface of the sample 50 is obtained.

This shape measuring operation is the same as the contact mode operation in the conventional scanning microscope.

In the present embodiment, since the position control of the moving device is performed by the open loop control, the moving devices 23, 25, 27 output from the arithmetic / control unit 31.
The control signal to corresponds to the position information of the mobile devices 23, 25, 27. Therefore, the calculation / control unit 31 stores the shape data of the surface of the sample 50 in the internal memory based on this control signal. When the position control of the moving devices 23, 25, 27 is performed by feedback control, for example, the moving devices 23, 25, 27 may be provided with a position detector.

Then, in the present embodiment, the arithmetic / control unit 31 processes the shape data to display an uneven image of the surface of the sample 50 on the display device.

Since the scanning of the probe 3 is common to the second heating operation and the shape measuring operation, these operations can be performed simultaneously.

Since the above-mentioned heating / shape measuring apparatus carries out each of the operations described above, it can be used as follows.

That is, the second heating operation and the third heating operation
By simultaneously performing the shape measurement operation described above, it is possible to simultaneously obtain the shape data of the surface of the sample 50 and heat the surface of the sample 50 entirely or locally.

Further, the shape data of the surface of the sample 50 before heating is acquired by the shape measurement operation, the heating point is determined based on this shape data, and then the position is locally changed by the second heating operation. It can be heated. That is, when it is desired to cause a thermal reaction at a singular point or an arbitrary position as a result of observing the unevenness of the sample 50 in the shape measuring operation, the position is locally heated by the second heating operation. It is possible. In this case, for example, by pointing out a part of the image of the unevenness of the surface of the sample 50 before heating displayed on the display device 33 with a mouse or the like as the input device 32, the portion is detected as the first image. It is preferable to build a user interface that is automatically heated by the second heating operation.

Further, the shape data of the surface of the sample 50 before heating is acquired by the shape measuring operation, the surface of the sample 50 is heated entirely or locally by the second heating operation, and then the shape measuring is performed again. Sample 5 after heating by operation
By acquiring the surface shape data of 0, it is also possible to observe the unevenness change of the surface of the sample 50 before and after heating.

The second heating operation and the shape measuring operation in the heating / shape measuring apparatus of the above-described embodiment are based on the contact mode in the scanning atomic force microscope.

However, by modifying the above-mentioned heating / shape measuring device as follows, it is possible to realize the heating operation and the shape measuring operation in other predetermined modes in the scanning atomic force microscope.

That is, in FIG. 8, the cantilever 2
A vibration unit that vibrates 1 and a vibration detection unit that detects the vibration state of the cantilever 21 are added.

The vibrating portion is, for example, a piezo element (not shown) provided on the flexible plate 2 of the cantilever 21, or a piezo element interposed between the cantilever holder 22 and the cantilever moving device 23. (Not shown) or the like can be employed. By applying an AC voltage to this piezo element, the cantilever 21
Vibrates. At this time, it is preferable that the frequency of the AC voltage applied to the piezo element is set to be a frequency slightly different from the natural frequency of the cantilever 21.

As the vibration detecting section, since the bending detecting section 30 is composed of a laser light source and a two-divided photodetector, this can be used as it is.
However, as the vibration detection unit, for example, a piezoresistor provided on the flexible plate 2 of the cantilever 21 can be adopted, and the vibration state can be detected from the resistance change of the piezoresistor.

The interatomic force acting between the probe 31 and the surface of the sample 50 changes according to the distance between the surface of the sample 50 and the probe 31, and the cantilever according to the interatomic force. When the resonance frequency of 21 shifts and the atomic force changes, the detection signal from the vibration detector changes. Therefore, based on the detection signal from the vibration detector, the distance between the sample 50 and the cantilever 21 is relatively moved in the vertical direction so that the interatomic force becomes constant.
By doing so, the distance between the sample 50 and the center of vibration of the cantilever 21 becomes constant, so that the heating amount of the sample surface can be made constant regardless of the unevenness of the surface of the sample 50, and at the same time, the sample 50 can be heated. The shape data of the surface of can be obtained.

Even if the heating / shape measuring apparatus described above is modified to perform the heating operation and the shape measuring operation in such a mode as described above, it is substantially the same as the heating / shape measuring apparatus described above. .

In the heating / shape measuring device described above,
Without heating the heating element 4 of the cantilever 21, the probe 3 is scanned in each of the above-described modes, and the sample 5 of the probe 3 is scanned.
It is also possible to measure the temperature distribution on the surface of the sample 50 by obtaining temperature data based on the thermoelectromotive force according to the relative position with respect to zero. In this case, it is possible to obtain a change in the temperature distribution on the surface of the sample after being heated once, which is more useful for analyzing the sample.

Although various embodiments of the present invention have been described above, the present invention is not limited to these embodiments.

[0072]

According to the present invention, it becomes possible to locally heat a minute region on the atomic or molecular order of a sample to a desired temperature.

Therefore, according to the present invention, the following specific application effects can be obtained.

The normal function of the biological sample in the living environment is 30 ° C to 40 ° C. Biological research is currently being carried out at the molecular level. According to the present invention, it is possible to finely observe the active state of living organisms by heating at a molecular level resolution in the range of 30 ° C to 40 ° C. In particular, in the present invention, since heating to a desired temperature is possible, it is possible to observe the active state of the organism due to a slight difference in temperature.

The temperature is also an important factor in controlling the protein activity and denaturation. Therefore, according to the present invention, the binding state can be examined at the molecular level by locally heating a protein having a large molecular weight.

Furthermore, in organic substances, the bonding state changes with temperature. Therefore, local heating of an organic substance having a large molecular weight can change the bonding state of molecular chains at the molecular level. Therefore, the present invention can also be applied to nanometer-order lithography.

[Brief description of drawings]

FIG. 1 is a schematic plan view showing a cantilever according to an embodiment of the present invention.

FIG. 2 is a schematic cross-sectional view taken along the line II-II in FIG.

FIG. 3 is a schematic cross-sectional view showing an example of a manufacturing process of the cantilever shown in FIGS. 1 and 2.

FIG. 4 is a schematic configuration diagram of a heating / shape measuring device according to an embodiment of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Support body 2 Flexible plate 3 Probe 4 Heating element 8 1st thermocouple structure part 10 2nd thermocouple structure part 21 Cantilever 23,25,27 Moving device 24,26,29 Drive circuit 28 Heat generation drive circuit 30 Deflection Detection Unit 31 Calculation / Control Unit 32 Input Device 33 Display Device 60 Thermoelectromotive Force Detection Circuit

Claims (6)

[Claims] 1. A cantilever comprising a support, a flexible plate whose one end is supported by the support, and a probe provided in a distal end side region of the flexible plate, wherein the probe is provided. A cantilever characterized in that a heating element for heating the distal end of the probe is provided, and a thermocouple is provided at the probe. 2. The cantilever according to claim 2, wherein at least a part of the metal material forming the thermocouple is also used as a high thermal conductor interposed between the heating element and the probe. . 3. The cantilever according to claim 1 or 2, a heat generation drive means for generating heat from the heat generating element, and the probe relatively moved with respect to the sample in a direction substantially parallel to the sample surface. Based on thermoelectromotive force from the thermocouple, first moving means for moving, second moving means for moving the probe relative to the sample in a direction substantially perpendicular to the sample surface, Temperature control means for controlling the heat generation driving means so that the temperature of the probe becomes a desired temperature, and in a state where the cantilever is bent and the probe is pressed against the sample surface, Control means for controlling the heat generation driving means and the first and second moving means so that only desired points are heated or respective points in desired areas of the sample surface are sequentially heated. A heating device characterized by having . 4. The cantilever according to claim 1 or 2, a heat generating drive means for causing the heating element to generate heat, a deflection detecting means for detecting deflection of the cantilever, and a direction substantially parallel to the sample surface. First moving means for moving the probe relative to the sample; second moving means for moving the probe relative to the sample in a direction substantially perpendicular to the sample surface; While controlling the second moving means so that the bending of the cantilever is constant based on the detection signal from the bending detecting means, the probe is opposed to a desired point on the sample surface or the sample Means for controlling the first moving means so as to sequentially scan each point of the desired area of the surface, and only the desired point of the sample surface is heated or each of the desired area of the sample surface So that the points are heated sequentially A means for controlling the heat generation driving means, and a temperature control means for controlling the heat generation driving means so that the temperature of the probe becomes a desired temperature based on the thermoelectromotive force from the thermocouple. A heating device characterized by being provided. 5. A cantilever according to claim 1 or 2, a heat generating drive means for causing the heating element to generate heat, a vibrating means for vibrating the cantilever, a vibration state detecting means for detecting a vibration state of the cantilever, First moving means for moving the probe relative to the sample in a direction substantially parallel to the sample surface, and the probe relative to the sample in a direction substantially perpendicular to the sample surface The second moving means for moving the first and the second moving means so that the atomic force acting between the probe of the cantilever and the sample surface becomes constant based on the detection signal from the vibration detecting means. While controlling the moving means, the first moving means is controlled so that the probe faces a desired point on the sample surface or sequentially scans each point in a desired area on the sample surface. Means and said A means for controlling the heat generation driving means so that only a desired point on the material surface is heated or each point in a desired area on the sample surface is sequentially heated, and a thermoelectromotive force from the thermocouple is applied. On the basis of the above, the heating device is provided with: temperature control means for controlling the heat generation driving means so that the temperature of the probe becomes a desired temperature. 6. The heating device according to claim 4, wherein the heating device is arranged in a direction substantially perpendicular to the sample surface, depending on a relative position of the probe with respect to the sample surface in a direction substantially parallel to the sample surface. A heating / shape measuring apparatus comprising: a unit that obtains information about a relative position of the probe with respect to the sample surface.