JP5627472B2 - Cantilever holder and scanning probe microscope having the same - Google Patents

Description

  The present invention relates to a scanning probe microscope that performs shape observation and physical property measurement by oscillating a cantilever having a probe at the tip while bringing the cantilever close to or in contact with a sample, and particularly relates to the cantilever holder.

  In a conventional scanning probe microscope, a cantilever having a probe at the tip is used to scan the sample with a triaxial fine movement mechanism, thereby measuring the shape image and physical properties of the sample surface. In the scanning probe microscope, the method of controlling the distance between the probe tip and the sample is roughly classified into a contact method and a vibration method.

  The vibration-type scanning probe microscope performs measurement according to the following principle. When a cantilever is vibrated in the vicinity of the primary resonance frequency with a piezoelectric element, the amplitude and phase of the cantilever are measured and the sample and probe are brought close to each other, a physical force such as an atomic force or an intermittent contact force is generated between the two. Works. This force changes the amplitude and phase of the cantilever or the resonance frequency. Since these changes depend on the distance between the sample and the probe, the distance between the sample and the probe is adjusted to a triaxial fine movement mechanism so that the change in the amplitude, phase, or resonance frequency of the cantilever is always constant. The distance in the height direction is controlled by controlling with the vertical fine movement mechanism provided. Furthermore, the sample and the probe are scanned relatively in the sample plane by the horizontal fine adjustment mechanism provided in the three-axis fine adjustment mechanism, and the displacement amount of the vertical fine adjustment mechanism is made to correspond to the height information of the sample. A shape image can be measured. In addition, electrical and magnetic properties due to electromagnetic signals acting between the sample and the probe, mechanical properties due to friction between the probe and the sample when the probe is pushed or pulled or scanned, etc. It is also possible to measure physical properties such as optical characteristics due to the interaction between the generated near-field light and the probe tip. The vibration-type distance control method has an advantage that the force exerted on the sample by the probe is lower than that in the contact mode, and measurement can be performed with little damage to the sample and the tip of the probe.

  The scanning probe microscope has an advantage that it can be measured in a solution in addition to the measurement in a general atmospheric environment. In solution, there are many samples with a soft surface, and measurement is often performed by a vibration method in order to prevent damage to the sample.

  In addition, in order to prevent sample corrosion or to investigate the reaction of the sample in the actual environment, the sample and the probe are arranged in a sealed space, and measurement may be performed in various gas environments.

  Here, the configuration of a conventional scanning probe microscope used in a solution is described in Patent Document 1. FIG. 13 is an overview of a conventional scanning probe microscope disclosed in Patent Document 1. In FIG. In FIG. 13, the cantilever fixing portion 105 is bonded and fixed to the glass base block 134 via the piezoelectric element 104, and the cantilever 106 fixed to the cantilever fixing portion 105 is forcibly vibrated near the resonance frequency of the cantilever by the piezoelectric element 104. The amplitude of the cantilever is measured by an optical lever type displacement detection mechanism 108. The displacement detection mechanism 108 emits laser light from the semiconductor laser 113, bends the optical path by the beam splitter 114, passes through the glass base block 134 and irradiates the back surface of the cantilever 106, and the reflected light passes through the glass base block 134. Thereafter, the optical path is bent by the mirror 115 and the displacement of the cantilever is detected by the quadrant photodetector 116.

  The sample 137 is fixed to the bottom surface of the petri dish 136, and the petri dish 136 is placed on a triaxial fine movement mechanism 118 constituted by a cylindrical piezoelectric element, and the sample 137 is scanned. A solution is placed in the petri dish 136, and the sample 137 is immersed in the solution. When the sample 137 and the probe 106a are brought closer to each other in this state, the projection 135 of the glass base block 134 is in contact with the liquid surface, the probe 106a is immersed in the solution, and the probe and the sample are in intermittent contact with each other. The amplitude of the cantilever changes according to the distance. At this time, while performing the distance control so that the amplitude of the cantilever becomes constant by the vertical fine movement mechanism of the three-axis fine movement mechanism 118, the shape of the sample in the solution is obtained by performing the raster scan by the horizontal fine movement mechanism of the three-axis fine movement mechanism. An image measurement is performed. In this prior art, since the cantilever fixing part 105 is directly fixed to the piezoelectric element 104, the cantilever can be vibrated efficiently even if it receives a viscous resistance from the solution.

  In Patent Document 2, as shown in FIG. 14, a cantilever 210 is attached to the tip of a glass holder 215, and a piezoelectric element 217 is arranged on the base of the holder 215 opposite to the side where the cantilever 210 is attached. The structure of a cantilever holder for a solution that causes the cantilever to vibrate by propagating vibration to the holder 215 is described.

Japanese Patent Laying-Open No. 2006-91002 (FIG. 5) International Publication No. 03/028036 Pamphlet (Figure 3)

  However, in the case of the technique described in Patent Document 1 described above, since the piezoelectric element is arranged on the solution side in which the sample is immersed and measurement is performed by immersing the piezoelectric element in the solution, there are the following problems. In other words, even if the piezoelectric element is coated with a molding agent such as silicone, depending on the type of solution in which the sample is immersed, the molding agent dissolves and a failure occurs in the piezoelectric element, or the molding agent is mixed into the solution and the sample Alteration may occur. In addition, the electrode of the piezoelectric element may come into contact with the solution, causing a short circuit or corrosion of the electrode, or the sample may be altered by an electrochemical reaction. Further, the adhesive that bonds the piezoelectric element also melts and the piezoelectric element is peeled off. When an organic solvent or the like is used, the molding agent may swell and the light path of the light lever may be blocked.

  Further, in the case of the technique described in Patent Document 2, there is little problem that the piezoelectric element has a problem due to the solution. However, since the vibration is propagated through the entire holder, the vibration transmission efficiency is poor and the amplitude of the cantilever is reduced. There was a problem of lowering. In order to increase the amplitude of the cantilever, it is necessary to increase the voltage applied to the piezoelectric element to increase the amplitude of the piezoelectric element. At this time, the various measuring parts and solutions mounted on the holder other than the cantilever are also increased. There is a problem in that vibrations occur, vibration peaks other than resonance of the cantilever occur, noise increases, and minute signal fluctuations cannot be captured and noise increases. Also, it may be difficult to determine the resonance peak of the cantilever during measurement.

  Further, when the probe and the sample are arranged in the sealed space, there is a problem that the electrodes of the piezoelectric element are deteriorated by the gas as in the measurement in the solution.

  The present invention has been made to solve the above-described problems, and cantilever holders that can be used in various environments and that can efficiently vibrate cantilevers, and scanning with improved cantilever holders. An object is to provide a scanning probe microscope.

  In order to achieve the above object, in the present invention, a cantilever holder for a scanning probe microscope is configured as follows.

Cantilever holder for scanning probe microscope of the present invention, a first base and a cantilever holding portion capable of holding one end of the cantilever, the end opposite to the side to hold the cantilever of the cantilever holding portion is fixed And a through hole that can pass through the cantilever holding portion, and a holding portion that holds the first base portion by hooking at least a part of the outer peripheral portion of the first base portion . Two base portions, a piezoelectric element placed on the opposite side of the cantilever holding portion of the first base portion to the fixed side, and a contact surface direction of the first base portion with respect to the piezoelectric element A piezoelectric element fixing member that tightly fixes the piezoelectric element to the first base portion by applying a preload .

According to the present invention, the piezoelectric element is fixed by applying a preload from the opposite surface, with one surface of the piezoelectric element contacting the edge of the first base portion. In this case, it is preferable that the piezoelectric element has a ring shape. Furthermore, a preload is applied to at least one surface of the piezoelectric element on the side in contact with or opposite to the first base portion via an elastic body.

Moreover, cantilever holder for scanning probe microscope of the present invention, the first in which the cantilever holding portion capable of holding one end of the cantilever, the end opposite to the side to hold the cantilever of the cantilever holding portion is fixed A base part, a through hole that can pass through the cantilever holding part, and a holding part that holds the first base part by hooking at least a part of the outer peripheral part of the first base part. A second base portion, a piezoelectric element placed on the opposite side of the first base portion to the fixed side of the cantilever holding portion, and one end placed on the first base portion of the piezoelectric element parts and is fixed to the end opposite, and a member having a heavier mass than the total mass of the mass of said first base portion of the mass and the cantilever holding portion.

  Furthermore, in the present invention, a laminated or plate-like piezoelectric element is used as the piezoelectric element.

  Further, the first base portion is made of a material capable of transmitting light having a wavelength in an arbitrary range of 200 nm to 2500 nm.

  In addition, the periphery of the cantilever held by the cantilever holding portion is configured to be immersed in the solution.

  Further, the cantilever holding part side and the piezoelectric element side are blocked by the first base part, and the cantilever holding part side is arranged in an environment different from the atmosphere.

  Furthermore, in the present invention, two electrodes functioning as a counter electrode and a reference electrode are disposed in the space immersed in the solution, and an electrode for functioning at least one of the sample and the cantilever as a working electrode is provided.

  Furthermore, the function which heats or cools the sample holder in which the sample arrange | positioned at the said cantilever holding | maintenance part or the cantilever opposing side was mounted was provided.

  By constructing a cantilever holder for a scanning probe microscope as described above, the piezoelectric element is not directly placed in a solution or gas environment, so that there is no dissolution or swelling of the molding agent, and the electrodes of the piezoelectric element Corrosion and adhesion peeling are also prevented. Therefore, measurement with a scanning probe microscope can be performed under various environments regardless of the type of solution or gas.

  In the present invention, the piezoelectric element is fixed by applying a preload to the first base part, or a member heavier than the total mass of the first base part and the cantilever holding part is provided on the terminal side of the piezoelectric element. By fixing, the cantilever can be vibrated efficiently and the measurement accuracy is improved.

  Further, according to the present invention, the piezoelectric element is fixed by applying one side of the piezoelectric element to the edge of the first base portion and applying a preload from the opposite surface. It is possible to prevent the base portion of the battery from being damaged. Furthermore, preload is applied to the first base part of the piezoelectric element on the side opposite to or opposite to the first base part via an elastic body to further prevent damage to the first base part and improve excitation efficiency. To do.

1 is a schematic view of a scanning probe microscope according to a first embodiment of the present invention. The top view of the cantilever holder which concerns on the 1st Embodiment of this invention. FIG. 5 is an overview diagram of a scanning probe microscope according to a second embodiment of the present invention. The top view of the cantilever holder which concerns on the 2nd Embodiment of this invention. FIG. 9 is an overview diagram of a scanning probe microscope according to a third embodiment of the present invention. The top view of the cantilever holder which concerns on the 3rd Embodiment of this invention. FIG. 9 is an overview diagram of a scanning probe microscope according to a fourth embodiment of the present invention. The top view of the cantilever holder which concerns on the 4th Embodiment of this invention. FIG. 10 is an overview diagram of a scanning probe microscope according to a fifth embodiment of the present invention. The top view of the cantilever holder which concerns on the 5th Embodiment of this invention. FIG. 10 is an overview diagram of a scanning probe microscope according to a sixth embodiment of the present invention. The top view of the cantilever holder which concerns on the 6th Embodiment of this invention. FIG. 6 is a schematic view of a conventional cantilever holder for a scanning probe microscope. FIG. 6 is a schematic view of a conventional cantilever holder for a scanning probe microscope.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the embodiments of the present invention, all have the function of a vibration type scanning probe microscope. In the following description, portions related to the present invention are described, and a part of drawings and descriptions of portions that are not related to the present invention in a known configuration of a scanning probe microscope are omitted.

<First Embodiment>
FIG. 1 is a schematic view showing the overall configuration of a scanning probe microscope according to the first embodiment of the present invention, and FIG. 2 is a plan view of a cantilever holder used in FIG.

  A scanning probe microscope 1 in FIG. 1 includes a three-axis fine movement mechanism 2 having a function of a horizontal fine movement mechanism 2a and a vertical fine movement mechanism 2b, and a three-axis fine movement, which are configured by a cylindrical piezoelectric element whose end is fixed to a base. The sample stage 3 fixed to the tip of the mechanism 2, the casing 4 of the unit, the displacement detection mechanism 6 installed in the casing 4 to detect the displacement of the cantilever 5, and the casing 4 The cantilever holder 7 is fixed.

  In the displacement detection mechanism 6, a semiconductor laser 9, a beam splitter 10, a total reflection mirror 11, a four-divided photodetector 12, and a preamplifier (not shown) are arranged in a housing 8 of the displacement detection mechanism. The laser beam 23 is bent by the beam splitter 10, irradiated onto the back surface of the cantilever 5, which will be described later, from directly above, the light reflected on the back surface of the cantilever 5 is bent by the total reflection mirror 11, and incident on the four-divided photodetector 12. The deflection direction of the cantilever 5 and the torsional displacement around the long axis are detected by the lever system.

  The cantilever holder 7 described in FIGS. 1 and 2 is used to fix a cantilever 5 integrally formed of silicone having a probe 5a at a distal end and a proximal end portion 5b at a distal end. The cantilever holder 7 vibrates the cantilever holding part 13, a first base part 14 that fixes the cantilever holding part 13, a second base part 15 that holds the first base part 14, and the cantilever 5. The piezoelectric element 16 for this is comprised.

  The cantilever holding portion 13 is formed by polishing the tip 13a of a cylindrical member made of quartz glass having a diameter of 12 mm and a length of 5 mm into a flat shape, and processing a part of the tip obliquely at an angle of 10 degrees with respect to the plane. An inclined flat surface portion 13b is provided, and the base end portion 5b of the cantilever is fixed to the inclined flat surface portion 13b. The cantilever 5 is fixed by providing a notch 13c in the cantilever holding portion 13 and fitting one end of a U-shaped plate spring 17 into the notch 13c, and tilting the base end 5b of the cantilever at the other end. The flat portion 13b was pressed and fixed.

  The first base portion 14 is made of quartz glass, has a disk shape with a diameter of 30 mm, a thickness of 3 mm, and is slightly larger than the diameter of the cantilever holding portion 13. Both surfaces of the first base portion 14 are polished. Yes. The end 13d of the cantilever holding portion 13 is fused to the flat portion 14a of the first base portion 14 so that the central axis coincides. Therefore. The first base portion 14 is a flange with respect to the cantilever holding portion 13, and the bonded joint surface is integrally formed with a constant refractive index.

  The second base portion 15 is made of a material made of titanium, has a square plate shape when viewed from above, and has a side length of 60 mm and a thickness of 6 mm. A through hole 15a having a diameter of 20 mm is provided at the center, and a holding portion 15b that is cut to a depth of 3 mm on the outer periphery substantially the same as the diameter of the first base portion 14 and protrudes to the central through hole 15a is provided. The first base portion 14 is engaged with the portion 15b.

  The piezoelectric element 16 is a stacked piezoelectric element in which electrodes of the same size as a square piezo thin film with a side of 5 mm are alternately stacked up to a length of 5 mm. The front end 16a of the piezoelectric element 16 is in contact with the position of the extension line of the inclined flat surface portion 13b of the cantilever holding portion 13 on the back surface 14b with respect to the surface to which the cantilever holding portion 13 of the first base portion 14 is fixed. Arranged. The other end 16 b of the multilayer piezoelectric element is in contact with the leaf spring 18, and both ends of the leaf spring 18 are fixed to the second base portion 15 with screws 19. At this time, the leaf spring 18 is bent and elastically deformed, whereby a preload is applied to the laminated piezoelectric element 16 and the first base portion 14 is fixed.

  The electrodes of the multilayer piezoelectric element 16 are connected to a driving power source (not shown), and the first base portion 14 is vibrated by applying an AC voltage from the driving power source.

  The first base portion 14 and the second base portion 15 are merely engaged without being bonded, and are fixed only by the preload of the leaf spring 18 via the laminated piezoelectric element 16.

  The both ends of the laminated piezoelectric element 16 are not bonded but are fixed only by the preload of the leaf spring 18, but the both ends or one of them may be bonded and fixed before applying the preload.

  In the present embodiment, measurement can be performed not only in the atmosphere but also in the liquid. When measurement is performed in the liquid, the petri dish 20 is placed on the sample stage 3 fixed to the tip of the triaxial fine movement mechanism 2 as shown in FIG. The sample 21 is placed on the bottom surface of the petri dish 20 and the solution 22 is placed. The solution is brought into contact with the tip 13a of the cantilever holding portion, and the cantilever 5 is immersed in the solution 22 for measurement.

  The displacement detection mechanism 6 is disposed immediately above the cantilever holder 7, and the laser beam 23 bent by the beam splitter 10 is substantially centered between the first base portion 14 and the cantilever holding portion 13 that are integrally formed. Incident along the axis, passes through the solution 22, reflects off the back surface of the cantilever 5, passes again through the cantilever holding part 13 and the first base part 14, is bent by the total reflection mirror 11, and enters the quadrant photodetector 12. Thus, the displacement of the cantilever 6 is detected. At this time, since the solution 22 and the tip 13a of the cantilever holding portion are in contact with each other, the laser beam 23 can be incident without being scattered on the liquid surface. The laminated piezoelectric element 16 and the leaf spring 18 described above are arranged at positions that do not obstruct the optical path of the laser.

  In this embodiment, a semiconductor laser having a wavelength of 670 nm is used as the wavelength of the laser beam 23. However, the sample may be altered by reaction with light, such as a semiconductor sample or a fluorescent sample. Wavelength light sources can be used. In some cases, the optical microscope 24 is disposed immediately above the displacement detection mechanism 6 to perform observation or spectroscopic analysis of the cantilever 5 or the sample 21. Therefore, at least the laser light 23 of the displacement detection mechanism 6 and the light transmitted from the optical microscope 24 of the first base part 14 and the cantilever holding part 13 are transmitted in the range of 200 nm to 2500 nm in accordance with these wavelength characteristics. It is comprised with the material which can permeate | transmit light of the arbitrary ranges among the following wavelengths.

Using the scanning probe microscope 1 configured as described above, the distance between the probe 5a and the sample 21 is set in the vertical direction so that the amplitude attenuation is constant while the cantilever 5 is vibrated in the vicinity of the primary resonance frequency. By performing feedback control with the fine movement mechanism 2b and raster scanning the probe 5a and the sample 21 with the horizontal fine movement mechanism 2a, the shape of the sample 21 in the solution 22 and mapping images of various physical properties can be measured. It is also possible to measure physical properties for each point.

  In the present embodiment, the piezoelectric element 16 for exciting the cantilever is disposed on the back surface 14b with respect to the surface on which the cantilever holding portion 13 of the first base portion 14 is fixed. It is possible to prevent the adhesion by the solution 22, the peeling and swelling of the molding agent, the corrosion of the electrode, the leakage of electric current, and the like, and various solutions such as an organic solvent as well as pure water can be disposed. Can be used.

  In particular, in the present invention, the tip 16a of the multilayer piezoelectric element 16 is brought into contact with the first base portion 14 and the other end 16b is brought into contact with the leaf spring 18, and both ends of the leaf spring 18 are connected to the second base portion 15 with screws 19. Since the plate spring 18 is bent and elastically deformed by bending it, the laminated piezoelectric element 16 is preloaded and the first base portion 14 is fixed in pressure. Compared to the case where the multilayer piezoelectric element 16 is fixed to the first base portion 14 without applying a force, the cantilever 5 can be vibrated more efficiently via the first base portion 14 and the cantilever holding portion 13. Measurement accuracy is improved.

  In particular, even when the cantilever is vibrated in a solution with viscous resistance as in this embodiment, the amplitude of the cantilever increases and the ratio of the amplitude signal to the noise increases, making it possible to perform low noise and high sensitivity measurement. .

  In addition, since the excitation amplitude of the cantilever can be secured even when the amplitude of the piezoelectric element is small, various measurement parts and solutions other than the cantilever mounted on the holder that was generated when the amplitude of the piezoelectric element was increased vibrated greatly. Further, vibration peaks other than resonance of the cantilever are generated and noise is increased, so that problems such as difficulty in determining the resonance peak of the cantilever during measurement and an increase in noise level of the measurement data itself can be avoided.

<Second Embodiment>
FIG. 3 is a schematic view showing the overall configuration of a scanning probe microscope according to the second embodiment of the present invention, and FIG. 4 is a plan view of a cantilever holder used in FIG.

  In this embodiment, since the configuration other than the cantilever holder 30 is the same as that of the first embodiment, the same members are denoted by the same reference numerals and detailed description thereof is omitted.

  Further, the cantilever holder 30 used in the scanning probe microscope 35 of FIG. 3 is the same as that of the first embodiment except for the position of the screw hole in the cantilever holding portion 13, the first base portion 14, and the second base portion 15. The material is used. These members are also denoted by the same reference numerals, and the detailed description is left to the description in the first embodiment.

  In the second embodiment shown in FIGS. 3 and 4, a donut-shaped single-plate piezoelectric element is used as the piezoelectric element 31 for cantilever excitation. The piezoelectric element 31 has an outer diameter of 22 mm, an inner diameter of 16 mm, a thickness of 2 mm, and is subjected to poling treatment in the thickness direction, and electrodes are provided on both surfaces 31a and 31b.

  The piezoelectric element 31 has one surface 31a disposed around a surface 14b opposite to the surface 14a to which the cantilever holding portion 13 of the first base portion 14 is fixed, and has an outer diameter of 60 mm, an inner diameter of 15 mm, and a thickness of 4 mm. Using a ring-shaped stainless steel piezoelectric element fixing member 32 having a groove 32a having a diameter of 30 mm and a depth of 1.5 mm on one surface, the other surface 31b of the piezoelectric element 31 is brought into contact with the groove 32a. The four locations around the piezoelectric element fixing member 32 are fixed to the second base portion 15 with screws 33.

  At this time, since a gap of 0.5 mm is formed between the second base portion 15 and the piezoelectric element fixing member 32, preload is applied by screwing, and the piezoelectric element 31 is attached to the first base portion 14. Fixed under pressure.

  In this embodiment as well as the first embodiment, the piezoelectric element 31 can be disposed outside the solution 22, and the adhesion of the solution 22, the peeling or swelling of the molding agent, electrode corrosion, current leakage, etc. In addition to pure water, various solutions such as organic solvents can be used. In addition, the cantilever can be vibrated efficiently via the first base portion 14 and the cantilever holding portion 13, and the measurement accuracy is improved.

  In the present invention, since the disk-shaped piezoelectric element 31 is used, the piezoelectric element 31 can be disposed without interfering with the optical path of the laser beam 23 of the displacement detection mechanism 6 and the microscope 24.

<Third Embodiment>
FIG. 5 is a schematic view showing the overall configuration of a scanning probe microscope according to the third embodiment of the present invention, and FIG. 6 is a plan view of a cantilever holder used in FIG.

  Also in this embodiment, since the configuration other than the cantilever holder 40 is the same as that of the first embodiment, the same members are denoted by the same reference numerals and detailed description thereof is omitted.

  Further, the cantilever holder 40 used in the scanning probe microscope 45 of FIG. 5 is the same as that of the first embodiment except for the position of the screw hole in the cantilever holding portion 13, the first base portion 14, and the second base portion 15. The material is used. These members are also denoted by the same reference numerals, and the detailed description is left to the description in the first embodiment.

  In the cantilever holder 40 of the third embodiment shown in FIGS. 5 and 6, the first base portion 14 is screwed to the second base portion 15 through the silicone rubber 42 with four claws 41 around the periphery. The

  Further, as the cantilever oscillating piezoelectric element 16, a laminated piezoelectric element in which electrodes having the same size as a square piezo thin film with a side of 5 mm are laminated to a length of 5 mm as in the first embodiment. The front end 16a of the piezoelectric element 16 is a surface 14b on the back side with respect to the surface 14a to which the cantilever holding portion 13 of the first base portion 14 is fixed, and is approximately at the position of the extension line of the inclined flat surface portion 13b of the cantilever holding portion 13. Bonded and fixed. For this reason, the multilayer piezoelectric element 16 is not immersed in the solution 22. A block 43 made of brass and having a length of 25 mm, a width of 12 mm, and a thickness of 20 mm is bonded and fixed to the other end 16 b of the multilayer piezoelectric element 16. At this time, the mass of the block 43 is about 52 g. On the other hand, the total mass of the first base portion 14 and the cantilever holding portion 13 is about 6 g. In this way, the first base portion is efficiently fixed by fixing the block 43 made of brass that is heavier than the total mass of the mass of the first base portion 14 and the mass of the cantilever holding portion 13 to the distal end side of the piezoelectric element 16. The measurement accuracy is improved.

  At this time, the greater the mass of the block 43 with respect to the total mass of the mass of the first base portion 14 and the cantilever holding portion 13, the greater the excitation effect.

<Fourth Embodiment>
FIG. 7 is a schematic view of a scanning probe microscope and a sealed cantilever holder according to a fourth embodiment. FIG. 8 is a plan view of a sealed cantilever holder used in the scanning probe microscope of FIG.

  Also in this embodiment, since the configuration other than the sealed cantilever holder 50 is the same as that of the first embodiment, the same members are denoted by the same reference numerals and detailed description thereof is omitted.

  The cantilever holder 50 used in the scanning probe microscope 66 of the present embodiment includes the cantilever 5 and the sample 21 in the sealed space 51, and a solution, gas, or the like is placed in the sealed space 51. It can be observed in a state close to a real environment, and is also used when a volatile organic solvent is used.

  In the sealed cantilever holder 50 of FIGS. 7 and 8, the cantilever holding part 52, the first base part 53 for fixing the cantilever holding part 52, and the second base part for holding the first base part 53 are provided. 54, a piezoelectric element 55 for exciting the cantilever 5, a Teflon (registered trademark) membrane film 56 forming a sealed space, a third base portion 57 for holding the membrane film 56, and an inner sample holder portion 58 Composed.

  The cantilever holding portion 52 is formed by polishing a tip 52a of a cylindrical member made of quartz glass having a diameter of 12 mm and a length of 5 mm into a flat shape, and machining a part of the tip 52a at an angle of 10 degrees with respect to the plane. The inclined flat surface portion 52b is provided, and the base end portion 5b of the cantilever is fixed to the inclined flat surface portion 52b. The cantilever 5 is fixed by providing a notch 52c in the cantilever holding part 52, fitting one end of the U-shaped plate spring 17 into the notch 52b, and the other end of the base end 5b of the cantilever with the inclined plane. It was made to press and fix to the part 52b.

  The first base portion 53 is made of quartz glass, has a diameter of 30 mm, a thickness of 3 mm, and a disk shape that is slightly larger than the diameter of the cantilever holding portion 52, and both surfaces 53 a and 53 b of the first base portion 53 are Polished. The end 52d of the cantilever holding portion is fused to the flat portion 53a of the first base portion 53 so that the central axis coincides. Therefore. The first base portion 53 is a flange with respect to the cantilever holding portion 52, and the fused bonding surface 52d is integrally formed with a constant refractive index.

  The second base portion 54 is made of a material made of polyether-ether-ketone resin (PEEK) having high chemical resistance. The second base portion 54 has a square plate shape as viewed from above and has a side length of 60 mm and a thickness of 6 mm. A through hole 54a having a diameter of 20 mm is provided at the center, and a holding portion 54b that is cut to a depth of 3 mm on the outer periphery substantially the same as the diameter of the first base portion 53 and protrudes to the central through hole 54a is provided. The first base portion 53 is engaged with the holding portion 54b via an O-ring 65 made of fluororesin.

  The piezoelectric element 55 is a ring-type stacked piezoelectric element in which thin film piezoelectric elements having an outer diameter of 22 mm and an inner diameter of 16 mm and electrodes are alternately stacked up to a thickness of 4 mm.

  The piezoelectric element 55 has one surface 55a disposed around the first base portion 53, and is a ring type having an outer diameter of 60 mm, an inner diameter of 15 mm, and a thickness of 4 mm. One surface has a diameter of 30 mm and a depth of 3.5 mm. Using the stainless steel piezoelectric element fixing member 59 provided with the groove 59a, the other surface 55b of the piezoelectric element 55 is brought into contact with the groove portion 59a, and the second base portion 54 is surrounded by the periphery 4 of the piezoelectric element fixing member 59. The location is fixed with screws 60.

  At this time, a gap of 0.5 mm is formed between the second base portion 54 and the piezoelectric element fixing member 59, so that the first base portion 53 is preloaded on the piezoelectric element 55 by screwing. It is fixed in a state where pressure is applied.

  Further, the O-ring 65 between the first base portion 53 and the second base portion 54 is also crushed by the preload via the piezoelectric element 55, and the space between the two is sealed by the O-ring 65.

  Further, on the ring-shaped third base 57 having an outer diameter of 60 mm, an inner diameter of 30 mm, and a thickness of 3 mm, a periphery of a Teflon (registered trademark) membrane film 56 for creating a sealed space is placed, An O-ring 62 is placed on the top and sandwiched between the second base portion 54 and the third base portion 57 and fixed with screws to seal the gap.

  An inner sample holder 58 is provided near the center of the membrane film 56, the membrane film 56 is sandwiched between the inner sample holder 58 and the sample holder 3 at the tip of the third fine movement mechanism, and the inner sample stage 58 operates in accordance with the operation 2 of the third fine movement mechanism. To do.

  In addition, since the membrane film 56 is soft, the movement of the triaxial fine movement mechanism 2 is not hindered.

  And the cantilever holder 50 is fixed by fixing the 3rd base part 57 to the housing | casing part 4 of a scanning probe microscope.

  By configuring the sealed cantilever holder 50 in this way, a sealed space can be secured in the region 51 surrounded by the first base portion 53, the second base portion 54, and the membrane film 56, and the sealed space The cantilever 5 and the sample 21 are arranged in 51.

  When a solution or gas is injected into the sealed space 51, the solution or gas is injected from an injection port 63 provided on the front surface of the cantilever holder 50 by a pump or a syringe.

  Further, a discharge port 64 is also provided on the front surface of the cantilever holder 50, so that it is possible to circulate in addition to exhaust of solution and gas. When the sealing state is set, the inlet 63 and the outlet 64 are sealed.

  Using the sealed cantilever holder 50 configured as described above, the electrode of the laminated piezoelectric element 55 is connected to a driving power source (not shown), and an AC voltage is applied from the driving power source to thereby form the first base portion. 53 is vibrated, and the cantilever 5 is vibrated through the cantilever holding portion 52.

  Using the scanning probe microscope configured as described above, the distance between the probe 5a and the sample 21 is set so that the attenuation of the amplitude is constant while the cantilever 5 is vibrated in the vicinity of the resonance frequency. Feedback control and raster scanning of the probe 5a and the sample 21 by the horizontal fine movement mechanism 5b can measure the shape of the sample 21 in the solution and mapping images of various physical properties. It is also possible to measure physical properties for each specific point.

  In the present embodiment, the piezoelectric element 55 for exciting the cantilever is arranged on the back surface 53b with respect to the surface 53a to which the cantilever holding portion 52 of the first base portion 53 is fixed. Can be placed outside the space, can prevent adhesion of piezoelectric elements, peeling and swelling of molding agents, corrosion of electrodes and leakage of current, etc., not only pure water, but also organic solvents and corrosive gases, Scanning probe microscope measurements can be performed under various environments such as nitrogen atmosphere.

  In particular, in the present invention, since the preload is applied to the multilayer piezoelectric element 55 and the first base portion 53 is applied with pressure, the multilayer piezoelectric element 55 is fixed to the first base portion 53 without preloading. Compared to the case where the element is fixed, the cantilever 5 can be vibrated efficiently via the first base portion 53, and the measurement accuracy is improved.

<Fifth Embodiment>
FIG. 9 is a schematic view showing the overall configuration of a scanning probe microscope according to the fifth embodiment of the present invention, and FIG. 10 is a plan view of a cantilever holder used in FIG.

  In the present embodiment, since the configuration is the same as that of the second embodiment described with reference to FIGS. 3 and 4 except for the ring-shaped elastic body 70, the same members are denoted by the same reference numerals and detailed description thereof is omitted. To do.

  Since the first base portion 14 is made of glass, if stress concentration occurs when preload is applied, the glass is likely to break. In particular, when the piezoelectric element is vibrated in a state where stress is applied, cracks are more likely to occur. In particular, there is a high possibility that the glass will break if it matches the resonance frequency of the first base portion.

  As in the second and fifth embodiments, one surface 31a of the ring-type piezoelectric element 31 is attached to the first base portion 14 at the edge near the fixed end of the disc-shaped first base portion 14. Is fixed to the first base portion 14 by the piezoelectric element fixing member 32 from the opposite surface 31b side, so that the preload is uniformly applied and the stress concentration is suppressed, so that the glass is not easily broken. Become.

  In the fifth embodiment, an elastic body having a thickness of 0.5 mm between the one surface 31b of the piezoelectric element 31 and the piezoelectric element fixing member 32 is sandwiched between the ring-type piezoelectric element and the piezoelectric element. A preload is applied by the fixing member 32. With this configuration, the preload is applied more uniformly, and it is difficult for the glass to break. In addition, the amplitude of the cantilever per unit voltage applied to the piezoelectric element 31 is improved, and the vibration transmission characteristics are also improved.

  Such an elastic body may be inserted between the other surface 31 a of the piezoelectric element 31 and the first base portion 14. Moreover, you may put in the both sides of the piezoelectric element 31. FIG. As a material of the elastic body, any material can be used as long as an elastic effect such as silicone rubber is obtained in addition to a Teflon (registered trademark) sheet.

<Sixth Embodiment>
FIG. 11 is a schematic view of a scanning probe microscope and a sealed cantilever holder used for electrochemical measurement according to a sixth embodiment of the present invention. 12 is a plan view of a sealed cantilever holder used in the scanning probe microscope of FIG.

  Since most of the configuration of the present embodiment is substantially the same as the sealed cantilever holder of the fourth embodiment shown in FIGS. 7 and 8, the same members are denoted by the same reference numerals and detailed description thereof is omitted. To do.

  In the present embodiment, a ring-type single plate piezoelectric element 81 is used, one surface 81a is disposed in contact with the edge of the first base portion 53, and the piezoelectric element fixing member is disposed from the opposite surface 81b side. 59 is fixed to the first base portion 53 via a ring-type elastic body 82 made of a Teflon (registered trademark) sheet, so that the preload is uniformly applied and stress concentration does not occur. It is difficult to crack.

  In the present embodiment, the electrodes forming the counter electrode and the reference electrode are inserted into the sealed space 51 from the side surface of the second base portion 54 of the sealed cantilever holder 80. The counter electrode 83 is composed of a platinum wire having an outer diameter of 1 mm, and is bent so as to form a semicircular arc electrode around the inside 51 of the sealed space immersed in the solution. The reference electrode 84 is made of a silver wire having an outer diameter of 1 mm, and is disposed by being bent around the periphery of the sealed space 51, except for the tip on the sealed space 51 side and the end on the atmosphere side. Insulation treatment is applied. A seal is applied to the introduction port from the second base portion 54 of each electrode.

  Further, contact pins 85 and 86 are arranged on the back side of the sample 91 or the back surface of the cantilever 92 so that the sample 91 or the cantilever 92 acts as a working electrode, and is electrically connected to the outside of the sealed space 51. The periphery of the contact pins 85 and 86 is sealed with O-rings 87 and 88.

  When using the sample 91 as a working electrode, an electrode is provided at a position where the sample is not in contact with the liquid on the back surface of the sample, and electrical contact between the electrode and the sample surface is ensured and contacted with this electrode. The pin 85 is brought into contact.

  When the cantilever 92 is used as a working electrode, the cantilever 92 is coated with gold, platinum, or the like, and a portion other than the tip is coated with an insulating film. Further, a part of the cantilever that is not coated with an insulator is provided, and is brought into contact with a contact pin 86 provided on the cantilever holder so as not to contact the solution.

  The first base portion 53 is made of quartz glass, the second base portion 54 and the sample holder 89 are made of PEEK material, the leaf spring 90 is made of Teflon (registered trademark), and the membrane film 56 is made of Teflon (registered trademark) film. There is no metal material other than each electrode that affects electrochemical measurements.

  Electrochemical measurement can be performed by connecting these counter electrode, reference electrode, and working electrode to a potentiostat provided outside. Either the sample 91 or the cantilever 92 is set as a working electrode in accordance with the purpose of measurement. It is also possible to connect both the cantilever 92 and the sample 91 to the bipotentiostat using the working electrode.

  In addition, the counter electrode and the reference electrode connect the tip on the atmosphere side to a potentiostat. The working electrode is connected to a potentiostat through a wiring material connected to the contact pin.

  If a piezoelectric element is placed in a solution when performing electrochemical measurement, the current applied to the piezoelectric element may leak and accurate electrochemical measurement may not be performed. In addition, the electrodes of the piezoelectric element may cause an electrochemical reaction. However, by arranging the piezoelectric element outside the sealed space in this way, accurate electrochemical is possible.

  Note that the material, shape, arrangement, and the like of each electrode are not limited to the present embodiment, and an arbitrary form is applied according to the measurement purpose. Further, an open type holder can be used in addition to the sealed type holder.

  Although the cantilever holder for a scanning probe microscope of the present invention has been described above, the present invention is not limited to the above invention and can be used in various forms.

    For example, an optical lever type displacement detection mechanism is used as the displacement detection mechanism, but a self-detection type cantilever that detects a displacement by changing a resistance value due to bending deformation by providing a resistor on the cantilever can also be used.

  In the case where an optical lever is not used, such as a self-detecting lever, or when observation with a microscope is not required, the cantilever holding portion and the first base portion may be made of a material that does not transmit light.

  Further, the cantilever holding portion and the first base portion may be configured as separate bodies or may be configured as an integral unit. Further, each component may be divided into a plurality of parts. Further, the cantilever holding portion may also serve as the first base portion.

  When light is transmitted through the first base part and the cantilever holding part, the whole may be made of a transmissive material, or a part thereof may be made of a transmissive material.

  In this embodiment, the sample side is driven by the triaxial fine movement mechanism. However, a triaxial fine movement mechanism may be provided on the cantilever side, and the horizontal fine movement mechanism and the vertical fine movement mechanism are arranged on the sample side and the cantilever side. It may be divided and arranged.

  In addition, the shape and material of the members constituting the cantilever holder, the shape of the piezoelectric element, the preloading means, the material and shape of the block at the end of the piezo, the sealing means, the cantilever fixing means, the shape and material of the cantilever, etc., any structure or method Can be used.

  The piezoelectric element is preferably a laminated piezoelectric element having a large displacement per unit applied voltage in terms of excitation efficiency, but a single plate type can also be used.

  Furthermore, the cantilever holding part side may be disposed in a vacuum, and the piezoelectric element side may be disposed in an atmospheric environment. In this case, generation of gas from the piezoelectric element or the adhesive can be prevented.

  Further, the cantilever holding part side may be disposed in a high humidity environment, and the piezoelectric element side may be disposed in an atmospheric environment. In this case, it is possible to prevent migration and corrosion of the electrodes due to humidity.

  Furthermore, the present invention can also be applied to a cantilever holder for a scanning probe microscope that performs measurement while heating the cantilever holding part or the sample holder. In this case, since the piezoelectric element can be moved away from the vicinity of the high temperature member, the poling of the piezoelectric element is prevented from being broken by heat.

  Further, the present invention can also be applied to a cantilever holder for a scanning probe microscope that performs measurement while cooling the cantilever holding part or the sample holder. In this case, since the piezoelectric element can be moved away from the vicinity of the cooling member, the phenomenon that the amplitude of the piezoelectric element is reduced by cooling and the excitation efficiency is deteriorated can be prevented.

  In the case of performing these heating or cooling, the effect is further improved by interposing a heat insulating member between the piezoelectric element and the first base portion or the cantilever holding portion.

  Furthermore, in order to reduce vibration noise, a damping material may be used for a leaf spring or a block for fixing the piezoelectric element, or the piezoelectric element may be fixed with the damping material interposed.

  In addition, the cantilever was vibrated near the primary resonance frequency and the distance was controlled by the amplitude attenuation. However, the cantilever is not limited to excitation at the primary resonance frequency or detection of the amplitude attenuation, but at any frequency. All the measurement means of a scanning probe microscope that performs measurement while exciting a cantilever with a piezo, such as a method of performing distance control by detecting phase change or frequency change, are applicable.

DESCRIPTION OF SYMBOLS 1, 35, 45, 66 Scanning probe microscope 2 3 axis | shaft fine movement mechanism 2a Horizontal direction fine movement mechanism 2b Vertical direction fine movement mechanism 3 Sample stage 4 Unit housing part 5 Cantilever 5a Probe 5b Cantilever base end part 6 Displacement detection mechanism 7, 30, 40 Cantilever holder 8 Displacement detection mechanism housing 9 Semiconductor laser 10 Beam splitter 11 Total reflection mirror 12 Four-divided photodetector 13, 52 Cantilever holding portion 14, 53 First base portion 15, 54 Second base portion 16, 31 , 55 Piezoelectric element 17 Plate spring 18 Plate spring 19, 33, 44, 60 Screw 20 Petri dish 21 Sample 22 Solution 23 Laser light 24 Optical microscope 32, 59 Piezoelectric element fixing member 34, 61 Gap 41 Claw 42 Silicone rubber 43 Block 50 Sealing Type cantilever holder DESCRIPTION OF SYMBOLS 1 Sealing space 56 Membrane film 57 3rd base part 58 Inner sample holder part 62, 65 O-ring 63 Inlet 64 Outlet 70 Elastic body 80 Sealing type cantilever holder 81 Piezoelectric element 82 Elastic body 83 Counter electrode 84 Reference electrode 85, 86 Contact pins 87, 88 O-ring 89 Inner sample holder 90 Plate spring 91 Sample 92 Cantilever 104 Piezoelectric element 105 Cantilever fixing part 106 Cantilever 106a Probe 108 Displacement detection mechanism 113 Semiconductor laser 114 Beam splitter 115 Mirror 116 Quadrant photodetector 118 Triaxial Fine movement mechanism 134 Glass base block 137 Sample 136 Petri dish 215 Glass holder 210 Cantilever 215 Holder 217 Piezoelectric element

Claims (13)

A cantilever holding portion capable of holding one end of the cantilever,
A first base portion to which an end opposite to the side holding the cantilever holding portion of the cantilever holding portion is fixed;
A second base having a through hole that can pass through the cantilever holding portion and a holding portion that holds the first base portion by hooking at least a part of the outer peripheral portion of the first base portion. And
A piezoelectric element placed on the side opposite to the fixed side of the cantilever holding part of the first base part ;
A piezoelectric element fixing member that tightly fixes the piezoelectric element to the first base portion by applying a preload to the piezoelectric element in a contact surface direction with the first base portion;
Cantilever holder for scanning probe microscope equipped with.   The cantilever holder for a scanning probe microscope according to claim 1, wherein the piezoelectric element is fixed by bringing one surface of the piezoelectric element into contact with an edge of the first base portion and applying a preload from the opposite surface.   The cantilever holder for a scanning probe microscope according to claim 2, wherein the piezoelectric element has a ring shape. The scanning probe microscope according to any one of claims 1 to 3, wherein a preload is applied to at least one surface of the piezoelectric element in contact with or opposite to the first base portion via an elastic body. Cantilever holder. A cantilever holding portion configured to hold one end of the cantilever,
A first base portion to which an end opposite to the side holding the cantilever holding portion of the cantilever holding portion is fixed;
A second base having a through hole that can pass through the cantilever holding portion and a holding portion that holds the first base portion by hooking at least a part of the outer peripheral portion of the first base portion. And
A piezoelectric element placed on the side opposite to the fixed side of the cantilever holding part of the first base part ;
The piezoelectric element is fixed to an end portion opposite to the one end portion mounted on the first base portion, and has a mass heavier than a total mass of the mass of the first base portion and the mass of the cantilever holding portion. Members ,
Cantilever holder for scanning probe microscope equipped with. Scanning probe cantilever holder for microscope according to any one of claims 1 to 5, wherein the piezoelectric element is a laminated piezoelectric element. Scanning probe cantilever holder for microscope according to any one of claims 1 to 5, wherein the piezoelectric element is a piezoelectric element plate.   The cantilever holder for a scanning probe microscope according to any one of claims 1 to 7, wherein the first base portion is made of a material that can transmit light having a wavelength in an arbitrary range of 200 nm to 2500 nm.   The cantilever holder for a scanning probe microscope according to any one of claims 1 to 8, wherein the cantilever holding portion held by the cantilever holding portion is soaked in a solution. The scanning probe microscope according to claim 9, wherein the cantilever holding part side and the piezoelectric element side are blocked by the first base part, and the cantilever holding part side is arranged in an environment different from the atmosphere. Cantilever holder. The scanning probe according to claim 10 , wherein two electrodes functioning as a counter electrode and a reference electrode are disposed in a space immersed in the solution, and further an electrode that functions as at least one of a sample or a cantilever as a working electrode is provided. Cantilever holder for microscope.   The scanning probe microscope according to any one of claims 1 to 11, which is used for a scanning probe microscope provided with a function of heating or cooling a sample holder on which a sample arranged on the cantilever holding part or the opposite side of the cantilever is placed. Cantilever holder for scanning probe microscope.   A scanning probe microscope comprising the cantilever holder for a scanning probe microscope according to claim 1.

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