Scanning probe microscope with electrochemical cell

FIELD: scanning probe microscopy.

SUBSTANCE: scanning probe microscope has sample holder, first platform, onto which case is mounted, and piezoscanner. Elastic membrane is placed between case and piezoscanner. There is unit for preliminary bringing sample and probe together, as well as housing and probe fixer. The second platform is introduced into the scanner, onto which unit for preliminary bringing sample and probe together. Base and sample holder is put together with cup by means of first hole and the second hole. Second hole is connected with inert gas source. Cup is made of chemically-proof material. Case is made to be air-proof. Locker of the probe is fastened to piezoscanner. Housing is mounted onto cup for interaction with airtight case. Aerostatic plain bearing is formed between housing and airtight case. Sample holder, cup, housing, airtight case, elastic membrane and probe locker form all together closed cavity of electrochemical cell.

EFFECT: simplified exploitation; widened operational abilities.

11 cl, 7 dwg

 

The invention relates to nanotechnology, and more specifically to devices, providing the analysis and modification of the sample surface in a liquid medium using methods of scanning probe microscopy.

Known scanning probe microscope (SPM) with an electrochemical cell containing a mechanical unit with the systems approach of the probe with the sample and the scanning control unit, as well as piezoscanner with the probe placed in the electrochemical cell [1].

The disadvantage of this device is to supply all functional elements from the open part of the electrochemical cell, which complicates its sealing and reduces reliability.

Also known scanning probe microscope with a liquid cell containing the platform with piezoscanner with a sample holder, the optical block tracking cantilever seal installed between the platform and the sample holder, the optical block tracking cantilever comprising a laser and a photodetector systems alignment shifts, optically coupled with the cantilever mounted so that one of the optical axes in the system of laser-cantilever-sensor perpendicular to the sample plane, as well as block pre-convergence of sample and cantilever mounted on the optical block [2].

First the second disadvantage associated with the use of elastic rings, installed between the platform and the sample holder, which hampers their mutual movement, and therefore, the study areas sample order 1×1 mm, and the receiving frame scan about 50×50 μm of this surface without deteriorating the resolution.

The second drawback is associated with a closed configuration of the device, which complicates the process of replacing the cantilever.

Also known scanning probe microscope with a liquid cell containing the platform on which you installed the enclosure, as well as pre-convergence of the sample with the probe, which enshrines piezoscanner with a sample holder, while between the housing and the sample holder is placed an elastic membrane, and the housing has a cover with holes for supplying and discharging the reagents, containing the holder of the probe [3].

The specified device is selected as a prototype of the proposed solution.

The first disadvantage of this device is difficult surgical access to the interior of the cell, which complicates the operation of the device.

The second drawback associated with inadequate treatment of the cells that will lead to the need for additional cleaning.

The third disadvantage associated with the use of an elastic membrane, as in the preliminary convergence, and when scanning that pre is jawset it increased requirements and complicates the process of convergence of the probe with the sample.

The fourth disadvantage is connected with the placement of the sample holder inside the electrochemical cell, which complicates the process of electrochemical studies, and also complicates the overall operation of the device.

All these disadvantages to some extent limit the functionality of the device.

The technical result of the invention is to simplify operation of the device and extend its functionality.

This technical result is achieved by the scanning probe microscope with an electrochemical cell containing the sample holder, the first platform on which is mounted a housing, as well as piezoscanner, while between the housing and piezoscanner posted elastic membrane, the pre-convergence of the sample with the probe housing, and the latch probe entered the second platform, which is equipped with the pre-convergence of the sample with the probe, and the base with a sample holder, paired with a Cup with the first hole, perpendicular to the plane of the coupling base, and a second hole connected to the first end with a source of inert gas, this Cup is made of chemically resistant material, the housing is airtight, the latch probe attached to piezoscanner, while the casing is mounted on the Cup with the possibility of the EOI is to interact with a sealed enclosure, education between the casing and a sealed enclosure aerostatic bearing and moving them relative to each other, while the sample holder, Cup, cover, sealed enclosure, the elastic membrane and the release of the probe form a closed cavity electrochemical cell, which includes the second end of the second hole.

There are ways in which the casing is made in the form of bellows or of optically transparent material.

Possible ways in which the sample holder of an arbitrary shape made in the form of plates with capture, covered with a chemically resistant material and secured between the base and the housing, the cylindrical sample holder is made in the form of a sleeve, made of chemically resistant material and secured between the base and the housing, and where the sample holder of the spherical shape using a tapered groove in the base.

There is also an option, in which the Cup is made of Teflon and is provided with a third hole, the first end connected to a source of electrolyte, and the second opening in a closed cavity.

It is possible that between the sample spherical shape and Cup set PTFE ring, mate Cup with base made using screws with elastic elements, the plant and between them and the base, and implemented installation between the Cup and the base of the elastic damper.

Figure 1 shows a scanning probe microscope with an electrochemical cell.

Figure 2 shows an embodiment of a shroud.

Figure 3, 4, 5 shows embodiments of the sample holder.

Figure 6 shows a variant of the fastening of the Cup.

Figure 7 presents accommodation elastic damper.

Scanning probe microscope (SPM) with electrochemical cell contains the first platform 1 (Fig 1), which includes a sealed housing 2, as well as piezoscanner 3 latch 4 probe 5. It should be noted that the probe 5 is fixed in the hole of the retainer 4 by frictional forces. It is also possible to do this using spring contacts inside the holes 4 and ensures the fixation of the probe 5 (not shown). However, the hermetic housing 2 and the retainer 4 probe 5 attached elastic membrane 6. The first platform 1 by means of three racks 7 are installed on the second platform 8, which is equipped with a device 9 for the rapprochement of sample 10 with probe 5. The sample 10 is fixed to the holder 11 disposed between the base 12 and the Cup 13 with an opening 14 made of chemically resistant material, which is most often used Teflon. It should be noted that it is possible the stop sample 10 directly on the base 12. The base 12 is usually made of metal and mounted on the device 9. Cup 13 includes an auxiliary electrode 15 and the reference electrode 16. It also made the second hole 17 which is connected to a source of inert gas 18, for example argon. On the Cup 13 has a casing 19, made for example of optically transparent material with the possibility of interaction through, for example, fluoroplastic sleeve 20 with a sealed enclosure 2. In between, the formation of aerostatic bearings. There is also the option of the Cup with the third hole 21 that is connected to a source of electrolyte 22.

In the proposed design of the holder 11 with the sample 10, the Cup 13, the casing 19, the hermetic housing 2, the elastic membrane 6 and the latch 4 form a closed cavity electrochemical cell.

Figure 1 SPM conventionally depicted, it is understood that the platform 1 includes a preamplifier and a control unit SPM. In detail these elements, see [4, 5].

In addition, the electrodes 15 and 16, the probe 5 and the sample 10 can be included in the circuit bipotentiality (not shown). Cm. in detail in [4].

There is an option in which the cover 19 is made in the form of bellows 23 (2), made, for example, PTFE.

You can run the sample holder 24 (Fig 3) in the form of a plate 25 with the capture of 26, representing the Wallpaper, for example, junction, covered with a chemically resistant material 27 (polyethylene, Teflon). In this case, the sample 24 can be of arbitrary shape.

You can also run a cylindrical sample holder 28 (figure 4) in the form of a sleeve 29, made of chemically resistant material, such as Teflon.

In the case of use as a sample spherical drops 30 (figure 5) with cut uppers 31, as its holder using a cone-shaped recess 32, is made in the base 33. However, you can use the Teflon ring 34 mounted between the Cup 35 and a drop of 30. Cup 35 in this case, you may have a different size bores, different from previous choices, determined by the size of the sample 30, and a somewhat modified form associated with the installation ring 34.

It should be noted that the installation of the cups 13 (6) in the case of any holder 36 (shown conventionally) is possible with the use of screws 37 and the elastic elements 38.

In all these cases, it is also possible to install elastic damper 39 (7) between the Cup 13 and the base 12, for example in the groove 40.

The device operates as follows.

Fix the sample 10 on the holder 11 by means of glue, seal, spring pads, not extending beyond the study sample surface (not shown), etc. Set forth RATEL 11 with the sample 10 on the base 12 and fix them to the base 12 by clamping the inner surface of the Cup 13 to the working surface of the sample 10, providing a tight connection at the expense of the yield of PTFE. The Cup 13 is fixed on the base 12 with screws, springs, etc. Set the probe 5 in the latch 4, if necessary, using the principle of forced bending [6]. After that, possible trial supply of the probe 5 to the sample 10, as described, for example, in [4, 5]. Next comes the removal of the probe 5 from the surface of the sample 10 and the filling of the electrolyte through the hole 21. It should be noted that quite often use the Gulf of electrolyte into the Cup 13, using, for example, microcapillary (not shown). At the time of installation of the sample 10, the first platform 1 SPM can be removed from the second platform 8 or casing 19 is elevated above the Cup 13.

After pouring the electrolyte include feeding an inert gas through the second hole 17, ensuring cleanliness in the electrochemical cell and carry out the supply of the probe 5 to the sample 10 using aerostatic bearing arising between the PTFE sleeve 20 and the hermetic housing 2 as a result of release of inert gas from the electrochemical cell. After that make electrochemical research sample, or other technological operations with them. See details in [4, 7].

Preparation of surfaces probes, samples, electrolytes and electrochemical cells described in [4].

In the case of manufacturing the casing 19 optical p is acronym possible observation of the process zone is selected, measurement, process supply, electrolyte level, etc.

When used as a casing 19 of the bellows 23 (2) simplifies the process of gross advances in the plane of the sample 10. The specifics of working with holder, made in the form of a plate 25 (figure 3), consists in the application of chemically resistant material (PTFE, polyethylene) on the elements in contact with the electrolyte.

When working with holder, made in the form of a sleeve 29 (4), must be sealed therein a cylindrical sample 28 by, for example, it is snug. In addition, you must create the electrical contact of the sample 28 with the base 12, which is provided, for example, due to the preliminary projection of the sample 28 of the sleeve hole 29. Figure 4 the clearance between the sleeve 29 and the base 12 are not shown, since in practice the deformation of PTFE after several installations of the sleeve 29 and he disappears on the periphery, but may remain in the center of the sleeve 29. In some cases, to reduce the likelihood of extrusion of the sample 28 of the sleeve 29 may be used thickening of the sample 28 from the base 12 (not shown).

The honors option is shown in figure 3, lies in the fact that it is reduced in comparison with the previous variant, the contact area of the Cup 35 with cut top 31 of the sample 30. In this case, it is possible to use shift the PTFE ring 34. Otherwise, due to the high residual deformation of the Teflon Cup 13 may be quickly damaged. Replacement rings 34 typically occurs through 4-7 terminals of the sample 30. It should be noted that the Teflon ring 34 can also be used in all previous versions.

When installed elastic damper 39 (7) in the groove 40 appears mediated interaction between the Cup 13 and the base 12. In this case, the elastic damper 39 performs the role of an additional sealer, and more evenly distributes the effort on the part screws onto the Cup 13.

The introduction of the second platform, which is equipped with the pre-convergence of the sample with the probe, and the base, paired with a Cup of ease-of-use device, as it is possible to manipulate the electrochemical cell in an open state.

Execution of the first hole in the Cup and pair it with the base allows you to use the Cup as a sample holder, which also simplifies operation and improves the quality of electrochemical research.

Make a second hole in the Cup connected to the first end with a source of inert gas, and a second end extending in a closed cavity, increases the purity of the inside of the electrochemical cell, simplifies cleaning and increases dostoverno the ü results.

Perform body tight and fastening it elastic membrane prevents the penetration of active ingredients of the electrolyte on the structural elements of the SPM.

Placing a flexible membrane sealed between the housing and the clamp probe with placement of the device prior convergence on the second platform reduces in comparison with the prototype of the mechanical effects on the elastic membrane. This is due to the fact that the movement of piezoscanner is hundreds of microns (proposed option), and moving the pre-convergence of the sample with the probe can reach 10 mm (prototype). As a result of this expanded choice of materials elastic membrane and simplifies the operation of the device.

Placing the cover on the Cup with the opportunity to interact with a sealed enclosure, the education between the casing and a sealed enclosure aerostatic bearing and moving them relative to each other increases the range of movement of the sample relative to the probe without depressurization of the electrochemical cell, which also simplifies the operation of the device.

The simplification of the operation of the SPM with the electrochemical cell, noted in the previous paragraphs leads to the expansion of the functionality of the device. For example, simplification of cleaning in the greater the degree allows the use of different electrolytes.

Increase range of movement of the sample relative to the probe also extends the functionality of the device through the use of samples of different thickness.

In addition, uniform exit of the inert gas on the periphery of the casing leads to a more uniform and orderly movement of inert gas inside the electrochemical cell, which increases the resolution of the device due to reduce the effect of inert gas on the probe.

Use as a casing of the bellows increases the reliability of the preliminary convergence of the sample with a probe that extends the functionality of the device.

The execution of the sample holder in the form of a plate with capture, in the form of a sleeve, and the use in the form of sample holder conical recesses in the base extends the functionality of the device.

Supply Cup third hole connected to a source of electrolyte, allows depressurization to add or delete an electrolyte that facilitates the operation of the device.

Making a Cup of PTFE increases the degree of sealing an electrochemical cell.

Use Teflon ring mounted between the Cup and the sample spherical shape, increases the degree of sealing an electrochemical cell.

Use screws with elastic elements with a gap from the deformation the purpose of the Teflon Cup increases the life of the Cup.

Installation of the elastic damper between the Cup and the base increases the degree of sealing an electrochemical cell.

Literature

1. Patent EP 0318289, 1988.

2. U.S. patent 34489, 1993.

3. Patent RU No. 2210818, 2003.

4. Scanning tunneling and atomic force microscopy in electrochemistry surface. Aigaiou, Uspekhi khimii 64 (8), 1995, s-833.

5. Probe microscopy for biology and medicine. Vasyukov and other Sensory systems, so 12, No. 1, 1998, s-121.

6. A positive decision on the application No. 2001129350.

7. Aigaiou. The nature of active centers, kinematics and mechanism of the initial stages of electrocrystallization copper. Abstract, M., 2002, 48 S.

1. Scanning probe microscope with an electrochemical cell containing the sample holder, the first platform on which you are building, as well as piezoscanner, while between the housing and piezoscanner posted elastic membrane, the pre-convergence of the sample with the probe housing, and the latch probe, characterized in that it introduced a second platform on which it is installed prior convergence of the sample with the probe, and the base with a sample holder, paired with a Cup with the first hole, perpendicular to the plane of base pairing with a Cup, and with a second hole connected to the first end with a source of inert gas that is ri this Cup is made of chemically resistant material, the case is airtight, the latch probe attached to piezoscanner, while the casing is mounted on the Cup with the opportunity to interact with a sealed enclosure, with the possibility of education between the casing and a sealed enclosure aerostatic bearing and moving them relative to each other, while the sample holder, Cup, cover, sealed enclosure, the elastic membrane and the release of the probe form a closed cavity electrochemical cell, which includes the second end of the second hole.

2. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the casing is made in the form of bellows.

3. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the casing is made of optically transparent material.

4. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the sample holder of an arbitrary shape made in the form of plates with capture, covered with a chemically resistant material, secured between the base and the housing.

5. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the cylindrical sample holder is made in the form of a sleeve, made of chemically resistant material and secured between the base and the housing.

6. Scanning unduly microscope with an electrochemical cell according to claim 1, characterized in that as the sample holder of the spherical shape using a tapered groove in the base.

7. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the Cup is provided with a third hole, the first end connected to a source of electrolyte, and the second opening in a closed cavity electrochemical cell.

8. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that the Cup is made of Teflon.

9. Scanning probe microscope with an electrochemical cell according to claims 1, 6 and 8, characterized in that between the sample spherical shape and Cup set PTFE ring.

10. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that for coupling the Cup with the base using screws with elastic elements placed between them and the base.

11. Scanning probe microscope with an electrochemical cell according to claim 1, characterized in that between the Cup and the base has an elastic damper.



 

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