Method for Producing a Probe Suitable for Scanning Probe Microscopy
20200278379 ยท 2020-09-03
Inventors
Cpc classification
C23C16/30
CHEMISTRY; METALLURGY
C23C16/045
CHEMISTRY; METALLURGY
C23C16/0272
CHEMISTRY; METALLURGY
C23C16/278
CHEMISTRY; METALLURGY
G01Q60/02
PHYSICS
International classification
Abstract
Example embodiments relate to methods for producing a probe suitable for scanning probe microscopy. One embodiment includes a method for producing a probe tip suitable for scanning probe microscopy. The method includes producing a probe tip body that includes at least an outer layer of a probe material. The method also includes, during the production of the probe tip body or after the production, forming a mask layer on the outer layer of probe material. Further, the method includes subjecting the probe tip body to a plasma etch procedure. The mask layer acts as an etch mask for the plasma etch procedure. The plasma etch procedure and the etch mask are configured to produce one or more tip portions formed of the probe material. The one or more tip portions are smaller and more pointed than the probe tip body prior to the plasma etch procedure.
Claims
1. A method for producing a probe tip suitable for scanning probe microscopy (SPM), comprising: producing a probe tip body comprising at least an outer layer of a probe material; during the production of the probe tip body or after the production, forming a mask layer on the outer layer of probe material; and subjecting the probe tip body to a plasma etch procedure, wherein the mask layer acts as an etch mask for the plasma etch procedure, wherein the plasma etch procedure and the etch mask are configured to produce one or more tip portions formed of the probe material, and wherein the one or more tip portions are smaller and more pointed than the probe tip body prior to the plasma etch procedure.
2. The method according to claim 1, wherein the mask layer comprises a layer of irregular thickness formed prior to the plasma etch procedure, and wherein the layer of irregular thickness acts as the etch mask for the plasma etch procedure.
3. The method according to claim 2, wherein the layer of irregular thickness comprises compounds formed spontaneously on a surface of the probe tip body after the production of the probe tip body and prior to the plasma etch procedure.
4. The method according to claim 2, wherein the layer of irregular thickness comprises particles deposited deliberately on the probe tip body after the production of the probe tip body and prior to the plasma etch procedure.
5. The method according to claim 2, wherein the probe tip body is produced by producing a mold in a substrate and by depositing the probe material in the mold, wherein seed particles are deposited in the mold prior to depositing the probe material therein, and wherein the layer of irregular thickness comprises the seed particles.
6. The method according to claim 5, wherein the layer of irregular thickness further comprises compounds formed spontaneously on a surface of the mold.
7. The method according to claim 2, wherein the plasma etch procedure comprises: a first etch process performed during a first etch time and configured to produce craters in the layer of irregular thickness; and a second etch process performed during a second etch time that is longer than the first etch time and configured to produce the one or more tip portions.
8. The method according to claim 1, wherein the probe tip body is attached to a cantilever, wherein particles of the cantilever are sputtered during the plasma etch procedure and deposited onto the probe tip body, and wherein the sputtered particles of the cantilever contribute to the formation of the mask layer during a remainder of the plasma etch procedure.
9. The method according to claim 1, wherein at an end of the plasma etch procedure, the one or more tip portions are distributed across a totality of the probe tip body.
10. The method according to claim 1, wherein the probe tip body is pyramid-shaped, and wherein, at an end of the plasma etch procedure, the one or more tip portions are present on an apex area of the probe tip body and no tip portions are present on side planes of the probe tip body because: a higher concentration of masking particles is deposited on the apex area than on the side planes during the plasma etch procedure; or the probe tip body comprises a core and, on the core, a layer of the probe material, wherein a thickness of the layer of the probe material is higher on the apex area than on the side planes such that, at the end of the plasma etch procedure, the probe material is removed from the side planes.
11. The method according to claim 1, wherein the probe material is diamond.
12. The method according to claim 1, further comprising the following steps performed after the plasma etch procedure: depositing a capping layer on the one or more tip portions, thereby covering the one or more tip portions entirely; and subjecting the one or more tip portions to an additional plasma etch process configured to remove the capping layer from a tip area of the one or more tip portions, while substantially maintaining the capping layer around a lateral surface of the one or more tip portions, wherein the tip area includes apexes of the one or more tip portions.
13. A probe tip suitable for scanning probe microscopy (SPM), comprising a probe tip body comprising at least an outer layer of a probe material, wherein a plurality of tip portions formed of the probe material are distributed across a totality of the probe tip body, and wherein the tip portions are smaller and more pointed than the probe tip body.
14. The probe tip according to claim 13, wherein the tip portions comprise a capping layer on their outer surface except on a tip area of the tip portions, and wherein the tip area comprises an apex of the tip portions.
15. A probe comprising: a cantilever; a holder to which the cantilever is attached; and a probe tip attached to a distal end of the cantilever, wherein the probe tip is suitable for scanning probe microscopy (SPM) and comprises a probe tip body comprising at least an outer layer of a probe material, wherein a plurality of tip portions formed of the probe material are distributed across a totality of the probe tip body, and wherein the tip portions are smaller and more pointed than the probe tip body.
16. The probe according to claim 15, wherein the tip portions comprise a capping layer on their outer surface except on a tip area of the tip portions, and wherein the tip area comprises an apex of the tip portions.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
[0050] Example methods are described in detail for the case of a diamond probe tip produced by a molding technique. The method is however applicable to tips formed of other materials and produced by other techniques.
[0051] According to this particular embodiment, at least a portion of these particles are non-doped diamond particles. The density of the particles when deposited in the mold may be in accordance with existing methods, for example between 1E10/cm.sup.2 and 5E10/cm.sup.2. The density may however be controlled within a larger range of 1E9/cm.sup.2 and 1E11/cm.sup.2 by adjusting the seeding dispersion chemistry, the particle and substrate potential and the seeding time. The applied density may enable the growth of a closed (i.e. fully coalesced) diamond layer in the mold. According to an embodiment, the particles consist of a mixture of non-doped diamond particles and doped diamond particles, deposited at any of the above-described densities. Both the doped and non-doped particles enable the growth of a closed diamond layer, but only the non-doped particles will act later on as masks for the creation of the nano-tips in accordance with example embodiments. The diameter of the individual particles is typically 3 to 5 nm but they often cluster to aggregates leading to a size distribution of typically 5 to 25 nm.
[0052] A doped diamond layer is then deposited for example by chemical vapor deposition (CVD). The dopant may be boron. The diamond layer is deposited in the mold 2 and on the surface of the substrate 1, after which it is patterned to form a patch 4 of the diamond layer inside and around the mold, as shown in
[0053] The diamond deposition is followed by the deposition and patterning of a metal layer stack 5 as illustrated in
[0054] The method step that characterizes this embodiment of the method is a step that is added to the above-described fabrication. The probe as shown in
[0055] As illustrated in
[0056] According to another etch procedure capable of obtaining the structure shown in
[0057] Apart from the SiO.sub.xC.sub.y layer 12 and the seed particles 3 acting as an etch mask, a third masking effect may occur during the plasma etch procedure itself. The energy of the plasma may release particles from materials inside the etch chamber and/or from the cantilever by sputtering, wherein the particles are deposited on the tip where they can also act as an etch mask for a given etch recipe. Also, polymeric etch residues deposited on the tip during the etch process may have the masking effect. In the particular case of a diamond tip produced by the above described molding technique on a Ni-cantilever, the sputtering of Ni particles from the cantilever may become an important contributor to the formation of the nanotips 15. Ni-particles are released from the cantilever by sputtering under the influence of the ion bombardment generated by O.sub.2, SF.sub.6 or SF.sub.6/O plasma. Also because of the bombardment with ions from the plasma, the pyramid gains static charge, resulting in an electric field, which attracts the Ni-particles. The Ni-particles are thereby deposited on the pyramid, but Ni is essentially not etched by SF.sub.6 nor by O.sub.2 plasma, so that the Ni-particles are also acting as etch masks in the same way as the seed particles 3 and SiO.sub.xC.sub.y layer portions 12. The field is stronger where the surface is sharper, i.e. at the pyramid plane edges and mostly at the apex, so the concentration of Ni-particles is higher in these areas, which may be exploited for the production of specific tip structures (see further). When the dry etch is stopped sufficiently early, i.e. before etching away the nanotips 15 themselves, the three above-described masking effects, the SiO.sub.xC.sub.y 12, the seed particles 3 and the Ni-particles have the combined effect of producing the hedgehog structure illustrated in
[0058] As stated, all three masking effects (seed particles 3, SiO.sub.xC.sub.y layer 12 and sputtered particles or etch residues) may contribute to the formation of the hedgehog structure in the case of diamond tip produced in a Si mold on a Ni cantilever. For tips produced from other materials and/or in molds of other materials, or by fabrication techniques other than the molding technique, not all the above-described effects are necessarily occurring simultaneously. In an example method, any one of the above masking effects may occur alone or in combination with the others. If the cantilever material is not a suitable etch mask, the sputtering effect is not or less relevant. It is also possible that a layer similar to the SiO.sub.xC.sub.y is not formed, or does not have a masking effect. The presence of seed particles in a mold is not always required, as is the case for a TiN probe tip, see further. On the other hand, particles which are to serve as a mask in the etch procedure may be deposited onto the tip body 10 after the probe fabrication process and prior to the etching procedure. For example, non-doped diamond particles may be deposited onto a diamond tip by colloidal deposition. This may be done in addition to one or more of the above-described masking effects, or when these effects are not applicable, for example when the seed particles are not suitable as a mask in a particular etching chemistry, or when the probe is not produced by a molding technique. It is also possible that the masking effect is only due to particles deposited on the tip during the etch procedure, such as sputtered particles from the cantilever or from the etch chamber. This may be the case when no seed particles are present and the spontaneously formed compounds, e.g. oxides do not have the masking effect.
[0059] In the light of the above descriptions, it is clear that the mask layer referred to in appended claim 1 may consist of various constituent parts. It may include a layer of irregular thickness, like layer 16 in
[0060] The etch procedures described above are stopped when the nanotips 15 have obtained a given shape and aspect ratio. In the case of the above-described O.sub.2 plasma etch of a diamond tip, the O.sub.2-etch duration defines the shape of the nanotips. At first, the nanotips are cone-shaped pillars, as illustrated in
[0061] The drawing in
[0062] When the probe tip illustrated in
[0063] The disclosure is not limited to the hedgehog type structure described above. According to an embodiment, the dry etch process is continued until the nanotips 15 are etched away on the side planes of the pyramid. However, one or more nanotips 15 are nevertheless formed on the apex area of the tip body 10, as schematically illustrated in
[0064] A second contributor to this tip on tip embodiment is the fact that the diamond layer may be thicker near the apex region compared to on the side planes of the pyramid. This is illustrated in
[0065] The disclosure is applicable to the production of any type of probe suitable for SPM scanning, produced by any standard technique and formed of any standard material, for example Si and Si-compound tips or metal and metal alloy tips. The method is equally applicable to diamond tips other than boron-doped diamond tips, for example phosphor-doped diamond, non-doped diamond, NV (Nitrogen Vacancy) diamond. A hedgehog probe tip including nano-tips 15 formed of TiN on a Ni cantilever may be produced. The probe was fabricated by a molding technique similar to the methods described above. However instead of a diamond CVD layer, a TiN layer, about 150 nm thick was deposited in the Si mold by sputtering of TiN. No seed particles were deposited in the mold. The layer of irregular thickness formed on the TiN is initially an oxide layer that spontaneously forms on the outer surface of the TiN pyramid, after its release from the mold. The oxide works as an etch mask in a plasma etch process under mixed SF.sub.6/O.sub.2 atmosphere, in the same way as the combined effect of the seed particles and SiO.sub.xC.sub.y described above, i.e. the oxide is slowly etched, so that the TiN layer underneath is locally exposed and subsequently etched at a faster rate. As the etch process progresses, sputtered Ni particles contribute to the mask layer, equally as described above. Exposure of the tip to a plasma etch under this atmosphere thereby produced the hedgehog structure with TiN nanotips 15. Details of suitable etch parameters are provide further in this description.
[0066] The disclosure is not limited to pyramid-shaped tips. The nanotips 15 may be produced on other tip geometries as well.
[0067] A number of additional method steps may be performed after completion of the method according to any of the embodiments described above. These additional method steps include: [0068] Deposition of a capping layer on the one or more nanotips 15, thereby covering the nanotips completely with the capping layer, [0069] Plasma etching the capping layer so as to remove the capping layer from a tip area of the nanotips, while maintaining the capping layer on the lateral surface of the nanotips. The tip area includes at least the apex of the nanotips.
[0070] In other words, after these additional steps, the capping layer forms a sleeve around the nanotips 15, leaving the apex of the nanotips exposed, so that the function of the nanotips in an SPM apparatus or other application is not inhibited. The capping layer reinforces the nanotips, i.e. it increases the mechanical resistance of the nanotips, while the tips remain capable of performing their function. This embodiment is beneficial especially in high-force applications, where the capping layer helps to protect the nanotips from breaking off. On a diamond tip or diamond coated tip as described above, the capping layer may be an SiO.sub.x layer (1<x<2) deposited on a hedgehog type probe tip as shown in
[0071] The additional steps as described in the previous paragraphs, for producing a capping layer on the one or more nanotips 15, can be applied also on a tip-on-tip probe, i.e. a probe tip including nanotips on the apex area of the tip body, but wherein the nanotips are produced by a method other than the above-described method involving the production of these nanotips by a self-aligned etch process. For example, the capping layer may be produced by the same steps as described above, on a probe tip produced by the method described in document U.S. Pat. No. 6,328,902. The present disclosure is therefore equally related to a method for producing a probe tip suitable for scanning probe microscopy (SPM), including the steps of: [0072] Producing a probe tip body 10 including an apex area and including on the apex area one or more tip portions being considerably smaller and more pointed than the tip body, while no tip portions are present on the remainder of the probe tip body, [0073] Depositing a capping layer on the one or more tip portions 15, thereby covering the tip portion or portions entirely, [0074] Subjecting the tip portions 15 to a plasma etch process, configured to remove the capping layer from a tip area of the one or more tip portions, the tip area including the apex of the one or more tip portions, while substantially maintaining the cap layer around the lateral surface of the one or more tip portions 15.
[0075] In view of the foregoing paragraphs, the disclosure is equally related to a probe tip suitable for scanning probe microscopy (SPM), including a probe tip body having an apex area and including one or more tip portions on the apex area of the tip body, and no tip portions on the remainder of the tip body, the tip portions being considerably smaller and more pointed than the tip body, wherein the tip portions include a capping layer on their outer surface except on a tip area of the tip portions, the tip area including the apex of the tip portions.
[0076] The example of suitable parameters for producing a capping layer described in the following section is applicable to a diamond probe tip of the tip on tip type, produced by the self-aligned etch method, by the method of U.S. Pat. No. 6,328,902 or by any other understood method.
ExamplesExperiments
[0077] A diamond full hedgehog tip on a probe was produced that includes a tip body produced by the above-described molding technique: Si mold, non-doped seed particles deposited in the mold (density about 1E10/cm.sup.2), Ni cantilever, diamond layer (about 800 nm thick) on Ni core. The following etch parameters were applied:
TABLE-US-00001 TABLE 1 Plasma reactor type ICP Plasma gas O.sub.2 Gas flow (of plasma gas) 50 sccm* RF power 25 W ICP power 1200 W Chamber pressure 9 mTorr ** Etch duration 2.5 min *the gas flow was supplied at 294K and 3 atm. Under these conditions 1 sccm equals about 9.09E9 m.sup.3/s. ** 1 Torr = 133,322 Pa
A diamond tip on tip probe as shown in
The TiN full hedgehog tip referred to above was produced by the following etch conditions:
TABLE-US-00002 TABLE 2 Plasma reactor type ICP Plasma gas Mixed SF.sub.6/O.sub.2 Gas flow (of plasma gas) 40 sccm (SF.sub.6)/10 sccm (O.sub.2)* RF power 50 W ICP power 300 W Chamber pressure 10 mTorr Etch duration 5 min *the gas flow was supplied at 294K and 3 atm
On a full hedgehog tip with diamond tips obtainable by the parameters of table 1, a SiO.sub.x layer was deposited by PECVD, with a thickness of about 50 nm. The tip was subsequently subjected to an SF.sub.6/O.sub.2 plasma etch with the parameters shown in Table 3.
TABLE-US-00003 TABLE 3 Plasma reactor type ICP Plasma gas Mixed SF.sub.6/O.sub.2 Gas flow (of plasma gas) 2.5 sccm (SF.sub.6)/50 sccm (O.sub.2)* RF power 25 W ICP power 1200 W Chamber pressure 10 mTorr Etch duration 5 min *the gas flow was supplied at 294K and 3 atm.
The result was that the SiO.sub.x layer was removed from the apex of the nanotips, while forming a reinforcing capping layer around the lateral surface of the nanotips.
[0080] While example embodiments have been illustrated and described in detail in the drawings and foregoing description, such illustration and description are to be considered illustrative and not restrictive. Other variations to the disclosed embodiments can be understood and effected in practicing the claims, from a study of the drawings, the disclosure, and the appended claims. In the claims, the word comprising does not exclude other elements or steps, and the indefinite article a or an does not exclude a plurality. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used. Any reference signs in the claims should not be construed as limiting the scope.