CN113504394A - Wafer-level preparation method of coated probe and coated probe - Google Patents
Wafer-level preparation method of coated probe and coated probe Download PDFInfo
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- CN113504394A CN113504394A CN202110787431.7A CN202110787431A CN113504394A CN 113504394 A CN113504394 A CN 113504394A CN 202110787431 A CN202110787431 A CN 202110787431A CN 113504394 A CN113504394 A CN 113504394A
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- 239000000523 sample Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 107
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 107
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- 238000000034 method Methods 0.000 claims abstract description 47
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 238000001312 dry etching Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 238000000347 anisotropic wet etching Methods 0.000 claims description 4
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
- G01Q70/16—Probe manufacture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
- G01Q60/40—Conductive probes
Abstract
The invention provides a wafer-level preparation method of a coated probe and the coated probe, wherein the preparation method comprises the following steps: forming a needle point pattern mask and a compensation structure pattern mask on a wafer-level substrate; forming a needle point blank structure and a compensation structure; sharpening the needle tip; etching the bulk silicon layer with anisotropic back; etching the exposed area of the oxygen burying layer and the bulk silicon layer on the front surface; removing the front deep etching mask layer and the back deep etching mask layer to form a base and a cantilever beam; and coating a film on the surface of the needle point to form a film-coated needle point, thereby completing the wafer-level preparation of the film-coated probe. By adopting the preparation method, the reliable preparation of the probe is realized, and the method is simple and reliable to operate; by optimizing the film deposition conditions, conformal deposition of film materials with different functions in a three-dimensional structure is realized, and the method can be widely applied to the manufacture of atom probes, nano-needle tip arrays and the like.
Description
Technical Field
The disclosure relates to the field of atomic force microscopes, in particular to a wafer-level preparation method of a coated probe and the coated probe.
Background
Scanning Probe Microscopy (SPM) is a generic name for a series of analytical instruments with atomic resolution for characterizing surface topography, thermal, force, electrical, magnetic, optical, etc. properties, and is widely used in the fields of nanotechnology, material science, surface science, bioengineering, high-density data storage, etc.
SPM uses a scanning probe to acquire signals, and therefore, the scanning probe is critical in SPM systems. The scanning probe consists of a base, a micro-cantilever and a nano-needle tip fixed at the free end of the micro-cantilever, wherein the nano-needle tip is a key component of the scanning probe. Firstly, in order to accurately reflect the surface information of a sample and improve the sensitivity of a scanning probe microscope, the sharp tip of a nanometer needle point is ensured as much as possible; secondly, in order to enable the scanning probe to characterize the electric and magnetic special performance parameters of the sample, different functional layers need to be deposited on the surface of the nanometer needle tip.
At present, there are various techniques for preparing scanning probes with special functions, for example, preparing a metal tip by electroplating or the like, and then preparing a probe by bonding or the like in combination with a micro-cantilever structure, or preparing a probe with special functions by a focused ion beam etching, Carbon Nanotube (CNT) deposition or the like in combination with a coating process.
However, the method can only realize the preparation of a single probe, cannot realize the large-scale preparation of the probe, and has higher preparation cost.
Disclosure of Invention
In view of the above, the present disclosure provides a method for manufacturing a coated probe and a coated probe, so as to at least partially solve one of the above-mentioned technical problems.
One aspect of the present disclosure provides a wafer-level manufacturing method of a coated probe, including:
forming a needle point pattern mask and a compensation structure pattern mask on a wafer-level substrate; wherein the substrate comprises a bulk silicon layer, an oxygen burying layer and a top silicon layer from bottom to top in sequence;
etching the top silicon layer by taking the needle point pattern mask and the compensation structure pattern mask as masks to form a needle point blank structure and a compensation structure;
removing the needle point pattern mask and the compensation structure pattern mask, and sharpening the needle point blank structure by a thermal oxidation method to form a needle point;
etching the top silicon layer to the buried oxide layer by using a photoetching technology;
forming a front deep etching mask layer and a back deep etching mask layer on the front surface of the substrate and the back surface of the substrate;
the back deep etching mask layer is used as a mask, and the bulk silicon layer is anisotropically deep etched; wherein, the etching depth of the anisotropic deep etching is less than the thickness of the bulk silicon layer;
etching the exposed area of the buried oxide layer and the bulk silicon layer by taking the front deep etching mask layer as a mask;
removing the front deep etching mask layer, the back deep etching mask layer and the exposed buried oxide layer; wherein, the top silicon layer with the needle tip and the compensation structure is used as a cantilever relative to the suspended part of the bulk silicon layer and the buried oxide layer; and the other parts of the substrate except the cantilever beam and the needle tip form a base.
And coating a film on the surface of the needle point to form a film-coated needle point, thereby finishing the preparation of the film-coated probe.
According to the embodiment of the disclosure, in the step of etching the top silicon layer by taking the needle point pattern mask and the compensation structure pattern mask as masks to form the needle point blank structure and the compensation structure, isotropic dry etching or anisotropic wet etching is adopted; wherein the depth of the etching or corrosion is larger than 10 μm and smaller than the thickness of the top silicon layer.
According to an embodiment of the present disclosure, in the step of sharpening the tip blank structure by the thermal oxidation method, the thermal oxidation temperature includes 900 ℃ to 1100 ℃.
According to the embodiment of the disclosure, in the step of anisotropically etching back the bulk silicon layer by using the back-side etch-back mask layer as a mask, the anisotropically etching back includes wet etching or dry etching.
According to an embodiment of the present disclosure, in the step of forming a plated needle tip by plating a film on the surface of the needle tip, the plating method includes: magnetron sputtering or electron beam evaporation;
wherein the sputtering power of the magnetron sputtering method comprises 100W-300W; wherein the substrate temperature of the magnetron sputtering method comprises 25-300 ℃.
According to the embodiment of the disclosure, the preparation method of the coated probe further comprises the following steps: annealing the coated device; wherein the annealing temperature comprises 200-700 ℃; wherein the annealing time is 0.5-3 h.
Another aspect of the present disclosure provides a coated probe, including: the wafer-level substrate sequentially comprises a bulk silicon layer, an oxygen buried layer and a top silicon layer from bottom to top;
the coated needle point comprises a needle point formed by etching the top silicon layer and a coated film covered on the surface of the needle point;
the compensation structure is formed by etching the top silicon layer and is used for improving the etching uniformity; wherein, the compensation structure is ridge-shaped; wherein, the compensation structure is arranged at intervals with the needle tip;
a cantilever formed by the top silicon layer in suspension except the needle tip;
a base composed of the other parts of the substrate except the cantilever beam and the coated needle tip; wherein, the base is step-shaped.
According to an embodiment of the present disclosure, the material of the plating film includes one of diamond, gold, platinum, titanium, nickel, metal alloy, and composite metal.
According to the embodiment of the disclosure, the radius of curvature of the finest part of the needle tip is less than 10 nm;
the thicknesses of the top silicon layer include: 5-30 μm;
the thickness of the buried oxide layer comprises: 0.5-2 μm;
the thicknesses of the bulk silicon layer include: 200-600 μm.
According to an embodiment of the present disclosure, the radius of curvature of the coated tip is less than 30 nm.
Compared with the prior art, the technical scheme has at least one or part of the following beneficial effects.
(1) The cantilever beam is formed by combining the anisotropic deep etching body silicon layer on the back surface of the substrate and the isotropic deep etching body silicon layer on the front surface of the substrate, so that the cantilever beam is gradually suspended, the stress is slowly released, and the cantilever beam is prevented from being broken from the root, therefore, the high-reliability preparation of the probe is realized.
(2) The method realizes conformal deposition of different functional film materials in a three-dimensional structure by optimizing the film deposition conditions, has simple operation and high reliability, and can be widely applied to the manufacture of atom probes, nano-needle tip arrays and the like.
Drawings
The above and other objects, features and advantages of the present disclosure will become more apparent from the following description of embodiments of the present disclosure with reference to the accompanying drawings, in which:
FIG. 1 schematically illustrates a flow diagram of a method of making a coated probe according to one embodiment of the present disclosure;
FIG. 2 schematically illustrates a schematic view of a tip patterning mask and a compensation structure patterning mask according to an embodiment of the present disclosure;
FIG. 3 schematically illustrates a schematic diagram of forming a tip proembryo structure and a compensation structure according to an embodiment of the present disclosure;
FIG. 4 schematically illustrates a schematic diagram of forming a silicon dioxide layer according to an embodiment of the present disclosure;
FIG. 5 schematically illustrates a schematic diagram of etching away a portion of a top silicon layer, according to an embodiment of the present disclosure;
FIG. 6 schematically illustrates a schematic diagram of forming a front side etch-back mask layer and a back side etch-back mask layer according to an embodiment of the present disclosure;
FIG. 7 schematically illustrates a schematic view of a substrate after front etching a bulk silicon layer, in accordance with an embodiment of the present disclosure;
FIG. 8 schematically illustrates a schematic diagram of forming a base and cantilever beam according to an embodiment of the present disclosure;
FIG. 9 schematically illustrates a schematic view of forming a coated tip according to an embodiment of the present disclosure; and
FIG. 10 schematically illustrates a coated probe obtained by the method of FIG. 1 according to an embodiment of the disclosure.
In the above drawings, the specific meanings of the reference numerals are as follows:
1. a top silicon layer; 2. an oxygen burying layer; 3. a bulk silicon layer; 4. a needle point pattern mask; 5. compensating the structural pattern mask; 6. a needle point blank structure; 7. a compensation structure; 8. a silicon dioxide layer; 9. the oxidized needle point blank structure; 10. a base; 11. a cantilever beam; 12. a needle tip; 13. coating a film layer; 14. and coating the film on the needle point.
Detailed Description
The present disclosure is described in further detail below with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the disclosure and not restrictive thereof, and that various features described in the embodiments may be combined to form multiple alternatives. It should be further noted that, for the convenience of description, only some of the structures relevant to the present disclosure are shown in the drawings, not all of them.
One aspect of the present disclosure provides a wafer-level manufacturing method of a coated probe, including:
forming a needle point pattern mask and a compensation structure pattern mask on a wafer-level substrate; the substrate comprises a bulk silicon layer, an oxygen burying layer and a top silicon layer from bottom to top in sequence;
etching the top silicon layer by taking the needle point pattern mask and the compensation structure pattern mask as masks to form a needle point blank structure and a compensation structure;
removing the needle point graphic mask and the compensation structure graphic mask, and sharpening the needle point blank structure by using a thermal oxidation method to form a needle point;
etching the top silicon layer to the oxygen burying layer by utilizing photoetching and etching technologies;
forming a front deep etching mask layer and a back deep etching mask layer on the front surface of the substrate and the back surface of the substrate;
the back deep etching mask layer is used as a mask, and the bulk silicon layer is anisotropically deep etched; wherein, the etching depth of the anisotropic deep etching is less than the thickness of the bulk silicon layer;
etching the exposed area of the buried oxide layer and the silicon layer by taking the front deep etching mask layer as a mask;
removing the front deep etching mask layer, the back deep etching mask layer and the exposed buried oxide layer; wherein, the suspended part of the top silicon layer with the needle tip and the compensation structure relative to the base is used as a cantilever beam; wherein the other parts of the substrate except the cantilever beam and the needle tip form a base.
And coating a film on the surface of the needle point to form a film-coated needle point, thereby finishing the preparation of the film-coated probe.
According to the embodiment of the disclosure, as the technical means of forming the cantilever beam by combining the anisotropic deep etching body silicon layer on the back surface of the substrate and the isotropic deep etching body silicon layer on the front surface of the substrate is adopted, the cantilever beam is gradually suspended, the stress is slowly released, and the cantilever beam is ensured not to be broken from the root, so that the high-reliability preparation of the probe is realized.
According to the embodiment of the disclosure, conformal deposition of different functional thin film materials in a three-dimensional structure is realized by optimizing thin film deposition conditions, and the method is simple to operate and high in reliability, and can be widely applied to manufacturing of atom probes, nano-tip arrays and the like.
According to the embodiment of the disclosure, in the step of etching the top silicon layer to form the needle point blank structure and the compensation structure by taking the needle point pattern mask and the compensation structure pattern mask as masks, isotropic dry etching or anisotropic wet etching is adopted; wherein the depth of the etching or corrosion is more than 10 μm and less than the thickness of the top silicon layer.
According to embodiments of the present disclosure, the depth to which the top silicon layer is etched or etched may be 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, or more, but the depth of the etch or etch is less than the thickness of the top silicon layer, as desired.
According to the embodiment of the disclosure, the deeper the etching or etching depth of the top silicon layer is, the higher the needle point can be obtained, and in a specific application, the higher the needle point can detect the topography at the deeper part of the gully of the target sample material to be detected, compared with the shorter needle point, for example, 3 μm, 4 μm, or 5 μm.
According to an embodiment of the present disclosure, the tip pattern mask may have one of a circular, square, and polygonal cross-sectional shape.
According to the embodiment of the disclosure, in the step of etching the top silicon layer by using the anisotropic wet method and forming the needle point blank structure below the needle point pattern mask, the cross section of the needle point pattern mask can be square or other polygons, so that the pyramid-shaped needle point can be obtained by utilizing the characteristic that the wet etching solution has different etching rates on different crystal faces; in the step of etching the top silicon layer by using an isotropic dry method and forming the needle point blank structure below the needle point pattern mask, the cross section of the needle point pattern mask is suitably circular, the surface of the etched needle point blank structure is uniform and round, the subsequent step of thermally oxidizing and sharpening the needle point is facilitated, and the needle point with a smooth and round surface is finally obtained.
According to the embodiment of the disclosure, when a plurality of probes are prepared on the same substrate, due to the etching load effect, the etching rate of the peripheral region of the substrate is faster than that of the central region of the substrate, so that the etching depths of different regions of the substrate are different in the same etching time, in order to make the etching rates of different regions of the substrate more uniform, the compensation pattern mask needs to be prepared to compensate the etching area, the etching exposure ratio of different positions of the whole wafer is changed, and the etching rate of the substrate is made more uniform.
According to the embodiment of the disclosure, in the step of sharpening the tip blank structure by using the thermal oxidation method, the thermal oxidation temperature includes 900 ℃ to 1100 ℃.
According to the embodiment of the disclosure, since the depth of the top silicon layer is etched or etched to be greater than 10 μm, the diameter of the finest portion of the tip blank structure is reduced with the increase of the depth of the top silicon layer, and at this time, the specific thermal oxidation temperature and the specific thermal oxidation time need to be judged according to the diameter of the finest portion of different tip blank structures, so as to ensure that the curvature radius of the finest portion of the tip can be smaller than 10 nm. For example, the thermal oxidation temperature may be 900 ℃ when the diameter maximum at the finest of the needle tips within the disc is 200 nm; for another example, the thermal oxidation temperature may be 1100 ℃ when the diameter maximum at the finest of the tips in the wafer is 500 nm.
According to the embodiment of the disclosure, the back side deep etching mask layer is used as a mask, and in the step of anisotropically deep etching the bulk silicon layer, the anisotropically deep etching comprises anisotropic wet etching or anisotropic dry etching.
According to the embodiment of the disclosure, the method for etching the exposed area of the buried oxide layer and the residual silicon layer by taking the front deep etching mask layer as a mask mainly adopts an isotropic deep etching process; if an anisotropic deep etching process is adopted, the buried oxide layer and the bulk silicon layer below the suspended top silicon layer cannot be etched, and then the cantilever beam cannot be formed.
According to the embodiment of the disclosure, in the step of coating the surface of the needle tip with a film to form a coated needle tip, the film coating method comprises the following steps: magnetron sputtering or electron beam evaporation;
wherein the sputtering power of the magnetron sputtering method comprises 100W-300W; wherein the substrate temperature of the magnetron sputtering method comprises 25-300 ℃.
According to an embodiment of the present disclosure, the method of manufacturing a coated probe further includes: annealing the coated device; wherein the annealing temperature comprises 200-700 ℃; wherein the annealing time is 0.5-3 h.
According to the embodiment of the disclosure, annealing treatment is carried out after the plated probe is formed, so that the conductivity or wear resistance of the plated film can be improved, for example, after the platinum is plated on the surface of the probe tip, the wear resistance of the plated probe can be improved by annealing at 550 ℃ for 1 h.
According to the embodiment of the disclosure, for the method for coating the film on the needle tip, a CoCr film can be deposited on the surface of the needle tip by utilizing a magnetron sputtering technology to obtain the magnetic needle tip coated with the CoCr film; wherein the sputtering power is 300W, the substrate temperature is 100 ℃, and the curvature radius of the coating needle tip is less than 30 nm.
Another aspect of the present disclosure provides a coated probe, including: the wafer-level substrate sequentially comprises a bulk silicon layer, an oxygen buried layer and a top silicon layer from bottom to top;
the coated needle point comprises a needle point formed by etching a top silicon layer and a coated film covered on the surface of the needle point;
the compensation structure is formed by etching the top silicon layer and is used for improving the etching uniformity; wherein, the compensation structure is ridge-shaped; wherein, the compensation structure is arranged at intervals with the needle tip;
the cantilever beam is formed by a suspended top silicon layer except the needle tip;
the base is composed of the other parts of the substrate except the cantilever beam and the coated needle point; wherein, the base is the step type.
According to the embodiment of the disclosure, when a step-type bulk silicon layer is formed by etching a bulk silicon layer by an anisotropic dry method, the side wall of the step is almost vertical to the surface of the substrate, and because the thickness of the bulk silicon layer is larger, when a cantilever beam formed by a required probe is shorter, the transmission of an optical path is influenced by the vertex of the step in the actual use process of the probe; and the design of the step-shaped base can move the vertex of the step backwards, so that the influence of the vertex of the step on a measuring light path is eliminated, and the size design of the micro-cantilever is more flexible.
According to an embodiment of the present disclosure, the material of the coating film includes one of diamond, gold, platinum, titanium, nickel, metal alloy, and composite metal.
According to the embodiment of the disclosure, the film coating probe of the disclosure can perform film coating of different materials on the surface of the probe tip according to the requirements of specific applications, and form the film coating probe of different material film coating materials. For example, a platinum plated probe, a titanium plated probe, and a nickel plated probe are formed.
According to an embodiment of the present disclosure, the radius of curvature at the thinnest point of the needle tip is less than 10 nm;
the thickness of the top silicon layer includes: 11-30 μm;
the thickness of the buried oxide layer comprises: 0.5-2 μm;
the thickness of the bulk silicon layer includes: 200-600 μm.
According to an embodiment of the present disclosure, the radius of curvature of the coated tip is less than 30 nm.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
Examples
FIG. 1 schematically illustrates a flow diagram of a wafer level fabrication method of a coated probe according to an embodiment of the disclosure.
As shown in fig. 1, the steps of the method for preparing a coated probe may include:
step S101: a tip pattern mask and a compensation structure pattern mask are formed on a wafer-level substrate.
Fig. 2 schematically illustrates a schematic view of a tip patterning mask and a compensation structure patterning mask according to an embodiment of the present disclosure.
As shown in fig. 2, the substrate comprises a top silicon layer 1, a buried oxide layer 2 and a bulk silicon layer 3 from bottom to top in sequence; wherein the thickness of the top silicon layer is 20 μm, the thickness of the buried oxide layer is 1 μm, and the thickness of the bulk silicon layer is 400 μm. Firstly, a silicon dioxide layer is formed on the top silicon layer 1 through thermal oxidation treatment at 1000 ℃, then photoresist with a needle point mask pattern and a compensation structure mask pattern is formed on the silicon dioxide layer, then the photoresist with the needle point mask pattern and the compensation structure mask pattern is used as a mask, the silicon dioxide layer is anisotropically etched to the top silicon layer 1 through the process of inductively coupled plasma, and finally a needle point pattern mask 4 and a compensation structure pattern mask 5 shown in figure 2 are formed on the top silicon layer 1.
Step S102: and etching the top silicon layer by taking the needle point pattern mask and the compensation structure pattern mask as masks to form a needle point blank structure and a compensation structure.
FIG. 3 schematically illustrates a schematic diagram of forming a tip proembryo structure and a compensation structure according to an embodiment of the present disclosure.
As shown in fig. 3, the top silicon layer 1 is isotropically etched by using the tip pattern mask 4 and the compensation structure pattern mask 5 as masks and using the process of inductively coupled plasma, the etching depth is 15 μm, a tip blank structure 6 is formed on the top silicon layer 1 under the tip pattern mask 4, a compensation structure 7 is formed on the top silicon layer 1 under the compensation structure pattern mask 5, and finally the structure shown in fig. 3 is formed.
Step S103: and sharpening the needle point blank structure by a thermal oxidation method to form the needle point.
FIG. 4 schematically illustrates a schematic diagram of forming a silicon dioxide layer according to an embodiment of the present disclosure;
as shown in fig. 3 and 4, the tip pattern mask 4 and the compensation structure pattern mask 5 are removed, and the exposed area on the upper surface of the top silicon layer 1 is subjected to a thermal oxidation process at 1000 ℃, so that a silicon dioxide layer 8 is formed on the surface of the top silicon layer, and the effect of sharpening the tip blank structure 6 is achieved, and an oxidized tip blank 9 is formed, thereby forming the structure shown in fig. 4.
Fig. 5 schematically illustrates a schematic diagram of etching away a portion of a top silicon layer according to an embodiment of the disclosure.
As shown in fig. 4 and 5, a patterned photoresist is formed on the silicon dioxide layer 8 shown in fig. 4, and the top silicon layer 1 is etched to the buried oxide layer 2 by using the patterned photoresist as a mask, and finally the structure shown in fig. 5 is formed.
Step S104: and forming a front deep etching mask layer and a back deep etching mask layer on the front surface and the back surface of the substrate.
FIG. 6 schematically illustrates a schematic diagram of forming a front side etch-back mask layer and a back side etch-back mask layer according to an embodiment of the present disclosure.
As shown in fig. 5 and 6, a silicon dioxide mask layer is formed on the exposed regions of the front and back surfaces of the substrate in fig. 5 by a plasma enhanced chemical vapor deposition process, then patterned photoresist is formed on the silicon dioxide mask layer of the front and back surfaces of the substrate, the silicon dioxide layer and the buried oxide layer 2 on the front surface of the substrate are etched to the bulk silicon layer 3 and the silicon dioxide layer on the back surface by a photolithography technique, and finally the front deep etching mask layer and the back deep etching mask layer shown in fig. 6 are formed.
Step S105: and the back deep etching mask layer is used as a mask, and the bulk silicon layer is anisotropically deep etched.
Step S106: and taking the front deep etching mask layer as a mask, and isotropically and deeply etching the bulk silicon layer.
FIG. 7 schematically illustrates a schematic view of a substrate after front etching a bulk silicon layer, in accordance with an embodiment of the present disclosure;
as shown in fig. 7, the back side deep etching mask layer is used as a mask, the bulk silicon layer 3 is anisotropically deep etched, the etching depth is suitably 200 μm, and the bulk silicon layer 3 is stepped; and taking the front deep etching mask layer as a mask, isotropically deep etching the right bulk silicon layer which is in a suspended state relative to the left bulk silicon layer, and finally forming the structure shown in fig. 7.
Step S107: and removing the back deep etching mask layer, the front deep etching mask layer and the exposed buried oxide layer to form a base and a cantilever beam.
FIG. 8 schematically illustrates a schematic diagram of forming a base and cantilever beam according to an embodiment of the present disclosure;
as shown in fig. 8, the back deep etching mask layer, the front deep etching mask layer and the exposed buried oxide layer are removed by using a hydrofluoric acid solution, the cantilever beam 11 is formed by the top silicon layer of the suspended part on the right side of the dotted line, and the etched residual bulk silicon layer, the buried oxide layer, the top silicon layer and the compensation structure on the left side of the dotted line jointly form a base 10, and finally the structure shown in fig. 8 is formed.
Step S108: and coating a film on the surface of the needle point to form a film-coated needle point, thereby finishing the preparation of the film-coated probe.
Fig. 9 schematically illustrates a schematic diagram of forming a coated tip according to an embodiment of the present disclosure.
As shown in fig. 9, a film 14 is formed on the exposed area of the upper surface of the structure shown in fig. 8 by using an electron beam evaporation technique, and a plated tip 13 is formed, the radius of curvature of the plated tip is less than 30nm, the film material is platinum, and finally the plated probe shown in fig. 9 is formed.
FIG. 10 schematically illustrates a coated probe obtained by the method of FIG. 1 according to an embodiment of the disclosure.
According to the embodiment of the disclosure, as shown in fig. 1 and 10, a technical means of forming the cantilever beam by combining the anisotropic deep etching bulk silicon layer on the back surface of the substrate and the isotropic deep etching bulk silicon layer on the front surface of the substrate is adopted, so that the cantilever beam is gradually suspended, the stress is slowly released, the cantilever beam is ensured not to break from the root, conformal deposition of different functional thin film materials in a three-dimensional structure is realized by optimizing thin film deposition conditions, and the film-coated probe shown in fig. 10 is finally obtained.
According to the embodiment of the disclosure, the method for preparing the probe is simple and reliable to operate, and can be widely applied to preparation of a suspension structure of a micro-electro-mechanical system; by optimizing the film deposition conditions, conformal deposition of film materials with different functions in a three-dimensional structure is realized, and the method can be widely applied to the manufacture of atom probes, nano-needle tip arrays and the like.
The above description is only exemplary of the present disclosure and should not be taken as limiting the disclosure, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present disclosure should be included in the scope of protection of the present disclosure.
Claims (10)
1. A wafer-level preparation method of a coated probe is characterized by comprising the following steps:
forming a needle point pattern mask and a compensation structure pattern mask on a wafer-level substrate; the substrate comprises a bulk silicon layer, an oxygen burying layer and a top silicon layer from bottom to top in sequence;
etching the top silicon layer by taking the needle point pattern mask and the compensation structure pattern mask as masks to form a needle point blank structure and a compensation structure;
removing the needle point graphic mask and the compensation structure graphic mask, and sharpening the needle point blank structure by using a thermal oxidation method to form a needle point;
etching the top silicon layer to the buried oxide layer by utilizing photoetching and etching technologies;
forming a front deep etching mask layer and a back deep etching mask layer on the front surface of the substrate and the back surface of the substrate;
the back deep etching mask layer is used as a mask, and the bulk silicon layer is anisotropically deep etched; wherein the etching depth of the anisotropic deep etching is less than the thickness of the bulk silicon layer;
etching the exposed area of the buried oxide layer and the bulk silicon layer by taking the front deep etching mask layer as a mask;
removing the front deep etching mask layer, the back deep etching mask layer and the exposed buried oxide layer; the top silicon layer with the needle tip and the compensation structure is used as a cantilever relative to the suspended parts of the bulk silicon layer and the buried oxide layer; wherein the other part of the substrate except the cantilever beam and the needle tip forms a base.
And coating a film on the surface of the needle point to form a film-coated needle point, thereby finishing the preparation of the film-coated probe.
2. The method of claim 1, wherein in the step of etching the top silicon layer to form the tip blank structure and the compensation structure by using the tip pattern mask and the compensation structure pattern mask as masks, isotropic dry etching or anisotropic wet etching is adopted; wherein the depth of the etching or corrosion is larger than 10 μm and smaller than the thickness of the top silicon layer.
3. The method of claim 1, wherein the step of sharpening the tip blank structure by thermal oxidation comprises a thermal oxidation temperature of 900 ℃ to 1100 ℃.
4. The method according to claim 1, wherein the step of anisotropically etching back the bulk silicon layer with the back side etch-back mask layer as a mask comprises wet etching or dry etching.
5. The method of claim 1, wherein in the step of coating the surface of the tip with a film to form a coated tip, the coating comprises: magnetron sputtering or electron beam evaporation;
wherein the sputtering power of the magnetron sputtering method comprises 100W-300W; wherein the substrate temperature of the magnetron sputtering method comprises 25-300 ℃.
6. The method of claim 1, wherein the method of making the coated probe further comprises: annealing the coated device; wherein the annealing temperature comprises 200-700 ℃; wherein the annealing time comprises 0.5 h-3 h.
7. A coated probe prepared according to the method of any one of claims 1 to 6, comprising:
the wafer-level substrate sequentially comprises a bulk silicon layer, an oxygen buried layer and a top silicon layer from bottom to top;
the coated needle point comprises a needle point formed by etching the top silicon layer and a coated film covered on the surface of the needle point;
a compensation structure formed by etching the top silicon layer for improving etching uniformity; wherein the compensation structure is ridge-shaped; wherein the compensation structure is arranged at intervals with the needle tip;
a cantilever formed from the top silicon layer in suspension except for the tip;
the base is formed by other parts of the substrate except the cantilever beam and the film-coated needle tip; wherein, the base is the step type.
8. The coated probe of claim 7, wherein the coating material comprises one of diamond, gold, platinum, titanium, nickel, metal alloys, and composite metals.
9. The coated probe of claim 7,
the radius of curvature of the thinnest part of the needle tip is less than 10 nm;
the thickness of the top silicon layer comprises: 5-30 μm;
the thickness of the oxygen buried layer comprises: 0.5-2 μm;
the thicknesses of the bulk silicon layer include: 200-600 μm.
10. The coated probe of claim 7, wherein the radius of curvature of the coated tip is less than 30 nm.
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