CN113504394B - Wafer level preparation method of coating probe and coating probe - Google Patents
Wafer level preparation method of coating probe and coating probe Download PDFInfo
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- CN113504394B CN113504394B CN202110787431.7A CN202110787431A CN113504394B CN 113504394 B CN113504394 B CN 113504394B CN 202110787431 A CN202110787431 A CN 202110787431A CN 113504394 B CN113504394 B CN 113504394B
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- 239000000523 sample Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011248 coating agent Substances 0.000 title claims abstract description 22
- 238000000576 coating method Methods 0.000 title claims abstract description 22
- 238000005530 etching Methods 0.000 claims abstract description 109
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 106
- 239000010703 silicon Substances 0.000 claims abstract description 106
- 238000000034 method Methods 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- 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
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 238000001312 dry etching Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000000347 anisotropic wet etching Methods 0.000 claims description 4
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 238000001039 wet etching Methods 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 238000001259 photo etching Methods 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 11
- 230000008021 deposition Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000003491 array Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 152
- 239000010408 film Substances 0.000 description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 27
- 235000012239 silicon dioxide Nutrition 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- 238000007747 plating Methods 0.000 description 11
- 238000010586 diagram Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 7
- 229920002120 photoresistant polymer Polymers 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000684 Cobalt-chrome Inorganic materials 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000010952 cobalt-chrome Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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 disclosure provides a wafer level preparation method of a coating probe and the coating probe, and 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; back anisotropic deep etching of the bulk silicon layer; etching the exposed area of the buried oxide 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; and (3) coating a film on the surface of the needle point to form a coated needle point, thus finishing wafer level preparation of the 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, the conformal deposition of different functional film materials in the three-dimensional structure is realized, and the method can be widely applied to the manufacture of atom probes, nanometer 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 coating probe and the coating probe.
Background
Scanning probe microscopy (SPM, scanning Probe Microscope) is a generic term for a series of analytical instruments with atomic resolution for characterizing surface morphology, 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 acquires signals using a scanning probe, and therefore, scanning probes are critical in SPM systems. The scanning probe consists of a base, a micro-cantilever beam and a nano needle point fixed at the free end of the micro-cantilever beam, wherein the nano needle point 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 sharpness of a nanometer needle point should be ensured as much as possible; secondly, in order to make the scanning probe capable of characterizing special performance parameters such as electricity, magnetism and the like of the sample, different functional layers need to be deposited on the surface of the nanometer needle tip.
At present, technologies for preparing a scanning probe with a special function are various, for example, a metal needle point is prepared by a method such as electroplating, then the probe is prepared by combining a method such as bonding with a micro-cantilever structure, or the preparation of the probe with the special function is realized by combining a film plating process such as focused ion beam etching, carbon nano tube (Carbon Nano Tubes, CNT) deposition and the like.
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 preparing a plating probe and a plating 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 preparation 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, a buried oxide 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 using a thermal oxidation method to form a needle point;
etching the top silicon layer to the buried oxide layer by using a photolithography technique;
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;
anisotropically etching the bulk silicon layer by taking the back deep etching mask layer as a mask; wherein, the etching depth of the anisotropic deep etching is smaller than the thickness of the bulk silicon layer;
etching the exposed area of the buried oxide layer and the bulk silicon layer by using 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 suspended relative to the bulk silicon layer and the oxygen-buried layer and serves as a cantilever; wherein the other parts of the substrate except the cantilever beam and the needle point form a base.
And coating a film on the surface of the needle tip to form a film-coated needle tip, thereby completing the preparation of the film-coated probe.
According to an embodiment of the present disclosure, in the step of forming the tip blank structure and the compensation structure by etching the top silicon layer using the tip pattern mask and the compensation structure pattern mask as masks, isotropic dry etching or anisotropic wet etching is adopted; wherein the etching or etching depth is greater than 10 μm and less than the thickness of the top silicon layer.
According to an embodiment of the present disclosure, in the step of sharpening the needle tip blank structure by the thermal oxidation method, the thermal oxidation temperature includes 900 ℃ to 1100 ℃.
According to an embodiment of the present disclosure, in the step of anisotropically etching the bulk silicon layer using the back side deep etching mask layer as a mask, the anisotropically deep etching includes wet etching or dry etching.
According to an embodiment of the present disclosure, in the step of forming the coated needle tip by coating the surface of the needle tip with a coating film, the method for coating the coating film 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 is 25 ℃ to 300 ℃.
According to an embodiment of the disclosure, the preparation method of the coated probe further includes: annealing the coated device; wherein the annealing temperature is 200-700 ℃; wherein the annealing time is 0.5 h-3 h.
Another aspect of the present disclosure provides a coated probe comprising: the wafer-level substrate comprises a bulk silicon layer, an oxygen-buried layer and a top silicon layer from bottom to top in sequence;
the coated needle tip comprises a needle tip formed by etching the top silicon layer and a coated film covered on the surface of the needle tip;
the compensation structure is formed by etching the top silicon layer and is used for improving etching uniformity; wherein the compensation structure is ridge-shaped; wherein the compensating structure is arranged at intervals with the needle tip;
the cantilever beam is formed by the suspended top silicon layer except the needle point;
a base formed of a portion of the substrate other than the cantilever and the coated needle tip; wherein, the base is step type.
According to an embodiment of the present disclosure, the material of the plating film includes one of diamond, gold, platinum, titanium, nickel, a metal alloy, and a composite metal.
According to an embodiment of the present disclosure, the radius of curvature of the finest part of the needle tip is less than 10nm;
the thickness of the top silicon layer includes: 5-30 μm;
the thickness of the buried oxide layer includes: 0.5-2 μm;
the thickness of the bulk silicon layer comprises: 200 μm to 600 μm.
According to the embodiment of the disclosure, the curvature radius of the coated needle tip is smaller than 30nm.
With the above technical solution, compared with the prior art, it has at least one of the following advantages or part of them.
(1) The cantilever beam is suspended gradually by adopting the technical means of 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 stress is released slowly, and the cantilever beam is ensured not to break from the root, therefore, the high-reliability preparation of the probe is realized, and the method is simple and reliable to operate and can be widely applied to the preparation of the suspended structure of the micro-electromechanical system.
(2) By optimizing the film deposition conditions, the conformal deposition of different functional film materials in the three-dimensional structure is realized, and the method is simple to operate and high in reliability, and can be widely applied to the manufacture of atom probes, nanometer 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 thereof with reference to the accompanying drawings in which:
FIG. 1 schematically illustrates a flow diagram of a method of preparing a coated probe according to an embodiment of the present disclosure;
FIG. 2 schematically illustrates a schematic view of forming a tip pattern mask and a compensation structure pattern mask in accordance with an embodiment of the present disclosure;
FIG. 3 schematically illustrates a schematic diagram of forming a needle tip blank structure and a compensating 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 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 deep etch mask layer and a back side deep etch mask layer in accordance with an embodiment of the present disclosure;
FIG. 7 schematically illustrates a schematic view of a substrate after front side etching of a bulk silicon layer in accordance with an embodiment of the present disclosure;
FIG. 8 schematically illustrates a schematic view of forming a base and a cantilever beam in accordance with an embodiment of the present disclosure;
FIG. 9 schematically illustrates a schematic view of forming a coated needle tip in accordance with an embodiment of the present disclosure; and
fig. 10 schematically illustrates a coated probe, as obtained by the manufacturing method of fig. 1, according to an embodiment of the disclosure.
In the above figures, 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 tip pattern mask; 5. compensating the structural graph mask; 6. a needlepoint blank structure; 7. a compensation structure; 8. a silicon dioxide layer; 9. oxidized needlepoint blank structure; 10. a base; 11. a cantilever beam; 12. a needle tip; 13. a coating layer; 14. and coating the pinpoint.
Detailed Description
The present disclosure is described in further detail below with reference to the drawings and examples. It will be appreciated that the specific embodiments described herein are merely illustrative of the disclosure and are not limiting of the disclosure, as various features described in the embodiments may be combined to form multiple alternatives. It should be further noted that, for convenience of description, only some, but not all of the structures related to the present disclosure are shown in the drawings.
One aspect of the present disclosure provides a wafer level preparation 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-buried 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 using 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;
using the back deep etching mask layer as a mask, and anisotropically etching the bulk silicon layer; wherein, the etching depth of the anisotropic deep etching is smaller 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 part of the top silicon layer with the needle point and the compensation structure, which is suspended relative to the base, is used as a cantilever beam; wherein the other parts of the substrate than the cantilever beam and the needle tip constitute a base.
And coating a film on the surface of the needle point to form a film-coated needle point, thereby completing the preparation of the film-coated probe.
According to the embodiment of the disclosure, the cantilever beam is suspended gradually by adopting 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, so that the stress is released slowly, and the cantilever beam is ensured not to break from the root, therefore, the high-reliability preparation of the probe is realized, and the method is simple and reliable to operate and can be widely applied to the preparation of the suspended structure of the micro-electromechanical system.
According to the embodiment of the disclosure, the conformal deposition of different functional film materials in the three-dimensional structure is realized by optimizing the film deposition conditions, and the method is simple to operate and high in reliability, and can be widely applied to the manufacture of atom probes, nanotip arrays and the like.
According to the embodiment of the disclosure, in the step of etching the top silicon layer by taking the needle tip pattern mask and the compensation structure pattern mask as masks to form the needle tip blank structure and the compensation structure, isotropic dry etching or anisotropic wet etching is adopted; wherein the depth of the etch or etch is greater than 10 μm and less than the thickness of the top silicon layer.
According to embodiments of the present disclosure, the depth of etching or corroding the top silicon layer may be 10 μm, 11 μm, 12 μm, 13 μm, 14 μm or more, as desired, but the etching or corroding depth is less than the thickness of the top silicon layer.
According to embodiments of the present disclosure, the deeper the top silicon layer is etched or etched, the higher the tip that can be obtained, and in particular applications, the higher the tip can detect a deeper morphology of the ravines of the target sample material to be measured relative to the shorter tips, e.g., 3 μm, 4 μm, 5 μm.
According to embodiments of the present disclosure, the cross-sectional shape of the tip pattern mask may be one of a circle, a square, and a polygon.
According to the embodiment of the disclosure, in the step of using the anisotropic wet etching top silicon layer and forming the needle tip blank structure below the needle tip pattern mask, the cross section shape of the needle tip pattern mask can be square or other polygons, so that the pyramid-shaped needle tip is obtained by utilizing the characteristic that wet etching solutions have different etching rates on different crystal faces; in the step of etching the top silicon layer by using an isotropic dry method and forming a needle tip blank structure below the needle tip pattern mask, the cross section shape of the needle tip pattern mask is suitable to be round, the surface of the etched needle tip blank structure is uniform and round, the subsequent step of thermally oxidizing and sharpening the needle tip is facilitated, and finally the needle tip with a smooth and round surface is obtained.
According to the embodiment of the disclosure, when a plurality of probes are prepared on the same substrate, the etching rate of the edge area of the substrate is faster than that of the central area of the substrate due to the etching load effect, so that the etching depths of different areas of the substrate are different within the same etching time, and in order to make the etching rates of different areas of the substrate more uniform, a compensation pattern mask is required to be prepared to compensate the etching area, so that the etching exposure ratio of different positions of the whole wafer is changed, and the etching rate of the substrate is more uniform.
In the step of sharpening the needle tip blank structure using the thermal oxidation method according to the embodiment of the present disclosure, the thermal oxidation temperature includes 900 to 1100 ℃.
According to the embodiment of the disclosure, since the depth of the etched or etched top silicon layer is greater than 10 μm, as the depth of the etched or etched top silicon layer increases, the diameter of the finest part of the needle tip blank structure is reduced, and at this time, specific thermal oxidation temperature and thermal oxidation time are required to be determined according to the diameters of the finest parts of different needle tip blank structures, so as to ensure that the radius of curvature of the finest part of the needle tip can be smaller than 10nm. For example, when the diameter at the narrowest point of the needle in the wafer is at a maximum of 200nm, the thermal oxidation temperature may be 900 ℃; for another example, the thermal oxidation temperature may be 1100 ℃ when the diameter at the narrowest point of the tip in the wafer is 500nm at maximum.
According to the embodiment of the disclosure, in the step of anisotropically etching the bulk silicon layer by taking the back deep etching mask layer as a mask, the anisotropically deep etching includes anisotropically wet etching or anisotropically dry etching.
According to the embodiment of the disclosure, the method for etching the exposed area of the buried oxide layer and the residual bulk silicon layer by taking the front deep etching mask layer as a mask mainly adopts an isotropic deep etching process; if the 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 thus the cantilever beam cannot be formed.
According to an embodiment of the present disclosure, in a step of plating a film on a surface of a needle tip to form a plated needle tip, a method of plating a film 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 an embodiment of the present disclosure, the method for preparing a coated probe further includes: annealing the coated device; wherein the annealing temperature comprises 200-700 ℃; wherein the annealing time is 0.5 h-3 h.
According to the embodiment of the disclosure, the conductive performance or the wear resistance of the plating film can be improved by performing annealing treatment after forming the plating film probe, for example, after the surface of the needle tip is platinized, the wear resistance of the platinized probe can be improved by annealing at 550 ℃ for 1 h.
According to the embodiment of the disclosure, for the method for coating the needle tip, a CoCr film can be deposited on the surface of the needle tip by utilizing a magnetron sputtering technology, so that a magnetic needle tip coated with the CoCr film is obtained; wherein, the sputtering power is suitably 300W, the substrate temperature is suitably 100 ℃, and the curvature radius of the coated needle point is less than 30nm.
Another aspect of the present disclosure provides a coated probe comprising: the wafer-level substrate comprises a bulk silicon layer, an oxygen-buried layer and a top silicon layer from bottom to top in sequence;
the coated needle tip comprises a needle tip formed by etching a top silicon layer and a coated film covered on the surface of the needle tip;
the compensation structure is formed by etching the top silicon layer and is used for improving etching uniformity; wherein the compensation structure is ridge-shaped; wherein the compensating structure is arranged at intervals with the needle tip;
the cantilever beam is formed by a suspended top silicon layer except the needle point;
the base consists of 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 the anisotropic dry etching is adopted to etch the bulk silicon layer to form the step-type bulk silicon layer, 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 the cantilever beam formed by the required probe is shorter, the vertex of the step can influence the transmission of the light path in the actual use process of the probe; the step-shaped base is designed, so that the vertex of the step can be moved backwards, the influence of the vertex of the step on a measuring light path is eliminated, and the size design of the micro-cantilever beam is more flexible.
According to an embodiment of the present disclosure, the material of the plating film includes one of diamond, gold, platinum, titanium, nickel, a metal alloy, and a composite metal.
According to the embodiment of the disclosure, the coated probe can be used for coating films of different materials on the surface of the needle tip according to the requirements of specific applications, and the coated probe with the coated materials of the different materials is formed. Such as forming a platinized probe, a titanized probe, a nickel plated probe.
According to embodiments of the present disclosure, the radius of curvature at the finest point of the needle tip is less than 10nm;
the thickness of the top silicon layer includes: 11-30 μm;
the thickness of the buried oxide layer includes: 0.5-2 μm;
the thickness of the bulk silicon layer includes: 200 μm to 600 μm.
According to embodiments of the present disclosure, the radius of curvature of the coated needle tip is less than 30nm.
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Examples
Fig. 1 schematically illustrates a flow chart of a wafer level manufacturing method of a plating probe according to an embodiment of the present disclosure.
As shown in fig. 1, the preparation method of the 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 diagram of forming a tip pattern mask and a compensation structure pattern mask according to an embodiment of the present disclosure.
As shown in fig. 2, the substrate sequentially comprises a top silicon layer 1, a buried oxide layer 2 and a bulk silicon layer 3 from bottom to top; 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 ℃, secondly, photoresist with a needle point mask pattern and a compensation structure mask pattern is formed on the silicon dioxide layer, then the silicon dioxide layer is anisotropically etched to the top silicon layer 1 through an inductively coupled plasma process by taking the photoresist with the needle point mask pattern and the compensation structure mask pattern as masks, and finally, a needle point pattern mask 4 and a compensation structure pattern mask 5 shown in fig. 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 of forming a needle tip blank structure and a compensating 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, 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, and 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: sharpening the needle point blank structure by using 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 disclosure;
as shown in fig. 3 and fig. 4, the tip pattern mask 4 and the compensation structure pattern mask 5 are removed first, and a thermal oxidation process treatment is performed at 1000 ℃ on the exposed area of the upper surface of the top silicon layer 1, so that a silicon dioxide layer 8 is formed on the surface of the silicon dioxide layer, the effect of sharpening the tip blank structure 6 is achieved, and an oxidized tip blank 9 is formed, so that the structure shown in fig. 4 is formed.
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 fig. 5, a patterned photoresist is formed on the silicon dioxide layer 8 shown in fig. 4, and the patterned photoresist is used as a mask to etch the top silicon layer 1 to the buried oxide layer 2, so as to finally form the structure shown in fig. 5.
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 deep etch mask layer and a back side deep etch 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 areas of the front and back surfaces of the substrate in fig. 5 through a plasma enhanced chemical vapor deposition process, then patterned photoresist is formed on the silicon dioxide mask layer on the front and back surfaces of the substrate, the silicon dioxide layer and the oxygen buried layer 2 on the front surface of the substrate are etched to the bulk silicon layer 3 through a photolithography technique, and the silicon dioxide layer on the back surface is finally formed, and finally the front deep etching mask layer and the back deep etching mask layer shown in fig. 6 are formed.
Step S105: and anisotropically etching the bulk silicon layer by taking the back deep etching mask layer as a mask.
Step S106: and isotropically etching the bulk silicon layer by taking the front deep etching mask layer as a mask.
FIG. 7 schematically illustrates a schematic view of a substrate after front side etching of a bulk silicon layer in accordance with an embodiment of the present disclosure;
as shown in fig. 7, the back deep etching mask layer is used as a mask, the bulk silicon layer 3 is anisotropically etched, the etching depth is suitably 200 μm, and the bulk silicon layer 3 is made to be step-shaped; and isotropically etching the right body silicon layer in a suspended state relative to the left body silicon layer by taking the front deep etching mask layer as a mask, 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 oxygen burying layer to form a base and a cantilever.
FIG. 8 schematically illustrates a schematic view of forming a base and a cantilever beam in accordance with 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, a cantilever beam 11 is formed by a top silicon layer of a suspended portion on the right side of a dotted line, and the body silicon layer, the buried oxide layer, the top silicon layer and the compensation structure remaining after etching on the left side of the dotted line together form a base 10, so as to finally form the structure shown in fig. 8.
Step S108: and coating a film on the surface of the needle point to form a film-coated needle point, thereby completing the preparation of the film-coated probe.
Fig. 9 schematically illustrates a schematic of forming a coated needle tip according to an embodiment of the disclosure.
As shown in fig. 9, a thin 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 technology, a coated needle tip 13 is formed, the curvature radius of the coated needle tip is smaller than 30nm, the thin film material is platinum, and finally the coated probe shown in fig. 9 is formed.
Fig. 10 schematically illustrates a coated probe, as obtained by the manufacturing method of fig. 1, according to an embodiment of the disclosure.
According to the embodiment of the disclosure, as shown in fig. 1 and fig. 10, a technical means of forming a cantilever beam by combining an anisotropic deep etching body silicon layer on the back side of a substrate and an isotropic deep etching body silicon layer on the front side of the substrate is adopted, so that the cantilever beam is suspended gradually, stress is released slowly, the cantilever beam is ensured not to break from the root, and conformal deposition of different functional film materials in a three-dimensional structure is realized by optimizing film deposition conditions, so that the film plating probe as 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 the preparation of the suspension structure of the micro-electromechanical system; and by optimizing 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 manufacture of atom probes, nanometer needle tip arrays and the like.
The foregoing description of the preferred embodiments of the present disclosure is not intended to limit the disclosure, but rather to cover all modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present disclosure.
Claims (10)
1. The wafer level preparation method of the coated probe is characterized by comprising the following steps of:
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-buried 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 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;
using the back deep etching mask layer as a mask, and anisotropically etching the bulk silicon layer; the etching depth of the anisotropic deep etching is smaller 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 part of the top silicon layer with the needle tip and the compensation structure, which is suspended relative to the bulk silicon layer and the oxygen-buried layer, is used as a cantilever; wherein the other parts of the substrate than the cantilever beam and the needle tip constitute a susceptor.
And coating a film on the surface of the needle point to form a film-coated needle point, thereby completing the preparation of the film-coated probe.
2. The method of claim 1, wherein in the step of forming the tip blank structure and the compensation structure by etching the top silicon layer using the tip pattern mask and the compensation structure pattern mask as masks, isotropic dry etching or anisotropic wet etching is used; wherein the depth of the etch or etch is greater than 10 μm and less than the thickness of the top silicon layer.
3. The method of claim 1, wherein the step of sharpening the needle tip blank structure by the thermal oxidation method comprises a thermal oxidation temperature of 900 ℃ to 1100 ℃.
4. The method of claim 1, wherein in anisotropically etching the bulk silicon layer using the backside etch mask layer as a mask, the anisotropically etching comprises wet etching or dry etching.
5. The method of claim 1, wherein in the step of coating the surface of the tip to form a coated tip, the method of 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 preparing the coated probe further comprises: annealing the coated device; wherein the annealing temperature comprises 200-700 ℃; wherein the annealing time is 0.5 h-3 h.
7. A coated probe prepared by the method of any one of claims 1 to 6, comprising:
the wafer-level substrate comprises a bulk silicon layer, an oxygen-buried layer and a top silicon layer from bottom to top in sequence;
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 etching uniformity; wherein the compensation structure is ridge-shaped; wherein the compensating structure is arranged at intervals with the needle tip;
a cantilever beam formed by the top silicon layer which is suspended except the needle point;
a base formed by other parts of the substrate except the cantilever beam and the coated needle point; wherein the base is of a step type.
8. The coated probe of claim 7, wherein the coated material comprises one of diamond, gold, platinum, titanium, nickel, a metal alloy, a composite metal.
9. The coated probe of claim 7, wherein,
the radius of curvature at the finest point of the needle tip is less than 10nm;
the thickness of the top silicon layer comprises: 5-30 μm;
the thickness of the buried oxide layer comprises: 0.5-2 μm;
the thickness of the bulk silicon layer comprises: 200 μm to 600 μm.
10. The coated probe of claim 7, wherein the radius of curvature of the coated tip is less than 30nm.
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