CN112158794B - Method for preparing atomic force microscope probe stepped substrate by adopting plasma etching - Google Patents
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- 239000000758 substrate Substances 0.000 title claims abstract description 94
- 239000000523 sample Substances 0.000 title claims abstract description 89
- 238000001020 plasma etching Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000005530 etching Methods 0.000 claims abstract description 38
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- 230000001105 regulatory effect Effects 0.000 claims abstract description 9
- 238000001259 photo etching Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 51
- 229910052710 silicon Inorganic materials 0.000 claims description 51
- 239000010703 silicon Substances 0.000 claims description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 229920002120 photoresistant polymer Polymers 0.000 claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- 238000009623 Bosch process Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910018503 SF6 Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 238000002161 passivation Methods 0.000 claims description 2
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 claims description 2
- 229960000909 sulfur hexafluoride Drugs 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 5
- 238000004630 atomic force microscopy Methods 0.000 description 27
- 238000010586 diagram Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00111—Tips, pillars, i.e. raised structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00388—Etch mask forming
- B81C1/00404—Mask characterised by its size, orientation or shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00531—Dry etching
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- 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
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- General Health & Medical Sciences (AREA)
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Abstract
A method for preparing an atomic force microscope probe stepped substrate by adopting plasma etching belongs to the technical field of micro-nano mechanical sensors. The method comprises the following steps: 1) Selecting SOI wafer as raw material; 2) Exposing by using a photoetching machine after the mask spin coating is finished, developing a sample under a special developer at room temperature after the exposure is finished, and then hardening the sample; 3) The reactive ion etching is performed in four steps. According to the method for preparing the atomic force microscope probe stepped substrate by adopting the plasma etching, different etching depths are obtained by utilizing different sizes of etching patterns, so that a stepped structure is manufactured by adopting the plasma etching, the three-step AFM probe substrate by adopting the plasma etching is realized, and the step depth can be regulated and controlled by regulating the side length of the rectangular array of the exposure patterns; an AFM probe having such a stepped substrate does not block the optical path of the reflected laser light.
Description
Technical Field
The invention belongs to the technical field of micro-nano mechanical sensors, and particularly relates to a method for preparing an atomic force microscope probe stepped substrate by adopting plasma etching.
Background
Atomic Force Microscopy (AFM) is widely used in a variety of industries to measure and study microscopic surface topography, such as semiconductors, solid state physics, polymer chemistry, medicine. Wherein an atomic force microscope probe (hereinafter referred to as an AFM probe) is an important component thereof. When the AFM probe is brought close to the sample, molecules or atoms on the surface of the sample interact with the probe to bend the cantilever beam of the probe. And constructing a 3D morphology graph of the sample surface according to different bending amounts when different areas are scanned. To meet the research demands of different degrees, there are also various improvements of AFM probes, such as edge probes with tips at the edges of cantilever beams, high Aspect Ratio (HAR) probes, and special probes with silver or gold plated surfaces to realize probe-surface enhanced raman spectroscopy.
The bending amount of the cantilever beam of the AFM probe is monitored by a set of laser reflection systems. In the measuring process, a beam of laser irradiates on the back of the cantilever beam to generate reflection and is captured by a feedback system, and the bending degree of the cantilever can be calculated by analyzing different reflection laser positions generated by bending the cantilever, so that the most basic requirement of the substrate of the AFM probe is that the reflection laser light path cannot be blocked, as shown in fig. 1.
The most widely used method of AFM probe fabrication today is wet etching, which uses KOH solution to anisotropically etch (100) the Si substrate. Since the etching rate of the (111) crystal face of silicon in KOH solution is far smaller than that of other crystal faces, the side of the substrate edge connected with the cantilever can naturally generate an inclined plane. Although the AFM probe can be manufactured in a large scale at low cost by the method, the inclined plane inclination angle of the joint of the cantilever and the base is 54.7 ℃, the base has only one plane because the inclined plane inclination angle cannot be changed, and the condition of blocking the reflected laser light path can occur in some cases.
Compared with wet etching, plasma etching (dry etching) can also be used for manufacturing AFM probes, is suitable for wafer-level mass production, and is compatible with the traditional MEMS process. However, the typical dry etching is vertical downward etching, and the connection between the AFM probe substrate and the cantilever will become right angles, so that no inclined surface can be generated, and thus the reflected laser light is blocked with a high probability, as shown in fig. 1 b.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a method for preparing an atomic force microscope probe stepped substrate by adopting plasma etching, which utilizes different sizes of etching patterns to obtain different etching depths, thereby manufacturing a stepped structure by plasma etching, realizing a three-step AFM probe substrate by plasma etching, and regulating and controlling the step depth by regulating the side length of a rectangular array of an exposure pattern; an AFM probe having such a stepped substrate does not block the optical path of the reflected laser light.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps of:
1) Selecting an SOI wafer as a raw material, wherein the SOI wafer consists of an SOI wafer device silicon layer, an SOI wafer silicon dioxide layer and an SOI wafer substrate silicon layer, the thickness of the SOI wafer device silicon layer is 5-20 mu m, the thickness of the SOI silicon dioxide layer is 0.5-2 mu m, and the thickness of the SOI wafer substrate silicon layer is 350-500 mu m; preparing a step AFM probe substrate by taking a silicon layer of an SOI wafer substrate as a top surface, spin-coating photoresist with the thickness of 10-12 mu m on the silicon layer of the SOI wafer substrate, and baking on a hot plate at the temperature of 90-100 ℃ for 5-15 minutes;
2) After the mask spin coating is completed, the mask spin coating is used for exposure by a photoetching machine, and the dose of an exposure area is 800-1200mJ/cm 2 Developing the sample under a special developer for 2-3.5 minutes at room temperature after exposure, and then placing the sample on a hot plate at 100-125 ℃ for hardening for 15-30 minutes;
3) The reactive ion etching is performed in four steps, and specifically comprises the following steps: deep silicon etching by Bosch process and O 2 Removing photoresist by plasma etching and adopting pure SF 6 Removing the side wall formed in the deep etching process by plasma, and performing deep silicon etching by using a Bosch process until the SOI wafer is oxidizedAnd a silicon layer.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps of: the thickness of the silicon layer of the SOI wafer device is 8-18 mu m, the thickness of the silicon dioxide layer of the SOI wafer is 0.7-1.8 mu m, and the thickness of the silicon layer of the SOI wafer substrate is 380-470 mu m; preferably: the thickness of the silicon layer of the SOI wafer device is 10-15 mu m, the thickness of the silicon dioxide layer of the SOI wafer is 1.0-1.5 mu m, and the thickness of the silicon layer of the SOI wafer substrate is 400-450 mu m; more preferably: the thickness of the silicon layer of the SOI wafer device is 12-14 μm, the thickness of the silicon dioxide layer of the SOI wafer is 1.2-1.3 μm, and the thickness of the silicon layer of the SOI wafer substrate is 420-430 μm.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps of: spin coating speeds of 1500-2500rpm, preferably 1800-2200rpm; spin coating time is 30-50 seconds, preferably 40-45 seconds; the thickness of the photoresist is 10.5-11 μm, the baking temperature is 95-98 ℃, and the baking time is 8-12 minutes.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps of: the dose of the exposure area is 900-1100mJ/cm 2 Preferably 1000-1050mJ/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the Developing for 2.5-3 min, and placing the sample on a hot plate at 110-120 ℃ for hardening for 20-25 min.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps of: the special developer is AZ400K developer with the volume ratio of 1:3-5: mixed solution of IPA deionized water.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized in that the step 3) adopts a Bosch process to carry out deep silicon etching, and specifically comprises the following steps: the deposition and etching gases being C 4 F 8 And SF (sulfur hexafluoride) 6 Passivation and etching are alternately carried out, and the etching depth is 250-350 mu m; the etching conditions are as follows: deposition cycle: 140-180sccm C 4 F 8 18-22 mTorr,18-22WRF,800-1200WICP,13-17 ℃; etching period: 140-180sccmSF 6 ,18-22mTorr, 18-22WRF,800-1200WICP,13-17℃。
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized in that O is adopted in the step 3) 2 The photoresist is removed by plasma etching, which comprises the following steps: performing pure oxygen reactive ion etching for 15-20 minutes to thoroughly remove the residual photoresist layer;
the method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized in that pure SF is adopted in the step 3) 6 The side wall formed in the deep etching process is removed by plasma, specifically: SF for 15-20 min 6 And (5) carrying out reactive ion etching to eliminate the side wall of the rectangular matrix pattern.
The method for preparing the atomic force microscope probe stepped substrate by adopting plasma etching is characterized in that the step 3) adopts a Bosch process to carry out deep silicon etching until SiO 2 The layer is specifically as follows: bosch etching to SiO in the region beyond the substrate 2 The layers are all exposed.
It will be appreciated by those skilled in the art that 250-300 μm in a Bosch etch refers to the etch depth in the plane of the wafer and not the actual etch depth of the microstructured array pattern. The actual depth of the microstructure array pattern is less than 250-300 μm.
The method for preparing the atomic force microscope probe stepped substrate by adopting the plasma etching utilizes the characteristic that the microstructures with different sizes are etched differently in the plasma etching, and the immediate etching rate is reduced along with the reduction of the size of the microstructure and the increase of the aspect ratio; dividing the vicinity of the substrate cantilever joint into a plurality of areas along the longitudinal axis direction of the substrate, designing micro-structure arrays with different sizes in each area, reducing the etching rate in each area along with the reduction of the micro-structure size, and combining anisotropic plasma etching and isotropic plasma etching to obtain different step heights inwards at the joint of the cantilever beam and the substrate.
Drawings
FIG. 1 is a schematic view of an AFM probe with a stepped substrate (a) and a vertical substrate (b) and a laser path; FIG. 2 is a schematic diagram of an exposure pattern of the present invention, showing two side-by-side probe substrates, wherein the side of the top having a rectangular array pattern is the junction of the substrate and the cantilever, wherein the gray area is the exposure portion and the white area is not exposed;
FIG. 3 is an enlarged schematic view of the top of a probe substrate of the present invention, again with gray areas exposed and white areas not exposed;
FIG. 4 is a flow chart of a step-type substrate manufacturing process according to the present invention;
FIG. 5 is a schematic diagram showing the result of the step 9) treatment in example 1 of the present invention;
FIG. 6 is a schematic diagram showing the result of the step 7) treatment in example 2 of the present invention;
FIG. 7 is a schematic diagram showing the result of the step 9) treatment in example 2 of the present invention;
in the figure: 1-AFM probe substrate, 2-AFM probe cantilever beam, 3-AFM probe tip, 4-incident laser and its reflection light path, 5-SOI wafer device silicon layer, 6-SOI wafer silicon dioxide layer, 7-SOI wafer substrate silicon layer, 8 photoresist.
Detailed Description
The process for preparing the stepped substrate by the method is described in detail below by way of specific examples. The present embodiments are to be considered in all respects as illustrative and not restrictive. In the following description and drawings, like elements are identified with like reference numerals.
Example 1
The AFM probe substrate in this example has dimensions of 3.1. 3.1 mm, 1.6. 1.6 mm, and 0.28. 0.28 mm. The process flow diagram shown in fig. 4 can be seen to include the steps of:
1) A double-sided polished SOI wafer is selected as a raw material, which consists of a 13 μm SOI wafer device silicon layer 5, a 0.5 μm SOI wafer silicon dioxide layer 6 and a 350 μm SOI wafer substrate silicon layer 7, and a substrate silicon layer is selected as a top surface to prepare a step AFM probe substrate (as shown in FIG. 4 a);
2) Spin-coating the silicon layer on one side of the substrate at 2000rpm for 40 seconds to obtain 11 μm thick photoresist AZ4620, and baking on a hot plate at 90 ℃ for 5 minutes (as shown in FIG. 4 b);
3) Photoetching the photoresist, selecting 405nm light with the dosage of 1000mJ/cm 2 Probe substrate topThe rectangular array at one end side is divided into two types, wherein the outer side is a 30 μm side rectangle, and the inner side is a 10 μm side rectangle (as shown in figures 2 and 3);
4) Immersing samples into AZ400K developing solution with the volume ratio of 1:4 at normal temperature: developing for 2.5 minutes in the mixed solution of IPA deionized water, then flushing with deionized water and drying;
5) Placing the sample on a hot plate at 120 ℃ and baking for 30 minutes to obtain a final mask pattern (shown in fig. 4 c);
6) Bosch etch 300 μm. The final etch depth is also different for the rectangular array pattern side lengths (as shown in fig. 4 d). The etching conditions are as follows: deposition cycle: 160sccm C 4 F 8 20mTorr,20WRF,1000WICP,15 ℃; etching period: 160sccmSF 6 ,20mTorr, 20WRF,1000WICP,15℃;
7) Removing the residual photoresist by oxygen plasma etching for 15 minutes (as shown in fig. 4 e);
8) 16 minutes pure SF 6 Plasma etch removes sidewall silicon (as shown in fig. 4 f): 160sccmSF 6 ,15mTorr,20WRF,1000W ICP,15℃;
9) Bosch etch 20 μm, this step is overetch, in order to make SiO 2 The layers were fully exposed and the final substrate thickness was about 250 μm (as shown in fig. 4 g). Example 1 step 9) results in a 70 degree tilt as shown in fig. 5.
The three-step AFM probe substrate for plasma etching is truly realized according to the implementation of the steps, and the step depth can be regulated and controlled by adjusting the side length of the rectangular array of the exposure pattern. An AFM probe with such a stepped substrate does not block the optical path of the reflected laser light (as shown in fig. 1 a).
Example 2
The AFM probe substrate in this example has dimensions of 3.1. 3.1 mm, 1.6. 1.6 mm, and 0.28. 0.28 mm. The process flow diagram shown in fig. 4 can be seen to include the steps of:
1) A double-sided polished SOI wafer was selected as a raw material, which consisted of a device silicon layer, a silicon dioxide layer, and a substrate silicon layer, with thicknesses of 15 μm,1.0 μm, and 380 μm, respectively. Preparing a stepped AFM probe base by taking a substrate silicon layer as a top surface (shown in FIG. 4 a);
2) Spin-coating on one side of the substrate silicon layer at 1800rpm for 50 seconds to obtain 13 μm thick photoresist AZ4620, and baking on a hot plate at 95deg.C for 8 minutes (as shown in FIG. 4 b);
3) Photoetching the photoresist, selecting 405nm light with the dosage of 1200mJ/cm 2 The rectangular array on one side of the top end of the probe substrate is divided into two types, wherein the outer side is 50 μm rectangular, and the inner side is 8 μm rectangular (as shown in figures 2 and 3);
4) Immersing the sample in AZ400K developing solution with the volume ratio of 1:3 at normal temperature: developing in IPA deionized water for 3.0 min, then rinsing with deionized water and drying;
5) Placing the sample on a hot plate at 100 ℃ and baking for 30 minutes to obtain a final mask pattern (shown in fig. 4 c);
6) Bosch etch 350 μm. The final etch depth is also different for the rectangular array pattern side lengths (as shown in fig. 4 d). The etching conditions are as follows: deposition cycle: 140sccm C 4 F 8 18mTorr,18WRF,800WICP,13 ℃; etching period: 140sccmSF 6 ,18mTorr,18WRF,800WICP,13℃;
7) Removing the residual photoresist by oxygen plasma etching for 20 minutes (as shown in fig. 4 e);
8) Pure SF for 15 minutes 6 Plasma etch removes sidewall silicon (as shown in fig. 4 f): 140sccmSF 6 ,18mTorr,18WRF,800W ICP,13℃;
9) Bosch etch 10 μm, this step is overetch, in order to make SiO 2 The layers were fully exposed and the final substrate thickness was about 380 μm (as shown in fig. 4 g).
Step 7), the result after photoresist removal is inclined at an angle of 15 degrees, as shown in fig. 6; 2, step 9), is tilted at an angle of 90 degrees, as shown in fig. 7.
The three-step AFM probe substrate for plasma etching is truly realized according to the implementation of the steps, and the step depth can be regulated and controlled by adjusting the side length of the rectangular array of the exposure pattern. An AFM probe with such a stepped substrate does not block the optical path of the reflected laser light (as shown in fig. 1 a).
Example 3
The AFM probe substrate in this example has dimensions of 3.1. 3.1 mm, 1.6. 1.6 mm, and 0.28. 0.28 mm. The process flow diagram shown in fig. 4 can be seen to include the steps of:
1) A double-sided polished SOI wafer was selected as a raw material, which consisted of a device silicon layer, a silicon dioxide layer, and a substrate silicon layer, with thicknesses of 10 μm,1.5 μm, and 450 μm, respectively. Preparing a stepped AFM probe base by taking a substrate silicon layer as a top surface (shown in FIG. 4 a);
2) Spin-coating on one side of the substrate silicon layer at 2200rpm for 45 seconds to obtain 10 μm thick photoresist AZ4620, and baking on a hot plate at 100deg.C for 5 minutes (as shown in FIG. 4 b);
3) Photoetching the photoresist, selecting 405nm light with the dosage of 800mJ/cm 2 The rectangular array on the top side of the probe substrate is divided into two types, wherein the outer side is 50 μm rectangular, and the inner side is 10 μm rectangular (as shown in figures 2 and 3);
4) Immersing the sample in AZ400K developing solution with the volume ratio of 1:5 at normal temperature: developing for 2.5 minutes in the mixed solution of IPA deionized water, then flushing with deionized water and drying;
5) The sample was placed on a 115 ℃ hotplate for 25 minutes to obtain the final mask pattern (as shown in fig. 4 c);
6) Bosch etch 250 μm. The final etch depth is also different for the rectangular array pattern side lengths (as shown in fig. 4 d). The etching conditions are as follows: deposition cycle: 180sccm C 4 F 8 22mTorr,22WRF,1200WICP,17 ℃; etching period: 180sccmSF 6 ,22mTorr,22WRF,1200WICP,17℃;
7) Removing the residual photoresist by oxygen plasma etching for 18 minutes (as shown in fig. 4 e);
8) 20 min pure SF 6 Plasma etch removes sidewall silicon (as shown in fig. 4 f): 180sccmSF 6 ,22mTorr,22WRF,1200W ICP,18℃;
9) Bosch etch 110 μm, this step is overetch, in order to make SiO 2 The layers were fully exposed and the final substrate thickness was about 250 μm (as shown in fig. 4 g).
The three-step AFM probe substrate for plasma etching is truly realized according to the implementation of the steps, and the step depth can be regulated and controlled by adjusting the side length of the rectangular array of the exposure pattern. An AFM probe with such a stepped substrate does not block the optical path of the reflected laser light (as shown in fig. 1 a).
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the principles and spirit of the invention, but such changes and modifications fall within the scope of the invention.
Claims (13)
1. A method for preparing an atomic force microscope probe stepped substrate by adopting plasma etching is characterized by comprising the following steps:
1) The SOI wafer is selected as a raw material, and consists of an SOI wafer device silicon layer (5), an SOI wafer silicon dioxide layer (6) and an SOI wafer substrate silicon layer (7), wherein the thickness of the SOI wafer device silicon layer (5) is 5-20 mu m, the thickness of the SOI silicon dioxide layer (6) is 0.5-2 mu m, and the thickness of the SOI wafer substrate silicon layer (7) is 350-500 mu m; preparing a stepped AFM probe substrate by taking a silicon layer (7) of an SOI wafer substrate as the top surface, spin-coating photoresist (8) with the thickness of 10-12 mu m on the silicon layer (7) of the SOI wafer substrate, and baking on a hot plate at the temperature of 90-100 ℃ for 5-15 minutes;
2) After the mask spin coating is completed, the mask spin coating is used for exposure by a photoetching machine, and the dose of an exposure area is 800-1200mJ/cm 2 Developing the sample under a special developer for 2-3.5 minutes at room temperature after exposure, and then placing the sample on a hot plate at 100-125 ℃ for hardening for 15-30 minutes;
3) The reactive ion etching is performed in four steps, and specifically comprises the following steps: deep silicon etching by Bosch process, removing photoresist (8) by oxygen plasma etching, and pure SF 6 Removing side wall formed in the deep etching process by plasma, and performing deep silicon etching by using Bosch process untilA silicon dioxide layer (6) of the SOI wafer;
the three-step AFM probe substrate for realizing plasma etching is implemented according to the steps, and the step depth is regulated and controlled by regulating the side length of the exposure pattern rectangular array, so that the AFM probe with the step-shaped substrate cannot block the light path of reflected laser.
2. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 1): the thickness of the SOI wafer device silicon layer (5) is 8-18 μm, the thickness of the SOI wafer silicon dioxide layer (6) is 0.7-1.8 μm, and the thickness of the SOI wafer substrate silicon layer (7) is 380-470 μm.
3. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 1): the thickness of the SOI wafer device silicon layer (5) is 10-15 μm, the thickness of the SOI wafer silicon dioxide layer (6) is 1.0-1.5 μm, and the thickness of the SOI wafer substrate silicon layer (7) is 400-450 μm.
4. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 1): the thickness of the SOI wafer device silicon layer (5) is 12-14 μm, the thickness of the SOI wafer silicon dioxide layer (6) is 1.2-1.3 μm, and the thickness of the SOI wafer substrate silicon layer (7) is 420-430 μm.
5. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 1): the spin coating speed is 1500-2500rpm, the spin coating time is 30-50 seconds, the thickness of the photoresist (8) is 10.5-11 mu m, the baking temperature is 95-98 ℃, and the baking time is 8-12 minutes.
6. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 1): the spin coating rotating speed is 1800-2200rpm; the spin coating time is 40-45 seconds.
7. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 2): the dose of the exposure area is 900-1100mJ/cm 2 Developing for 2.5-3 min, and placing the sample on a hot plate at 110-120 ℃ for hardening for 20-25 min.
8. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 2): the dose of the exposure area is 1000-1050mJ/cm 2 。
9. A method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in step 2): the special developer is AZ400K developer with the volume ratio of 1:3-5: mixed solution of IPA deionized water.
10. The method for preparing the atomic force microscope probe stepped substrate by plasma etching according to claim 1, wherein in the step 3), deep silicon etching is performed by using a Bosch process, specifically: the deposition and etching gases being C 4 F 8 And SF (sulfur hexafluoride) 6 Passivation and etching are alternately carried out, and the etching depth is 250-350 mu m; the etching conditions are as follows: deposition cycle: 140-180sccm C 4 F 8 18-22 mTorr,18-22WRF,800-1200WICP,13-17 ℃; etching period: 140-180sccmSF 6 ,18-22mTorr, 18-22WRF,800-1200WICP,13-17℃。
11. The method for preparing the atomic force microscope probe stepped substrate by plasma etching according to claim 1, wherein in the step 3), the photoresist is removed by oxygen plasma etching, specifically: and (5) carrying out pure oxygen reactive ion etching for 15-20 minutes, and thoroughly removing the residual photoresist layer.
12. The method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein pure SF is used in the step 3) 6 The side wall formed in the deep etching process is removed by plasma, specifically: SF for 15-20 min 6 And (5) carrying out reactive ion etching to eliminate the side wall of the rectangular matrix pattern.
13. The method for preparing a stepped substrate for an atomic force microscope probe by plasma etching according to claim 1, wherein in the step 3), deep silicon etching is performed by using a Bosch process until SiO 2 The layer is specifically as follows: bosch etching to SiO in the region beyond the substrate 2 The layers are all exposed.
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Citations (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0888162A (en) * | 1994-09-19 | 1996-04-02 | Fujitsu Ltd | Manufacture of semiconductor device |
JPH08262041A (en) * | 1995-03-17 | 1996-10-11 | Olympus Optical Co Ltd | Afm cantilever and manufacture thereof |
US5705443A (en) * | 1995-05-30 | 1998-01-06 | Advanced Technology Materials, Inc. | Etching method for refractory materials |
JPH11271347A (en) * | 1998-03-23 | 1999-10-08 | Olympus Optical Co Ltd | Cantilever for scanning type probe microscope and its manufacture |
JP2001242061A (en) * | 2000-03-02 | 2001-09-07 | Olympus Optical Co Ltd | Cantilever for scan type probe microscope and its manufacturing method |
US6458206B1 (en) * | 1998-05-13 | 2002-10-01 | Crystals And Technologies, Ltd. | Cantilever with whisker-grown probe and method for producing thereof |
JP2003315242A (en) * | 2002-04-25 | 2003-11-06 | Seiko Instruments Inc | Cantilever and its producing method |
EP1544865A1 (en) * | 2003-12-17 | 2005-06-22 | Interuniversitair Micro-Elektronica Centrum (IMEC) | A method for making probes for atomic force microscopy |
KR100771851B1 (en) * | 2006-07-21 | 2007-10-31 | 전자부품연구원 | Afm cantilever having fet and method for manufacturing the same |
RU2407101C1 (en) * | 2009-09-07 | 2010-12-20 | Учреждение Российской академии наук Институт физики полупроводников им. А.В. Ржанова Сибирского отделения РАН (ИФП СО РАН) | Method for manufacturing of stepped altitude calibration standard for profilometry and scanning probe microscopy |
DE102009060223A1 (en) * | 2009-12-23 | 2011-06-30 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V., 80539 | Cone-shaped nanostructures on substrate surfaces, in particular optical elements, methods for their production and their use |
CN102435785A (en) * | 2011-11-18 | 2012-05-02 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tilting AFM probe with huge aspect ratio and preparation method thereof |
CN102798615A (en) * | 2011-05-23 | 2012-11-28 | 中国科学院微电子研究所 | Periodic nanostructure-based biosensor and preparation method thereof |
CN103091982A (en) * | 2013-01-23 | 2013-05-08 | 华中科技大学 | Microtube fabrication process |
CN105189821A (en) * | 2013-04-18 | 2015-12-23 | 崔波 | Method of fabricating nano-scale structures and nano-scale structures fabricated using the method |
WO2016018880A1 (en) * | 2014-07-29 | 2016-02-04 | Northwestern University | Apertureless cantilever-free tip arrays for scanning optical lithography and photochemical printing |
JP2016126319A (en) * | 2014-12-26 | 2016-07-11 | Hoya株式会社 | Reflection type mask blank, reflection type mask and method of producing the same, and method of producing semiconductor device |
CN106017385A (en) * | 2016-07-21 | 2016-10-12 | 中国电子科技集团公司第十三研究所 | Preparation method of step height standard sample block with nominal height ranging from 10 mu m to 100 mu m |
CN111134654A (en) * | 2019-12-25 | 2020-05-12 | 上海交通大学 | Photoelectric nerve probe integrated with internal metal shielding layer and preparation method thereof |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002005810A (en) * | 2000-06-16 | 2002-01-09 | Canon Inc | Probe and its manufacturing method, surface-observing device, exposing device, and information-processing device |
WO2005020243A1 (en) * | 2003-07-16 | 2005-03-03 | Japan Science And Technology Agency | Probe for scannning probe microscope and method of producing the same |
KR100766407B1 (en) * | 2007-05-02 | 2007-10-12 | (주)엠투엔 | Method of manufacturing probe tip and probe for use in scanning probe microscope |
US8023191B2 (en) * | 2008-05-07 | 2011-09-20 | Qualcomm Mems Technologies, Inc. | Printable static interferometric images |
JP6746703B2 (en) * | 2016-08-31 | 2020-08-26 | 株式会社日立ハイテク | Particle measuring method and particle measuring device |
-
2020
- 2020-09-04 CN CN202010921867.6A patent/CN112158794B/en active Active
Patent Citations (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0888162A (en) * | 1994-09-19 | 1996-04-02 | Fujitsu Ltd | Manufacture of semiconductor device |
JPH08262041A (en) * | 1995-03-17 | 1996-10-11 | Olympus Optical Co Ltd | Afm cantilever and manufacture thereof |
US5705443A (en) * | 1995-05-30 | 1998-01-06 | Advanced Technology Materials, Inc. | Etching method for refractory materials |
JPH11271347A (en) * | 1998-03-23 | 1999-10-08 | Olympus Optical Co Ltd | Cantilever for scanning type probe microscope and its manufacture |
US6458206B1 (en) * | 1998-05-13 | 2002-10-01 | Crystals And Technologies, Ltd. | Cantilever with whisker-grown probe and method for producing thereof |
JP2001242061A (en) * | 2000-03-02 | 2001-09-07 | Olympus Optical Co Ltd | Cantilever for scan type probe microscope and its manufacturing method |
JP2003315242A (en) * | 2002-04-25 | 2003-11-06 | Seiko Instruments Inc | Cantilever and its producing method |
EP1544865A1 (en) * | 2003-12-17 | 2005-06-22 | Interuniversitair Micro-Elektronica Centrum (IMEC) | A method for making probes for atomic force microscopy |
KR100771851B1 (en) * | 2006-07-21 | 2007-10-31 | 전자부품연구원 | Afm cantilever having fet and method for manufacturing the same |
RU2407101C1 (en) * | 2009-09-07 | 2010-12-20 | Учреждение Российской академии наук Институт физики полупроводников им. А.В. Ржанова Сибирского отделения РАН (ИФП СО РАН) | Method for manufacturing of stepped altitude calibration standard for profilometry and scanning probe microscopy |
DE102009060223A1 (en) * | 2009-12-23 | 2011-06-30 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V., 80539 | Cone-shaped nanostructures on substrate surfaces, in particular optical elements, methods for their production and their use |
CN102798615A (en) * | 2011-05-23 | 2012-11-28 | 中国科学院微电子研究所 | Periodic nanostructure-based biosensor and preparation method thereof |
CN102435785A (en) * | 2011-11-18 | 2012-05-02 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tilting AFM probe with huge aspect ratio and preparation method thereof |
CN103091982A (en) * | 2013-01-23 | 2013-05-08 | 华中科技大学 | Microtube fabrication process |
CN105189821A (en) * | 2013-04-18 | 2015-12-23 | 崔波 | Method of fabricating nano-scale structures and nano-scale structures fabricated using the method |
WO2016018880A1 (en) * | 2014-07-29 | 2016-02-04 | Northwestern University | Apertureless cantilever-free tip arrays for scanning optical lithography and photochemical printing |
JP2016126319A (en) * | 2014-12-26 | 2016-07-11 | Hoya株式会社 | Reflection type mask blank, reflection type mask and method of producing the same, and method of producing semiconductor device |
CN106017385A (en) * | 2016-07-21 | 2016-10-12 | 中国电子科技集团公司第十三研究所 | Preparation method of step height standard sample block with nominal height ranging from 10 mu m to 100 mu m |
CN111134654A (en) * | 2019-12-25 | 2020-05-12 | 上海交通大学 | Photoelectric nerve probe integrated with internal metal shielding layer and preparation method thereof |
Non-Patent Citations (5)
Title |
---|
SU-8胶光刻工艺研究;张立国, 陈迪, 杨帆, 李以贵;光学精密工程;20020630(第03期);第36-39页 * |
原子力显微镜探针批量制备工艺分析;李加东;苗斌;张轲;吴东岷;;微纳电子技术(第02期);第56-60页 * |
原子力显微镜的力传感器;薛实福,刘永生,李庆祥,高宏,徐毓娴,于水;电子工业专用设备;19950730(第03期);第9-15页 * |
基底温度对中阶梯光栅厚铝膜质量的影响;孙梦至;高劲松;李资政;杨海贵;王笑夷;;中国光学(第06期);第48-54页 * |
微米柱阵列ICF埋点靶的制备;王衍斌;唐永建;朱效立;张林;陈志梅;马小军;;原子能科学技术(第04期);第71-74页 * |
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