CN103803484B - Based on the silicon nitride film/silicon micro-nano processing method of friction induction selective etch - Google Patents

Based on the silicon nitride film/silicon micro-nano processing method of friction induction selective etch Download PDF

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CN103803484B
CN103803484B CN201310732868.6A CN201310732868A CN103803484B CN 103803484 B CN103803484 B CN 103803484B CN 201310732868 A CN201310732868 A CN 201310732868A CN 103803484 B CN103803484 B CN 103803484B
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nitride film
silicon nitride
silicon
micro
solution
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CN103803484A (en
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钱林茂
郭剑
余丙军
王晓东
宋晨飞
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Southwest Jiaotong University
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Abstract

A kind of silicon nitride film based on friction induction selective etch/silicon micro-nano processing method, its operation is: be that spherical probe is arranged on scanning probe microscopy or the micro-nano process equipment of Multi-contact by tip, silicon nitride film/silicon is fixed on sample stage, the normal load being not less than critical load is applied to probe, and make probe along the track of setting, delineate; Delineation is placed in HF solution and etches the regular hour, delineation district silicon base is exposed, then uses the mixed solution of KOH solution and isopropyl alcohol to etch, can process required micro nano structure.The method changes material etch characteristic by friction induction delineation, and then forms the selective etch of particular solution.The method is to silicon base not damaged, and the micro nano structure obtained has more reliable service ability; Can process darker/higher micro nano structure, improve the depth-to-width ratio/depth-width ratio of micro nano structure, the scope of application is wide; And its processing is simple, processing cost is low.

Description

Based on the silicon nitride film/silicon micro-nano processing method of friction induction selective etch
Technical field
The present invention relates to the micro-nano manufacturing method of monocrystalline silicon surface.
Background technology
Nanosecond science and technology have started the New Times of 21 century human lives, and nanometer manufacture supports the basis that nanosecond science and technology move towards application.China is subject to the restriction that nano-fabrication technique falls behind, micro-/nano electromechanical systems (MEMS/NEMS) practical comparatively delayed.While the original processing technology of improvement, seek new nanofabrication technique extremely urgent.Therefore, carry out the fundamental and applied research of nanoprocessing aspect, no matter for the development of MEMS/NEMS, or in new round science and technology competition, keep catbird seat for China, all tool is of great significance.
Monocrystalline silicon, because of its outstanding mechanical performance and physical property, is widely used in MEMS/NEMS.According to different principles, the micro-nano manufacturing method being applied to monocrystalline silicon surface at present mainly contains photoetching technique, nanometer embossing etc.Along with improving constantly of machining accuracy, the cost of lithography process is more and more higher, and limitation is increasing.Such as, the minimum feature of DUV lithography processing can reach 24nm, but DUV is easily by absorption of air, and this technology is also immature at present; In addition, nanometer embossing also faces many technical bottlenecks and challenge at present, and such as knockout course is serious on the impression impact such as effect, die life, and moulding process easily causes damage to matrix material in addition.
In recent years, due to advantages such as Scanning probe technique have high accuracy, multi-functional, be applicable to micro-nano manufacture field.The scanning probe lithography method of common based single crystal silicon generally depends on anodic oxidation or local " mask " is carried out in rubbing action, and anodised governing factor is numerous and diverse, high to the requirement of environment, and this greatly reduces the controllability of processing; And " mask " of friction induction is strongly depend on friction chemical reaction or malformation, " mask " of friction induction is fine and close not, and chemical resistance etching power is limited, fettered process the height/depth of micro nano structure.
Summary of the invention
The object of this invention is to provide a kind of silicon nitride film based on friction induction selective etch/silicon micro-nano processing method, the method is to silicon base not damaged, and the micro nano structure obtained has more reliable service ability; Can process darker/higher micro nano structure, improve the depth-width ratio of micro nano structure, the scope of application is wide; And its processing is simple, processing cost is low.
The present invention is for realizing its goal of the invention, and the technical scheme adopted is, a kind of silicon nitride film based on friction induction selective etch/silicon micro-nano processing method, and its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy or the micro-nano process equipment of Multi-contact by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory;
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in mass concentration is that the HF solution of 1-5% etches 30-50 minute;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 10-25% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:4-6; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution and etches 2-60 minute;
D, the HF solution that the silicon nitride film/monocrystal silicon substrate after C step etching is placed in 1-5% is again etched 10-20 minute.
Process and the mechanism of the inventive method are:
Be deposited on the silicon nitride film of monocrystalline silicon surface in the scoring process of probe, micro-crack is created under the effect of residual stress, in follow-up HF solution etches, scored area silicon nitride film micro-crack promotes the diffusion of etching agent, therefore its etch rate is greater than the etch rate of not delineating district and is preferentially optionally removed, thus exposes silicon base.The silicon in delineation district is etched fast by follow-up KOH solution, and the district of not delineating still with stabilized silicon nitride thin layer is not etched.Under the mask ability that silicon nitride film is outstanding, darker micro nano structure can be processed, finally by HF solution, the silicon nitride mask of remnants be removed again.
Compared with prior art, the invention has the beneficial effects as follows:
One, probe is delineated on silicon nitride film, and to silicon base not damaged, the micro nano structure not damaged therefore finally obtained, has reliable service ability.
Two, process and can carry out under normal temperature, atmospheric pressure environment, do not need the particular surroundings such as vacuum, constant temperature, processing is simple, and processing cost is low.KOH solution in etching process and HF solution are easy to obtain.
Three, silicon nitride film compact structure, anti-KOH solution corrosion ability is strong, and KOH solution is also difficult to erode silicon nitride mask for a long time, thus under its mask effect, KOH solution can etch darker micro-nano recessed structure to the monocrystalline silicon region removing mask.
Below in conjunction with accompanying drawing and concrete embodiment, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the AFM figure of the monocrystalline silicon surface groove structure that embodiment one processing obtains.
Fig. 2 is the AFM figure of the monocrystalline silicon surface groove structure that embodiment two processing obtains.
Fig. 3 is the AFM figure of the monocrystalline silicon surface groove structure that embodiment three processing obtains.
Fig. 4 is the AFM figure of the monocrystalline silicon surface groove structure that embodiment four processing obtains.
Fig. 5 a is the AFM figure of the monocrystalline silicon surface groove structure that embodiment slender acanthopanax work obtains.
Fig. 5 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that embodiment slender acanthopanax work obtains.
Fig. 6 a is the AFM figure of the monocrystalline silicon surface groove structure that embodiment six processing obtains.
Fig. 6 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that embodiment six processing obtains.
Fig. 7 a is the AFM figure of the monocrystalline silicon surface groove structure that embodiment seven processing obtains.
Fig. 7 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that embodiment seven processing obtains.
Fig. 8 a is the AFM figure of the monocrystalline silicon surface groove structure that embodiment eight processing obtains.
Fig. 8 b is the cross section profile figure of the monocrystalline silicon that obtains of embodiment eight processing along groove axis.
Fig. 9 a is the AFM figure of the monocrystalline silicon surface groove structure that embodiment nine processing obtains.
Fig. 9 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that embodiment nine processing obtains.
Figure 10 is the scanning electron microscope (SEM) photograph of the monocrystalline silicon surface large area linear array structure local that embodiment ten processing obtains.
Detailed description of the invention
Embodiment one
Based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory; The radius of curvature of the diamond spherical probe tip of this example is 1.5 μm, and the normal load F of setting is 3mN, and desired trajectory is straight line.
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in mass concentration be 2% HF solution etching 30 minutes;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 20% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:5; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution etching 30 minutes;
D, by C step etching after silicon nitride film/monocrystal silicon substrate be again placed in 2% HF solution etching 10 minutes.
Fig. 1 is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 1 shows that this example has processed the groove of wide about 0.5 μm, dark about 200nm at monocrystalline silicon surface.
Embodiment two
The operation of this example is substantially identical with embodiment one, and different is only that normal load changes 4mN into.
Fig. 2 is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 2 shows that this example has processed the groove of wide about 0.6 μm, dark about 300nm at monocrystalline silicon surface.
Embodiment three
The operation of this example is substantially identical with embodiment one, and different is only that normal load changes 4.5mN into.
Fig. 3 is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 3 shows that this example has processed the groove of wide about 0.75 μm, dark about 360nm at monocrystalline silicon surface.
Embodiment four
The operation of this example is substantially identical with embodiment one, and different is only that normal load changes 5mN into.
Fig. 4 is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 4 shows that this example has processed the groove of wide about 0.95 μm, dark about 400nm at monocrystalline silicon surface.
Embodiment one to embodiment four shows: load is larger, and the final groove structure obtained is darker.
Embodiment five
Based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory; Radius of curvature R=1.5 μm of the diamond spherical probe tip of this example, the normal load F of setting is 4mN, and desired trajectory is straight line.
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in mass concentration be 1% HF solution etching 40 minutes;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 10% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:4; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution etching 5 minutes;
D, by C step etching after silicon nitride film/monocrystal silicon substrate be again placed in 1% HF solution etching 15 minutes.
Fig. 5 a is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained, Fig. 5 b is the cross-sectional profiles figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 5 a and Fig. 5 b shows that this example has processed the groove of wide about 0.6 μm, dark about 100nm at monocrystalline silicon surface.
Embodiment six
The operation of this example is substantially identical with embodiment five, and the etch period in C step that different is only changes 15 minutes into.
Fig. 5 a is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained, Fig. 5 b is the cross-sectional profiles figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 5 a and Fig. 5 b shows that this example has processed the groove of wide about 0.6 μm, dark about 150nm at monocrystalline silicon surface.
Embodiment seven
The operation of this example is substantially identical with embodiment five, and the etch period in C step that different is only changes 30 minutes into.
Fig. 5 a is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained, Fig. 5 b is the cross-sectional profiles figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 5 a and Fig. 5 b shows that this example has processed the groove of wide about 0.6 μm, dark about 240nm at monocrystalline silicon surface.
Embodiment five to embodiment seven shows: the etch period of KOH, isopropyl alcohol mixture is longer, and the groove structure processed is darker.
Embodiment eight
Based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory; Radius of curvature R=1.5 μm of the diamond spherical probe tip of this example, the normal load F of setting is the varying load changing to 6mN from 3mN linearly, and desired trajectory is straight line.
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in mass concentration be 5% HF solution etching 30 minutes;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 25% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:6; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution etching 35 minutes;
D, by C step etching after silicon nitride film/monocrystal silicon substrate be again placed in 5% HF solution etching 20 minutes.
Fig. 8 a is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 8 b is that this example processes the monocrystalline silicon that the obtains profile diagram along the cross section of groove axis.Fig. 8 a and Fig. 8 b shows that this example has processed at monocrystalline silicon surface and adds general orientation along load, wide from about 0.5 μm to 1 μm, dark in about 120nm to 380nm continually varying groove.
Embodiment nine
Based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory; The normal load F of this example setting is 3.5mN, and desired trajectory is the linear array that many parallel lines are formed.
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in mass concentration be 3% HF solution etching 50 minutes;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 20% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:5; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution etching 30 minutes;
D, by C step etching after silicon nitride film/monocrystal silicon substrate be again placed in 4% HF solution etching 13 minutes.
Fig. 9 a is the AFM figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 9 b is the cross-sectional profiles figure that this example processes the monocrystalline silicon surface groove structure obtained.Fig. 9 a and Fig. 9 b show this example monocrystalline silicon surface processed wide about 0.55 μm, dark about 300nm the linear array structure of multiple grooves compositions.
Embodiment ten
Based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on the micro-nano process equipment of Multi-contact by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory; Radius of curvature R=5 μm of the diamond spherical probe tip of this example, the normal load F of setting is 50mN.Desired trajectory is the linear array that within the scope of 5mm × 5mm, many straight lines are delineated simultaneously; The micro-nano process equipment of Multi-contact " the large area friction induction micron order processing unit (plant) under Multi-contact pattern " disclosed in ZL201220331439.9 patent used.
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in mass concentration be 2% HF solution etching 30 minutes;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 20% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:5; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution etching 60 minutes;
D, by C step etching after silicon nitride film/monocrystal silicon substrate be again placed in 2% HF solution etching 10 minutes.
Figure 10 is the scanning electron microscope (SEM) photograph that this example processes the monocrystalline silicon surface large area linear array structure local obtained.Figure 10 shows that this example has processed at monocrystalline silicon surface the large area linear array structure that wide about 1.8 μm, dark about 0.7 μm multiple grooves form.In array, the depth-to-width ratio of groove is close to 0.4.
Above-described embodiment shows, by controlling delineation track, delineation scope, parameter such as delineation load, etch period etc., can show to process various micro nano structure at monocrystalline silicon, as the structure of constant depth, ramp structure, linear array structure, large area textured structure etc.Experiment proves, delineation load, etch period all with working depth positive correlation, can delineate by conservative control the micro-nano groove structure that load and etch period obtain desired depth in actual processed and applied.

Claims (1)

1., based on silicon nitride film/silicon micro-nano processing method of friction induction selective etch, its concrete operation step is followed successively by:
A, be that spherical probe is arranged on scanning probe microscopy or the micro-nano process equipment of Multi-contact by tip, again cleaned silicon nitride film/monocrystal silicon substrate is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to the normal load set and desired trajectory;
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in mass concentration is that the HF solution of 1-5% etches 30-50 minute;
C, isopropyl alcohol joined mass concentration be in the KOH solution of 10-25% mixed solution, the volume ratio adding fashionable isopropyl alcohol and KOH solution is 1:4-6; Again silicon nitride film/the monocrystal silicon substrate after B step etching is placed in mixed solution and etches 2-60 minute;
D, the HF solution that the silicon nitride film/monocrystal silicon substrate after C step etching is placed in 1-5% is again etched 10-20 minute.
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CN109437085A (en) * 2018-10-25 2019-03-08 西南交通大学 A kind of not damaged friction induction nanoprocessing method
CN109850842A (en) * 2019-03-05 2019-06-07 西南交通大学 A kind of lossless processing method of monocrystalline silicon surface nanometer hole
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