CN103803484A - Silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching - Google Patents
Silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching Download PDFInfo
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Abstract
The invention discloses a silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching. The method comprises the following operating steps: mounting a probe of which the tip is spherical on a scanning probe microscope or multipoint contact micro-nano processing equipment, fixing a silicon nitride film/silicon on a sample stage, applying a normal load which is not larger than a critical load to the probe, and enabling the probe to mark along a set track; etching the probe in an HF solution for a certain time after marking, so that a silicon substrate is exposed in a marking area, and etching by using a mixed solution of a KOH solution and isopropanol, thus processing the needed micro-nano structure. According to the method, the etching characteristics of the material are changed through friction-induced marking, and selective etching of a specific solution is formed. According to the method, the silicon substrate is not damaged, and the obtained micro-nano structure has reliable service capacity; a deeper/higher micro-nano structure can be processed, a depth-to-width ratio/height-width ratio of the micro-nano structure is improved, and an application range is wide; and the method is simple in processing operation and low in processing cost.
Description
Technical field
The present invention relates to the micro-nano manufacturing method of monocrystalline silicon surface.
Background technology
Nanosecond science and technology have been started 21 century human lives's New Times, and nanometer manufacture is to support nanosecond science and technology to move towards the basis of applying.China is subject to the restriction that nano-fabrication technique falls behind, and micro-/the practical of Mechatronic Systems (MEMS/NEMS) of receiving comparatively lags behind.In improving original processing technology, 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 that is applied at present monocrystalline silicon surface 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.For example, the minimum feature of DUV lithography processing can reach 24nm, but DUV is easily by absorption of air, and this technology is at present also immature; In addition, nanometer embossing also faces many technical bottlenecks and challenge at present, and such as knockout course is serious on impacts such as impression effect, die lifes, 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 scan-probe processing method of common based single crystal silicon generally depends on anodic oxidation or part " mask " is carried out in rubbing action, and anodised governing factor is numerous and diverse, to environment require highly, this greatly reduces the controllability of processing; And " mask " of friction induction depends on friction chemical reaction or malformation strongly, " mask " of friction induction is fine and close not, and anti-chemical etching is limited in one's ability, has fettered the height/depth of the micro nano structure of processing.
Summary of the invention
The object of this invention is to provide a kind of silicon nitride film/silicon micro-nano processing method based on friction induction selective etch, the method is to silicon base not damaged, and the micro nano structure obtaining 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, and processing cost is low.
The present invention is for realizing its goal of the invention, and the technical scheme adopting is, a kind of silicon nitride film/silicon micro-nano processing method based on friction induction selective etch, 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set;
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in the HF solution etching 30-50 minute that mass concentration is 1-5%;
C, isopropyl alcohol is joined in the KOH solution that mass concentration is 10-25% to obtain to mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:4-6; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 2-60 minute;
D, C is walked to silicon nitride film/monocrystal silicon substrate after etching and is again placed in the HF solution etching 10-20 minute of 1-5%.
Process and the mechanism of the inventive method are:
Be deposited on the silicon nitride film of monocrystalline silicon surface in the delineation process of probe, under the effect of residual stress, produce micro-crack, in follow-up HF solution etching, scored area silicon nitride film micro-crack promotes the diffusion of etching agent, therefore its etch rate is greater than and does not delineate the etch rate in district and preferentially optionally removed, thereby exposes silicon base.The silicon in delineation district is by the follow-up quick etching of KOH solution, and the not delineation district still with stabilized silicon nitride thin layer is not etched.Can, under the outstanding mask ability of silicon nitride film, process darker micro nano structure, the last HF solution that passes through is again removed remaining silicon nitride mask.
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 obtaining, has reliable service ability.
Two, processing can be carried out under normal temperature, atmospheric pressure environment, does not need the particular surroundings such as vacuum, constant temperature, and processing is simple, and processing cost is low.KOH solution and HF solution in etching process 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 removing the monocrystalline silicon region of 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 obtains of embodiment mono-processing.
Fig. 2 is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment bis-processing.
Fig. 3 is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment tri-processing.
Fig. 4 is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment tetra-processing.
Fig. 5 a is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment slender acanthopanax work.
Fig. 5 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that obtains of embodiment slender acanthopanax work.
Fig. 6 a is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment six processing.
Fig. 6 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that obtains of embodiment six processing.
Fig. 7 a is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment seven processing.
Fig. 7 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that obtains of embodiment seven processing.
Fig. 8 a is the AFM figure of the monocrystalline silicon surface groove structure that obtains of embodiment eight processing.
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 obtains of embodiment nine processing.
Fig. 9 b is the cross-sectional profiles figure of the monocrystalline silicon surface groove structure that obtains of embodiment nine processing.
Figure 10 is the scanning electron microscope (SEM) photograph of the monocrystalline silicon surface large area linear array structure part that obtains of embodiment ten processing.
The specific embodiment
Embodiment mono-
Silicon nitride film/silicon micro-nano processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set; The radius of curvature of this routine diamond spherical probe tip is 1.5 μ m, and the normal load F of setting is 3mN, and desired trajectory is straight line.
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in to mass concentration is 2% HF solution etching 30 minutes;
C, by isopropyl alcohol join mass concentration be in 20% KOH solution mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:5; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 30 minutes;
D, C walked to silicon nitride film/monocrystal silicon substrate after etching be again placed in 2% HF solution etching 10 minutes.
Fig. 1 is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 1 shows that this example has processed the groove of wide approximately 0.5 μ m, dark about 200nm at monocrystalline silicon surface.
Embodiment bis-
The operation of this example and embodiment mono-are basic identical, and different is only that normal load changes 4mN into.
Fig. 2 is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 2 shows that this example has processed the groove of wide approximately 0.6 μ m, dark about 300nm at monocrystalline silicon surface.
Embodiment tri-
The operation of this example and embodiment mono-are basic identical, and different is only that normal load changes 4.5mN into.
Fig. 3 is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 3 shows that this example has processed the groove of wide approximately 0.75 μ m, dark about 360nm at monocrystalline silicon surface.
Embodiment tetra-
The operation of this example and embodiment mono-are basic identical, and different is only that normal load changes 5mN into.
Fig. 4 is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 4 shows that this example has processed the groove of wide approximately 0.95 μ m, dark about 400nm at monocrystalline silicon surface.
Embodiment mono-to embodiment tetra-shows: load is larger, and the final groove structure obtaining is darker.
Embodiment five
Silicon nitride film/silicon micro-nano processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set; Radius of curvature R=1.5 μ the m of this routine diamond spherical probe tip, the normal load F of setting is 4mN, desired trajectory is straight line.
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in to mass concentration is 1% HF solution etching 40 minutes;
C, by isopropyl alcohol join mass concentration be in 10% KOH solution mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:4; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 5 minutes;
D, C walked to silicon nitride film/monocrystal silicon substrate after etching be again placed in 1% HF solution etching 15 minutes.
Fig. 5 a is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining, and Fig. 5 b is the cross-sectional profiles figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 5 a and Fig. 5 b show that this example has processed the groove of wide approximately 0.6 μ m, dark about 100nm at monocrystalline silicon surface.
Embodiment six
The operation of this example and embodiment five are basic identical, 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 is processed the monocrystalline silicon surface groove structure obtaining, and Fig. 5 b is the cross-sectional profiles figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 5 a and Fig. 5 b show that this example has processed the groove of wide approximately 0.6 μ m, dark about 150nm at monocrystalline silicon surface.
Embodiment seven
The operation of this example and embodiment five are basic identical, 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 is processed the monocrystalline silicon surface groove structure obtaining, and Fig. 5 b is the cross-sectional profiles figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 5 a and Fig. 5 b show that this example has processed the groove of wide approximately 0.6 μ m, 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 processing is darker.
Embodiment eight
Silicon nitride film/silicon micro-nano processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set; Radius of curvature R=1.5 μ the m of this routine diamond spherical probe tip, the normal load F of setting is the varying load that changes to linearly 6mN from 3mN, desired trajectory is straight line.
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in to mass concentration is 5% HF solution etching 30 minutes;
C, by isopropyl alcohol join mass concentration be in 25% KOH solution mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:6; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 35 minutes;
D, C walked to silicon nitride film/monocrystal silicon substrate after etching be again placed in 5% HF solution etching 20 minutes.
Fig. 8 a is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 8 b is that this example is processed the monocrystalline silicon that the obtains profile diagram along the cross section of groove axis.Fig. 8 a and Fig. 8 b show that this example has processed along load and added general orientation at monocrystalline silicon surface, wide from approximately 0.5 μ m to 1 μ m, deeply from about 120nm to 380nm continually varying groove.
Embodiment nine
Silicon nitride film/silicon micro-nano processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set; The normal load F that this example is set is 3.5mN, and desired trajectory is the linear array that many parallel lines form.
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in to mass concentration is 3% HF solution etching 50 minutes;
C, by isopropyl alcohol join mass concentration be in 20% KOH solution mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:5; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 30 minutes;
D, C walked to silicon nitride film/monocrystal silicon substrate after etching be again placed in 4% HF solution etching 13 minutes.
Fig. 9 a is the AFM figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 9 b is the cross-sectional profiles figure that this example is processed the monocrystalline silicon surface groove structure obtaining.Fig. 9 a and Fig. 9 b show this example monocrystalline silicon surface processed wide approximately 0.55 μ m, dark about 300nm the linear array structure of multiple grooves composition.
Embodiment ten
Silicon nitride film/silicon micro-nano processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set; Radius of curvature R=5 μ the m of this routine diamond spherical probe tip, the normal load F of setting is 50mN.Desired trajectory is many linear arrays that straight line is delineated simultaneously within the scope of 5mm × 5mm; The micro-nano process equipment of Multi-contact using is ZL201220331439.9 patent disclosed " the large area friction induction micron order processing unit (plant) under Multi-contact pattern ".
B, the silicon nitride film/monocrystal silicon substrate after delineation is placed in to mass concentration is 2% HF solution etching 30 minutes;
C, by isopropyl alcohol join mass concentration be in 20% KOH solution mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:5; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 60 minutes;
D, C walked to silicon nitride film/monocrystal silicon substrate after etching be again placed in 2% HF solution etching 10 minutes.
Figure 10 is the scanning electron microscope (SEM) photograph that this example is processed the monocrystalline silicon surface large area linear array structure part obtaining.Figure 10 shows that this example has processed the large area linear array structure of multiple groove compositions of wide approximately 1.8 μ m, dark approximately 0.7 μ m at monocrystalline silicon surface.In array, the depth-to-width ratio of groove approaches 0.4.
Above-described embodiment shows, delineate the parameters such as track, delineation scope, delineation load, etch period by control, can show to process various micro nano structures at monocrystalline silicon, structure as constant in the degree of depth, ramp structure, linear array structure, large area texturing structure etc.Experiment showed, delineation load, etch period all with working depth positive correlation, in actual processed and applied, can delineate load and etch period and obtain by reasonable control the micro-nano groove structure of desired depth.
Claims (1)
1. silicon nitride film/silicon micro-nano the processing method based on 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 silicon nitride film/the monocrystal silicon substrate of cleaning is fixed on sample stage, starting device, controls probe and delineates on silicon nitride film/monocrystal silicon substrate surface according to normal load and the desired trajectory set;
B, by delineation after silicon nitride film/monocrystal silicon substrate be placed in the HF solution etching 30-50 minute that mass concentration is 1-5%;
C, isopropyl alcohol is joined in the KOH solution that mass concentration is 10-25% to obtain to mixed solution, the volume ratio that adds fashionable isopropyl alcohol and KOH solution is 1:4-6; Silicon nitride film/the monocrystal silicon substrate again B being walked after etching is placed in mixed solution etching 2-60 minute;
D, C is walked to silicon nitride film/monocrystal silicon substrate after etching and is again placed in the HF solution etching 10-20 minute of 1-5%.
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| CN107265398A (en) * | 2017-06-15 | 2017-10-20 | 西南交通大学 | The silicon that is etched based on mechanical scratching and metal catalytic is micro-/micro-nano structure preparation method |
| CN108821230A (en) * | 2018-06-25 | 2018-11-16 | 西南交通大学 | A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation- |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110482486A (en) * | 2019-07-15 | 2019-11-22 | 电子科技大学 | A kind of silicon substrate graphene nano male structure and preparation method thereof reducing frictional force |
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