CN109850842A - A kind of lossless processing method of monocrystalline silicon surface nanometer hole - Google Patents
A kind of lossless processing method of monocrystalline silicon surface nanometer hole Download PDFInfo
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- CN109850842A CN109850842A CN201910163123.XA CN201910163123A CN109850842A CN 109850842 A CN109850842 A CN 109850842A CN 201910163123 A CN201910163123 A CN 201910163123A CN 109850842 A CN109850842 A CN 109850842A
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- monocrystalline silicon
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Abstract
The invention discloses a kind of lossless processing methods of monocrystalline silicon surface nanometer hole, the following steps are included: S1, to monocrystal silicon sample carry out cleaning and corrosion treatment, to remove the natural oxidizing layer on monocrystal silicon sample surface, and obtain the monocrystalline silicon surface that hydrogen atom or hydroxyl terminate；S2, it after carrying out deionized water flushing to monocrystalline silicon surface, successively places into alcoholic solution and deionized water and is cleaned by ultrasonic, to remove monocrystalline silicon surface pollution；S3, monocrystalline silicon surface is processed using the probe on scanning probe microscopy, indentation-lock out operation is repeated to set contact pressure, time of contact or cycle-index in Working position in probe, so that the silicon atom removed at Working position obtains the nanometer hole without lattice defect.For this method to processing environment without particular/special requirement, finished surface lattice keeps complete, and for base material without residual impairment, the nanometer hole structure for processing acquisition has highly reliable military service performance；Procedure of processing is simple and flexibility is high, and processing cost is low.
Description
Technical field
The invention belongs to technical field of nano-processing, and in particular to a kind of lossless processing method of monocrystalline silicon surface nanometer hole.
Background technique
With the microminiaturization process of micro-nano device, the processing technology under nanosecond science and technology and nanoscale obtains tremendous development
It is also faced with huge challenge simultaneously.Carry out the fundamental and applied research in terms of nanoprocessing, no matter for advanced manufacturing technology
Development, or catbird seat is kept in new round science and technology competition for China, all had a very important significance.
The micro- texture in surface (nanometer hole, nano wire, nano-pattern) is not only to make the base of novel MEMS (MEMS)
Plinth and premise, and it is also widely used for that located growth, surface be modified, anti-attrition drop is rubbed, therefore by researchers at home and abroad
Extensive concern.Wherein, the nanometer hole of monocrystalline silicon surface is mainly used for the fixed point growth of quantum dot, the processing master in Conventional nano hole
There are the methods of laser holographic lithography, nano impression, ion beam etching, electron beam lithography.These methods are expensive, parameter not
It is easy to control, step is complex and inevitably causes to damage to substrate.After preparatory processing goes out nanometer hole, usually also want
Redeposited one layer of silicon crystal is to eliminate the influence of substrate amorphous, dislocation equivalent damage to following process.
In recent years, due to having many advantages, such as that flexibility is big, precision is higher, Scanning probe technique is gradually widely used in micro-
Receive manufacture field.It is mainly delineated by anodic oxidation or friction for the conventional sweep probe processing method of monocrystalline silicon.Its middle-jiao yang, function of the spleen and stomach
Pole oxidation needs special needle point, and environment interdependency is high, and influence factor is more, therefore processing cost is higher；And the delineation that rubs generally is adopted
It realizes that surface processes under big contact pressure with high rigidity Diamond tip, inevitably substrate is caused to damage.
Summary of the invention
Present invention aim to address the above problems, provide a kind of lossless processing method of monocrystalline silicon surface nanometer hole, are one
Kind realizes the simple and easy method of the lossless processing of monocrystalline silicon surface nanometer hole based on " indentation-separation " ad-hesion removal rate under minimal stress,
This method without particular/special requirement, carries out processing environment under normal temperature and pressure environment, and finished surface lattice keeps complete, substrate
For material without residual impairment, the nanometer hole structure for processing acquisition has highly reliable military service performance；Only by changing contact pressure, contact
Depth-width ratio of the parameters such as time or cycle-index with regard to flexibly changing nanometer hole；And the processing is simple, required step is few, processing cost
It is low.
In order to solve the above technical problems, the technical scheme is that a kind of lossless processing side of monocrystalline silicon surface nanometer hole
Method, comprising the following steps:
S1, cleaning and corrosion treatment are carried out to monocrystal silicon sample, to remove the natural oxidizing layer on monocrystal silicon sample surface, and
Obtain the monocrystalline silicon surface that hydrogen atom or hydroxyl terminate；
S2, it after carrying out deionized water flushing to monocrystalline silicon surface, successively places into ultrasonic in alcoholic solution and deionized water
Cleaning, to remove monocrystalline silicon surface pollution；
S3, monocrystalline silicon surface is processed using the probe on scanning probe microscopy, probe with set contact pressure,
Indentation-lock out operation is repeated in Working position in time of contact or cycle-index, to remove the silicon atom at Working position
Obtain the nanometer hole without lattice defect.
In the above-mentioned lossless processing method of monocrystalline silicon surface nanometer hole, as long as it is anti-mechanochemistry to occur between needle point and surface
It answers, form key bridge i.e. and can produce material removal, the surface that hydrogen atom and hydroxyl terminate is capable of forming key bridge, the preferred hydrogen of the present invention
Atom terminates monocrystalline silicon surface.The monocrystalline silicon surface that removal and hydrogenation/hydroxyl for monocrystalline substrate oxide layer terminates obtains
, concrete operations are this field routine operation means.The hydrofluoric acid solution for being preferably 20% by mass concentration in the step S1
It mixed, diluted with the ratio of 1:4 with deionized water, then monocrystal silicon sample is placed in solution and handles 3-5min, to remove monocrystalline
The natural oxidizing layer of silicon face, and obtain the monocrystalline silicon surface of hydrogen atom termination.
In the above-mentioned lossless processing method of monocrystalline silicon surface nanometer hole, deionized water and alcohol washes are used in the step S2
Purpose be raffinate in order to remove step S1 on monocrystalline silicon surface, therefore under the premise of reaching above-mentioned purpose, can adopt
With the mode of operation of other general areas raffinates in this field.In the present invention preferably, after first being rinsed using a large amount of deionized waters,
It is cleaned by ultrasonic 3-5min in alcoholic solution, then is cleaned by ultrasonic 1-3min in deionized water.
In the above-mentioned lossless processing method of monocrystalline silicon surface nanometer hole, special limitation is had no to probe, as long as meeting needle point
Mechanico-chemical reaction can occur between surface, formation key bridge can produce material removal.Preferred silica probe in the present invention,
Such needle point is widely used, is easily obtained, and the technics comparing of this needle point is mature, and price is more cheap.
In the above-mentioned lossless processing method of monocrystalline silicon surface nanometer hole, when to probe tip radius of curvature, contact pressure, contact
Between or circulation time, press-in speed and lift speed, the quiescent time at Working position is not particularly limited, can basis
Actual demand is adjusted.The needle point of same radius of curvature obtains the substantially uniform-diameter of nanometer hole, the depth of nanometer hole with follow
Ring number is in a linear relationship；Between at the time of contact within 10s, the depth of nanometer hole and time of contact are in a linear relationship, and 10s or more connects
The time is touched on the depth of nanometer hole then without influence；Within the scope of experiment condition (< 1.1Gpa), depth is exponentially closed with contact pressure
System.The preferred contact pressure of the present invention is 0.75-1.15GPa, and preferably time of contact is within 10s.
Process and mechanism of the invention is as follows: the natural oxidizing layer of monocrystalline silicon surface is removed using hydrofluoric acid (HF) solution,
And obtain the monocrystalline silicon surface terminated with hydrogen atom；Make probe (silica probe) on this surface under Minor contact pressure
The silicon atom of " indentation-separation ", monocrystalline silicon surface is gradually removed under adhesive attraction.Since this method depends on contact surface
Between adhesion removal based on mechanico-chemical reaction, contact pressure used in processing is well below causing single crystal silicon material
The critical contact pressure of surrender, therefore the plastic deformation or material damage of material will not be caused.Therefore the matrix material of nanometer hole is obtained
Material still maintains mono-crystalline structures, therefore method provided by the invention is a kind of undamaged nanoprocessing method.
The lossless processing method of monocrystalline silicon surface nanometer hole provided by the invention has the advantages that
1, this method depends on the adhesion removal of material, and contact pressure of the probe in " indentation-separation " processing can
Control is within 1GPa, far below the critical contact pressure (about 11GPa) that monocrystalline silicon is surrendered, therefore can avoid introducing and add
The surrender and destruction of work surfacing；
2, with traditional nanometer hole manufacturing process (laser holographic lithography, nano impression, ion beam etching, electron beam lithography
Deng) compare, the present invention only passes through probe and simply " indentation-separation " can be obtained in monocrystalline silicon surface, and cost is lower,
Manufacturing process is simpler；
3, nanometer hole structure can be regulated and controled by contact pressure, time of contact or cycle-index, therefore the present invention has
The process flexibility of height.
Detailed description of the invention
Fig. 1 is the atomic force microscope images for the nanometer hole structure that embodiment one is processed on monocrystal silicon sample surface；
Fig. 2 is the cross-sectional profiles figure for the nanometer hole structure that embodiment one is processed on monocrystal silicon sample surface；
Fig. 3 is the atomic force microscope images for the nanometer hole structure that embodiment two is processed on monocrystal silicon sample surface；
Fig. 4 is the cross-sectional profiles figure for the nanometer hole structure that embodiment two is processed on monocrystal silicon sample surface；
Fig. 5 is the atomic force microscopy for the nanometer hole linear array structure that embodiment three is processed on monocrystal silicon sample surface
Mirror image；
Fig. 6 is the cross-sectional profiles for the nanometer hole linear array structure that embodiment three is processed on monocrystal silicon sample surface
Figure.
Specific embodiment
The present invention is described further in the following with reference to the drawings and specific embodiments:
Embodiment one
The lossless processing method of monocrystalline silicon surface nanometer hole in the present embodiment, specifically includes the following steps:
S1, by mass concentration be 20% hydrofluoric acid solution and deionized water mixed with the ratio of 1:4, dilution, then by ruler
It is very little to be placed in solution for 10mm × 10mm × 1mm monocrystal silicon sample and handle 5min, to remove the natural oxidizing layer of monocrystalline silicon surface,
And obtain the monocrystalline silicon surface of hydrogen atom termination；
S2, after carrying out deionized water flushing to monocrystalline silicon surface, 5min is cleaned by ultrasonic in alcoholic solution, then in deionization
It is cleaned by ultrasonic 3min in water, to remove monocrystalline silicon surface pollution；
S3, monocrystalline silicon surface is processed using the preparing spherical SiO 2 probe being mounted on scanning probe microscopy,
The radius of curvature of preparing spherical SiO 2 probe is 1 μm, and probe is with the load of 3.2 μ N in Working position " indentation-separation " 100 repeatedly
It is secondary, press-in speed and to lift speed be 2 μm/s, after being pressed into depth capacity, processing probe in the static 2s of Working position, due to
Adhesive attraction based on mechanico-chemical reaction, the silicon atom of Working position can be processed probe removal, lack to obtain without lattice
Sunken nanometer hole.
Fig. 1 is the atomic force microscope images for the nanometer hole structure that the present embodiment is processed on monocrystal silicon sample surface.
Fig. 2 is the cross-sectional profiles figure of the nanometer hole structure.Using the processing method of the present embodiment, in monocrystal silicon sample table
Face obtains diameter 100nm, and depth is the nanometer hole structure without lattice defect of 5.5nm.
Embodiment two
The lossless processing method of monocrystalline silicon surface nanometer hole in the present embodiment, specifically includes the following steps:
S1, by mass concentration be 20% hydrofluoric acid solution and deionized water mixed with the ratio of 1:4, dilution, then by ruler
It is very little to be placed in solution for 10mm × 10mm × 1mm monocrystal silicon sample and handle 5min, to remove the natural oxidizing layer of monocrystalline silicon surface,
And obtain the monocrystalline silicon surface of hydrogen atom termination；
S2, after carrying out deionized water flushing to monocrystalline silicon surface, 5min is cleaned by ultrasonic in alcoholic solution, then in deionization
It is cleaned by ultrasonic 3min in water, to remove monocrystalline silicon surface pollution；
S3, monocrystalline silicon surface is processed using the preparing spherical SiO 2 probe being mounted on scanning probe microscopy,
The radius of curvature of preparing spherical SiO 2 probe is 1 μm, and probe is with the load of 3.2 μ N in Working position " indentation-separation " 50 repeatedly
Secondary, press-in speed and to lift speed be 2 μm/s, after being pressed into depth capacity, processing probe obtains nothing in the static 1s of Working position
The nanometer hole of lattice defect.
Fig. 3 is the atomic force microscope images for the nanometer hole structure that the present embodiment is processed on monocrystal silicon sample surface.
Fig. 4 is the cross-sectional profiles figure of the nanometer hole structure.Using the processing method of the present embodiment, in monocrystal silicon sample table
Face obtains diameter 100nm, and depth is the nanometer hole structure without lattice defect of 1.4nm.
Embodiment three
The lossless processing method of monocrystalline silicon surface nanometer hole in the present embodiment, specifically includes the following steps:
S1, by mass concentration be 20% hydrofluoric acid solution and deionized water mixed with the ratio of 1:4, dilution, then by ruler
It is very little to be placed in solution for 10mm × 10mm × 1mm monocrystal silicon sample and handle 5min, to remove the natural oxidizing layer of monocrystalline silicon surface,
And obtain the monocrystalline silicon surface of hydrogen atom termination；
S2, after carrying out deionized water flushing to monocrystalline silicon surface, 5min is cleaned by ultrasonic in alcoholic solution, then in deionization
It is cleaned by ultrasonic 3min in water, to remove monocrystalline silicon surface pollution；
S3, monocrystalline silicon surface is processed using the preparing spherical SiO 2 probe being mounted on scanning probe microscopy,
The radius of curvature of preparing spherical SiO 2 probe is 1 μm, and probe is with the load of 3.2 μ N in Working position " indentation-separation " 25 repeatedly
Secondary, press-in speed and to lift speed be 2 μm/s after being pressed into depth capacity, processes probe in the static 1s of Working position, a position
Needle point is moved after setting immediately to next Working position, point-blank Continuous maching, obtains the nanometer without lattice defect
Cheat linear array structure.
Fig. 5 is the atomic force microscopy for the nanometer hole linear array structure that the present embodiment is obtained in the processing of monocrystal silicon sample surface
Mirror image.
Fig. 6 is the partial cross sectional profile diagram of the nanometer hole linear array structure.Using the processing method of the present embodiment,
Monocrystal silicon sample surface obtains diameter 100nm, depth 0.7nm, the nanometer hole linear array structure that quantity is 16.
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair
Bright principle, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.This field
Those of ordinary skill disclosed the technical disclosures can make according to the present invention and various not depart from the other each of essence of the invention
The specific variations and combinations of kind, these variations and combinations are still within the scope of the present invention.
Claims (6)
1. a kind of lossless processing method of monocrystalline silicon surface nanometer hole, it is characterised in that: the following steps are included:
S1, cleaning and corrosion treatment are carried out to monocrystal silicon sample, to remove the natural oxidizing layer on monocrystal silicon sample surface, and obtained
The monocrystalline silicon surface that hydrogen atom or hydroxyl terminate；
S2, it after carrying out deionized water flushing to monocrystalline silicon surface, successively places into alcoholic solution and deionized water and is cleaned by ultrasonic,
To remove monocrystalline silicon surface pollution；
S3, monocrystalline silicon surface is processed using the probe on scanning probe microscopy, probe is to set contact pressure, contact
Indentation-lock out operation is repeated in Working position in time or cycle-index, so that the silicon atom removed at Working position obtains
Nanometer hole without lattice defect.
2. the lossless processing method of monocrystalline silicon surface nanometer hole according to claim 1, it is characterised in that: the step S1
In, by mass concentration be 20% hydrofluoric acid solution and deionized water mixed with the ratio of 1:4, dilution, then by monocrystal silicon sample
It is placed in solution and handles 3-5min, to remove the natural oxidizing layer of monocrystalline silicon surface, and obtain the monocrystalline silicon table of hydrogen atom termination
Face.
3. the lossless processing method of monocrystalline silicon surface nanometer hole according to claim 1, it is characterised in that: the step S2
In, 3-5min is cleaned by ultrasonic in alcoholic solution, then be cleaned by ultrasonic 1-3min in deionized water.
4. the lossless processing method of monocrystalline silicon surface nanometer hole according to claim 1, it is characterised in that: the probe is two
Aoxidize silicon probe.
5. the lossless processing method of monocrystalline silicon surface nanometer hole according to claim 1 to 4, it is characterised in that: described to connect
Touch pressure is 0.75-1.15GPa.
6. the lossless processing method of monocrystalline silicon surface nanometer hole according to claim 1 to 4, it is characterised in that: described to connect
Touching the time is within 10s.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010063599A (en) * | 1999-12-23 | 2001-07-09 | 박종섭 | Method for forming isolation layer in semiconductor device |
| US7476418B2 (en) * | 2003-10-03 | 2009-01-13 | Sii Nanotechnology Inc. | Method for fabricating nanometer-scale structure |
| CN103738912A (en) * | 2013-12-27 | 2014-04-23 | 西南交通大学 | Monocrystalline silicon non-destructive surface nanometer machining method based on tribo-chemistry induction etching |
| CN103803484A (en) * | 2013-12-27 | 2014-05-21 | 西南交通大学 | Silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching |
| CN106744671A (en) * | 2016-11-30 | 2017-05-31 | 西南交通大学 | A kind of monocrystalline silicon surface nanoprocessing method based on UV ozone |
-
2019
- 2019-03-05 CN CN201910163123.XA patent/CN109850842A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010063599A (en) * | 1999-12-23 | 2001-07-09 | 박종섭 | Method for forming isolation layer in semiconductor device |
| US7476418B2 (en) * | 2003-10-03 | 2009-01-13 | Sii Nanotechnology Inc. | Method for fabricating nanometer-scale structure |
| CN103738912A (en) * | 2013-12-27 | 2014-04-23 | 西南交通大学 | Monocrystalline silicon non-destructive surface nanometer machining method based on tribo-chemistry induction etching |
| CN103803484A (en) * | 2013-12-27 | 2014-05-21 | 西南交通大学 | Silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching |
| CN106744671A (en) * | 2016-11-30 | 2017-05-31 | 西南交通大学 | A kind of monocrystalline silicon surface nanoprocessing method based on UV ozone |
Non-Patent Citations (1)
| Title |
|---|
| 陈诚: ""单晶硅机械化学耦合去除机理研究"", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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