CN101973507A - Friction induction-based single crystal quartz surface selective etching method - Google Patents

Friction induction-based single crystal quartz surface selective etching method Download PDF

Info

Publication number
CN101973507A
CN101973507A CN 201010222382 CN201010222382A CN101973507A CN 101973507 A CN101973507 A CN 101973507A CN 201010222382 CN201010222382 CN 201010222382 CN 201010222382 A CN201010222382 A CN 201010222382A CN 101973507 A CN101973507 A CN 101973507A
Authority
CN
China
Prior art keywords
single crystal
scanning
crystal quartz
probe
load
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 201010222382
Other languages
Chinese (zh)
Other versions
CN101973507B (en
Inventor
钱林茂
宋晨飞
周仲荣
余家欣
余丙军
陈磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Southwest Jiaotong University
Original Assignee
Southwest Jiaotong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southwest Jiaotong University filed Critical Southwest Jiaotong University
Priority to CN2010102223824A priority Critical patent/CN101973507B/en
Publication of CN101973507A publication Critical patent/CN101973507A/en
Application granted granted Critical
Publication of CN101973507B publication Critical patent/CN101973507B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention discloses a friction induction-based single crystal quartz surface selective etching method. The method comprises the following steps of: arranging a probe with ball coronary tip on an atomic force microscope, fixing single crystal quartz on a sample platform, starting the atomic force microscope, and applying constant load F or variable load F' to the probe, wherein the value of the F or the variable range of the F' is 0.03 to 0.14 times critical load Fy of yield on the quartz surface; performing scanning on the surface of the single crystal quartz along the set track and cycle times by the probe; and after scanning, corroding the single crystal quartz for over 2.5 hours by using 15 to 25 percent KOH solution. The method can effectively perform nano processing by combining scanning under extremely low load and subsequent corrosion, does not need a mask or repeated corrosion, and can process a multistage nano structure. The method does not damage or pollute the structure and the surface outside the processed area, and is a simple, accurate and clean nano quartz processing method.

Description

A kind of single crystal quartz surface selectivity lithographic method based on friction induction
Technical field
The present invention relates to quartzy micro-nano manufacturing method.
Background technology
Micro-nano device is widely used in fields such as advanced manufacturing, Aero-Space, military affairs, biotechnology, Computers and Communication.Quartz not only has excellent electric insulating and chemical stability, and degree of will speed up, pressure etc. are converted into the signal of telecommunication easily, is a kind of piezoelectric of excellent performance.Therefore, quartz is an important materials of making micro-nano device, often is used to make micro-acceleration gauge, micropressure sensor, biochip, MEMS dielectric base etc.
According to different process principles, processing method at quartzy micro element mainly contains at present: the processing of (1) FIB: utilize plus high-voltage field to quicken metal ion, under the control of deflecting electric field, form directed high energy ion beam, bombard, cut by ion pair single crystal quartz surface, reach the purpose of processing.This method need be protected the gold-plated film of quartz surfaces, and a part of ion can be injected into quartz crystal inside in the process, and single crystal quartz is polluted.In addition, this method process complexity, used focused ion beam system costliness is unfavorable for large-scale production.(2) reaction particle bundle etching: optionally plate mask at quartz surfaces, utilize SF 6+ O 2Perhaps Cl 2+ HBr etc. have corrosive particle beams etching, the removal that is corroded of uncoated quartz.The inherent defect of this method is that machining accuracy is low, and reaction rate is low, and poisonous, harmful material such as fluorine, chlorine is arranged in process, diminishes operating personnel's health, and contaminated environment.(3) lithography: utilize steps such as template, resist coating, preceding baking, exposure, development, back baking that the structure graph of micro-nano device is transmitted to the single crystal quartz surface, utilize not gluing zone of HF acid solution chemical attack again, the processing of removing photoresist then finally processes the structure corresponding with template at quartz surfaces.The method process complexity, each step all influences final precision.Simultaneously, HF acid has volatility, and is harmful.Photoresist can come off in HF acid for a long time, causes the zone of the corresponding protection of HF acid to produce corrosion.If need the multistage ledge structure of processing, then need repeated multiple times to use template, repeat corrosion, the template of each time is difficult to realize nano level accurate location, makes it be difficult to be applied to the processing of multistage ledge structure.Equally, other above-mentioned method also is applied to plane processing more, is difficult to process structures such as slope.
In recent years, the scanning probe microscopy that comprises AFM is applied to the nanoprocessing field gradually.At present, conventional scanning probe microscopy machining process is to utilize the direct cutting material of scan-probe cutter, and material is removed.The method certainly will produce a large amount of abrasive dusts, and is also very serious to the wearing and tearing of scan-probe.In addition, the edge of materials after the cutting can produce serious plastic deformation, influences the character of material.Can utilize the original position anodizing at conductor or semiconductor surface processing mask based on the anodizing of AFM, in conjunction with chemical attack, can process nanostructured, but the method can't be applied to insulator surfaces such as quartz.However, because AFM has advantages such as multi-functional, high accuracy, be highly suitable for the nanoprocessing field.Therefore, at the growth requirement of quartzy micro element processing, need badly exploitation a kind of based on AFM simple, accurately, the nanoscale single crystal quartz processing method of cleaning.
Summary of the invention
The purpose of this invention is to provide a kind of single crystal quartz surface selectivity lithographic method based on friction induction, this method can etching process the micro/nano level structure on single crystal quartz, be a kind of simple, accurately, the single crystal quartz micro nano structure processing method of cleaning; It need not mask, and the single corrosion can process nanoscale structures such as multistage step, inclined-plane on single crystal quartz.
The present invention is for solving its goal of the invention, and the technical scheme that is adopted is:
A kind of single crystal quartz surface selectivity lithographic method based on friction induction, its concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform, start AFM, apply to probe and to decide load F, perhaps varying load F ', and probe is scanned on the single crystal quartz surface along track and the cycle-index set, adding the man-hour sweep speed is 6-20 μ m/s;
The theoretical critical fire area load value F that destroys takes place during for the single crystal quartz Surface Machining that calculates according to the hertz contact formula in described value of deciding load F y0.03-0.14 doubly;
The theoretical critical fire area load value F that destroys takes place during for the single crystal quartz Surface Machining that calculates according to the hertz contact formula in the excursion of described varying load F ' y0.03-0.14 doubly;
It is 15~25% KOH solution that B, the single crystal quartz after will scanning place mass concentration, and corrosion got final product more than 2.5 hours.
Mechanism of the present invention and process are: quartzy top layer is in the exerting pressure of probe, scanning process, and the direct stress of vertical direction and the shearing stress of horizontal direction induce the single crystal quartz top layer that inelastic deformation takes place, and makes quartzy lattice take place to destroy and distortion.Induce the quartz areas after the deformation to produce the chemical attack effect with potassium hydroxide, the quartz areas that does not produce deformation then can not produce the chemical attack effect with potassium hydroxide, thereby single crystal quartz is soaked in the potassium hydroxide solution and can etches the corresponding groove structure in scanned zone.
Compared with prior art, the advantage that has of the present invention is:
One, the present invention does not need extra electric field, does not need specially treated is carried out on the single crystal quartz surface.Compare with machine cut, required load is minimum, and is little to the single crystal quartz surface damage, also less relatively to the wearing and tearing of needle point.And oxidation reaction (quartz has been a stable oxide) does not take place in the scanning process, do not introduce impurity, do not change the chemical composition of material, the roughness of material initial surface changes also little before and after the corrosion.
Two, adopt repeatedly scanning, the area of each scanning is not exclusively overlapping, because the scanning times of zones of different is different, can make quartzy top layer generation inelastic deformation in various degree, the zone that scanning times is many more, its variation is dark more, again through corrosion, can etch the different step-like micro-nano groove structure of the degree of depth at different levels easily at last.Because during each time scanning, probe is fixedly mounted on the AFM all the time, probe is not subjected to displacement, and guarantee accurately resetting of AFM, and the KOH corrosion process is finished once, without any need for mask, therefore, can accurately etch multistage ledge structure, than mask and corrosion repeatedly repeatedly, its working (machining) efficiency obviously improves, and the etching shape is more accurately controlled.
Three, adopt the varying load scan mode, because the scanning load that different single crystal quartz surface zones of different is subjected to is inconsistent, the inelastic deformation degree varies that takes place in its top layer causes, the place that load is big more, the distortion Shaoxing opera of its generation is strong, thereby can process the ramped shaped structure that prior art is difficult to process easily.
Four, in scanning, have only the regional top layer that has produced inelastic deformation just can be eroded fully, the crystal region top layer that does not produce inelastic deformation then can not be corroded; Therefore, the long-time stable existence of the micro nano structure that processing obtains energy in etchant solutions such as KOH has good anti-corrosion and stability.
Five, process can realize under normal temperature, atmospheric pressure environment, does not need particular surroundings such as vacuum, constant temperature, constant humidity, is easy to processing, and processing cost is low.And the corrosive agent KOH in the corrosion process is easy to obtain, and does not need the concentration of corrosive agent is accurately set.The mass concentration of rough preparation has also greatly reduced operation easier and cost for the KOH of 15%-25% can provide quartz reaction after enough hydroxide ion and the delineation.
Six, based on the multifunctionality of AFM, after machining, the spherical crown shape probe of processing usefulness is taken off, and processed single crystal quartz is motionless, the silicon nitride probe that replacing is exclusively used in the prong shape of scanning pattern carries out pattern scanning, can directly obtain the in-situ three-dimensional pattern of institute's processing structure.If processing result does not meet the demands, can carry out accurate original position reparation processing again, until being processed into certified products.After the test by small amount of sample, can accurately set machined parameters, carry out large batch of high accuracy processing.Less wastage in the process, the qualification rate height.
The track while scan of above-mentioned probe is face scanning, and the cycle-index of scanning is for once.Like this, can process easily and etch the micro/nano level groove structure.
The track while scan of above-mentioned probe is face scanning, and the cycle-index of scanning is more than 2 times, and back time scanning is littler than the area of last time scanning, but scanning center's unanimity.Like this, can process interior dark, the outer shallow micro-nano groove structure of multistage step.
The track while scan of above-mentioned probe is face scanning, and the cycle-index of scanning is more than 2 times, and the area of each time scanning is identical, and scanning center is inconsistent.Like this, can process a plurality of overlapping or nonoverlapping a plurality of micro/nano level groove structures; When two groove structures are close, also can think between two groove structures, to have processed the bulge-structure of a strip.
The present invention is described in further detail below in conjunction with accompanying drawing and concrete embodiment.
Description of drawings
Fig. 1 is in the method for the embodiment of the invention one, and processed single crystal quartz surface is at the shape appearance figure in each stage.Wherein, the silicon nitride probe scanning shape appearance figure when A, B, C, D, E component etching time are respectively 0h (not corrosion after the scanning processing), 0.5h, 1h, 2h, 3h, a, b, c, d, e component then are respectively the profile diagram of A, B, C, D, E component.
Fig. 2 is in the method for the embodiment of the invention two, and processed single crystal quartz surface is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component are respectively the forward and backward silicon nitride probe scanning shape appearance figure of corrosion, and a, b component then are respectively the profile diagram of A, B component.
Fig. 3 is in the method for the embodiment of the invention three, and processed single crystal quartz surface is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component are respectively the forward and backward silicon nitride probe scanning shape appearance figure of corrosion, and a, b component then are respectively the profile diagram of A, B component.
Fig. 4 is in the method for the embodiment of the invention three, and the corrosion depth on inclined-plane is with the rule of load change.
Fig. 5 is in the method for the embodiment of the invention four, and processed single crystal quartz surface is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component are respectively the forward and backward silicon nitride probe scanning shape appearance figure of corrosion, and a, b component then are respectively the profile diagram of A, B component.
Fig. 6 is in the method for the embodiment of the invention five, and processed single crystal quartz surface is being corroded forward and backward and machined the shape appearance figure that corrosion is continued in the back.Wherein, A, B, C, D component etching time are respectively the silicon nitride probe scanning shape appearance figure of 0h (not corrosion after the scanning processing), 2.5h (etch also and promptly machine), 5h (corroding again after machining 2.5 hours), 7.5h (corroding again after machining 5 hours), and a, b, c, d component then are respectively the profile diagram of A, B, C, D component.
Fig. 7 is in the method for the embodiment of the invention six, and processed single crystal quartz surface is at the shape appearance figure in each stage.Wherein, the silicon nitride probe scanning shape appearance figure when A, B, C component etching time are respectively 0h (not corrosion after the scanning processing), 3.5h, 5h, a, b, c component then are respectively the profile diagram of A, B, C component.
The specific embodiment
Embodiment one
A kind of specific embodiment of the present invention is, a kind of single crystal quartz surface selectivity lithographic method based on friction induction, and its concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform of AFM, start AFM, apply to probe and to decide load F, and probe is scanned on the single crystal quartz surface along track and the cycle-index set, adding the man-hour sweep speed is 12 μ m/s.
The value of deciding load F of this example is 5 μ N, and the theoretical critical fire area load value F that destroys takes place when it is the single crystal quartz Surface Machining that calculates according to the hertz contact formula y0.047 times of=106 μ N.
Processed single crystal quartz is specially X-cut type single crystal quartz, and employed spherical crown shape probe is the diamond probe, because single crystal quartz (X-cut) and adamantine elastic modelling quantity are respectively 78.3GPa and 1141GPa, Poisson's ratio is respectively 0.17 and 0.07; The yield limit of single crystal quartz is 8.4GPa.The coefficient of friction on diamond needle point and single crystal quartz surface is 0.26.Under this routine slip scan contact mode, the corresponding critical load F of surrender takes place in single crystal quartz yBe 106 μ N as calculated.
It is 20% KOH solution that B, the single crystal quartz after will scanning place mass concentration, corrodes 3 hours, can obtain the micro/nano level groove structure of single crystal quartz.
The track while scan of the probe that this is routine is face scanning, and the cycle-index of scanning is for once.Concrete scan area during face scanning is 3 μ m * 3 μ m.
Fig. 1 is the shape appearance figure of the processed single crystal quartz surface of present embodiment in each stage.Wherein, the silicon nitride probe scanning shape appearance figure when A, B, C, D, E component etching time are respectively 0h (not corrosion after the scanning processing), 0.5h, 1h, 2h, 3h, a, b, c, d, e component then are respectively the profile diagram of A, B, C, D, E component.
Can obtain from Fig. 1, along with the growth of etching time, corrosion depth increases gradually and tends towards stability, and the degree of depth no longer changes after 2 hours, and the height of the micro/nano level groove structure step that forms is 1.1nm.From C, the c of Fig. 1, D, d, E, e component, can find that scanning area does not have significant change, illustrate that this process optionally occurs in the scanned zone of diamond needle point, does not influence the structure of other position on the single crystal quartz initial surface.
Embodiment two
This routine concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform of AFM, start AFM, apply to probe and to decide load F, and probe is scanned on the single crystal quartz surface along track and the cycle-index set.
The value of deciding load F of this example is 8 μ N, and the theoretical critical fire area load value F that destroys takes place when it is the single crystal quartz Surface Machining that calculates according to the hertz contact formula y0.075 times of=106 μ N.
The material type of the single crystal quartz that this example is processed and employed spherical crown shape probe and embodiment one are just the same, and therefore, the corresponding critical load F of surrender takes place its single crystal quartz yAlso be 106 μ N.
It is 15% KOH solution that B, the single crystal quartz after will scanning place mass concentration, corrodes 3 hours, gets final product.
The track while scan of the probe that this is routine is face scanning, and the cycle-index of scanning is 3 times, and back time scanning is littler than the area of last time scanning, but scanning center's unanimity.Concrete scan area during face scanning for the first time is 5 μ m * 5 μ m, and sweep speed is 20 μ m/s; Scanning in zone line 3 μ m * 3 mu m ranges of face scanning carrying out for the second time, sweep speed is 12 μ m/s; Carry out the scanning in center 1.5 μ m * 1.5 μ m zones for the third time again, sweep speed is 6 μ m/s.This routine this scanning center is constant, and the scanning that scan area diminishes one by one can be described as embedded scanning.
Adopt this routine scan mode can form multistage stepped recesses structure on the single crystal quartz surface at last:
Fig. 2 is that the processed single crystal quartz surface of present embodiment is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component are respectively the forward and backward silicon nitride probe scanning shape appearance figure of corrosion, and a, b component then are respectively the profile diagram of A, B component.
From the B of Fig. 2, b component as can be seen, the example method processing back has formed three grades of stepped recesses structures of micro/nano level on the single crystal quartz top layer, be reference with the initial surface, and three grades of steps absolute depth from outside to inside are respectively 2nm, 4nm, 5.2nm; Three grades of steps relative depth from outside to inside are respectively 2nm, 2nm and 1.2nm; As seen, under the constant situation of load, along with the increase of scanning times, the corrosion depth of single crystal quartz constantly increases.
Embodiment three
This routine concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform of AFM, start AFM, apply varying load F ' to probe, and probe is scanned on the single crystal quartz surface along track and the cycle-index set, the sweep speed that adds man-hour is 12 μ m/s.
The theoretical critical fire area load value F that destroys when being the single crystal quartz Surface Machining that calculates according to the hertz contact formula, the excursion of the varying load F ' that this is routine takes place yThe 0.03-0.14 of (106 μ N) also is the excursion 3.2 μ N-15 μ N of varying load F ' doubly.
The material type of the single crystal quartz that this example is processed and employed spherical crown shape probe and embodiment one are just the same, and therefore, the corresponding critical load F of surrender takes place its single crystal quartz yAlso be 106 μ N.
In this example, from small to large unidirectional of being changed to of varying load F ' once changes, and is even variation (promptly the variable quantity at constituent parts varying load F ' in the time is identical).
It is 20% KOH solution that B, the single crystal quartz after will scanning place mass concentration, corrodes 3 hours, gets final product.
The track while scan of the probe that this is routine is face scanning, and the cycle-index of scanning is for once.Concrete scan area during face scanning is 3 μ m * 3 μ m.
Adopt this routine variable load scan method can process the inclined plane groove structure:
Fig. 3 is in this routine method, and processed single crystal quartz surface is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component corrode forward and backward silicon nitride probe scanning shape appearance figure respectively, and a, b component then are respectively the profile diagram of A, B component.
Fig. 4 is that the corrosion depth on inclined-plane is with the rule of load change in this routine method.Can find that from Fig. 4 along with the even increase of load, the degree of depth after the corrosion increases gradually, the increment rate of the degree of depth is slowed down gradually, and when load was 15 μ N, corrosion depth reached 2.5nm, and the change in depth rate is very slow.The scanning of variable load face can form the inclined plane groove structure on single crystal quartz.
Certainly, when implementing, the variation of varying load also can be in the single pass process, and change direction is two-way, and is promptly earlier big from little change, again from diminishing greatly, even a plurality of two-way circulation, the variable of varying load also not necessarily is even variation.Like this, both can process the slope groove structure of undaform, or the inconsistent groove structure of slope everywhere.
Embodiment four
The concrete practice of this example is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform of AFM, start AFM, apply to probe and to decide load F, and probe is scanned on the single crystal quartz surface along track and the cycle-index set, the sweep speed that adds man-hour is 12 μ m/s.
The value of deciding load F of this example is 3.2 μ N, and the theoretical critical fire area load value F that destroys takes place when it is the single crystal quartz Surface Machining that calculates according to the hertz contact formula y0.03 times of=106 μ N.
The material type of the single crystal quartz that this example is processed and employed spherical crown shape probe and embodiment one are just the same, and therefore, the corresponding critical load F of surrender takes place its single crystal quartz yAlso be 106 μ N.
It is 25% KOH solution that B, the single crystal quartz after will scanning place mass concentration, corrodes 3 hours, gets final product.
The track while scan of the probe that this is routine is face scanning, and the cycle-index of scanning is 2 times, and the area of each time scanning is identical, and scanning center is inconsistent.The area of twice scanning of this example all is 3 μ m * 3 μ m, finish scanning for the first time after, scanning center carries out scanning second time to right translation 3.6 μ m, thereby forms the groove structure of two 3 μ m * 3 μ m, then forms the strip bulge structure between these two grooves.Twice sweep speed is 12 μ m/s.
Fig. 5 is in this routine method, and processed single crystal quartz surface is at the forward and backward shape appearance figure of corrosion.Wherein, A, B component are respectively the forward and backward silicon nitride probe scanning shape appearance figure of corrosion, and a, b component then are respectively the profile diagram of A, B component.
As can be seen from Figure 5, the example method has then formed a strip bulge structure at the groove structure of two 3 μ m * 3 μ m of single crystal quartz Surface Machining formation between these two grooves.The length of strip bulge structure is 3 μ m, and width is 0.6 μ m, height 0.8nm.
Embodiment five
This routine concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform of AFM, start AFM, apply to probe and to decide load F, and probe is scanned on the single crystal quartz surface along track and the cycle-index set;
The value of deciding load F of this example is 6 μ N, and the theoretical critical fire area load value F that destroys takes place when it is the single crystal quartz Surface Machining that calculates according to the hertz contact formula y0.057 times of=106 μ N.
The material type of the single crystal quartz that this example is processed and employed spherical crown shape probe and embodiment one are just the same, and therefore, the corresponding critical load F of surrender takes place its single crystal quartz yAlso be 106 μ N.
It is 20% KOH solution that B, the single crystal quartz after will scanning place mass concentration, corrodes 2.5 hours, gets final product.
The track while scan of the probe that this is routine is face scanning, and the cycle-index of scanning is 2 times, and back time scanning is littler than the area of last time scanning, but scanning center's unanimity.Concrete scan area during face scanning for the first time is 4 μ m * 4 μ m, and sweep speed is 16 μ m/s; Scanning in zone line 1.5 μ m * 1.5 mu m ranges of face scanning carrying out for the second time, sweep speed is 6 μ m/s.
Adopt this routine scan mode can form two-stage stepped recesses structure on the single crystal quartz surface at last:
Fig. 6 is in this routine method, and processed single crystal quartz surface is being corroded forward and backward and machined the shape appearance figure that back continuation corrosion obtains.Wherein, A, B, C, D component etching time are respectively the silicon nitride probe scanning shape appearance figure of 0h (not corrosion after the scanning processing), 2.5h (etch also and promptly machine), 5h (corroding again after machining 2.5 hours), 7.5h (corroding again after machining 5 hours), and a, b, c, d component then are respectively the profile diagram of A, B, C, D component.A from Fig. 6, a, B, b component as can be seen, the height that this routine method is processed to form on single crystal quartz is that 1.7nm, area are 1.5 μ m * 1.5 μ m and is that highly 0.8nm, area are two steps that the center is overlapping of 4 μ m * 4 μ m.
It can also be seen that from C, c, D, the d component of Fig. 6, proceed corrosion after machining again, its probe shape appearance figure and corresponding profile diagram do not have significant change.Illustrate the structure that obtains of processing for a long time stable existence in corrosive agent, confirm the decay resistance that structure that the method processing obtains has excellence.Therefore, when corrosion processing is carried out in other zone of together individual sample, can not influence the stability of original structure, this superiority helps repeatedly processing, and repairs processing.
Embodiment six
The practice that this is routine and embodiment one are basic identical, and different only is: the value of deciding load F that applies to probe is 15 μ N, and the theoretical critical fire area load value F that destroys takes place when it is the single crystal quartz Surface Machining that calculates according to the hertz contact formula y0.14 times of=106 μ N; The mass concentration of KOH is 18% during corrosion.
Fig. 7 is in this routine method, and processed single crystal quartz surface is at the shape appearance figure in each stage.Wherein, the silicon nitride probe scanning shape appearance figure when A, B, C component etching time are respectively 0h (not corrosion after the scanning processing), 3.5h, 5h, a, b, c component then are respectively the profile diagram of A, B, C component.As can be seen, the degree of depth that corrosion 3.5h is processed to form on single crystal quartz is that 2.5nm, area are the one-level step of 3 μ m * 3 μ m in B from Fig. 7, the b component.As can be seen, continue corrosion 1.5 hours from C, c component, etching time reaches 5 hours, and the ledge structure degree of depth remains unchanged, and is 2.5nm.
Etching time of the present invention, can determine concrete etching time with the variation tendency of etching time according to corrosion depth in actual applications, it is the time point that the degree of depth no longer changes, but as long as etching time reaches 2.5 hours, corrosion completely just can take place substantially, corrodes and can guarantee in 3 hours to have taken place to corrode completely; Though also can carry out the corrosion of more time, also inessential.
The above-mentioned specific embodiment shows, by control load, sweep limits, scan mode and number of times, this method can show and process various nanostructureds that the structure after the processing has excellent corrosion resistance and stability at quartz.Experiment showed, that corrosion depth becomes positive correlation with load, scanning times.The slope on inclined-plane is relevant with variable load speed.Can set machined parameters according to concrete condition in the practical application.

Claims (4)

1. single crystal quartz surface selectivity lithographic method based on friction induction, its concrete operation method is:
A, be that the probe of spherical crown shape is installed on the AFM with the tip, the single crystal quartz of cleaning is fixed on the sample platform, start AFM, apply to probe and to decide load F, perhaps varying load F ', and probe is scanned on the single crystal quartz surface along track and the cycle-index set, adding the man-hour sweep speed is 6-20 μ m/s;
The theoretical critical fire area load value F that destroys takes place during for the single crystal quartz Surface Machining that calculates according to the hertz contact formula in described value of deciding load F y0.03-0.14 doubly;
The theoretical critical fire area load value F that destroys takes place during for the single crystal quartz Surface Machining that calculates according to the hertz contact formula in the excursion of described varying load F ' y0.03-0.14 doubly;
It is 15~25% KOH solution that B, the single crystal quartz after will scanning place mass concentration, and corrosion got final product more than 2.5 hours.
2. a kind of single crystal quartz surface selectivity lithographic method based on friction induction according to claim 1 is characterized in that: the track while scan of described probe is face scanning, and the cycle-index of scanning is for once.
3. a kind of single crystal quartz surface selectivity lithographic method according to claim 1 based on friction induction, it is characterized in that: the track while scan of described probe is face scanning, the cycle-index of scanning is more than 2 times, and back time scanning is littler than the area of last time scanning, but scanning center's unanimity.
4. a kind of single crystal quartz surface selectivity lithographic method according to claim 1 based on friction induction, it is characterized in that: the track while scan of described probe is face scanning, the cycle-index of scanning is more than 2 times, and the area of each time scanning is identical, and scanning center is inconsistent.
CN2010102223824A 2010-07-09 2010-07-09 Friction induction-based single crystal quartz surface selective etching method Expired - Fee Related CN101973507B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010102223824A CN101973507B (en) 2010-07-09 2010-07-09 Friction induction-based single crystal quartz surface selective etching method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102223824A CN101973507B (en) 2010-07-09 2010-07-09 Friction induction-based single crystal quartz surface selective etching method

Publications (2)

Publication Number Publication Date
CN101973507A true CN101973507A (en) 2011-02-16
CN101973507B CN101973507B (en) 2012-07-11

Family

ID=43573423

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010102223824A Expired - Fee Related CN101973507B (en) 2010-07-09 2010-07-09 Friction induction-based single crystal quartz surface selective etching method

Country Status (1)

Country Link
CN (1) CN101973507B (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503155A (en) * 2011-12-01 2012-06-20 西南交通大学 Glass surface nanofabrication method based on friction-induced selective etching
CN102730631A (en) * 2012-07-10 2012-10-17 西南交通大学 Method for texturing large-area silicon surface in multipoint contact mode
CN102736410A (en) * 2012-07-10 2012-10-17 西南交通大学 Method for machining large-area nanoimprint silicon die under multi-point contact mode
CN103738911A (en) * 2013-12-27 2014-04-23 西南交通大学 Gallium arsenide surface micro/nano machining method based on friction-induced selectivity 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
CN104034296A (en) * 2014-06-30 2014-09-10 西南交通大学 Detection method for thickness of monocrystalline silicon surface scratch damaged layer
CN109179314A (en) * 2018-10-24 2019-01-11 西南交通大学 Based on hydrofluoric acid/nitric acid mixed solution friction induction nanoprocessing method
CN109437085A (en) * 2018-10-25 2019-03-08 西南交通大学 A kind of not damaged friction induction nanoprocessing method
CN114758942A (en) * 2022-03-24 2022-07-15 中国科学院光电技术研究所 Reactive ion etching mask

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101549853A (en) * 2009-05-13 2009-10-07 西南交通大学 Processing method for constructing nano projection structure on surface of single crystal silicon based on friction induction
CN101723318A (en) * 2009-12-03 2010-06-09 西南交通大学 Micro-nano manufacturing method for surfaces of quartz and glass materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101549853A (en) * 2009-05-13 2009-10-07 西南交通大学 Processing method for constructing nano projection structure on surface of single crystal silicon based on friction induction
CN101723318A (en) * 2009-12-03 2010-06-09 西南交通大学 Micro-nano manufacturing method for surfaces of quartz and glass materials

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《农业机械学报》 20070831 蒋洪奎等 基于AFM的纳米机械刻蚀加工研究 第205-207页 1-4 第38卷, 第8期 2 *
《黑龙江大学自然科学学报》 20060630 袁福龙等 利用AFM和碱溶液在单晶硅表面微加工及其电化学机理 "1 实验部分","2 结构和讨论" 1-4 第23卷, 第3期 2 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503155A (en) * 2011-12-01 2012-06-20 西南交通大学 Glass surface nanofabrication method based on friction-induced selective etching
CN102730631B (en) * 2012-07-10 2015-05-20 西南交通大学 Method for texturing large-area silicon surface in multipoint contact mode
CN102730631A (en) * 2012-07-10 2012-10-17 西南交通大学 Method for texturing large-area silicon surface in multipoint contact mode
CN102736410A (en) * 2012-07-10 2012-10-17 西南交通大学 Method for machining large-area nanoimprint silicon die under multi-point contact mode
CN102736410B (en) * 2012-07-10 2013-12-11 西南交通大学 Method for machining large-area nanoimprint silicon die under multi-point contact mode
CN103738911B (en) * 2013-12-27 2016-03-02 西南交通大学 Based on the gallium arsenide surface micro-nano manufacturing method of friction induction selective etch
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
CN103803484B (en) * 2013-12-27 2016-02-03 西南交通大学 Based on the silicon nitride film/silicon micro-nano processing method of friction induction selective etch
CN103738911A (en) * 2013-12-27 2014-04-23 西南交通大学 Gallium arsenide surface micro/nano machining method based on friction-induced selectivity etching
CN104034296A (en) * 2014-06-30 2014-09-10 西南交通大学 Detection method for thickness of monocrystalline silicon surface scratch damaged layer
CN109179314A (en) * 2018-10-24 2019-01-11 西南交通大学 Based on hydrofluoric acid/nitric acid mixed solution friction induction nanoprocessing method
CN109437085A (en) * 2018-10-25 2019-03-08 西南交通大学 A kind of not damaged friction induction nanoprocessing method
CN114758942A (en) * 2022-03-24 2022-07-15 中国科学院光电技术研究所 Reactive ion etching mask
CN114758942B (en) * 2022-03-24 2023-05-30 中国科学院光电技术研究所 Reactive ion etching mask

Also Published As

Publication number Publication date
CN101973507B (en) 2012-07-11

Similar Documents

Publication Publication Date Title
CN101973507B (en) Friction induction-based single crystal quartz surface selective etching method
CN103449731B (en) A kind of method promoting fused quartz optical component damage threshold
EP2202208A1 (en) Glass substrate and method for manufacturing the same
Zheng et al. A novel wet etching process of Pb (Zr, Ti) O3 thin films for applications in microelectromechanical system
EP2161612A1 (en) Display and its manufacturing method
CN104498957A (en) Preparation method of super-hydrophobic micro-nano structure on titanium alloy surface
Rouhi et al. Optimisation of nanooxide mask fabricated by atomic force microscopy nanolithography: a response surface methodology application
Larsen et al. Investigations of the isotropic etch of an ICP source for silicon microlens mold fabrication
JP2007119290A (en) Method for manufacturing glass strip
Wu et al. Toward controllable wet etching of monocrystalline silicon: roles of mechanically driven defects
Vos et al. Silicon nano-pillar test structures for quantitative evaluation of wafer drying induced pattern collapse
CN101549853A (en) Processing method for constructing nano projection structure on surface of single crystal silicon based on friction induction
CN102007394A (en) Etching composition, in particular for strained or stressed silicon materials, method for characterizing defects on surfaces of such materials and process of treating such surfaces with the etching composition
Woo et al. Critical bending radius of thin single-crystalline silicon with dome and pyramid surface texturing
Wu et al. Tuning the plasma etching mode for the atomic-scale smoothing of single-crystal silicon
TW201544577A (en) Composition and method for healing glass, and glass treated with the composition
CN102503155B (en) A kind of glass surface nanoprocessing method based on friction induction selective etch
CN110526203A (en) Method based on the quasi- three-dimensional micro-nano structure of AFM write-through stress-electric coupling lithography
CN103803484A (en) Silicon nitride film/silicon micro-nano processing method based on friction-induced selective etching
CN103738912B (en) Based on the monocrystalline silicon surface non-destructive nano processing method of tribochemistry induction etching
CN101723318B (en) Micro-nano manufacturing method for surfaces of quartz and glass materials
CN106744671A (en) A kind of monocrystalline silicon surface nanoprocessing method based on UV ozone
JP2016521593A (en) Method for marking material, system for marking material, and material marked by the method
Liu et al. Corrosion mechanism and surface passivation strategies of polycrystalline silicon electrodes
CN112071740A (en) Method for preparing silicon carbide structure by picosecond laser irradiation

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20120711

Termination date: 20180709

CF01 Termination of patent right due to non-payment of annual fee