CN108821230A - A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation- - Google Patents
A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation- Download PDFInfo
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- CN108821230A CN108821230A CN201810659326.3A CN201810659326A CN108821230A CN 108821230 A CN108821230 A CN 108821230A CN 201810659326 A CN201810659326 A CN 201810659326A CN 108821230 A CN108821230 A CN 108821230A
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- anodic oxidation
- nano structure
- monocrystalline silicon
- processing method
- lossless
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00388—Etch mask forming
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00539—Wet etching
Abstract
The invention discloses a kind of lossless micro-nano structure processing methods secondarily etched based on anodic oxidation-, include the following steps:S1, monocrystalline silicon (100) substrate surface is subjected to oxide layer removal processing, then its surface is cleaned;S2, using atomic force microscope probe, one layer of oxide film pattern is processed on monocrystalline silicon (100) substrate surface by anodic oxidation as exposure mask;S3, monocrystalline silicon (100) substrate surface is performed etching using TMAH solution, obtains required nanostructure;S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using HF solution, to completely remove oxide film, lossless micro-nano structure needed for obtaining.This method is easy to operate, flexible, efficient, low in cost, the substrat structure processed using this method, compared to the light transmissive substrate of other epitaxial growths, has the characteristics that not damage substrate.
Description
Technical field
The invention belongs to semiconductor processing technology fields, and in particular to a kind of based on secondarily etched lossless of anodic oxidation-
Micro-nano structure processing method.
Background technique
It is important how to realize that the substrate texture of high quality has in technical field of micro and nano fabrication especially optics display field
Meaning.Molecule epitaxial growth or the method for vapor deposition are to realize the important channel of high-performance optical display device.Due to
Some optical materials are expensive, need to answer in substrate material surface using molecule epitaxial growth or gas phase deposition technology come sedimentary facies
Optical material, such as monocrystalline substrate surface deposit GaN.In optical material epitaxial process, substrate material surface
Defect will be transferred to epitaxial layer, be unfavorable for the promotion of optical device performance.Studies have shown that through texturing treated lining
Bottom can effectively weaken the generation of this growth defect;Further, lossless texture (damage without lattice by the structure that texture is included
Wound), it is not only avoided that epitaxial growth defect, more can utmostly improve device light emitting efficiency.Therefore, lossless substrate knot is realized
The processing of structure is particularly important.
It is expected to process lossless substrate texture based on the secondarily etched processing method of anodic oxidation-, which knits
Structure can be used as the epitaxial growth substrate of optical material.It is (thin for forming perfect extension lattice material since it is not damaged
Film), to having vital effect in the luminescent devices such as following process high efficiency laser, LED.Anodic oxidation-secondary quarter
Erosion has high efficiency, low cost, undamaged advantage, can be used as a kind of new method for processing lossless substrat structure.
Summary of the invention
Present invention aim to address the above problems, provide a kind of lossless micro-nano knot secondarily etched based on anodic oxidation-
Structure processing method, the processing method are capable of processing the not damaged substrate that can be used as grown epitaxial layer.
In order to solve the above technical problems, the technical scheme is that:One kind is secondarily etched lossless micro- based on anodic oxidation-
The processing method of micro-nano structure, includes the following steps:
S1, monocrystalline silicon (100) substrate surface is subjected to oxide layer removal processing, then its surface is cleaned;
S2, using atomic force microscope probe, one layer of oxygen is processed on monocrystalline silicon (100) substrate surface by anodic oxidation
Change film figure as exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using TMAH solution, obtains required nanostructure;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using HF solution, to completely remove oxidation
Film, lossless micro-nano structure needed for obtaining.
In above-mentioned technical proposal, in the step S1, hydrofluoric acid (HF) solution etches monocrystalline silicon of preferred mass concentration 5%
(100) substrate surface 5min, then monocrystalline silicon (100) substrate surface is cleaned using dehydrated alcohol and secondary deionized water,
Scavenging period is 5min.In the present invention, the purpose for using HF solution to perform etching monocrystalline silicon (100) substrate is to remove
The natural oxidizing layer on its surface, and using the purpose of dehydrated alcohol and secondary deionized water is the net HF solution residual of cleaning, therefore,
Oxide layer removal processing is carried out to monocrystalline silicon (100) substrate surface, then its surface is cleaned, is not limited to the above method, it is all
Under thought guidance of the invention, other regular oxidation layer removal processing and cleaning way, also belong to this in this field of use
In invention protection scope.
In above-mentioned technical proposal, in the step S2, due under lower bias, the oxidation mask thickness of processing compared with
Low, the effect of exposure mask is poor;And bias it is excessively high when, the diameter for generating oxidation film can become larger.Therefore in the present invention, preferably in atomic force
The bias that the needle point of microscope probe applies is 0.5V~10V, further preferably 7V~9V.Relative humidity also has shadow to processing
It rings, the stability for keeping humidity is had to during anodic oxidation, excessive or too small will lead to processes the uneven of structure, excellent
Selecting humidity is 40%~70%, is further preferably 45%-55%.Further, since needle point scanning excessive velocities, will affect anode
The uniformity of the oxidation film generated is aoxidized, and then will affect the effect of exposure mask.In the present invention, the needle point of preferably processing oxidation film is fast
Degree is no more than 2 μm/s, further preferably 2 μm/s.
In above-mentioned technical proposal, in the step S3, tetramethylammonium hydroxide (TMAH) solution concentration is excessively high to be influenced whether
The roughness of etch rate and silicon face, and 25% TMAH solution is exactly the equalization point between rate and roughness.With quarter
The increase of time is lost, processed structure can collapse.Therefore in terms of the effect that processed structure is presented, preferred TMAH solution quality
Concentration is 25%, and etch period is 1min~8min, and within the scope of the etch period, the nanostructure height processed is with quarter
It loses the time and increases.Further, preferably etch period is 8min.Inventor tests discovery, when etch period is 8min, this
When can get maximum etching height, the shape and height of resulting nanostructure are most uniform.
In above-mentioned technical proposal, in the step S4, preferably HF concentration of polymer solution is 5%, etch period 5min.It needs
It is noted that being performed etching using HF solution to monocrystalline silicon (100) substrate by step S3 processing, its purpose is to complete
The oxidation film processed in full removal step S2, is solved with obtaining lossless nanometer.Therefore, it is normal that other in this field can also be used
The oxidation film minimizing technology of rule.It is all under the guidance of inventive concept, using other oxidation film removing methods of this field routine,
Also belong to protection scope of the present invention.
The principle of the present invention is described in detail below, further to show advantages of the present invention:The present invention first passes through
It presses certain positive bias, leads on sample (monocrystalline silicon (100) substrate) in the conductive pinpoint of atomic force microscope probe (AFM)
It crosses anodic oxidation and generates layer oxide film, which can be used as the exposure mask of subsequent etching;Then sample is placed in TAMH solution
Middle carry out selective etch has masked areas to highlight at this point, exposure mask peripheral region will be etched quickly;Finally, will be
Substrate after TMAH etching is put into HF solution, to remove oxide film dissolving.It is tested by the electric conductivity of AFM, if surface conductance situation
Unanimously, show that the surface texture of processing is undamaged.
The lossless micro-nano structure processing method secondarily etched based on anodic oxidation-provided by the invention has below beneficial to effect
Fruit:
1, the substrate texture processed using method provided by the invention, compared to the light transmissive substrate of other epitaxial growths,
Have the characteristics that not damage;
2, by the path of control atomic force microscope (AFM) probe tip, the figure of various needs can flexibly be processed
Case, strong applicability;
3, the TMAH solution in etching process and HF solution are readily available, and etching process is completed under room temperature, normal pressure, only need
Control etch period can be obtained certain etching height, and wet etching pollution is few, relative to other methods, etching at
This is lower, speed is fast, surface quality is high;
4, this method is when carrying out anodic oxidation, the facing when contact pressure between needle point and silicon wafer is surrendered much smaller than silicon wafer
Boundary's contact pressure will not damage silicon base.
Detailed description of the invention
Fig. 1 is that the present invention is based on the step processes of the secondarily etched not damaged micro-nano structure processing method of anodic oxidation-to show
It is intended to;
Fig. 2 be embodiment one process nano dot etched respectively in TMAH solution 0min (a), 2min (b), 6min (c),
Atomic force microscope shape appearance figure after 8min (d), 10min (e), 16min (f);
Fig. 3 is its height of nano dot of the processing of embodiment one with the increased variation diagram of etch period in TMAH solution;
Fig. 4 be embodiment two process nanostructure respectively in HF solution etch 0min (a), 3min (b), 5min (c),
Atomic force microscope shape appearance figure after 8min (d), 10min (e);
Fig. 5 is its height of nanostructure of the processing of embodiment two with the increased variation diagram of etch period in HF solution;
Fig. 6 is embodiment three respectively by the original of step S2 (a), step S3 (b), step S4 (c) nanostructure processed
Sub- force microscope shape appearance figure and current graph;
Fig. 7 is using the present invention is based on the processing methods of the secondarily etched not damaged micro-nano structure of anodic oxidation-to prepare
The atomic force microscopy diagram of not damaged micro-nano structure.
Specific embodiment
The present invention is described further in the following with reference to the drawings and specific embodiments:
As shown in Figure 1, a kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation-of the invention, packet
Include following steps:
S1, HF solution etches monocrystalline silicon (100) substrate surface 5min using mass concentration 5% remove its surface oneself
Right oxide layer, then successively monocrystalline silicon (100) substrate surface is cleaned by ultrasonic using dehydrated alcohol and secondary deionized water, clearly
Washing the time is 5min;
S2, apply the bias of 0.5V~10V in the needle point of atomic force microscope probe, and control humidity 40%~
70%, stylus velocity is 2 μm/s, processes layer oxide film pattern work on monocrystalline silicon (100) substrate surface by anodic oxidation
For exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using the TMAH solution of mass concentration 25%, etch period is
1min~8min obtains required nanostructure;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using the HF solution of mass concentration 5%,
Etch period 5min, to remove oxide film dissolving, lossless micro-nano structure needed for obtaining.
After step S1~S4 processing, conductive pinpoint can be used, scanning speed is controlled in 1 μm/s hereinafter, carrying out
The electric conductivity of finished surface is tested.According to current graph it is found that the structure after HF removes removing oxide layer is with silicon substrate be as
, it be the structure of processing is undamaged.
As shown in fig. 7, being inventor by procedure of processing flow diagram shown in FIG. 1, using base provided by the invention
In the atom for the not damaged micro-nano structure pattern that the processing method of the secondarily etched lossless micro-nano structure of anodic oxidation-processes
Force microscope figure.The lossless substrate shown disclosure is particularly well suited to process high-performance optical.
Below by way of specific embodiment, the invention will be further described.
Embodiment one
A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation-of the present embodiment, including following step
Suddenly:
S1, HF solution etches monocrystalline silicon (100) substrate surface 5min using mass concentration 5% remove its surface oneself
Right oxide layer, then dehydrated alcohol and secondary deionized water is successively respectively adopted, ultrasound is carried out clearly to monocrystalline silicon (100) substrate surface
Wash 5min;
S2, atomic force microscope probe needle point application+7V bias, and control relative humidity be 50%, needle point speed
2 μm/s is spent, processes layer oxide film pattern on monocrystalline silicon (100) substrate surface by anodic oxidation as exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using the TMAH solution of mass concentration 25%, etch period point
Not Wei 0min, 2min, 6min, 8min, 10min, 16min, obtain required nano dot;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using the HF solution of mass concentration 5%,
Etch period is 5min, to remove oxide film dissolving, lossless micro-nano structure needed for obtaining.
As shown in Figure 2, it can be seen that in TMAH solution, the height and shape of the nano dot that different time points etches
Shape.
As shown in figure 3, after TMAH solution etches 8min, the shape of nanostructure is in contrast under this processing conditions
More preferably, height is also more suitable.
Embodiment two
A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation-of the present embodiment, including following step
Suddenly:
S1, HF solution etches monocrystalline silicon (100) substrate surface 5min using mass concentration 5% remove its surface oneself
Right oxide layer, then dehydrated alcohol and secondary deionized water is successively respectively adopted, ultrasound is carried out clearly to monocrystalline silicon (100) substrate surface
Wash 5min;
S2, atomic force microscope probe needle point application+7V bias, and control relative humidity be 50%, needle point speed
2 μm/s is spent, processes layer oxide film pattern on monocrystalline silicon (100) substrate surface by anodic oxidation as exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using the TMAH solution of mass concentration 25%, etch period
2min obtains required nanostructure;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using the HF solution of mass concentration 5%,
Etch period is respectively 0min, 3min, 5min, 8min, 10min, lossless micro-nano structure needed for obtaining.
As illustrated in figures 4-5, after 5% HF solution etches 5min, oxidation film has been completely removed, and can calculate oxygen
The thickness for changing film is about 4nm.
Embodiment three
A kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation-of the present embodiment, including following step
Suddenly:
S1, HF solution etches monocrystalline silicon (100) substrate surface 5min using mass concentration 5% remove its surface oneself
Right oxide layer, then dehydrated alcohol and secondary deionized water is successively respectively adopted, ultrasound is carried out clearly to monocrystalline silicon (100) substrate surface
Wash 5min;
S2, atomic force microscope probe needle point application+7V bias, and control relative humidity be 50%, needle point speed
2 μm/s is spent, processes layer oxide film pattern on monocrystalline silicon (100) substrate surface by anodic oxidation as exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using the TMAH solution of mass concentration 25%, etch period
2min obtains nanostructure;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using the HF solution of mass concentration 5%,
Etch period 5min, lossless micro-nano structure needed for obtaining.
It carries out sweeping conductive pattern using the conductive module of AFM, since scanning speed can have an impact its result, in order to obtain
More accurate data, scanning speed are set as 0.6 μm/s, and the bias of scanning is -2V.
As shown in fig. 6, after the HF solution etches 5min using 5%, it can be seen from current graph when electric current passes through,
Silicon base and the structure of processing are consistent, and without any otherness, show that the structure of processing is undamaged.
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 (9)
1. a kind of lossless micro-nano structure processing method secondarily etched based on anodic oxidation-, it is characterised in that:Including following step
Suddenly:
S1, monocrystalline silicon (100) substrate surface is subjected to oxide layer removal processing, then its surface is cleaned;
S2, using atomic force microscope probe, layer oxide film is processed on monocrystalline silicon (100) substrate surface by anodic oxidation
Pattern is as exposure mask;
S3, monocrystalline silicon (100) substrate surface is performed etching using TMAH solution, obtains required nanostructure;
S4, monocrystalline silicon (100) substrate by step S3 processing is performed etching using HF solution, to completely remove oxidation film,
Lossless micro-nano structure needed for obtaining.
2. the lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1, feature exist
In:In the step S2, apply the bias of 0.5V~10V on the needle point of atomic force microscope probe, controls humidity 40%
~70%, to process oxidation film no more than 2 μm/s needle point scanning speed.
3. the lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 2, feature exist
In:It is 7V~9V in the bias that the needle point of atomic force microscope probe applies, humid control is in 45%- in the step S2
55%.
4. the lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 2, feature exist
In:In the step S2, the 2 μm/s of stylus velocity of oxidation film is processed.
5. the lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1, feature exist
In:In the step S3, the TMAH solution mass concentration is 25%, and the etch period is 1min~8min.
6. -5 any lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1,
It is characterized in that:In the step S1, using HF solution etches monocrystalline silicon (100) substrate surface 5min of mass concentration 5%, to remove
Remove the natural oxidizing layer on its surface.
7. -5 any lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1,
It is characterized in that:In the step S1, successively monocrystalline silicon (100) substrate surface is carried out using dehydrated alcohol and secondary deionized water
Cleaning, scavenging period is 5min.
8. -5 any lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1,
It is characterized in that:HF concentration of polymer solution is 5% in the step S4.
9. -5 any lossless micro-nano structure processing method secondarily etched based on anodic oxidation-according to claim 1,
It is characterized in that:Etch period in the step S4 is 5min.
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