CN109399558A - Gallium arsenide surface nanoprocessing method based on photochemistry assisted selective etching - Google Patents
Gallium arsenide surface nanoprocessing method based on photochemistry assisted selective etching Download PDFInfo
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- CN109399558A CN109399558A CN201811343464.7A CN201811343464A CN109399558A CN 109399558 A CN109399558 A CN 109399558A CN 201811343464 A CN201811343464 A CN 201811343464A CN 109399558 A CN109399558 A CN 109399558A
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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
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/00492—Processes for surface micromachining not provided for in groups B81C1/0046 - B81C1/00484
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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
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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
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0156—Lithographic techniques
- B81C2201/0159—Lithographic techniques not provided for in B81C2201/0157
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Abstract
The invention discloses a kind of gallium arsenide surface nanoprocessing methods based on photochemistry assisted selective etching, comprising the following steps: S1, carries out scratch or impression processing in clean gallium arsenide surface using mechanical scratching or indentation equipment；S2, ultraviolet light chemistry auxiliary etch is carried out to gallium arsenide surface using mixing etching agent, gallium arsenide surface is cleaned after the completion of etching, obtains the gallium arsenide surface nanostructure of high quality.The processing method can be realized the processing of gallium arsenide surface random two-dimensional structure, be not necessarily to template, easy to operate, at low cost；Further, the process of this method carries out at normal temperatures and pressures, does not generate polluted gas, and the etching agent after processing is easy to handle；In addition, this method quickly can process the pattern and optical texture of high quality in gallium arsenide surface, compared with conventional etch, process velocity is fast, quality is high.
Description
Technical field
The invention belongs to GaAs Technology fields, and in particular to a kind of GaAs based on photochemistry assisted selective etching
Nano surface processing method.
Background technique
Due to the excellent photoelectric characteristic of GaAs (such as direct band gap and high electron mobility), it has been widely used in
Field of optoelectronic devices, such as solar battery, Schottky diode and photodetector.Under normal conditions, the work of device
Region has important meaning on surface, therefore in the nanoprocessing method of gallium arsenide surface development high-precision, high efficiency and low cost
Justice.
Currently, the typical micro-nano processing method of gallium arsenide surface include photoetching, nano impression, ion/electron beam lithography and
Photoetching (SPL) etc. based on scanning probe.The features such as SPL is due to its at low cost, easy to operate and strong flexibility, it has also become a kind of
Very attractive nanoprocessing method.In recent years, in conjunction with the scraping of scanning probe and wet etching, friction induction selective etch
Technology has been employed for the surface micronano processing of the materials such as GaAs, monocrystalline silicon and glass.For GaAs material, scrape
Residual compressive stress and the lattice densification that process generates are considered as resisting the principal element of selective etch.However, still needing
It further to improve etch rate and reduce surface roughness to realize the high quality processing of gallium arsenide surface, and it also requires
Further elucidate selective etch mechanism.Therefore, friction induction selective etch based on GaAs need further to explore and
Optimization.
It is worth noting that, the wet-etch rate of GaAs can assist greatly improving by ultraviolet (UV) light, this master
It is attributed to its internal photoelectric effect.Its specific principle are as follows: when being applied more than GaAs forbidden band during wet etching
When the illumination of the energy of width, etch rate can be obviously improved under the catalytic action of photoelectron-hole pair.In addition, photochemical
Learning etching has many advantages, such as that process time is short and etching surface is uniform, therefore it is possible to prevente effectively from high caused by traditional chemical etching
Surface roughness.
Although photochemistry etching has many advantages, such as etch rate fastly and etching is uniform, whether no stencil-chosen can be promoted
Property etching relative etch rate come realize rapid nano process, be still not clear at present.Proposed adoption photochemistry auxiliary choosing of the present invention
Selecting property lithographic method, the quick no templating nanoparticles processing for gallium arsenide surface.By the load of control scratch or impression, carve
The parameters such as time are lost, surface random two-dimensional pattern and the processing of high quality optical structure are fast implemented.
Summary of the invention
Present invention aim to address the above problems, provide a kind of arsenic based on photochemistry assisted selective etching principle
Quickly the nanoprocessing method without template, this method can improve gallium arsenide surface etching quality and improve etching efficiency on gallium surface.
The present invention is suitable for the random two-dimensional nanoscale structures of gallium arsenide surface and the processing of partial optical structure.
In order to solve the above technical problems, the technical scheme is that it is a kind of based on photochemistry assisted selective etching
Gallium arsenide surface nanoprocessing method, comprising the following steps:
S1, scratch or impression processing are carried out in clean gallium arsenide surface using mechanical scratching or indentation equipment；
S2, ultraviolet light chemistry auxiliary etch is carried out to gallium arsenide surface using mixing etching agent, to arsenic after the completion of etching
Gallium surface is cleaned, and gallium arsenide surface nanostructure is obtained.
In above-mentioned technical proposal, the ultraviolet light chemistry auxiliary etch refers to be performed etching under ultraviolet environments, in this hair
Employed in bright is the PSDP UV-8T type ultraviolet light chemistry auxiliary system of Novascan company, the U.S., and low pressure mercury lamp can
Launch wavelength is the ultraviolet light of 184.9nm and 253.7nm.It is worth noting that ultraviolet light chemistry auxiliary system has no special limit
System, can also be used other ultraviolet light chemistry auxiliary systems commonly used in the art.
In above-mentioned technical proposal, in the step S1, scratch is carried out using the Diamond tip of scanning probe microscopy and is added
Work, or impression processing is carried out using nano-hardness tester Bo Shi (Berkovich) pressure head.Diamond tip for scratch production
Tip curvature radius is 20nm-5 μm, and preferably 100nm-2 μm, nano-hardness tester impression processes preferred Berkovich diamond
Pressure head.
In above-mentioned technical proposal, in the step S2, the type and ratio for mixing etching agent directly affect selective quarter
Lose the roughness of rate and gallium arsenide surface.The mixing etching agent of preferably sulfuric acid and hydrogen peroxide of the present invention, volume ratio are as follows:
98%H2SO4: 30%H2O2: H2(98% and 30% respectively indicates H to O=1:0.5:1002SO4And H2O2Mass fraction；Following letter
Claim " 3H " solution), etching surface roughness is low under this mixed species and concentration, and Etch selectivity with higher ratio.With
The increase of selective etch time, etching height shows as gradually collapsing after first increasing, and photochemistry auxiliary etch
Structure is apparently higher than traditional chemical etching.From the experimental results, preferably etch period is 30s-20min, is further preferably carved
The erosion time is 5min-15min, and within the scope of the etch period, etching structure has biggish height and preferable quality.
In above-mentioned technical proposal, in the step S2, due to GaAs in etching process may adsorption reaction object or
Impurity needs to carry out surface cleaning processing to gallium arsenide film after processing.The preferred acetone of the present invention and dehydrated alcohol clean,
Successively it is cleaned by ultrasonic 3min in acetone and dehydrated alcohol first, then rinses gallium arsenide surface 10min with continuous deionized water.It needs
It is noted that being not limited to the above method to gallium arsenide surface cleaning treatment.It is all under thought guidance of the invention, with realize
The method of gallium arsenide surface cleaning is within the 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 exists first
Scratch (impression) processing is carried out on mechanical scoring device (scanning probe microscopy, nano impress/impression instrument), makes gallium arsenide surface
It deforms, which can be as the exposure mask of subsequent etching process.Then GaAs sample is immersed in mixing etching agent, and
Selective etch processing is carried out in photochemical system.Since that there are etch rates is poor for scored area and untreated areas, and produce
Raw photoelectron-hole is to further increasing selective etch speed difference, therefore compared to conventional etch, photochemistry auxiliary etch
The highly higher and preferable nanostructure of quality can be processed within a short period of time.
Gallium arsenide surface nanoprocessing method provided by the invention based on photochemistry assisted selective etching has following
The utility model has the advantages that
1, the processing method can be realized the processing of gallium arsenide surface random two-dimensional structure, be not necessarily to template, easy to operate, at
This is low；
2, the processing method is to carry out at normal temperatures and pressures in process, does not generate polluted gas, and after processing
Etching agent it is easy to handle；
3, the processing method quickly can process the pattern and optical texture of high quality in gallium arsenide surface, carve with tradition
Erosion is compared, and process velocity is fast, quality is high.
Detailed description of the invention
Fig. 1 is that the present invention is based on the step processes of the gallium arsenide surface nanoprocessing method of photochemistry assisted selective etching
Schematic diagram；
Fig. 2 is one GaAs of embodiment in " 3H " solution, traditional chemical etching and photochemistry Assisted Chemical Etching Process 5min
Under the conditions of be formed by the scanning probe microscopy pattern comparison diagram of nanostructure；
Fig. 3 is two GaAs of embodiment in " 3H " solution and under the conditions of photochemistry auxiliary etch, scratch under different loads
Nanostructure height comparison diagram is formed by after etching different time；
Fig. 4 is three GaAs of embodiment in " 3H " solution and under the conditions of photochemistry auxiliary etch, under different normal loads
Impression it is etched after be formed by nanostructure scanning probe microscopy shape appearance figure；
Fig. 5 is the scanning probe microscopy shape appearance figure for the nano-pattern that example IV is processed in gallium arsenide surface；
Fig. 6 is the scanning probe microscopy shape appearance figure for the nanocomposite optical structure that embodiment five is processed in gallium arsenide surface.
Specific embodiment
The present invention is described further in the following with reference to the drawings and specific embodiments, in the following embodiments with GaAs
(100) it is illustrated for surface processing:
As shown in Figure 1, the gallium arsenide surface nanoprocessing method of the invention based on photochemistry assisted selective etching, packet
Include following steps:
S1, scratch or impression processing are carried out in clean gallium arsenide surface using mechanical scoring device；
Specifically, successively GaAs sample ultrasonic is cleaned using acetone and dehydrated alcohol before scratch or impression processing,
And rinsed with continuous deionized water to remove the pollutant on surface, the GaAs sample for carrying out above-mentioned surface treatment is put into and is swept
In the sample cavity for retouching probe microscope or nano-hardness tester, select appropriate scratch or impression processing load, scanning probe aobvious
The tip curvature radius of the Diamond tip of micro mirror is about 200nm, and nano-hardness tester selects Berkovich pressure head；
S2, ultraviolet light chemistry auxiliary etch is carried out to gallium arsenide surface using mixing etching agent, to arsenic after the completion of etching
Gallium surface is cleaned, and gallium arsenide surface nanostructure is obtained；
Specifically, selection mixing etching agent (98%H2SO4: 30%H2O2: H2O=1:0.5:100) to gallium arsenide surface into
Row etching, etch period 30s-20min, to obtain the nanostructure of different height, after the completion of etching, successively in acetone and nothing
Water-ethanol is cleaned by ultrasonic 3min, then rinses gallium arsenide surface 10min with continuous deionized water to remove the absorption of sample surfaces
Object obtains the nanostructure of gallium arsenide surface high quality.
Since GaAs may adsorption reaction product or impurity in etching process, it is therefore desirable to right after each processing
Gallium arsenide film carries out surface cleaning processing, and obtains the primary morphology of scratch or impression by scanning probe microscopy；
Below by way of specific embodiment, the invention will be further described.
Embodiment one
The nanoprocessing method of the gallium arsenide surface based on photochemistry assisted selective etching of the present embodiment, including it is following
Step:
S1, clean gallium arsenide wafer is put into the sample cavity of scanning probe microscopy, using Diamond tip in arsenic
Change the delineation of gallium surface, processing load is divided into 0.1 μ N, 0.25 μ N, 0.5 μ N, 1 μ N, 2 μ N, 4 μ N；
S2, the GaAs Jing Guo above-mentioned processing is divided into two groups, then immerses mixing etching agent (98%H2SO4: 30%H2O2:
H2O=1:0.5:100 surface etch is carried out in), one group is etched using traditional chemical, and another set is under ultraviolet light chemical environment
It carries out, etch period is 5min, after the completion of etching, is successively cleaned by ultrasonic 3min in acetone and dehydrated alcohol, then with continuously
Deionized water rinses gallium arsenide surface 10min to remove the adsorbate of sample surfaces, to obtain GaAs table under two kinds of operating conditions
The nanostructure in face.
As shown in Fig. 2, being divided into 0.25 μ N, 0.5 μ N, 1 μ N, 2 μ N, 4 μ N for load manufactured in the present embodiment, in etching 5min
The scanning probe microscopy pattern comparison diagram of acquired nanostructure under latter two operating condition.
Embodiment two
The nanoprocessing method of the gallium arsenide surface based on photochemistry assisted selective etching of the present embodiment, including it is following
Step:
S1, gallium arsenide wafer is put into the sample cavity of scanning probe microscopy, using Diamond tip in GaAs table
Face carries out needle point delineation, and processing load is divided into 2 μ N, 4 μ N, 8 μ N, 16 μ N；
S3, the GaAs Jing Guo above-mentioned processing is immersed to mixing etching agent (98%H2SO4: 30%H2O2: H2O=1:0.5:
100) in carry out surface etch, etching carried out under ultraviolet lighting environment, etch period be respectively 0s, 30s, 1min, 5min,
10min, 15min, 20min, after the completion of etching, be successively cleaned by ultrasonic 3min in acetone and dehydrated alcohol, then with it is continuous go from
Sub- water rinses gallium arsenide surface 10min to remove the adsorbate of sample surfaces, to obtain the nanostructure of gallium arsenide surface.
As shown in figure 3, being respectively 2 μ N, 4 μ N, 8 μ N, 16 μ N for load manufactured in the present embodiment, under ultraviolet lighting environment
The degree of contrast figure of acquired nanostructure after etching 0s, 30s, 1min, 5min, 10min, 15min, 20min.
Embodiment three
A kind of nanoprocessing method of the gallium arsenide surface based on photochemistry assisted selective etching of the present embodiment, including
Following steps:
S1, gallium arsenide wafer is put into the sample cavity of nano-hardness tester, using Berkovich pressure head in gallium arsenide surface
Impression processing is carried out, processing load is 0.5-4.5mN；
S2, the GaAs Jing Guo above-mentioned processing is immersed to mixing etching agent (98%H2SO4: 30%H2O2: H2O=1:0.5:
100) in carry out surface etch, etching carried out under ultraviolet lighting environment, etch period be respectively 0s (not etching), 30s,
1min, 5min, 10min, 15min, 20min after the completion of etching, are successively cleaned by ultrasonic 3min in acetone and dehydrated alcohol, then use
Continuous deionized water rinses gallium arsenide surface 10min to remove the adsorbate of sample surfaces, to obtain gallium arsenide surface
Nanostructure.
As shown in figure 4, for load manufactured in the present embodiment be 0.5-4.5mN, etching 0s, 1min, 5min, 10min,
The scanning probe microscopy pattern comparison diagram of the formed nanostructure of 20min.
Example IV
A kind of nanoprocessing method of the gallium arsenide surface based on photochemistry assisted selective etching of the present embodiment, including
Following steps:
S1, gallium arsenide wafer is put into the sample cavity of scanning probe microscopy, using Diamond tip in GaAs table
Face is delineated according to scheduled parameter (track, load and speed), and processing load is divided into 4 μ N；
S2, the GaAs Jing Guo above-mentioned processing is immersed to mixing etching agent (98%H2SO4: 30%H2O2: H2O=1:0.5:
100) surface etch is carried out in, etching carries out under ultraviolet lighting environment, etch period 5min, after the completion of etching, successively third
Ketone and dehydrated alcohol are cleaned by ultrasonic 3min, then rinse gallium arsenide surface 10min with continuous deionized water to remove sample surfaces
Adsorbate, obtain the nano-pattern of gallium arsenide surface.
As shown in figure 5, the scanning probe microscopy shape appearance figure of the nano-pattern for the present embodiment processing.
Embodiment five
A kind of nanoprocessing method of the gallium arsenide surface based on photochemistry assisted selective etching of the present embodiment, including
Following steps:
S1, gallium arsenide wafer is put into the sample cavity of scanning probe microscopy or nano-hardness tester, using scanning probe
Microscopical Diamond tip is delineated in gallium arsenide surface according to scheduled load and speed, using nano-hardness tester
Berkovich pressure head gallium arsenide surface carries out impression processing；
S2, the GaAs Jing Guo above-mentioned processing is immersed to mixing etching agent (98%H2SO4: 30%H2O2: H2O=1:0.5:
100) surface etch is carried out in, etching carries out under ultraviolet lighting environment, etch period 15min, after the completion of etching, successively third
Ketone and dehydrated alcohol are cleaned by ultrasonic 3min, then rinse gallium arsenide surface 10min with continuous deionized water to remove sample surfaces
Adsorbate, obtain the optical texture of gallium arsenide surface.
As shown in figure 5, the scanning probe microscopy shape appearance figure of the optical texture for the present embodiment processing.
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. it is a kind of based on photochemistry assisted selective etching gallium arsenide surface nanoprocessing method, it is characterised in that: including with
Lower step:
S1, scratch or impression processing are carried out in clean gallium arsenide surface using mechanical scratching or indentation equipment；
S2, ultraviolet light chemistry auxiliary etch is carried out to gallium arsenide surface using mixing etching agent, to GaAs table after the completion of etching
Face is cleaned, and gallium arsenide surface nanostructure is obtained.
2. the gallium arsenide surface nanoprocessing method according to claim 1 based on photochemistry assisted selective etching,
It is characterized in that: in the step S1, carrying out scratch processing using the Diamond tip of scanning probe microscopy, or use nanometer pressure
Trace instrument Berkovich pressure head carries out impression processing.
3. the gallium arsenide surface nanoprocessing method according to claim 2 based on photochemistry assisted selective etching,
Be characterized in that: in the step S1, the tip curvature radius of the Diamond tip for scratch production is 20nm-5 μm, preferably
100nm-2μm；It is Berkovich diamond penetrator for impression production.
4. the gallium arsenide surface nanoprocessing method according to claim 1 based on photochemistry assisted selective etching,
Be characterized in that: the low pressure mercury lamp launch wavelength of the photochemistry auxiliary etch device is the ultraviolet light of 184.9nm and 253.7nm.
5. the gallium arsenide surface nanoprocessing method according to claim 1 based on photochemistry assisted selective etching,
Be characterized in that: in the step S2, the mixing etching agent is the mixing etching agent of sulfuric acid and hydrogen peroxide, h 2 so 4 concentration
It is 30% for 98%, hydrogen peroxide mass concentration, volume ratio H2SO4: H2O2: H2O=1:0.5:100, etch period 30s-
20min。
6. -5 any gallium arsenide surface nanoprocessing side based on photochemistry assisted selective etching according to claim 1
Method, it is characterised in that: in the step S2, successively GaAs is cleaned by ultrasonic using acetone and dehydrated alcohol, ultrasonic time is equal
For 3min, and rinsed with continuous deionized water to remove the adsorbate on surface, washing time 10min, then place is dried
Reason.
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Cited By (1)
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| CN114002043A (en) * | 2021-09-16 | 2022-02-01 | 西南科技大学 | Method for testing chemical stability of glass based on nano scratches |
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