CN104576813B - A kind of nanostructured matte on photoelectric material surface and preparation method thereof - Google Patents
A kind of nanostructured matte on photoelectric material surface and preparation method thereof Download PDFInfo
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- CN104576813B CN104576813B CN201310480369.2A CN201310480369A CN104576813B CN 104576813 B CN104576813 B CN 104576813B CN 201310480369 A CN201310480369 A CN 201310480369A CN 104576813 B CN104576813 B CN 104576813B
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 4
- 239000002110 nanocone Substances 0.000 claims description 4
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- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 3
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to a kind of nanostructured matte on photoelectric material surface and preparation method thereof, a kind of preparation method of the reconstruct nanostructured matte on photoelectric material surface is specifically disclosed, is comprised the following steps：(a) substrate is provided, initial nanostructured is formed by dry etching or wet etching in the substrate surface；(b) oxidation processes are carried out to described initial nanostructured, oxide layer is formed on the surface of initial nanostructured；(c) described oxide layer is partly or entirely removed, nanostructured matte is obtained.The invention also discloses a kind of reconstruct nanostructured matte prepared by this method.The characteristics of nanostructured matte made from the method for the present invention has high light trapping, low specific surface area, its reflectivity can be stablized below 3% in wider wavelength band, be particularly suitable for the preparation of high efficiency solar cell.And it is expected to form the black silion cell technology applied towards scale of future generation.
Description
Technical field
The present invention relates to optoelectronic materials technology, more particularly to a kind of nanostructured matte on photoelectric material surface
Preparation method and the nanostructured matte prepared by this method.
Background technology
On the road towards green, renewable electric power of future generation, the energy conversion based on photovoltaic effect is an extremely pass
Important technology.In various solar cells (PV) technology, silicon (Si) base battery technology occupies leading position, wherein polysilicon
And monocrystalline silicon (c-Si) battery accounts for the whole solar cell market share more than 85%, and this share is within the coming years (P-Si)
The trend also further increased.However, based on reducing the inherently required of cost, it is necessary to consider the battery material of reduction unit power
Expect usage amount.One feasible selection is exactly the 160- that for example main flow battery at this stage is commonly used using thinner silicon chip technology
The Si pieces of 200 μ m thicks are thinned as tens microns, you can to substantially reduce cost.Unfortunately, Si is a kind of indirect band gap
Semiconductor, its absorbability to solar spectrum is weaker, particularly near infrared band.Thin silicon chip technology is necessarily required to more multiple
Miscellaneous, more efficient sunken light technology.Refractive index further requirement higher Si efficient broadband antireflective technology reduces incidence
Reflection loss of the light on surface.Multilayer antireflective plated film and the surface based on photoetching technique are generally used in high-efficiency battery technology
Making herbs into wool reaches above-mentioned both sides purpose.However, above-mentioned high-efficiency battery technology clearly not applys to the requirement of inexpensive volume production.
Pyramid knot is typically obtained using anisotropic alkaline random surface making herbs into wool technology in commercialization standard solar cell technology
Structure matte（Just in c-Si）, the matte can help to obtain about 10% or so average reflectance（To P-Si）.The opposing party
Face, traditional general making herbs into wool depth of pyramid suede structure is in 3~10 μ ms, the depth and thin Si pieces（Such as 20 μm）Physics
Thickness can compare, hence it is evident that not be a good selection.
However, common nanometer suede structure can reach specific sunken light requirement along with very big specific surface area increase
Nanostructured surface product be usually more than 10 times of flat board Si areas, considerably increase photo-generated carrier answering in material surface
Probability is closed, causes the reduction of battery efficiency.Efficiency of solar cell based on nano wire and nanometer hole is currently below 10%, much low
In the level of traditional c-Si battery~25%.The c-Si batteries based on nanometer suede structure currently reported（Black silion cell）Highest
Efficiency only has 18.2%.A main cause for causing these battery efficiencies relatively low is exactly the carrier directly related with surface area
High recombination rate, carrier surface recombination rate an order of magnitude about higher than flat board Si in these batteries.Therefore, towards of future generation high
The sunken light technology of performance battery must possess following characteristics：1）Broadband antiradar reflectivity；2）Relatively low surface area increase；3）Compared with
Few raw materials consumption.Battery efficiency can not only be improved by meeting the exploitation of the sunken light technology of novel nano of above-mentioned requirements, simultaneously
Make it possible the promoting the use of of thin silicon wafer, with comparatively fast reducing the potentiality of cost.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nanostructured matte on photoelectric material surface and by this
Nanostructured matte prepared by method.
First aspect present invention provides a kind of preparation method of the reconstruct nanostructured matte on photoelectric material surface, including
Following steps：
(a) substrate is provided, initial nanostructured is formed in the substrate surface by dry etching or wet etching；
(b) dry or wet oxidation processes are carried out to described initial nanostructured, in the surface shape of initial nanostructured
Into oxide layer；
(c) described oxide layer is partly or entirely removed, obtains reconstructing nanostructured matte.
In another preference, the substrate thickness is 1-1000 μm.
In another preference, the dry etching includes：Template, plasma etching, the dry etching based on photoetching.
In another preference, the wet etching includes：Electrochemical etching, metal inducement etching, metal assistant chemical
Etching.Preferably metal assistant chemical etch（Such as the corrosion of self-assembled nanometer Ag particles assistant chemical）.
In another preference, in step (b), the oxide layer formed is the oxide layer of non-uniform thickness, oxide layer
Thickness is 10-1000nm.
In another preference, in step (c), described oxide layer is fully removed.
In another preference, in step (c), described oxide layer is partially removed, and part is retained in weight after removing
The thickness of the oxide layer of structure nanostructured textured surfaces is 0.1-100nm.
In another preference, the substrate is the photoelectric semiconductor material that can be oxidized, and is selected from：Monocrystalline silicon, polysilicon,
Non-crystalline silicon, germanium, GaAs, indium phosphide.
In another preference, described initial nanostructured is selected from：Nano thread structure, nanometer hole structure, nanocone knot
Structure, nanometer rod structure, nanometer band structure or its combination.
In another preference, described initial nanostructured has some construction units, the transverse direction of the construction unit
Size is 1nm~1 μm（Preferably 20-200nm）, making herbs into wool corrosion depth is 20nm~3 μm（Preferably 100-500nm）.
In another preference, in step (b), oxidation temperature is 25-1410 DEG C, and oxidation treatment time is 1-
100000s.（Preferably 60-1800s）
In another preference, the oxidation processes are dry oxidation process, and treatment temperature is 500-1000 DEG C.
In another preference, the oxidation processes are wet oxidation process, and treatment temperature is 25-150 DEG C.
In another preference, in step (c), the removal of oxide layer is including the use of acid or alkaline corrosion solution to oxidation
The step of layer carries out corrosion treatment, the acid or alkaline corrosion solution has corrosivity to oxide layer, to substrate not damaged.
In another preference, corrosion treatment includes dry etching processing and wet etching processing.Preferably wet method is rotten
Erosion is handled.
In another preference, described acidic corrosion solution is selected from：Hydrofluoric acid solution, hydrochloric acid solution etc. or its combination.
In another preference, described alkaline corrosion solution is selected from：NaOH solution, KOH solution etc. or its combination.
In another preference, the hydrofluoric acid solution is the volume ratio of the aqueous solution, wherein hydrofluoric acid and water of hydrofluoric acid
For 1：1000-100：1（Preferably 1：10）.
In another preference, the reconstruct nanostructured matte has one or more of feature：
(i) have top air gap big, the small structure of bottom air gap, the characteristic with effective refractive index gradual change, from top to
Bottom, the excursion of effective refractive index is 1-n, and n is the refractive index of substrate.Preferably, when substrate is crystalline silicon, n is
3.5；
(ii) reconstruct nanostructured matte have spill bowl-shape or convex taper construction unit, the system of the construction unit
Suede corrosion depth is 10-500nm；
(iii) reconstruct nanostructured matte compared with flat board photoelectric material, its surface area increase 0.5-3 times, more preferably for
0.5-2 times；
(iv) in 400-1100nm wave bands, the average reflectance of reconstruct nanostructured matte is 2-8%, preferably
2-3%.
Second aspect of the present invention provides a kind of photoelectric material, and the material, which includes surface, has reconstruct nanostructured matte
Substrate, the reconstruct nanostructured matte has top air gap big, the small structure of bottom air gap, and bowl-shape or convex with spill
The construction unit of type taper.
In another preference, the making herbs into wool corrosion depth of the construction unit is 10-500nm, spill bowl structure unit
Top diameter be 20nm-1 μm（Preferably 80-150nm）, base diameter is 10-700nm（Preferably 30-
100nm）；The top diameter of convex cone structure unit is 10-700nm（Preferably 30-100nm）, base diameter is
20nm-1μm（Preferably 80-150nm）.
In another preference, the reconstruct nanostructured matte is prepared from by the method described in first aspect.
It should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the invention and have in below (eg embodiment)
It can be combined with each other between each technical characteristic of body description, so as to constitute new or preferred technical scheme.As space is limited, exist
This no longer tires out one by one states.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of preparation method of the present invention.Wherein, Fig. 1-1 is substrate schematic cross-section；Fig. 1-2 is first
Beginning nanostructured schematic cross-section；Schematic cross-sections of the Fig. 1-3 for initial nanostructured after oxidation-treated；Fig. 1-4 is deoxidation
Change the schematic cross-section of the reconstruct nanostructured matte after layer.
Fig. 2 is the preparation method schematic flow sheet of the embodiment of the present invention 1.Wherein, Fig. 2-1 represents that evaporation Ag is thin on Si pieces
Film；Fig. 2-2 is rapid thermal annealing（RTP）Ag nano particle schematic diagrames are formed afterwards；Fig. 2-3 is that chemical attack obtains initial nanometer
Hole structural representation；Fig. 2-4 to Fig. 2-6 is that nanostructured matte reconstructs schematic flow sheet.
Fig. 3 schemes for the SEM of the corresponding nanostructured of each step in embodiment 1.Wherein, Fig. 3-1 (a) is to pass through RTP processes
The Ag nano particles SEM figures formed afterwards；Fig. 3-1 (b) is that correspondence nano particle is empty via the nanometer obtained after 150s chemical attacks
Hole structure matte section SEM schemes；Fig. 3-2 is that nano-void structure is received via the reconstruct formed after 1000 DEG C of oxidations and oxide layer
The SEM figures of rice structure matte.
Fig. 4 is initial nanostructured, reconstruct nanostructured matte and commercialization c-Si batteries in embodiment 1 in visible ray model
Enclose internal reflection spectrogram.
Fig. 5 is the SEM figures of the corresponding nanostructured of each step in embodiment 2.Wherein, wherein Fig. 5-1 and Fig. 5-4 is first
Beginning nanostructured section SEM pictures；Fig. 5-2 and Fig. 5-5 is oxidation-treated initial nanostructured section SEM pictures；Fig. 5-3
With section SEM pictures of the Fig. 5-6 for reconstruct nanostructured matte.
Fig. 6 is initial nanostructured in embodiment 2（6-1）, oxidation-treated initial nanostructured（6-2）, reconstruct receive
Rice structure matte（6-3）In visible-range internal reflection spectrogram.
Embodiment
Inventor has found by research extensively and profoundly, on the basis of the initial nanostructured that substrate surface is formed,
The structure aoxidize-reconstruction processing of deoxidation after, a kind of novel nano structure matte, the nanostructured can be obtained
The characteristics of matte has high light trapping, low specific surface area, and the reflectivity of the structure can stablize in wider wavelength band
Below 3%, effective collection of carrier can be ensured while absorbing incident light is increased, be particularly suitable for the high efficiency sun
The preparation of battery.The present invention is completed on this basis.
Initial nanostructured and preparation method thereof
In the nanostructured matte preparation method of the present invention, substrate is the photoelectric semiconductor material that can be oxidized, including but
It is not limited to：Silicon, germanium, GaAs, indium phosphide.Wherein, silicon chip can be more than 99.9999% P or N-type solar energy level silicon for purity
Piece, purity are more than 99.9999999999% P or N-type integrated circuit level silicon wafer, include polysilicon（P-Si）, monocrystalline silicon（c-
Si）And non-crystalline silicon（a-Si）Deng base material.The thickness of substrate is generally 1-1000 μm.
Initial nanostructured refers to receive by one kind of the methods such as etching formation on more smooth photovoltaic substrate surface
The suede structure of meter level, to increase light path, reduces the reflection of light.
As used herein, " initial nanostructured ", " initial nanometer suede structure ", " initial nanostructured matte " is interchangeable
Use.
In the present invention, initial nanostructured can have periodicity or aperiodic structure.Initial nanostructured
Can be single shape and structure, or the combination of a variety of single shape and structures, structure preferably includes but is not limited to：Nanometer
Cable architecture, nanometer hole structure, nanocone structures, nanometer rod structure, nanometer band structure or its combination.
Every kind of initial nanostructured includes multiple construction units, and construction unit as described herein is the initial nano junction of composition
The minimum basic unit of structure.Lateral dimension average out to 1nm~1 μm of each construction unit（Preferably 20-200nm）, making herbs into wool
Corrosion depth average out to 20nm~3 μm（Preferably 100-500nm）.
Herein, when initial nanostructured is nano thread structure, nanometer hole structure or nanometer rod structure, its initial nanometer
The lateral dimension of construction unit is the diameter of the construction unit, and when initial nanostructured is nanocone structures, it is initially received
The lateral dimension of rice construction unit is the diameter that the construction unit bores bottom.
The preparation method of the initial nanostructured of the present invention is not particularly limited, can be according to selected substrate material
Difference selected.Generally, can be by the conventional method including dry etching and wet etching on photovoltaic substrate surface
Prepared, the preferred dry etching of a class includes（But it is not limited to）：Template, plasma etching, the dry etching based on photoetching
Erosion.The preferred wet etching of one class includes（But it is not limited to）：Electrochemical etching, metal inducement etching, metal Assisted Chemical Etching Process.
The present invention more preferably metal assistant chemical etch（MaCE）（Such as the corrosion of self-assembled nanometer Ag particles assistant chemical）
In photoelectric material（Such as silicon chip）Surface forms initial nanostructured.Corrosion process includes following two steps：
(1) with AgNO3Preliminary treatment is carried out with HF mixed solution, processing time is 1~10000s（Preferably 1-
1000s）, AgNO3Molal volume ratio with HF is 1:1~1:2000, preferably 1：1~1：500；
(2) with HF and H2O2Mixed solution for etchant solution carry out corrosion treatment, processing time be 1~10000s（Preferably
Ground is 1-1000s）, HF and H2O2Molal volume ratio be 200：1~1：1, preferably 50：1~1：1.
Oxidation treatment step
In the preparation process in accordance with the present invention, oxidation processes are carried out to initial nanostructured to refer to the initial of the present invention
The photovoltaic substrate of nanostructured is placed in containing oxidation reaction is carried out in the environment of oxygen, so that in the surface shape of initial nanostructured
Into oxide layer.
Oxidation processes can be carried out under oxygen atmosphere, can also be carried out in atmosphere.Oxidation processes include dry method oxygen
Change processing and wet oxidation process, described dry oxidation process refers in heating furnace by being passed through oxidizing gas（Such as sky
Gas, oxygen etc.）, at a certain temperature aoxidize substrate sample surface, described wet oxidation process refers to oxygen
In the solution for the property changed（Such as H2O2、HNO3Deng）, substrate sample surface is formed oxide layer.The present invention is preferably dry oxidation process.
Oxidation temperature is 50-1410 DEG C, it is preferred that when oxidation processes are dry oxidation process, treatment temperature is
500-1000℃.When oxidation processes are wet oxidation process, treatment temperature is 25-150 DEG C.Oxidation treatment time is 1-
100000s.（Preferably 60-1800s）
In the oxidation processes of the present invention, because initial nanostructured top and bottom are different by oxygen area, lead
Cause the oxidation rate of upper and lower ends different, therefore the thickness of the oxide layer formed on its surface corrodes deep along initial nanostructured
Degree direction is tapered into from top to bottom, is the oxide layer of non-uniform thickness, and the thickness of oxide layer is general in 10-1000nm.
Oxidation-treated initial nanostructured, the oxide layer filling that its gap is substantially formed, oxide layer
Medium it is typically corresponding with selected substrate material, for the oxidation state species corresponding to the substrate material.For example, working as substrate
When material is silicon, the oxide layer formed is silica（SiOx）Layer.When substrate material is germanium, the oxide layer formed is oxygen
Change germanium（GeO2）Layer.
Go removing oxide layer step
In the preparation process in accordance with the present invention, removing oxide layer step is gone to refer to by etchant solution to being formed and initial nano junction
The oxide layer on structure surface carries out corrosion treatment, so as to form the reconstruct nanostructured matte of the present invention.
Wherein, etchant solution of the invention will not cause damage to substrate, while there is good oxide layer effect, can
To reach the effect that selective removal oxide layer is carried out to the substrate containing oxide layer.Etchant solution used in the present invention includes
Acidic corrosion solution and alkaline corrosion solution, the preferred acidic corrosion solution of a class include（But it is not limited to）：Hydrofluoric acid solution（HF
Acid solution）, hydrochloric acid solution, more preferably hydrofluoric acid solution.
The preferred alkaline corrosion solution of one class includes（But it is not limited to）：The hydroxide solution of alkali metal（Such as NaOH,
KOH）.
The acidic corrosion solution and alkaline corrosion solution of the present invention refers to corresponding acid or alkali soluble formed in solvent
Solution, the solvent may be selected from the common solvent in this area, such as alcohols solvent, water, and the present invention is preferably acid or alkali
The aqueous solution, such as SiOx, corrosive liquid is that the volume ratio of hydrofluoric acid aqueous solution, wherein HF and water is 1：1000-100：1（Preferably
Ground is 1：10）
By the concentration of acid or alkaline matter in control corrosion rate solution, or by controlling during corrosion during oxide layer
Between, to reach the effect for partly or entirely removing removing oxide layer.I.e. oxide layer can be completely removed, can also be in whole nanometer
Retain certain thickness oxide layer on structure matte（Preferably thickness is 0.1-100nm）.Retained certain thickness oxide layer both
Antireflective effect can be played, the purpose of efficient surface passivation can also be reached.Preferably oxide layer of the invention is fully removed.
The selection of etching time can be according to the oxidated layer thickness of the corrosive power of etchant solution, concentration and required corrosion
Difference is selected.For example to SiOx, when use quality fraction is 40% HF solution, corrode 10-1000nm oxide layers when institute
Take time generally 0.01-1000s, preferably 10-300s.
Reconstruct nanostructured matte
The reconstruct of the present invention refers to initial nanostructured is carried out to aoxidize-deoxidation processing procedure." reconstruct nanostructured
Matte " and " nanostructured matte " are used interchangeably, and refer both to the nanostructured matte of gained after oxidation-deoxidation processing.At this
In invention, reconstruct nanostructured matte is in irregular alveolate texture（With the construction unit that spill is bowl-shape）, or pointed cone
Shape arrangement architecture（With convex cone structure unit）.The construction unit of reconstruct nanostructured matte as described herein is heavy to constitute
The minimum basic unit of structure nanostructured matte.The making herbs into wool corrosion depth of construction unit is 10-500nm, spill bowl structure list
The top diameter of member is 20nm-1 μm, preferably 80-150nm.Base diameter is 10-700nm, preferably 30-
100nm, the top diameter of convex cone structure unit is 10-700nm, and preferably 30-100nm, base diameter is 20nm-1
μm, preferably 80-150nm.
The spatial joint clearance of the construction unit of nanostructured matte from top to bottom is reconstructed from large to small, from superficial layer to body
The different local air dielectric of material internal is different with silicon medium proportion, therefore with effective refractive index roll-off characteristic, is usually
From small to large.The excursion of effective refractive index is 1-n, and n is the refractive index of substrate.It is preferred that when substrate is crystalline silicon, n
For 3.5（Such as：From top to bottom, the excursion of effective refractive index is 1-3.5 to crystalline silicon substrate）, i.e. impedance matching property.Therefore
Incident light reflects in the Propagation that effective refractive index continuity changes to be effectively suppressed.
The specific surface area of the reconstruct nanostructured matte of the present invention and flat board photoelectric material（Such as flat board silicon）Compare, its surface
Product only increases 0.5-3 times, is more preferably 0.5-2 times.
In 400-1100nm wave bands, the average reflectance of reconstruct nanostructured matte is 2-8%, preferably 2-3%.
The preparation method of the reconstruct nanostructured matte of the present invention, is preferably comprised following steps：
(1) pre-treatment step, as Figure 1-1, by substrate 101 after over cleaning and hydrophilic treated it is stand-by；
(2) preparation process of initial nanostructured, as shown in Figure 1-2, is prepared on substrate by dry or wet etch
Initial nanostructured 102；
(3) oxidation treatment step, as Figure 1-3, carries out oxidation processes to initial nanostructured 102 at high temperature, from
And in initial nanostructured surface formation oxide layer 103；
(4) oxide layer step, as Figure 1-4, using rotten by wet method to the selective etchant solution of oxide layer
Etching off removing oxide layer 103, forms reconstruct nanostructured matte 104.
Compared with prior art, main advantages of the present invention include：
(1) present invention develops a kind of new process for etching, and this method is simple and easy to apply, compatible with existing industrial manufacture process
Property is good, suitable for popularization and application.
(2) reconstruct nanostructured matte produced by the present invention has making herbs into wool corrosion depth shallow, the low spy of matte specific surface area
Point.While the reflectivity of nanostructured matte after reconstruct can be stablized below 3% in wider wavelength band, and
Surface area is only doubled, far below the surface area increase of other nanostructured mattes（General more than 10 times）, effectively suppress
Carrier is in the compound of surface.
(3) it is produced by the present invention reconstruct nanostructured matte have spill bowl-shape or convex taper construction unit, structure
The spatial joint clearance of unit from top to bottom inhibits Jie that incident light changes in effective refractive index continuity from large to small, effectively
Reflection when being propagated in matter.
(4) preparation method applicability of the invention is wide, and can all kinds of photoelectric semiconductor materials be carried out with making herbs into wool, and with fine
Making herbs into wool effect.
(5) there is the characteristics of small cost of thickness is low by photoelectric semiconductor material made from the method for the present invention, especially fits
For thin battery piece.
(6) preparation method of the invention can take into account surface passivation and sunken optical property, without surface antireflective plated film, be conducive to
Efficiency of solar cell is improved, battery preparation flow and corresponding equipment investment is reduced, production cost is reduced.
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to conventional strip
Part or according to the condition proposed by manufacturer.
Unless otherwise defined, all specialties used in text known to scientific words and one skilled in the art with anticipating
Justice is identical.In addition, any method similar or impartial to described content and material all can be applied in the inventive method.Wen Zhong
Described preferable implementation only presents a demonstration with material to be used.
Embodiment 1
1. reconstruct the preparation of nanostructured matte
In the present embodiment, initial nanostructured is corroded using self-assembled nanometer Ag particles assistant chemical to be prepared.
The preparation of 1.1 initial nanostructureds
There is provided a thickness it is 625 μm as shown in Fig. 2-1, crystal face is（100）C-Si pieces 201, resistivity be 1-10 Ω
cm.The thick Ag films 202 of one layer of about 20nm are deposited using thermal evaporation after being cleaned to c-Si substrates.
As shown in Fig. 2-2, by structure shown in Fig. 2-1 in H2Under gas shielded, 800 DEG C of progress, the rapid thermal annealing of 5 minutes,
Wherein rate of temperature fall control is 30 DEG C/min, the spontaneous cluster formation rule nano particle 203 of Ag films 202.
As Figure 2-3, under the catalytic action of Ag nano particles, in HF：H2O2Mol ratio is 10：Carried out in 1 solution
The corrosion of 150 seconds, nano particle is gradually fallen into c-Si, forms the regular nano-void structure 204 erect.
As in Figure 2-4, the initial nano-void structure shown in Fig. 2-3 is soaked 3 minutes in concentrated nitric acid, removes Ag residual
It is remaining.
1.2 oxidation processes
As shown in Figure 2-5, to the initial nano-void structure at a high temperature of 1000 DEG C, carry out 100 minutes in atmosphere
Oxidation processes, c-Si surface formed silica（SiOx）Layer 205.
1.3 oxide layer
As shown in figures 2-6, using the HF aqueous solution（HF：H2O volume ratio 1:10）Silicon oxide layer is eroded, so that weight is made
Structure nanostructured matte 206.
2. the nanostructured in reconstruct nanostructured matte preparation method corresponding to each step compares
It can be drawn from Fig. 3-1 and 3-2, alveolate texture is presented in reconstruct nanostructured matte, and its construction unit is relative
Homogeneous spill bowl structure.The maximum making herbs into wool corrosion depth of construction unit is about 200nm, and the top and bottom of construction unit are straight
Footpath respectively may be about 120nm and 70nm.
The spatial joint clearance of the construction unit from top to bottom from large to small, therefore has effective refractive index roll-off characteristic
（From top to bottom, the excursion of effective refractive index is 1-3.5）, effectively inhibit incident light to change in effective refractive index continuity
Propagation when reflection.
The maximum making herbs into wool corrosion depth of the construction unit is only 200nm, the average making herbs into wool with traditional pyramid suede structure
3-10 μm of depth is compared, and reconstruct nanostructured matte of the invention can provide more effective wide band antireflective and stronger near-infrared
Wave band efficiently falls into light effect.
The surface area for generally reaching the nanostructured matte of specific sunken light requirement is usually identical size flat-panel silicon area
More than 10 times, the surface area of reconstruct nanostructured matte of the invention is about 2 times or so of identical dimension plane silicon, i.e., with it is identical
Dimension plane silicon is compared, and surface area only increases by 1 times.Less surface area can substantially reduce carrier being combined on surface, thus
The photoelectric transformation efficiency through battery made from the material can be improved.
3. reconstruct the average reflectance of nanostructured matte
The measurement of reflectivity uses AudioDev GmbH HELIOS LAB-RE model reflectance tests in the present embodiment
Instrument is measured.In the present embodiment, initial nanostructured（401）, cellular nano structure matte after reconstruct（402）And it is attached
There is the pyramid structure matte of the commercialization c-Si batteries of SiNx antireflective coatings（403）Each wavelength under corresponding reflectivity measurement
As a result it is as shown in table 1：
Table 1
The initial nanostructured of the present invention is can be seen that from table 1 and Fig. 4（401）In the average anti-of 400-1100nm wave bands
It is 7.2%, the cellular nano structure matte after reconstruct to penetrate rate（402）It is about 2.5% in the average reflectance of the wave band, and it is current
Pyramid structure made from the anisotropic alkaline random surface making herbs into wool technology typically used in commercialization standard solar cell
Matte（Just in c-Si）, its average reflectance（To P-Si）About 10%.Even in the golden word of commercialization c-Si batteries at present
Pass through additional SiN on tower structure mattexAntireflective coating（403）, its average reflectance is also only down to 3%.
It can thus be seen that the reconstruct nanostructured matte of the present invention has more efficient sunken light effect.
Current existing commercial c-Si battery surfaces are pyramid matte, and also use high-quality SiNxAntireflective
Layer.Therefore under intimate identical optical enhancement assimilation effect, reconstruct nanostructured matte of the invention is without surface antireflective
Plated film, reduces battery preparation flow and corresponding equipment investment, contributes to the reduction of cost.
Embodiment 2
1. reconstruct the preparation of nanostructured matte
In the present embodiment, initial nanostructured uses AgNO3The metal of solution is aided in without electrochemical corrosion（MaCE）Method
Prepare.
1.1 pretreatment
To 300 μ m thicks, crystal face is（100）, resistivity is 1-10 Ω cm c-Si pieces according to acetone, alcohol, deionization
The sequencing of water is cleaned by ultrasonic.C-Si pieces after cleaning are in H2SO4And H2O2Mixed solution（H2SO4：H2O2Volume
Than 3:1）Middle immersion 30 minutes, removes the residual impurities such as surface organic matter, and Si pieces surface is had certain hydrophily；As schemed
Shown in 6-2, after the c-Si substrates after hydrophilic treated are cleaned with deionized water, dried up, in c-Si backside coating a thin layer nails
Oil is protected.
The preparation of 1.2 initial nanostructureds
C-Si substrates by pretreatment are kept flat into HF and AgNO3Mixed solution（HF：AgNO3Mol ratio be 240:
1）Middle 90s, Ag nano particle can be deposited evenly on c-Si upper surfaces.Then, the c-Si substrates for being coated with Ag particles are put into HF
And H2O2Mixed solution（HF：H2O2Mol ratio be 30:1）Middle progress 20s corrosion treatment, under Ag catalytic action,
C-Si upper surface, which can corrode, homogeneous initial nanostructured.C-Si substrates with initial nanostructured are successively put into dense
HNO3With each 3 minutes in acetone soln, remaining and the back side the nail polish of Ag is removed respectively.
1.3 oxidation processes
Initial nanostructured obtained in 2.2 is put into tubular heater under air atmosphere, sintered at 1000 DEG C
30 minutes, in initial nanostructured surface formation oxide layer.The thickness of the oxide layer corrodes from the upper end edge of initial nanostructured
Depth direction is tapered into.
1.4 oxide layer
Substrate after oxidation is put into HF and H2O mixed solution（HF：H2O volume ratio 1:10）Middle corrosion 150 seconds, oxygen
Change layer to be completely removed, so that reconstruct nanostructured matte is made.
2. the nanostructured in reconstruct nanostructured matte preparation method corresponding to each step compares
It can be drawn from Fig. 5-1 and Fig. 5-4, the making herbs into wool corrosion depth of initial nanostructured is about 400nm, be presented irregular
Nano-void shape structure.From Fig. 5-2 and Fig. 5-5 as can be seen that the top nano-void knot of the initial nanostructured after oxidation
Structure is oxidized layer and filled substantially.From Fig. 5-3 and Fig. 5-6 as can be seen that the reconstruct nanostructured matte after oxide layer is removed is same
Sample shows irregular alveolate texture, and concave is equally presented in its construction unit.Compared with initial nanostructured, reconstruct
Nanostructured matte afterwards has smaller specific surface area.
3. reconstruct the average reflectance of nanostructured matte
From fig. 6, it can be seen that in embodiment 2, in 400-1100nm spectral regions, at initial nanostructured 6-1, oxidation
The average reflectance of the random cellular nano structure 6-3 after nanostructured 6-2, reconstruct after reason is respectively 6.8%, 6.4% and
2.9%.Compared with initial nanostructured, the cellular nano structure matte after reconstruct shows full wave anti-reflective effect, its
2% is below in the reflectivity of the main photo-absorption regions of the c-Si of 500nm-1000nm scopes.
All documents referred in the present invention are all incorporated as reference in this application, independent just as each document
It is incorporated as with reference to such.In addition, it is to be understood that after the above-mentioned instruction content of the present invention has been read, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
Claims (12)
1. the preparation method of the reconstruct nanostructured matte on a kind of photoelectric material surface, it is characterised in that comprise the following steps：
(a) substrate is provided, initial nanostructured is formed in the substrate surface by dry etching or wet etching；
(b) dry oxidation process is carried out to described initial nanostructured, oxide layer is formed on the surface of initial nanostructured；
(c) described oxide layer is partly or entirely removed, obtains reconstructing nanostructured matte；
Also, the reconstruct nanostructured matte has top air gap big, the small structure of bottom air gap, with effective refractive index gradually
The characteristic of change, from the top to the bottom, the excursion of effective refractive index is 1-n, and n is the refractive index of substrate；
Wherein, described dry oxidation process refers to be passed through oxidizing gas in heating furnace, and base material sample is made at a certain temperature
Product surface is aoxidized；
Also, the treatment temperature of the dry oxidation process is 500-1000 DEG C；
Also, in step (c), the removal of oxide layer carries out corrosion treatment including the use of acid or alkaline corrosion solution to oxide layer
The step of, the acid or alkaline corrosion solution has corrosivity to oxide layer, to substrate not damaged.
2. preparation method as claimed in claim 1, it is characterised in that the substrate is the semiconductor optoelectronic material that can be oxidized
Material, is selected from：Monocrystalline silicon, polysilicon, non-crystalline silicon, germanium, GaAs, indium phosphide.
3. preparation method as claimed in claim 1, it is characterised in that described initial nanostructured is selected from：Nano thread structure,
Nanometer hole structure, nanocone structures, nanometer rod structure, nanometer band structure or its combination.
4. preparation method as claimed in claim 1, it is characterised in that if described initial nanostructured has stem structure list
Member, the lateral dimension of the construction unit is 1nm~1 μm, and making herbs into wool corrosion depth is 20nm~3 μm.
5. preparation method as claimed in claim 1, it is characterised in that in step (b), oxidation temperature is 500-1000
DEG C, oxidation treatment time is 1-100000s.
6. preparation method as claimed in claim 1, it is characterised in that in 400-1100nm wave bands, reconstructs nanostructured suede
The average reflectance in face is 2-3%.
7. preparation method as claimed in claim 1, it is characterised in that the reconstruct nanostructured matte have it is following a kind of or
Various features：
(i) when substrate is crystalline silicon, n is 3.5, and from top to bottom, the excursion of effective refractive index is 1- to crystalline silicon substrate
3.5；
(ii) reconstruct nanostructured matte have spill bowl-shape or convex taper construction unit, the making herbs into wool of the construction unit is rotten
Erosion depth is 10-500nm；
(iii) reconstruct nanostructured matte is compared with flat board photoelectric material, and its surface area increases 0.5-3 times；
(iv) in 400-1100nm wave bands, the average reflectance of reconstruct nanostructured matte is 2-8%.
8. a kind of photoelectric material, it is characterised in that the material includes the substrate that surface has reconstruct nanostructured matte, described
Reconstruct nanostructured matte has top air gap big, the small structure of bottom air gap, and has spill bowl-shape or convex taper knot
Structure unit；And the reconstruct nanostructured matte is prepared from by the method described in claim 1；
Also, the reconstruct nanostructured matte has effective refractive index roll-off characteristic, and from the top to the bottom, effective refractive index
Excursion be 1-n, n is the refractive index of substrate；
Also, in 400-1100nm wave bands, the average reflectance of the reconstruct nanostructured matte is 2-8%.
9. photoelectric material as claimed in claim 8, it is characterised in that the making herbs into wool corrosion depth of the construction unit is 10-
500nm, the top diameter of spill bowl structure unit is 20nm-1 μm, and base diameter is 10-700nm；Convex cone structure list
The top diameter of member is 10-700nm, and base diameter is 20nm-1 μm.
10. photoelectric material as claimed in claim 8, it is characterised in that when substrate is crystalline silicon, n is 3.5, crystal silicon substrate
From top to bottom, the excursion of effective refractive index is 1-3.5 to piece.
11. photoelectric material as claimed in claim 8, it is characterised in that the specific surface area of the reconstruct nanostructured matte with
Flat board photoelectric material is compared, and its surface area increases 0.5-3 times.
12. photoelectric material as claimed in claim 8, it is characterised in that in 400-1100nm wave bands, the reconstruct nano junction
The average reflectance of structure matte is 2-3%.
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| CN105390909A (en) * | 2015-11-04 | 2016-03-09 | 上海无线电设备研究所 | Terahertz source based on intrinsic semiconductor layer with micro-nano structure and preparation method |
| CN106129168A (en) * | 2016-08-26 | 2016-11-16 | 电子科技大学 | Infrared enhancing Si PIN detector and preparation method thereof is etched based on metal inducement |
| CN106997915A (en) * | 2017-04-01 | 2017-08-01 | 江苏辉伦太阳能科技有限公司 | A kind of monocrystalline silicon surface honey comb structure and preparation method thereof |
| CN107068805A (en) * | 2017-04-01 | 2017-08-18 | 江苏辉伦太阳能科技有限公司 | A kind of polysilicon surface honey comb structure and preparation method thereof |
| CN107902918B (en) * | 2017-12-08 | 2020-03-31 | 福耀玻璃工业集团股份有限公司 | Preparation method of anti-reflection and anti-reflection film layer |
| CN113651290A (en) * | 2021-07-07 | 2021-11-16 | 北京大学 | Novel silicon-based micro-nano structure modification method |
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