CN102660776A - Method for preparing black silicon through Mn ion catalysis and corrosion - Google Patents
Method for preparing black silicon through Mn ion catalysis and corrosion Download PDFInfo
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- CN102660776A CN102660776A CN2012101400977A CN201210140097A CN102660776A CN 102660776 A CN102660776 A CN 102660776A CN 2012101400977 A CN2012101400977 A CN 2012101400977A CN 201210140097 A CN201210140097 A CN 201210140097A CN 102660776 A CN102660776 A CN 102660776A
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Abstract
The invention relates to a method for preparing black silicon in low cost. The method is characterized in that as follows: firstly, ultrasonic cleaning is performed on monocrystal silicon chip by using acetone, alcohol and ultrapure water in sequence, so as to remove oil fouling and metal ions on the surface of a silicon chip; then, the silicon chip is placed into NaO solution with high concentration for corrosion for minutes so as to remove a surface damage layer; then, the silicon chip is placed into the NaOH solution with low concentration for corrosion for dozens of minutes so as to form a pyramid-shaped structure on the surface of the silicon chip; and finally, the pyramid-shaped structure is placed into mixed solution of HF, any one of manganese salts (Mn (No3)2, or Mn (NO3)3, k2MnO4 and MnO4) and ultrapure water, for chemical corrosion so as to prepare the black silicon with an antireflection nano structure on the pyramid. The method provided by the invention has the advantages that complex equipment is not required, the preparing process is simple, the preparing cost is low, and the preparation of large-area black silicon can be achieved.
Description
Technical field
The invention belongs to technical field of semiconductors, relate to the method for a kind of low-cost preparation " black silicon ".
Background technology
Global energy shortage, environmental pollution, climate warming are just day by day seriously perplexing human society.Seek green substitute energy, realize Sustainable development, become the problem that countries in the world face jointly.In the long run, renewable energy source will be following human main energy sources source.In the utilization of the renewable energy source of new development, the tool potentiality of solar cell.
Silicon storage on earth is abundant, is prone to purify, and is high temperature resistant, forms natural oxide easily, has good semiconducting insulation bed interface, so crystalline silicon is by a large amount of solar cell and SIC fields of being used for.But the high-reflectivity of crystalline silicon itself makes that its performance in the application of solar cell and photoelectric device is not good.In order to reduce the reflectivity on crystal silicon solar energy battery surface, increase photoabsorption, general method is to fall into light microstructure and deposition antireflection film in the silicon face preparation; Preparation antireflective microstructure mainly is meant utilizes the mixing solutions of NaOH (or KOH) and Virahol (or ethanol) to prepare pyramid structure in the silicon chip surface wet method; But etching method not only has requirement to the crystal orientation of crystalline material; And can only in very narrow wavelength band, reduce surface albedo; Reflectivity is not enough to satisfy the requirement that reduces the silicon chip surface reflectivity to greatest extent still more than 10%.The preparation antireflective coating is meant that methods such as utilizing PECVD is at silicon chip surface deposition one deck anti-reflective film (SiO
x, TiO
x, ZnO, ITO or Si
3N
4), and the anti-reflective film thickness is relevant with the specific refractory power of lambda1-wavelength and anti-reflective film, this has just determined anti-reflective film can only play the antireflection effect of limited spectral range, and incident angle of light is also had restriction.
" black silicon " has the consistent reflection high-absorbable ability of hanging down as a kind of reflectivity very low silicon face or silica-base film in the very wide wavelength band of near ultraviolet-near infrared.The method of preparation at present " black silicon " has the femtosecond pulse method, plasma etching method, electrochemical erosion method metals ion assistant chemical etch." black silicon " is at SF the earliest by people [Applied Physics Letters, 1998,73 (12): 1673-1675] such as Mazur E
6With femto-second laser pulse active silicon surface, the little surface of the tip-like that obtains is because SF in the atmosphere
6Gas forms H under the laser pulse effect
2Toxic gases such as S, the researchist adopts " the black silicon " of the method for knitting of plasma surface in the silicon chip surface preparation, and in 400～1100 nm wavelength band, average reflectance is 2.6%; Yoo J [the Solar Energy of Korea Energy Source Inst; 2010; 84 (4): 730-734] utilize " the black silicon " of reactive ion etching method preparation, surface topography is the pyramid at crater, at 300～850 nm wave band average reflectances 8.9%; Under the situation of no traditional antireflective coating, the efficiency of solar cell of preparation is 16.7%.[the Applied Physics Letters of the Hou Xiao of Fudan University seminar far away; 2006; 88 (17): 171907 (1-3)] adopt the pulse corrosion electric current to prepare multi-layer porous " the black silicon " of gradually changed refractive index, its reflectivity is lower than 5% in the wide band scope, bear Zu Hong seminar of Southwestern University [Acta Physica Sinica; 2007; 57 (01): 514-518] adopt computer-controlled electrolytic corrosion silicon single crystal, obtain gradual " black silicon " thin film layer of specific refractory power, be lower than 5% at 400-800 nm reflectivity by exponential attenuation.Since femtosecond pulse method and plasma method apparatus expensive, complex process, and area is little for " the black silicon " of preparation, and the technological operation of electrochemical erosion method is unfavorable for industrialization production.Metal assistant chemical etch preparation cost is low, and technology is simple, can realize big area industrialization production.2009; [Applied physics letters such as the breadboard Yuan H of U.S.'s renewable energy source C; 2009,95 (12): 123501 (1-3)] reported that as solar cell, the battery efficiency that obtains is 16.8% for " the black silicon " of step nano particle catalysis etching preparation.During one step nano particle catalysis etching preparation " black silicon ", get the p type twin polishing silicon chip of (100), silicon chip is immersed contain 0.4 mM HAuCl
4Solution, add HF:H with amount
2O
2: H
2In the O=1:5:2 mixing solutions, in ultrasonic tank, handle 1～8 min then, use I
2The ultrasonic Au that removes the surface of/KI solution uses deionized water rinsing and N again
2Dry up.At last through compromise reflectivity and internal quantum, its efficient reaches 16. 8% under the situation of traditional antireflective film not having through thick " black silicon " solar cell of the 500nm of 3min etching preparation.2011, [Applied Surface Science, 2011,257 (17): 7411-7414] such as the Liu Aimin of Dalian University of Technology utilize the auxiliary etch of Ag particle to prepare average reflectance 250 ~ 1000nm scope in was " deceiving silicon " structure of 0.9%.They at first prepare the pyramid matte with silicon chip in NaOH solution, pass through magnetron sputtering then at the netted silver-colored thin layer of matte surface deposition one deck, then adopt HF and H
2O
2Mixing solutions corrode.2011; The breadboard Fatima Toor of U.S.'s renewable energy source etc. [In:the 37th IEEE Photovoltaic Specialists Conference [C]. Seattle; Washington:Alliance for Sustainable Energy; 2011] further improved the performance of solar cell through adding the making herbs into wool step again, they use p type (100) silicon chip, soak 1min with 10%HF earlier and remove the silicon chip surface natural oxidizing layer.Then silicon chip is put into the KOH of 600ml 2.5% and the mixing solutions of 200ml Virahol preparation, in water-bath, corrode 25min under 80 ℃ of temperature.Then the silicon chip of making herbs into wool is put into 80 ℃ HCl:H
2O
2: H
2Leave standstill 10min in the O=1:1:5 solution to remove residual potassium impurity, make battery efficiency rise to 17.1%.In the same year, Xia Yang seminar of Microelectronic Institute of China Chinese Academy of Sciences [Solar Energy, 2011,85:1574-1578] has prepared " black silicon " through the reactive ion etching method, is 1.79% at the average reflectance of 300 ~ 1000nm scope.With being somebody's turn to do the transformation efficiency that makes " deceiving silicon " battery is 15.68%, and wherein packing factor is 0.783.But the metal that in existing metal assistant chemical etch, is utilized all is a precious metal, and this is unfavorable for the reduction of production cost very much.Therefore, the metals ion of seeking a kind of cheapness is the key of preparation low-cost " black silicon ".
Summary of the invention
The method of a kind of low-cost preparation " black silicon ".Method used in the present invention have preparation technology simple, need not complex apparatus, preparation cost is low and can realizes characteristics such as big area industrialization production; Alternative traditional antireflective coating; Reduce the luminous reflectance of silicon chip surface; Improve the solar cell transformation efficiency, finally reduce the preparation cost of solar cell.
The method of low cost preparation " black silicon " involved in the present invention realizes through following technical scheme, specifically comprises following step:
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into inferior quality fractional NaOH solution, thereby under the water-bath environment, corrode for some time in silicon chip surface formation pyramid shape structure;
(4) be placed on subsequently in the mixing solutions of HF, manganese salt and ultrapure water and carry out chemical corrosion on pyramid, to prepare nano-micro structure, i.e. " black silicon ".
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
Wherein, the purity of step (1), (2) and (3) described acetone, ethanol and NaOH is analytical pure;
The massfraction of NaOH is 2% ~ 2.5% in the step (3), and bath temperature is 70 ~ 85 ℃, and etching time is 20 ~ 40min.
The described manganese salt of step (4) comprises Mn (NO
3)
2, Mn (NO
3)
3, K
2MnO
4And KMnO
4
The described HF concentration of step (4) is 1 ~ 20M, Mn (NO
3)
2, Mn (NO
3)
3, K
2MnO
4And KMnO
4Concentration is 0.1 ~ 1M, and etching time is 5 ~ 60min, and corrosion temperature is 0 ~ 80 ℃.
The principle of the invention:
Use Mn ion assistant chemical etch corrosion monocrystalline silicon piece, through control corrosive fluid concentration and etching time, at pyramid surface preparation nano-micro structure, promptly black silicon, this structure has excellent reflection preventing ability.Particularly, in HF, add Mn (NO
3)
2, Mn (NO
3)
3, K
2MnO
4And KMnO
4In after any, when adding Mn (NO
3)
2The time, generated HNO in the solution
3, Mn
2+By HNO
3Be oxidized to Mn
3+And MnO
2Deposition, Mn
3+Has oxidisability, at Mn
3+And HNO
3Dual function under, Si loses electronics and is corroded into nano-micro structure; And when adding Mn (NO
3)
3The time, Mn
3+And HNO
3Can directly corrode silicon jointly; K
2MnO
4And KMnO
4Middle Mn ion is in high price, and the tool strong oxidizing property can directly be corroded silicon.
Mn ion assistant chemical etch be a kind of simple, low-cost, can realize big area industrialization " black silicon " preparation method.
Beneficial effect
1, the present invention compares with existing Au, Pt, Ag assistant chemical etch; Used cheap Mn ion to carry out assistant chemical corrosion monocrystalline silicon piece with preparation " black silicon " structure; Through control etchant solution concentration and etching time, go out nano-micro structure to reach antireflecting effect in the pyramid surface preparation;
2, the present invention and femtosecond pulse method, methods such as plasma processing method compare that to have technology simple, need not expensive equipment, advantage such as preparation cost is low; Compare with electrochemical erosion method, metals ion assistant chemical etch need not additional power source, and operation is extremely simple, and raising solar cell efficiency of conversion is reduced cost has potential using value.
Description of drawings
Fig. 1 is the photomacrograph before and after embodiment 1 corrosion; Before wherein (a) corrodes for the Mn ion is auxiliary, (b) for after the auxiliary corrosion of Mn ion;
Fig. 2 is the SEM figure after embodiment 1 corrosion: (a) cross-sectional view, (b) vertical view;
Fig. 3 is the SEM figure after embodiment 7 corrosion: (a) cross-sectional view, (b) vertical view;
Fig. 4 is the reflectance curve before and after the sample corrosion among Fig. 2: (a) before the corrosion, (b) after the corrosion.
Embodiment
Below in conjunction with embodiment the present invention is further described, but should not limit protection scope of the present invention with this.
Embodiment 1
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2.5% NaOH solution, thus 70 ℃ down corrosion 40min form the pyramid shape structure at silicon chip surface;
(4) be placed on 20M HF, 1 M Mn (NO subsequently
3)
2With under 80 ℃, carry out chemical rotten 5min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.6% in 200 ~ 1000nm scope.
Embodiment 2
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2% NaOH solution, thus 85 ℃ down corrosion 20min form the pyramid shape structure at silicon chip surface;
(4) be placed on 1M HF, 0.2M Mn (NO subsequently
3)
2With under 0 ℃, carry out chemical rotten 60min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.76% in 200 ~ 1000nm scope.
Embodiment 3
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2.5% NaOH solution, thus 70 ℃ down corrosion 40min form the pyramid shape structure at silicon chip surface;
(4) be placed on 20M HF, 1 M Mn (NO subsequently
3)
3With under 80 ℃, carry out chemical rotten 5min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.5% in 200 ~ 1000nm scope.
Embodiment 4
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2% NaOH solution, thus 85 ℃ down corrosion 20min form the pyramid shape structure at silicon chip surface;
(4) be placed on 1M HF, 0.2M Mn (NO subsequently
3)
3With under 0 ℃, carry out chemical rotten 60min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.61% in 200 ~ 1000nm scope.
Embodiment 5
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2.5% NaOH solution, thus 70 ℃ down corrosion 40min form the pyramid shape structure at silicon chip surface;
(4) be placed on 20M HF, 1 M K subsequently
2MnO
4With under 80 ℃, carry out chemical rotten 5min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.63% in 200 ~ 1000nm scope.
Embodiment 6
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2% NaOH solution, thus 85 ℃ down corrosion 20min form the pyramid shape structure at silicon chip surface;
(4) be placed on 1M HF, 0.2M K subsequently
2MnO
4With under 0 ℃, carry out chemical rotten 60min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.71% in 200 ~ 1000nm scope.
Embodiment 7
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2.5% NaOH solution, thus 70 ℃ down corrosion 40min form the pyramid shape structure at silicon chip surface;
(4) be placed on 20M HF, 1 M KMnO subsequently
4With under 80 ℃, carry out chemical rotten 5min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.54% in 200 ~ 1000nm scope.
Embodiment 8
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece, to remove
Silicon chip surface greasy dirt and metals ion;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down,
Remove the silicon chip affected layer on two surfaces up and down;
(3) then will go the silicon chip of affected layer to put into massfraction is 2% NaOH solution, thus 85 ℃ down corrosion 20min form the pyramid shape structure at silicon chip surface;
(4) be placed on 1M HF, 0.2M KMnO subsequently
4With under 0 ℃, carry out chemical rotten 60min in the mixing solutions of ultrapure water;
(5) with a large amount of ultrapure waters sample is washed at last, with impurity such as removal kish ions.
The result: average reflectance is 2.48% in 200 ~ 1000nm scope.
Claims (5)
1. the method for a low-cost preparation " black silicon " is characterized in that, comprises the steps:
(1) at first use acetone, ethanol and ultrapure water successively to each ultrasonic cleaning 10min of monocrystalline silicon piece;
(2) then silicon chip being put into massfraction is 25% NaOH solution, at 85 ℃ of corrosion 5min down;
(3) silicon chip is put into NaOH solution, thereby corrosion forms the pyramid shape structure at silicon chip surface under the water-bath environment;
(4) be placed on subsequently in the mixing solutions of HF, manganese salt and ultrapure water and carry out chemical corrosion on pyramid, to prepare nano-micro structure, i.e. " black silicon ";
(5) with ultrapure water sample is washed at last, remove impurity.
2. the method for a kind of low-cost preparation according to claim 1 " black silicon " is characterized in that the purity of step (1), (2) and (3) described acetone, ethanol and NaOH is analytical pure.
3. " method of black silicon is characterized in that, the massfraction of NaOH is 2% ~ 2.5% in the step (3), and bath temperature is 70 ~ 85 ℃, and etching time is 20 ~ 40min in a kind of low-cost preparation according to claim 1.
4. the method for a kind of low-cost preparation according to claim 1 " black silicon " is characterized in that the described manganese salt of step (4) comprises Mn (NO
3)
2, Mn (NO
3)
3, K
2MnO
4And KMnO
4
5. the method for a kind of low-cost preparation according to claim 1 " black silicon " is characterized in that the described HF concentration of step (4) is 1 ~ 20M, and manganese salt is Mn (NO
3)
2, Mn (NO
3)
3, K
2MnO
4Or KMnO
4,Above-mentioned manganese salt concn is 0.1 ~ 1M, and etching time is 5 ~ 60min, and corrosion temperature is 0 ~ 80 ℃.
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|---|---|---|---|---|
| CN103489942A (en) * | 2013-10-14 | 2014-01-01 | 南开大学 | Light trapping structure based on nano-zinc oxide silicon heterojunction battery, and preparation method of the light trapping structure |
| CN104332526A (en) * | 2014-08-26 | 2015-02-04 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing black silicon |
| CN104576813A (en) * | 2013-10-14 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Nanostructure suede of photoelectric material surface and preparation method of nanostructure suede |
| CN108447943A (en) * | 2018-03-23 | 2018-08-24 | 浙江师范大学 | Simple and effective store method after a kind of Wafer Cleaning |
| CN110265296A (en) * | 2019-06-25 | 2019-09-20 | 中国科学院电工研究所 | A kind of method of silicon chip erosion, the method in silicon chip surface preparation antireflective flannelette and the method in silicon chip surface etching special pattern |
| CN111040766A (en) * | 2019-12-25 | 2020-04-21 | 中国科学院电工研究所 | Polycrystalline silicon wafer texturing solution, preparation method of black silicon material and application of black silicon material in accelerating PERC battery LeTID recovery |
| CN111139076A (en) * | 2018-11-06 | 2020-05-12 | 中国科学院电工研究所 | Chemical corrosive liquid and application thereof |
| CN113707740A (en) * | 2020-05-06 | 2021-11-26 | 南京理工大学 | Preparation method of black silicon material |
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| CN103489942A (en) * | 2013-10-14 | 2014-01-01 | 南开大学 | Light trapping structure based on nano-zinc oxide silicon heterojunction battery, and preparation method of the light trapping structure |
| CN104576813A (en) * | 2013-10-14 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Nanostructure suede of photoelectric material surface and preparation method of nanostructure suede |
| CN104576813B (en) * | 2013-10-14 | 2017-10-13 | 中国科学院宁波材料技术与工程研究所 | A kind of nanostructured matte on photoelectric material surface and preparation method thereof |
| CN104332526A (en) * | 2014-08-26 | 2015-02-04 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing black silicon |
| CN108447943A (en) * | 2018-03-23 | 2018-08-24 | 浙江师范大学 | Simple and effective store method after a kind of Wafer Cleaning |
| CN111139076A (en) * | 2018-11-06 | 2020-05-12 | 中国科学院电工研究所 | Chemical corrosive liquid and application thereof |
| CN111139076B (en) * | 2018-11-06 | 2021-04-16 | 中国科学院电工研究所 | Application of chemical corrosion liquid in texturing of surface of silicon wafer |
| CN110265296A (en) * | 2019-06-25 | 2019-09-20 | 中国科学院电工研究所 | A kind of method of silicon chip erosion, the method in silicon chip surface preparation antireflective flannelette and the method in silicon chip surface etching special pattern |
| CN110265296B (en) * | 2019-06-25 | 2022-03-01 | 中国科学院电工研究所 | Method for etching silicon wafer, method for preparing anti-reflection texture surface on surface of silicon wafer and method for etching specific pattern on surface of silicon wafer |
| CN111040766A (en) * | 2019-12-25 | 2020-04-21 | 中国科学院电工研究所 | Polycrystalline silicon wafer texturing solution, preparation method of black silicon material and application of black silicon material in accelerating PERC battery LeTID recovery |
| CN111040766B (en) * | 2019-12-25 | 2021-05-25 | 中国科学院电工研究所 | Polycrystalline silicon wafer texturing solution, preparation method of black silicon material and application of black silicon material in accelerating PERC battery LeTID recovery |
| CN113707740A (en) * | 2020-05-06 | 2021-11-26 | 南京理工大学 | Preparation method of black silicon material |
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Application publication date: 20120912 Assignee: Jiangsu KangBo new Mstar Technology Ltd Assignor: Nanjing University of Aeronautics and Astronautics Contract record no.: 2019320000048 Denomination of invention: Method for preparing black silicon through Mn ion catalysis and corrosion Granted publication date: 20150701 License type: Exclusive License Record date: 20190321 |