CN103022266A - Method for manufacturing novel light-trapping synergetic antireflection structure on basis of LSP (localized surface plasma) effect - Google Patents
Method for manufacturing novel light-trapping synergetic antireflection structure on basis of LSP (localized surface plasma) effect Download PDFInfo
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- CN103022266A CN103022266A CN2013100092973A CN201310009297A CN103022266A CN 103022266 A CN103022266 A CN 103022266A CN 2013100092973 A CN2013100092973 A CN 2013100092973A CN 201310009297 A CN201310009297 A CN 201310009297A CN 103022266 A CN103022266 A CN 103022266A
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Abstract
The invention belongs to the technical field of solar cells, and particularly relates to a method for manufacturing a novel light-trapping synergetic antireflection structure on the basis of an LSP (localized surface plasma) effect. The method includes etching a cone shape on the surface of monocrystalline silicon by alkali; and depositing a layer of discontinuous silver nanoparticles on the surface of a cone by means of sputtering and annealing to obtain the novel light-trapping structure with the silver nanoparticles and a cone structure which are compounded with one another. The reflectivity of the novel light-trapping synergetic antireflection structure is reduced by 3.4% within the total solar spectrum range as compared with a pure cone structure. The method for manufacturing the effective light-trapping structure includes simple and practical silicon wafer cleaning and silver nanoparticle sputtering and depositing technological procedures, and a constant-temperature wet etching means is combined with the LSP effect, so that an excellent antireflection effect is realized as compared with the traditional structure manufactured by alkaline etching, and design and manufacturing processes of the method provide novel technical means for improving the efficiency of silicon and the efficiency of a thin film silicon solar cell.
Description
Technical field
The invention belongs to technical field of solar batteries, particularly a kind of preparation method who falls into the novel anti-reflection structure of light synergy based on the LSP effect.
Technical background
Silicon is semiconductor element the abundantest on the earth's crust, smelts purification technique technique comparative maturity, therefore becomes the primary raw material of solid electronic device.At present, the silicon materials growth rate that is applied in the photovoltaic field has been higher than it in the growth rate of integrated circuit fields.Because the silicon materials wide material sources, cost is lower, at solar cell market dominate.Along with development and the progress of solar battery technology, improving the conversion efficiency of solar cell and reducing cost is the research emphasis in solar cell field.Wherein, reduce battery surface to the incident reflection of light and improve a kind of important means that the incident Optical Absorption is raising solar cell photoelectric conversion efficiency.Traditional antireflective measure mainly is that the sensitive surface at surface of silicon or battery prepares TiO
x(x≤2), SiN
xDeng antireflective coating.These methods generally need complicated equipment, and process is complicated, operation easier is large, and preparation cost is higher.And the silicon chip surface that utilizes wet etching to obtain has good anti-reflective effect, and the method just can be carried out at normal temperatures, equipment requirement is simple, processing ease, controllability are good, has good reappearance, with respect to preparing antireflective coating on the Si surface, the etching cost reduces greatly, and can combine with solar cell preparation technology, is conducive to suitability for industrialized production.On the wet etching basis, utilize the means such as plating, sputter, silver mirror reaction, evaporation or self assembly to be used for exciting the LSP effect at the silicon chip surface deposition equally distributed nanometer of one deck or submicron order thickness, discrete noble metal granule, the surface that can further improve solar cell falls into optical efficiency.In these technological means, because the characteristics such as the method for sputter is simple, coating is even more and more are subject to people's favor.This shows that traditional cone surface light trapping structure falls into light synergy in conjunction with the LSP of silver nano-grain, has very real using value in the preparation of solar cell top layer light trapping structure.
Summary of the invention
Not enough for prior art, the invention provides a kind of preparation method who falls into the novel anti-reflection structure of light synergy based on the LSP effect.
A kind of preparation method who falls into the novel anti-reflection structure of light synergy based on the LSP effect, utilize first alkaline etching to etch the cone pattern at monocrystalline silicon surface, then utilize sputter-annealing means in the method for the discrete silver nano-grain of cone surface deposition one deck, obtained by the compound novel light trapping structure of silver nano-grain and cone structure, concrete steps are as follows:
A. (100) monocrystalline silicon piece that with resistivity is 8 Ω cm ~ 13 Ω cm is immersed in the acetone soln, ultrasonic 10 min ~ 20 min in 35 ℃ of water-baths; Then after rinsing well with deionized water, ultrasonic 10 min ~ 15 min; Take out sample, be placed on soak at room temperature 3 min ~ 5 min in the CP4A cleaning fluid, described CP4A cleaning fluid is that mass fraction is that 40% hydrofluoric acid, acetic acid, mass fraction are the mixed solution that 65% ~ 68% nitric acid and ultra-pure water form, and wherein mass fraction is that 40% hydrofluoric acid, acetic acid, mass fraction are that 65% ~ 68% nitric acid and the volume ratio of ultra-pure water are 3:5:3:22; Be after 14% hydrofluoric acid solution soaks 2 min ~ 3 min with mass fraction at last, take out and rinse well with deionized water that then dry up with nitrogen, it is for subsequent use to put into drier;
B. be that 3% NaOH, volume fraction are 8% isopropyl alcohol configuration etching liquid with mass fraction, wherein mass fraction is that 3% NaOH and volume fraction are that the volume ratio of 8% aqueous isopropanol is 25:2, sample 30 min that etching is handled well through step 1 under 80 ℃ of water bath condition ~ 50 min etch cone structure at silicon face;
C. utilize high-resolution magnetron sputtering instrument at the cone structure electroplate of etching, sputtering current is that 15 mA ~ 50 mA, sputtering time are 15 s ~ 30 s;
D. step c gained cone structure electroplate sample is under nitrogen protection; under 350 ℃ ~ 400 ℃ conditions; 2 h ~ 3 h anneal; after cooling; form the discontinuous silver nano-grain of one deck particle diameter between 40 nm ~ 100 nm at silicon face, namely obtain falling into the novel anti-reflection structure of light synergy based on the LSP effect.
Described (100) monocrystalline silicon piece is of a size of 2 cm * 2 cm.
Described deionized water resistivity is not less than 16 Ω cm.
Described cone pattern is one or more in pyramid, square cone, circular cone and the tetrahedral structure pattern.
Beneficial effect of the present invention is:
Utilize method of the present invention to prepare silicon face and fall into the light Synergistic structure, by the method for the discontinuous silver nano-grain of surface coverage, so that the cone structure that surface coverage has a discontinuous silver nano-grain obtains synergy in the full solar spectrum scope optical property of caving in.Concrete effect shows as: in full solar spectrum scope, the surface be coated with the simple cone light trapping structure of the luminance factor of light trapping structure of discontinuous silver nano-grain cone low 3.4%.The method provides new effective technology means for the conversion efficiency that improves silica-based solar cell, for exploitation and the industrialization of solar cell provides new approaches.The present invention utilizes simple wet etching means, and is simple without specific condition requirement, processing ease, equipment requirement; The silver nano-grain sputter deposition craft is simpler than chemical synthesis process, save time, and the silver nano-grain that obtains is even, can excite well the LSP effect, thereby has guaranteed the reflection preventing ability that structure is higher.
Description of drawings
The electromicroscopic photograph of the surperficial cone light trapping structure that Fig. 1 obtains after 35 minutes for (100) monocrystalline silicon etching;
Fig. 2 is the electromicroscopic photograph at the discontinuous silver nano-grain of cone structure plated surface last layer;
Fig. 3 is that full solar spectrum scope inner surface is coated with the cone light trapping structure of silver-colored particle and the comparison curves of simple cone light trapping structure reflectivity.
Embodiment
The invention provides a kind of preparation method based on the sunken novel anti-reflection structure of light synergy of LSP effect, the present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
1. be resistivity the sample that (100) monocrystalline silicon piece of 12 Ω cm cuts into 2 * 2 cm, then be immersed in the acetone soln ultrasonic 10 min in 35 ℃ of water-baths; Then be immersed in deionized water for ultrasonic 10 min with behind the deionized water rinsing 3 times; Take out sample, be placed on soak at room temperature 5 min in the CP4A cleaning fluid; Be after 14% hydrofluoric acid solution soaks 2 min with mass fraction at last, take out sample, with deionized water rinsing 3 times, then dry up with nitrogen, it is for subsequent use to put into drier.
2. with etching liquid sample 40 min that etching is handled well through step 1 under 80 ℃ of water bath condition, obtain the silicon chip of surperficial cone structure, can be observed a large amount of bubbles on the surface of silicon chip in etching process and generate on every side, the silicon face of light is along with the increase of etch period dimmed tarnishing gradually.After etching finishes, with the sample after the deionized water rinsing etching, then use ultrasonic 10 min of deionized water, use again deionized water rinsing 3 times, dry up with nitrogen at last.
3. utilize high-resolution magnetron sputtering instrument silver-plated: sputtering current is that 30 mA, sputtering time are 30 s, the silicon chip sample plated surface last layer silverskin after process step 2 etching.
4. nitrogen atmosphere annealing: under the environment of nitrogen atmosphere protection, be annealing 3 h under 400 ℃ the temperature in temperature, so that the silverskin of sample surfaces is agglomerated into nano particle, thereby form the discrete silver nano-grain of one deck on cone light trapping structure surface, as shown in Figure 2.
5. the test comparison of reflectivity, the cone light trapping structure that is coated with silver-colored particle at full solar spectrum scope inner surface is lower by 3.4% than simple cone light trapping structure, as shown in Figure 3.
The present invention adopts (100) monocrystalline silicon piece, utilizes simple silicon wafer cleaning process, obtains the sample of cleaning surfaces, avoided the conventional clean method consuming time, complex process, efficient is lower and the shortcoming of equipment requirement harshness.For the monocrystalline silicon piece after cleaning, the mixed solution with NaOH and isopropyl alcohol carries out etching to sample first, can be observed silicon chip in the course of reaction on every side and there is bubble formation on the surface, along with the carrying out of etching, and the disappearance of the metallic luster of silicon chip surface.Formed the cone light trapping structure at monocrystalline silicon surface after the etching; Then sputter one deck silverskin by annealing process, forms the silver nano-grain of the discontinuous distribution of one deck on the surface of cone light trapping structure, finally obtain by the compound novel light trapping structure of silver nano-grain and cone structure.
Claims (4)
1. preparation method who falls into the novel anti-reflection structure of light synergy based on the LSP effect, it is characterized in that, utilize first alkaline etching to etch the cone pattern at monocrystalline silicon surface, then utilize sputter-annealing means in the method for the discrete silver nano-grain of cone surface deposition one deck, obtained by the compound novel light trapping structure of silver nano-grain and cone structure, concrete steps are as follows:
A. (100) monocrystalline silicon piece that with resistivity is 8 Ω cm ~ 13 Ω cm is immersed in the acetone soln, ultrasonic 10 min ~ 20 min in 35 ℃ of water-baths; Then after rinsing well with deionized water, ultrasonic 10 min ~ 15 min; Take out sample, be placed on soak at room temperature 3 min ~ 5 min in the CP4A cleaning fluid, described CP4A cleaning fluid is that mass fraction is that 40% hydrofluoric acid, acetic acid, mass fraction are the mixed solution that 65% ~ 68% nitric acid and ultra-pure water form, and wherein mass fraction is that 40% hydrofluoric acid, acetic acid, mass fraction are that 65% ~ 68% nitric acid and the volume ratio of ultra-pure water are 3:5:3:22; Be after 14% hydrofluoric acid solution soaks 2 min ~ 3 min with mass fraction at last, take out and rinse well with deionized water that then dry up with nitrogen, it is for subsequent use to put into drier;
B. be that 3% NaOH, volume fraction are 8% isopropyl alcohol configuration etching liquid with mass fraction, wherein mass fraction is that 3% NaOH and volume fraction are that the volume ratio of 8% aqueous isopropanol is 25:2, sample 30 min that etching is handled well through step 1 under 80 ℃ of water bath condition ~ 50 min etch cone structure at silicon face;
C. utilize high-resolution magnetron sputtering instrument at the cone structure electroplate of etching, sputtering current is that 15 mA ~ 50 mA, sputtering time are 15 s ~ 30 s;
D. step c gained cone structure electroplate sample is under nitrogen protection; under 350 ℃ ~ 400 ℃ conditions; 2 h ~ 3 h anneal; after cooling; form the discontinuous silver nano-grain of one deck particle diameter between 40 nm ~ 100 nm at silicon face, namely obtain falling into the novel anti-reflection structure of light synergy based on the LSP effect.
2. method according to claim 1, it is characterized in that: described (100) monocrystalline silicon piece is of a size of 2 cm * 2 cm.
3. method according to claim 1, it is characterized in that: described deionized water resistivity is not less than 16 Ω cm.
4. method according to claim 1, it is characterized in that: described cone pattern is one or more in pyramid, square cone, circular cone and the tetrahedral structure pattern.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103258718A (en) * | 2013-05-16 | 2013-08-21 | 华北电力大学 | Method for preparing crater-type porous silicon structure based on LSP effect |
| CN103866246A (en) * | 2014-01-24 | 2014-06-18 | 中国科学院长春光学精密机械与物理研究所 | Ag nano-material having ultraviolet band with hybrid quadrupole and preparation method thereof |
| CN104372301A (en) * | 2014-11-21 | 2015-02-25 | 国家纳米科学中心 | Method for preparing monodisperse size-controllable nanosilver particles by using radio frequency magnetron sputtering method |
| CN106206778A (en) * | 2016-08-30 | 2016-12-07 | 陕西师范大学 | A kind of crystalline silicon solaode and nano surface composite construction preparation method thereof |
| CN107046066A (en) * | 2017-03-09 | 2017-08-15 | 深圳大学 | With suede structure monocrystalline silicon piece and preparation method thereof and silicon solar cell |
| CN107302040A (en) * | 2017-06-22 | 2017-10-27 | 烟台南山学院 | The preparation method of Ag nano wire light trapping structures is inlayed based on wet etching silicon face |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103258718A (en) * | 2013-05-16 | 2013-08-21 | 华北电力大学 | Method for preparing crater-type porous silicon structure based on LSP effect |
| CN103258718B (en) * | 2013-05-16 | 2015-10-21 | 华北电力大学 | A kind of method based on LSP effect preparation " cratering " Porous Silicon structures |
| CN103866246A (en) * | 2014-01-24 | 2014-06-18 | 中国科学院长春光学精密机械与物理研究所 | Ag nano-material having ultraviolet band with hybrid quadrupole and preparation method thereof |
| CN104372301A (en) * | 2014-11-21 | 2015-02-25 | 国家纳米科学中心 | Method for preparing monodisperse size-controllable nanosilver particles by using radio frequency magnetron sputtering method |
| CN106206778A (en) * | 2016-08-30 | 2016-12-07 | 陕西师范大学 | A kind of crystalline silicon solaode and nano surface composite construction preparation method thereof |
| CN106206778B (en) * | 2016-08-30 | 2019-01-22 | 陕西师范大学 | A kind of crystalline silicon solar battery and its nano surface composite construction preparation method |
| CN107046066A (en) * | 2017-03-09 | 2017-08-15 | 深圳大学 | With suede structure monocrystalline silicon piece and preparation method thereof and silicon solar cell |
| CN107302040A (en) * | 2017-06-22 | 2017-10-27 | 烟台南山学院 | The preparation method of Ag nano wire light trapping structures is inlayed based on wet etching silicon face |
| CN107302040B (en) * | 2017-06-22 | 2018-11-20 | 烟台南山学院 | The preparation method of Ag nano wire light trapping structure is inlayed based on wet etching silicon face |
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