CN103022266B - 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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- CN103022266B CN103022266B CN201310009297.3A CN201310009297A CN103022266B CN 103022266 B CN103022266 B CN 103022266B CN 201310009297 A CN201310009297 A CN 201310009297A CN 103022266 B CN103022266 B CN 103022266B
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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 falling into light synergy anti-reflection structure based on LSP effect.
Technical background
Silicon is semiconductor element the abundantest on the earth's crust, smelts purification technique technics comparing ripe, therefore becomes the primary raw material of solid electronic device.At present, silicon materials be applied in photovoltaic art growth rate higher than its growth rate in integrated circuit fields.Due to silicon materials wide material sources, cost is lower, at solar cell market dominate.Along with development and the progress of solar battery technology, improve the conversion efficiency of solar cell and to reduce costs be the research emphasis in solar cell field.Wherein, reducing the absorption of battery surface to the reflection of incident light and raising incident light is a kind of important means improving solar cell photoelectric conversion efficiency.Traditional antireflective measure mainly prepares TiO at the sensitive surface of surface of silicon or battery
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 utilizing 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, there is good reappearance, antireflective coating is prepared relative on Si surface, etching cost reduces greatly, and can combine with solar cell preparation technology, is conducive to suitability for industrialized production.On wet etching basis, utilize that the means such as plating, sputtering, silver mirror reaction, evaporation or self assembly deposit the equally distributed nanometer of one deck or submicrometer-thick at silicon chip surface, discrete noble metal granule is used for exciting LSP effect, the surface can improving solar cell further falls into optical efficiency.In these technological means, due to features such as the method for sputtering are simple, coating is even, be more and more subject to the favor of people.Traditional cone surface light trapping structure falls into light synergy in conjunction with the LSP of silver nano-grain as can be seen here, and light trapping structure preparation in solar cell top layer has very real using value.
Summary of the invention
Not enough for prior art, the invention provides a kind of preparation method falling into light synergy anti-reflection structure based on LSP effect.
A kind of preparation method falling into light synergy anti-reflection structure based on LSP effect, alkaline etching is first utilized to etch cone pattern at monocrystalline silicon surface, then sputtering-annealing means are utilized to deposit the method for the discrete silver nano-grain of one deck at cone surface, obtain the light trapping structure by silver nano-grain and cone structure compound, concrete steps are as follows:
A. be that (100) monocrystalline silicon piece of 8 Ω cm ~ 13 Ω cm is immersed in acetone soln by resistivity, ultrasonic 10min ~ 20min in 35 DEG C of water-baths; Then after clean with deionized water rinsing, ultrasonic 10min ~ 15min; Take out sample, be placed on soak at room temperature 3min ~ 5min in CP4A cleaning fluid, described CP4A cleaning fluid to be mass fraction be 40% hydrofluoric acid, acetic acid, mass fraction be the nitric acid of 65% ~ 68% and the mixed solution of ultra-pure water composition, wherein mass fraction is hydrofluoric acid, acetic acid, the mass fraction of 40% be the nitric acid of 65% ~ 68% and the volume ratio of ultra-pure water is 3:5:3:22; After finally soaking 2min ~ 3min with the hydrofluoric acid solution that mass fraction is 14%, taking-up is clean with deionized water rinsing, then dries up with nitrogen, puts into drier for subsequent use;
B. be the isopropyl alcohol configuration etching liquid of 8% by NaOH, volume fraction that mass fraction is 3%, wherein mass fraction be 3% NaOH and volume fraction be the volume ratio of the aqueous isopropanol of 8% be 25:2, under 80 DEG C of water bath condition, etch the sample 30min ~ 50min handled well through step a, etch cone structure at silicon face;
C. utilize the cone structure electroplate that high-resolution magnetron sputtering instrument is etching, sputtering current is 15mA ~ 50mA, sputtering time is 15s ~ 30s;
D. step c gained cone structure electroplate sample under nitrogen protection; under 350 DEG C ~ 400 DEG C conditions, annealing 2h ~ 3h, after cooling; form the discontinuous silver nano-grain of one deck particle diameter between 40nm ~ 100nm at silicon face, namely obtain falling into light synergy anti-reflection structure based on LSP effect.
Described (100) monocrystalline silicon piece is of a size of 2cm × 2cm.
Described deionized water resistivity is not less than 16 Ω cm.
Described cone pattern is one or more in pyramid, side's cone, circular cone and tetrahedral structure pattern.
Beneficial effect of the present invention is:
Utilize method of the present invention to prepare silicon face and fall into light Synergistic structure, by the method for the discontinuous silver nano-grain of surface coverage, make surface coverage have the cone structure of discontinuous silver nano-grain to obtain synergy in full solar spectrum scope optical property of caving in.Concrete effect shows as: in full solar spectrum scope, and it is low by 3.4% that surface is coated with the luminance factor of the light trapping structure of discontinuous silver nano-grain cone simple cone light trapping structure.The method is improve the conversion efficiency of silica-based solar cell to provide new effective technology means, for the exploitation of solar cell and industrialization provide new approaches.The present invention utilizes simple wet etching means, simple without specific condition requirement, processing ease, equipment requirement; Silver nano-grain sputter deposition craft is simpler than chemical synthesis process, save time, and the silver nano-grain obtained is even, can excite LSP effect well, thus ensure that the reflection preventing ability that structure is higher.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of the surperficial cone light trapping structure obtained after (100) monocrystalline silicon etches 35 minutes;
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 boundary inner surface is coated with the cone light trapping structure of Argent grain and the comparison curves of simple cone light trapping structure reflectivity.
Embodiment
The invention provides a kind of preparation method falling into light synergy anti-reflection structure based on LSP effect, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
1. (100) monocrystalline silicon piece being 12 Ω cm resistivity cuts into the sample of 2 × 2cm, is then immersed in acetone soln, ultrasonic 10min in 35 DEG C of water-baths; Then deionized water for ultrasonic 10min is immersed in after deionized water rinsing 3 times; Take out sample, be placed on soak at room temperature 5min in CP4A cleaning fluid; Finally soak after 2min with the hydrofluoric acid solution that mass fraction is 14%, take out sample, with deionized water rinsing 3 times, then dry up with nitrogen, put into drier for subsequent use.
2. under 80 DEG C of water bath condition, the sample 40min handled well through step 1 is etched with etching liquid, obtain the silicon chip of surperficial cone structure, can be observed in etching process a large amount of bubble the surface of silicon chip and around generate, the silicon face of light tarnishes along with the increase of etch period is dimmed gradually.After etching terminates, with the sample after deionized water rinsing etching, then use the ultrasonic 10min of deionized water, then use deionized water rinsing 3 times, finally dry up with nitrogen.
3. utilize high-resolution magnetron sputtering instrument silver-plated: sputtering current is 30mA, sputtering time is 30s, the silicon chip sample plated surface last layer silverskin after etching through step 2.
4. nitrogen atmosphere annealing: under the environment of nitrogen atmosphere protection, is the 3h that anneals at the temperature of 400 DEG C in temperature, makes the silverskin of sample surfaces be agglomerated into nano particle, thus forms 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 being coated with Argent grain at full solar spectrum boundary 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 surface cleaning, avoid Conventional cleaning methods consuming time, complex process, efficiency are lower and the shortcoming of equipment requirement harshness.For the monocrystalline silicon piece after cleaning, first etch sample with the mixed solution of NaOH and isopropyl alcohol, can be observed there is bubble formation with surface around silicon chip in course of reaction, along with the carrying out of etching, the metallic luster of silicon chip surface disappears.Cone light trapping structure is defined at monocrystalline silicon surface after etching; Then sputter one deck silverskin, by annealing process, form the silver nano-grain of the discontinuous distribution of one deck on the surface of cone light trapping structure, finally obtain the light trapping structure by silver nano-grain and cone structure compound.
Claims (4)
1. one kind is fallen into the preparation method of light synergy anti-reflection structure based on LSP effect, it is characterized in that, alkaline etching is first utilized to etch cone pattern at monocrystalline silicon surface, then sputtering-annealing means are utilized to deposit the method for the discrete silver nano-grain of one deck at cone surface, obtain the light trapping structure by silver nano-grain and cone structure compound, concrete steps are as follows:
A. be that (100) monocrystalline silicon piece of 8 Ω cm ~ 13 Ω cm is immersed in acetone soln by resistivity, ultrasonic 10min ~ 20min in 35 DEG C of water-baths; Then after clean with deionized water rinsing, ultrasonic 10min ~ 15min; Take out sample, be placed on soak at room temperature 3min ~ 5min in CP4A cleaning fluid, described CP4A cleaning fluid to be mass fraction be 40% hydrofluoric acid, acetic acid, mass fraction be the nitric acid of 65% ~ 68% and the mixed solution of ultra-pure water composition, wherein mass fraction is hydrofluoric acid, acetic acid, the mass fraction of 40% be the nitric acid of 65% ~ 68% and the volume ratio of ultra-pure water is 3:5:3:22; After finally soaking 2min ~ 3min with the hydrofluoric acid solution that mass fraction is 14%, taking-up is clean with deionized water rinsing, then dries up with nitrogen, puts into drier for subsequent use;
B. be the isopropyl alcohol configuration etching liquid of 8% by NaOH, volume fraction that mass fraction is 3%, wherein mass fraction be 3% NaOH and volume fraction be the volume ratio of the aqueous isopropanol of 8% be 25:2, under 80 DEG C of water bath condition, etch the sample 30min ~ 50min handled well through step a, etch cone structure at silicon face;
C. utilize the cone structure electroplate that high-resolution magnetron sputtering instrument is etching, sputtering current is 15mA ~ 50mA, sputtering time is 15s ~ 30s;
D. step c gained cone structure electroplate sample under nitrogen protection; under 350 DEG C ~ 400 DEG C conditions, annealing 2h ~ 3h, after cooling; form the discontinuous silver nano-grain of one deck particle diameter between 40nm ~ 100nm at silicon face, namely obtain falling into light synergy anti-reflection structure based on LSP effect.
2. method according to claim 1, is characterized in that: described (100) monocrystalline silicon piece is of a size of 2cm × 2cm.
3. method according to claim 1, is characterized in that: described deionized water resistivity is not less than 16 Ω cm.
4. method according to claim 1, is characterized in that: one or both in the described cone pattern side of being cone and conical structure pattern.
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| 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 |
| CN104372301B (en) * | 2014-11-21 | 2017-06-23 | 国家纳米科学中心 | A kind of utilization radio-frequency magnetron sputter method prepares single dispersing, the method for controllable nanon size Argent grain |
| 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 |
| 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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| EP2034339A1 (en) * | 2006-06-16 | 2009-03-11 | FUJIFILM Corporation | Polarizing film for window and front window for vehicle |
| CN102299207A (en) * | 2011-08-30 | 2011-12-28 | 华北电力大学 | Method for manufacturing porous pyramid-type silicon surface light trapping structure for solar cell |
| CN102610692A (en) * | 2012-03-09 | 2012-07-25 | 润峰电力有限公司 | Method for preparing crystalline silicon nanometer and micrometer composite texture surface |
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| EP2034339A1 (en) * | 2006-06-16 | 2009-03-11 | FUJIFILM Corporation | Polarizing film for window and front window for vehicle |
| CN102299207A (en) * | 2011-08-30 | 2011-12-28 | 华北电力大学 | Method for manufacturing porous pyramid-type silicon surface light trapping structure for solar cell |
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