CN102097535A - Method for preparing moth-eye structure for antireflection on surface of solar battery - Google Patents
Method for preparing moth-eye structure for antireflection on surface of solar battery Download PDFInfo
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Abstract
The invention discloses a method for preparing a moth-eye structure for antireflection on the surface of a solar battery, which comprises the following steps: 1, cleaning an epitaxial wafer used by the solar batter; 2, spin-coating photoresist on the epitaxial wafer; 3, prebaking the photoresist to form a sample; 4, carrying out double exposure and development on the sample by two-beam interference exposure equipment to form a two-dimension periodic photoresist mask pattern; 5, carrying out after-baking on the developed sample; 6, performing dry etching on the sample; and 7 removing the photoresist mask pattern in order to complete the preparation of the moth-eye structure.
Description
Technical field
The present invention relates to the semiconductor photoelectric device technical field, refer more particularly to the preparation method who is used for the antireflecting moth ocular structure of solar cell surface.
Background technology
Sunlight enters semiconductor layer from air, and air refraction is 1, and semi-conducting material such as GaAs, and the Si refractive index is more than 3, thereby can form big refractive index step at the interface, and consequent Fresnel reflection can the energy of loss more than 30%.General solution is to adopt the deielectric-coating of 1/4 λ wavelength as anti-reflecting layer at present, but its limited bandwidth; The multilayer dielectricity anti-reflecting layer has wide spectrum anti-reflection effect, but be subject to the selection and the coupling of layers of material refractive index, the thermal coefficient of expansion difference on rete border, and the problems such as diffuse of rete interface appearance, device reliability and stability are not good, particularly work as work under extreme conditions, as excessive temperature, this type of problem is particularly outstanding.Be subjected to the inspiration of the wide spectrum anti-reflection function of nature moth ocular structure, we propose to prepare class moth ocular structure, and it is used for solar cell as anti-reflecting layer, to improve absorption and the increase cell photoelectric conversion efficiency to light.The moth ocular structure is actual to be a kind of two-dimentional sub-wavelength binary cycle nanostructure, and sidewall slope can equivalence be the anti-reflecting layer with graded index.Only there is zero order light reflected in the character of its sub-wavelength when making light incident, has suppressed reflection further, and this character is particularly evident when varied angle incident, makes reflectance spectrum insensitive to the variation of incident angle.Moth eye anti-reflection structure is compared with the anti-reflection structure of assembly of thin films, has higher reliability, because the subsurface material homogeneity of itself and device does not exist the material coefficient of thermal expansion coefficient not match and the interfacial diffusion problem, be particularly suitable under extreme conditions, as working in the space.
Because of we towards to as if solar spectrum, the cycle of prepared moth ocular structure must be littler than the lower limit-350nm of solar spectrum.Prepare the periodic structure under the yardstick like this, can use electron beam exposure, focused-ion-beam lithography is realized.Though they have the high resolution and the graphic making degree of freedom, productive rate is very low, and is not suitable for large-scale industrial production.Though there is not this problem in nanometer embossing, its employed template need be made earlier by other micro-nano process technologies.Self-organizing growth technology efficiency-cost ratio height, but its long-range periodicity is relatively poor, and different Semiconductor substrate is not had versatility.It is the most effective to interfere exposure technique to be considered to prepare the large tracts of land periodic nano-structure, one of Jing Ji method the most, and be widely used in the middle of the preparation of commercial Distributed Feedback Laser modeling grating.
In order to prepare the moth eye anti-reflection structure that can be used on the solar cell, need etching depth greater than 300nm, in order to realize this point, need the pattern arrangement of preparation tight.Require its sidewall slope to distribute in addition to form graded index.These have all proposed very high requirement to preparation method and technology.
Summary of the invention
The objective of the invention is to, a kind of preparation method who is used for the antireflecting moth ocular structure of solar battery surface is provided, it is to utilize the two-beam interference exposure, in conjunction with the light distribution of the uniqueness that double exposes and the non-linear exposure response effect of photoresist, and preparation two-dimension periodic photoresist mask.Especially, compare with the photoresist dot matrix of traditional interference exposure preparation, prepared counterfeit rhombus array photoresist mask has bigger duty ratio, the water chestnut taper moth ocular structure that utilizes its dry etching to obtain, by theoretical with experimental results show that, traditional round taper moth ocular structure than being gone out by circular dot matrix photoresist mask etching has more excellent anti-reflection effect.
The invention provides a kind of preparation method who is used for the antireflecting moth ocular structure of solar battery surface, may further comprise the steps:
Step 1: get the used epitaxial wafer of a solar cell, epitaxial wafer is cleaned;
Step 2: spin coating photoresist on epitaxial wafer;
Step 3: photoresist is carried out preceding baking, form sample;
Step 4: adopt the two-beam interference exposure sources,, form two-dimension periodic photoresist mask pattern to sample double exposure, development;
Step 5: the sample after developing is carried out the back baking;
Step 6: sample is carried out dry etching;
Step 7: remove the photoresist mask pattern, finish the preparation of moth ocular structure.
Beneficial effect of the present invention, specific as follows:
Two-beam interference exposure preparation sub-wavelength scale lithography glue mask pattern is compared with other micro-nano process technologies, has low cost, large tracts of land, and the clear superiority of high yield is more suitable for suitability for industrialized production." counterfeit rhombus " photoresist mask technique and " photoresist expansion " technology of utilizing this patent to propose in addition, can overcome the shortcoming that the conventional interference exposure can only prepare the low duty ratio figure, obtain the dense arrangement figure of big space rate, help suppressing further boundary reflection.Because moth eye antireflecting structure needs enough degree of depth, and the cycle also is inferior solar spectral yardstick, wet etching can't reach needed constructional depth, thus adopt the inductively coupled plasma dry etching, and finally obtained the moth ocular structure of high-aspect-ratio.Through actual test shows, under nearly vertical incidence situation, all can realize good anti-reflection effect, only be 1.1% especially at AM1.5 spectrum average reflectance.
Description of drawings
For further specifying technical characterictic of the present invention, in conjunction with the following drawings, the present invention is done a detailed description, wherein:
Fig. 1 is the process chart that is used for the antireflecting moth ocular structure of solar cell surface;
Fig. 2 (a) is water chestnut taper moth eye anti-reflection structure figure;
Fig. 2 (b) is conical moth eye anti-reflection structure figure;
Fig. 3 is the exposure dose circle of equal altitudes that twice two-beam interference exposure forms on the photoresist surface;
Fig. 4 is the reflection spectrogram of the conical moth ocular structure under the 8 degree angle incident conditions;
Fig. 5 is the reflection spectrogram of the water chestnut taper moth ocular structure under the 8 degree angle incident conditions;
Fig. 6 is the reflection spectrogram of the big space rate water chestnut taper moth ocular structure under the 8 degree angle incident conditions.
Embodiment
See also shown in Fig. 1,2,3, a kind of preparation method who is used for the antireflecting moth ocular structure of solar battery surface of the present invention may further comprise the steps:
Step 1: get the used epitaxial wafer of a solar cell, epitaxial wafer is cleaned, this epitaxial wafer is single crystalline Si or GaAs based solar battery structure;
The cleaning method of GaAs base epitaxial wafer is: epitaxial wafer is placed acetone respectively, absolute ethyl alcohol, 55 ℃ were heated 3-5 minute, then rinse well with deionized water, nitrogen dries up, then put into boiling 15 minutes of negative glue stripper again, deionized water rinsing is clean, then puts into 120 ℃ of baking oven bakings 30 minutes; For Si base epitaxial wafer, use standard RCA ablution, to improve the adhesiveness of photoresist to substrate.
Step 2: need before the spin coating photoresist on epitaxial wafer, gluing institute is diluted with photoresist.In order to prepare needed two-dimension periodic photoresist mask pattern, the S9912 eurymeric photoresist that adopts Shipley company to produce, and cooperate corresponding D A3004 dilution is beneficial to obtain having behind the whirl coating glue-line of different-thickness.Especially, we adopt 5000 rev/mins rotating speed whirl coating 40s, obtained thickness and be the glue-line about 120nm, this glue is thick, and to access sidewall vertical, two-dimension periodic rhombus, circular array photoresist mask pattern, and make mask thicknesses be controlled at about 100nm, be beneficial to the figure that the later stage dry etching goes out high-aspect-ratio.
Step 3: photoresist is carried out preceding baking, form sample.The temperature of photoresist being carried out preceding baking is 90 ℃, and the time is 20 minutes;
Step 4: adopt the two-beam interference exposure sources,, form two-dimension periodic photoresist mask pattern to sample double exposure, development;
The exposure light source that adopts is that operation wavelength is the He-Cd laser of 325nm, and the minimum theoretical limit cycle that it can prepare is 170nm, therefore can be used in the making of Asia-Pacific sunlight spectrum periodic structure.To each exposure of sample, determine the periodicity of a direction.The moth ocular structure is a two-dimensionally periodic structure, therefore need double expose.And the angle of double exposure direction has determined that the distribution form of two-dimension periodic figure, angle are 60 degree, forms the triangular crystal lattice lattice structure, and angle is 90 when spending, and forms square grid lattice structure (consulting Fig. 3).
Utilize the character of the non-linear exposure response of photoresist, concrete control by exposure dose and development conditions, make shown in Figure 3 in, with exposure dose 4 contours as cutting apart, the exposure area that is higher than it shows in development fully to be gone, be lower than then after having developed, still keeping of its, thereby formed counterfeit rhombus two-dimension periodic pattern.Further, as cutting apart, the exposure area that is higher than it shows fully to be gone, and has then realized the preparation of two-dimension periodic dot matrix with exposure dose 2 contours.
The developer solution that adopts is tetramethyl ammonium hydroxide solution or Shipley Microposit 351 developer solutions.In the developing process of reality, need it dilutes to developer solution.Because used bondline thickness is less than 200nm, the concentration of developer solution should be less than 1: 5.
Accurately set the dual-beam angle of exposure, be 250nm performance period, and yardstick is less than the preparation of the structure of solar spectrum.The wavelength band of solar spectral is about 350-1000nm, in order to realize the effective inhibition to whole spectral reflectance, needs the careful cycle of selecting the moth ocular structure.Cycle, its reflecting effect to shortwave was not good greater than 350nm; Cycle, then long wave spectrum anti-reflection effect was not good less than 200nm.Thereby the optimal period scope is between the 200-350nm.
Step 5: the sample after developing is carried out the back baking, and the back baking time is 120 degree, and the time is 20 minutes, to remove the residual solvent in the photoresist, improves the anti-etching ability of photoresist mask.Interfered the limitation of the low contrast that exposes, the periodic pattern duty ratio that this technology prepares is less than normal, generally below 0.6.In order to form the pattern of big space rate, further, adopt 210 degree heat treated, heating 15s, duty ratio reaches 0.7, heating 22s, duty ratio reaches about 0.9.
Step 6: sample is carried out dry etching.Dry etching does not need to consider the influence in epitaxial wafer crystal orientation, in addition by the control etching parameters, can access the etching figure of advanced money ratio, satisfies the requirement of the moth eye anti-reflection structure degree of depth greater than 300nm.As adopt wet etching, under this yardstick, be difficult to obtain the figure of the degree of depth greater than 100nm.Because the moth ocular structure comes down to a kind of graded index structure, therefore requiring also needs to keep the sidewall slope of structure when obtaining expecting etching depth.Referring to water chestnut taper shown in Figure 2 and conical moth ocular structure, the top is sharp-pointed, and duty ratio is little; Duty ratio progressively increases from top to bottom, and reaches maximum in the bottom of moth ocular structure.
Step 7: remove the photoresist mask pattern, adopt hot acetone or oxygen gas plasma to remove photoresist.
Key problem in technology of the present invention mainly contains the following aspects:
The selection of the concrete thickness of photoresist
Learn that by calculating towards the moth ocular structure that improves efficiency of solar cell, the cycle is less than the lower limit of solar spectrum, i.e. 350nm.Best periodic regime should be between the 200-350nm.And to prepare the nanostructure of yardstick like this, can only the selection work wavelength less than the uv-exposure light source of 400nm.Use the He-Cd laser of wavelength in the present invention as 325nm.Under this wavelength, photoresist absorption of incident light be can not ignore.Consider the low contrast of interfering exposure self in addition, and we used be the high reflectance substrate, form minimum point for fear of vertical standing wave effect, usually thick half that is less than the vertical direction standing wave cycle of glue is (for the situation in 250nm cycle on the GaAs substrate, the vertical standing wave cycle is about 100nm), and this way can't obtain the steep photoresist figure of sidewall, and this external cause mask thickness is limited, can't obtain the etching figure of high-aspect-ratio.We utilize photoresist thickness mudulation effect (CN101738662A), select the thick photoresist of 110-130nm for use, and it is thick in more than the 100nm finally to obtain glue, the two-dimension periodic photoresist mask pattern of counterfeit rhombus and circular dot-matrix array, and sidewall is vertical.
The difference of the manufacture craft of " counterfeit-rhombus " and dot matrix
The limitation of being interfered the self-technique that exposes can't obtain the figure of high duty ratio.And high duty ratio actual be exactly more compact arranged distribution, for obtaining of utmost point antiradar reflectivity, play crucial effects.Consider after the double exposure that in the light distribution (referring to Fig. 3) on photoresist glue-line surface when preparing circular dot matrix, that in fact takes only stays the zone that exposure dose is 0-2, and must control all the other zones of removal by exposure dose and development conditions.In this course, if only make high exposure area (greater than 4) be removed, keep low exposure and intermediate exposures amount district, then can obtain shown in Figure 3 is the formed rhombus array of contour of " 4 " by dosage.The round dot matrix that the rhombus that forms by the contour in the comparison diagram 3 " 4 " and contour are " 2 ", rhombus tightr than circular dot matrix arrangement occupies bigger area in single single primitive unit cell as can be seen.Be the glue-line that has adopted 120nm thick equally, high exposure area (greater than 6) district can show clean fully, and sidewall is steep, and low exposure area (0-2) does not then almost change, and the intermediate exposure that falls between can be embodied in the variation of glue-line height along with the difference of concrete exposure dose.Consider the isotropism in the process of actual development, actually can't obtain proper lozenge diagram, so we are with its called after " counterfeit rhombus " pattern.Counterfeit rhombus array photoresist pattern as etching mask, is obtained water chestnut taper moth ocular structure; Round dot matrix photoresist pattern as etching mask, is obtained conical moth ocular structure;
Change the duty ratio of mask by the photoresist flow technique
Propose the counterfeit rhombus pattern of preparation above us, obtained the more pattern of dense arrangement.On this basis, we propose the duty ratio that the photoresist flow technique further improves figure.It is compared with the method that developing time is controlled duty ratio with simple control exposure, has better reliability and repeatability.The photoresist flow technique is actual to be to have utilized photoresist can become these characteristics for colloid after being higher than vitrification point.Photoresist mask pattern by heating has formed makes photoresist become colloid, and is subjected to capillary effect, and the photoresist that becomes colloid is promptly constantly filled original zone that is not capped for little by little expanding towards horizontal direction.Simultaneously, highly also can diminish gradually.
In actual fabrication, we adopt following technological process:
The cleaning of solar battery epitaxial wafer
GaAs based solar battery epitaxial wafer is put into acetone successively, absolute ethyl alcohol, 55 ℃ were heated 3-5 minute down, carried out ultrasonic cleaning simultaneously and handled.Then use deionized water rinsing 40 times, the N2 air-blowing is done.Further place negative glue stripper to boil 15 minutes, then use washed with de-ionized water, the N2 air-blowing is done.The epitaxial wafer that cleaning is finished is put in the culture dish, puts into 120 ℃ of dehydrations 30 minutes in the lump.
For single crystalline Si based solar battery epitaxial wafer, then adopt the RCA method of standard clear.
Whirl coating obtains the bondline thickness of 120nm
The photoresist good with dilution evenly is coated in the epitaxial wafer surface, and adjusting whirl coating platform rotating speed is 5000 rev/mins, gets rid of 40 seconds.And dried by the fire 20 minutes before being placed on 90 ℃ of baking ovens.
Adopt the He-Cd laser of 325nm that sample is exposed.Prepare counterfeit rhombus, the needed single exposure time of circular array pattern is respectively 55s and 60s.In order to obtain a square grid array, after exposure is finished for the first time, sample revolved turn 90 degrees, and then carry out next step exposure.Along with the adjustment of interfering exposure system and the variation of light source power, the time for exposure is not unalterable, and what therefore really need control is total exposure dose, and this can realize by main passive exposure striped reponse system;
Developing time is decided according to the exposure that reality adopts.The developer solution that adopts is that (Tetramethylammonium hydroxide: proportioning deionized water), actual developing time was judged in the variation of dissolving by the real-time monitored photoresist in developing process (as can be by the change of diffraction intensity) in 1: 8.For counterfeit-argyle design, developing time is generally 10-15s; For the dot matrix pattern, developing time is 20-25s.
After having developed sample was put into 120 ℃ of baking oven post bakes 20 minutes, to improve adhesive force and the etch resistance of glue to substrate.If need carry out the photoresist flowing process to improve duty ratio, 210 ℃ of heating, duty ratio control heating time according to actual needs to sample.
Sample is put into inductively coupled plasma etching machine carry out etching processing, by changing process conditions, as gases used, pressure etc. obtain the moth eye GaAs with sloped sidewall of different aspect ratios, Si anti-reflection structure.
Sample after etching is finished is put in hot acetone and removes photoresist, and also can use oxygen plasma to remove photoresist, and obtains clean sample surfaces.
Be concrete example of making result below, the GaAs moth eye anti-reflection structure that checking the present invention prepares has good antireflective property.
Example 1: water chestnut taper GaAs moth eye surface anti-reflection structure
Preparation water chestnut taper GaAs moth eye surface anti-reflection structure needs counterfeit rhombus array photoresist mask.Referring to exposure dose Two dimensional Distribution shown in Figure 3, ideally resultingly should be rhombus but not Kong Zhen, but because the isotropism of developing process, and the space fluctuation of exposure dose in the exposure process, the nonideal diamond shape of the shape of real income.But counterfeit rhombus duty ratio is 1, only is 0.5 circular array photoresist mask greater than the prepared duty ratio of usual method.Through after the dry etching, obtain being similar to the water chestnut taper moth ocular structure of Fig. 2 (a), duty ratio is 1 also, the degree of depth has reached 450nm.Its reflectance spectrum measured under any polarised light 8 degree angle incident conditions as shown in Figure 4.Can calculate water chestnut taper moth eye surface anti-reflection structure for AM1.5 spectrum, average reflectance is 1.1%.
Example 2: conical GaAs moth eye surface anti-reflection structure
Prepare conical GaAs moth ocular structure, adopt the circular dot array mask of two-dimension periodic, obtain conical structure shown in Fig. 2 (b) by dry etching.Concrete steps are: the thick photoresist of (1) spin coating 120nm is in the GaAs substrate; (2) be put in before 90 ℃ in the baking oven baking 20 minutes; (3) two-beam interference exposure system exposure, double exposure gap rotation substrate 90 degree obtain a square dot matrix grid; (4) the control exposure is exposed the zone greater than contour 2 shown in Figure 3 fully, obtains potential circular port battle array; (5) carefully control developing time, show the two-dimensional circular dot-matrix array; (6) back baking; (7) ICP dry etching.Prepared conical GaAs moth ocular structure is similar to Fig. 2 (b), and the degree of depth is about 400nm, and duty ratio is between the 0.5-0.6.Under the situation of arbitrarily polarised light 8 degree angle incidents, measured reflectance spectrum as shown in Figure 5, with AM1.5 spectrum as a reference, the average reflectance that calculates gained is 2.56%.
Example 3: the GaAs moth eye surface anti-reflection structure that expands the counterfeit diamond shaped mask preparation of glue
The duty ratio that " counterfeit rhombus " mask is mentioned in the front can reach 1.But the rhombus pattern still can't occupy square single primitive unit cell zone that the length of side equals the cycle fully.The optimal square that is shaped as that occupies the unit born of the same parents fully, but sub-micrometer scale is difficult to utilize the method for crystal orientation wet etching to realize this purpose.Therefore the photoresist hot reflux method that adopts us to propose further enlarges the duty ratio of " counterfeit rhombus " mask single primitive unit cell cycle.Adopt 210 degree heating 22s, can further increase the area coverage of moth ocular structure, get on refractive index rank at the interface with subsurface material thereby reduce the moth ocular structure at single primitive unit cell.After the dry etching, obtain maximum etching depth 330nm.Its corresponding reflectance spectrum as shown in Figure 6, and to calculate its average reflectance be 2.9%.
Claims (10)
1. preparation method who is used for the antireflecting moth ocular structure of solar battery surface may further comprise the steps:
Step 1: get the used epitaxial wafer of a solar cell, epitaxial wafer is cleaned;
Step 2: spin coating photoresist on epitaxial wafer;
Step 3: photoresist is carried out preceding baking, form sample;
Step 4: adopt the two-beam interference exposure sources,, form two-dimension periodic photoresist mask pattern to sample double exposure, development;
Step 5: the sample after developing is carried out the back baking;
Step 6: sample is carried out at the method etching;
Step 7: remove the photoresist mask pattern, finish the preparation of moth ocular structure.
2. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, wherein used epitaxial wafer is single crystalline Si or GaAs based solar battery structure.
3. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, wherein said spin coating photoresist at first dilutes photoresist, and with 5000 rev/mins rotating speed whirl coating 40s, the thickness of spin coating photoresist is 100-130nm.
4. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1 wherein carries out preceding baking to photoresist, and temperature is 90 ℃, and the time is 20 minutes.
5. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, wherein said to sample double exposure, be the dual-beam angle of setting exposure, performance period, yardstick was less than the preparation of the structure of 350nm.
6. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1 wherein between the double exposure, with the sample rotation, obtains the two-dimension periodic interference optical field and distributes.
7. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, the developer solution of wherein selecting for use is tetramethyl ammonium hydroxide solution or Shipley Microposit351 developer solution, development 10-15s obtains counterfeit rhombus array pattern, and development 20-25s obtains the circular array pattern.
8. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, wherein sample carries out the back baking, and temperature is 120 ℃, and the time is 20 minutes, and the back baking temperature of big space rate figure is 210 ℃.
9. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1, wherein carry out dry etching, the degree of depth that makes the etching figure is greater than 300nm, and controls the sidewall slope that etching condition keeps the etching figure simultaneously, forms the graded index structure.
10. the preparation method who is used for the antireflecting moth ocular structure of solar battery surface according to claim 1 wherein adopts hot acetone or oxygen gas plasma to remove the photoresist mask pattern.
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| CN102263144A (en) * | 2011-07-29 | 2011-11-30 | 清华大学 | Semiconductor heterojunction solar cell based on bionic moth eye and manufacturing method thereof |
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| CN103107252B (en) * | 2013-02-27 | 2016-01-27 | 中国科学院物理研究所 | The method of class spherical structure is prepared on the GaP surface of AlGaInP base LED |
| CN103199161A (en) * | 2013-03-22 | 2013-07-10 | 中国科学院物理研究所 | Method for preparing cone-shaped structure on gallium phosphide (GaP) surface |
| CN103199161B (en) * | 2013-03-22 | 2016-01-06 | 中国科学院物理研究所 | A kind of method preparing cone structure on GaP surface |
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| CN107204386A (en) * | 2017-05-31 | 2017-09-26 | 浙江工业大学 | The method and thin-film solar cell structure of enhanced film solar cell photon absorption efficiency |
| WO2018231316A1 (en) * | 2017-06-16 | 2018-12-20 | Lawrence Livermore National Security, Llc | Nanostructured layer for graded index freeform optics |
| US10612145B2 (en) | 2017-06-16 | 2020-04-07 | Lawrence Livermore National Security, Llc | Nanostructured layer for graded index freeform optics |
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