CN101876088B - Polycrystalline silicon texturing method - Google Patents
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- CN101876088B CN101876088B CN201010134689.9A CN201010134689A CN101876088B CN 101876088 B CN101876088 B CN 101876088B CN 201010134689 A CN201010134689 A CN 201010134689A CN 101876088 B CN101876088 B CN 101876088B
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- 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
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Abstract
The invention discloses a polycrystalline silicon texturing method which comprises low-temperature high-concentration acidizing fluid texturing, normal-temperature low-concentration acidizing fluid, alkali cleaning, ion removal and passivation. The invention provides more a proper acid treatment fluid and a corrosion texturing process for the polycrystalline silicon texturing to ensure that the removal of a mechanical damage layer on the surface of a silicon slice and the texturing are easier to control, can accurately control the texturing degree of the surface of the silicon slice and the thickness reduction of the silicon slice, shorten the texturing time, improve the texturing yield of a battery, reduce the surface reflectivity, increase the light absorption and the short-circuit current, and improve the photo-electricity conversion efficiency of the battery.
Description
[technical field]
The present invention relates to the manufacturing technology of solar cell, particularly relate to the making herbs into wool technology of polysilicon chip.
[background technology]
In recent years, polysilicon solar cell is higher with its efficiency of conversion, the feature of stable performance and moderate cost and obtain applying more and more widely, and its output has surmounted silicon single crystal, occupies the dominant position in market.
In order to improve the photoelectric transformation efficiency of solar cell, when making, need first to carry out chemical treatment to silicon chip, silicon face is made to make an effigurate matte of tool, due to the existence of matte, the reflectivity of body surface will reduce greatly, thus increases the absorption of light.The making herbs into wool of polysilicon chip carries out isotropic etch by chemical reaction at silicon chip surface, form intensive pit shape surface tissue, add the order of reflection of light at silicon chip surface, reduce light reflectance to greatest extent, increase the absorption of light, improve short-circuit current (Isc), and then improve photoelectric transformation efficiency.
At present, domestic solar energy polycrystalline silicon battery manufacturers etching device used has two classes, and a class is the flat etching device of import type, as the rena of Germany; Another kind of is domestic groove type etching equipment, and main manufacturing enterprise has: Shenzhen Jie Jiachuan company, Changsha the 48th institute, Beijing group of Sevenstar-HC etc.At home in solar energy polycrystalline silicon battery production enterprise, this two kind equipment all has application, and the flat equipment of external import is slightly many, and the cost of domestic groove type etching equipment is more much lower than the flat etching device of import, has more competitive superiority.The all suitable acid solution making herbs into wool method of this two classes etching device, its making herbs into wool flow process is: with nitric acid (HNO
3), hydrofluoric acid (HF), water (H
2o) and the mixing solutions of additive carry out making herbs into wool, and then wash through diluted alkaline, remove ion and passivation.According to polycrystalline corrosion technology development trend, groove type etching equipment is more suitable for large-scale low-cost and produces.Requirement for acid solution making herbs into wool is, should remove the mechanical damage layer of silicon chip surface comparatively up hill and dale, can carry out texturing making herbs into wool again to silicon chip surface.Can obtain without flower basket mark, corrosion matte without serious grain boundary corrosion, surface uniform, or obtain the effect of desirable " having little corrosion pit in large corrosion pit ", increase the order of reflection of light at silicon chip surface, thus reduce light reflectance, improve extinction efficiency.In existing leather producing process, acidic treatment liquid used generally adopts rich nitric acid system, nitric acid (HNO
3) volume fraction > 60%, hydrofluoric acid (HF) volume fraction > 20%, pure water (H
2and suitable additives (CH O)
3cOOH or dense H
2sO4 or dense H
3pO
4) mixing solutions, liquid temperature, at 5 DEG C-10 DEG C, must carry out circulating cooling.In actual production process, making herbs into wool speed and making herbs into wool effect are difficult to control.
In long-term production process, applicant learns through repetition test and observation analysis, it is not identical for carrying out removing mechanical damage layer with the acidic treatment liquid system needed for making herbs into wool and processing condition to polysilicon chip, remove silicon chip surface mechanical damage layer and need low temperature and high concentration acidic treatment liquid corrosion system, meticulous making herbs into wool then needs normal temperature lower concentration acidic treatment liquid corrosion system.An acid liquid corrosion making herbs into wool method, takes same acid system to remove affected layer simultaneously and making herbs into wool treatment process is unscientific, cannot accomplish that thoroughly can remove affected layer can obtain again desirable making herbs into wool effect.
Such as in groove type etching, adopt circulating cooling method, and at bottom land drawing liquid, the overflow of groove top completes circulation, and cause silicon chip bottom solution temperature relatively low, upper temp is relatively high, make between different chips and different sites making herbs into wool on same wafer uneven, affect making herbs into wool effect.Adding the last time, to enter sheet quantity more, cause speed of cooling relatively slow, because silicon chip surface temperature in making herbs into wool process rises very fast, and surface temperature is relatively high, be difficult to, while effectively removing affected layer, carry out desirable surface-texturing by traditional groove type etching method.
In view of the above problems, be necessary to provide a kind of new polycrystalline silicon texturing method to solve the problems referred to above.
[summary of the invention]
The object of this invention is to provide a kind of polycrystalline silicon texturing method, it can remove the mechanical damage layer on polysilicon chip surface better, the texturing making herbs into wool effect on polysilicon chip surface can be improved again, reduce the reflectivity of polysilicon chip, thus improve electricity conversion.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of polycrystalline silicon texturing method, it comprises the following steps: sour making herbs into wool, diluted alkaline is washed, remove ion and passivation, it is characterized in that: described sour making herbs into wool comprises the low temperature and high concentration acid making herbs into wool and normal temperature lower concentration acid making herbs into wool two steps implemented successively, and two step acid making herbs into wool acidic treatment liquid used is the mixed acid solution of nitric acid, hydrofluoric acid and pure water.
As the improvement of the technical program, in low temperature and high concentration acid making herbs into wool process, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein, and nitric acid (HNO
3) volume fraction be 40%-60%, the volume fraction of hydrofluoric acid (HF) is 10%-25%, pure water (H
2o) volume fraction is 15%-50%, under 0.1MPa air pressure, circulating cooling condition, controls liquid temperature at-10 DEG C-20 DEG C, and pass into 0.1-1.0m in mixed acid solution
3/ h nitrogen carries out disturbance, corrosion treatment 20 seconds-240 seconds, removes polysilicon chip surface mechanical damage layer, and realizes elementary making herbs into wool.
Further, in low temperature and high concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 46.5%, 18.6%, 34.9%, is put by polysilicon chip and states in mixed acid solution, in mixed acid solution, pass into 0.2m
3the nitrogen of/h carries out disturbance, and liquid temperature 15 DEG C, pressure is 0.1Mpa, under circulating cooling condition, corrodes 80 seconds.
Further, in low temperature and high concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 56.9%, 20.3%, 22.8%, polysilicon chip is put and states in mixed acid solution, in mixed acid solution, pass into 0.1m
3the nitrogen of/h carries out disturbance, and liquid temperature 8 DEG C, pressure is 0.1Mpa, and circulating cooling condition corrodes 50 seconds.
As the improvement of the technical program, in normal temperature lower concentration acid making herbs into wool process, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein nitric acid (HNO
3) volume fraction be 10%-20%, the volume fraction of hydrofluoric acid (HF) is 1%-8%, pure water (H
2o) volume fraction is 72%-89%, under room temperature, 0.1MPa air pressure conditions, passes into 0.1m to mixed acid solution
3/ h-1.0m
3/ h nitrogen carries out disturbance, corrodes 100 seconds-360 seconds, realizes the secondary hardening making herbs into wool on polysilicon chip surface.
Further, in normal temperature lower concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 18.2%, 6.5%, 75.3%, at room temperature, 0.1MPa, passes into 0.5m
3under the nitrogen of/h carries out disturbed conditions, corrosion making herbs into wool 120 seconds.
Further, in normal temperature lower concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 15.5%, 5.5%, 79%, at room temperature, 0.1MPa, passes into 0.8m
3under/h nitrogen carries out disturbed conditions, corrosion making herbs into wool 150 seconds.
Because existing sour making herbs into wool process decomposition is become low temperature and high concentration acid making herbs into wool and normal temperature lower concentration acid making herbs into wool two procedure by the present invention, and provide corresponding acidic treatment liquid system and corrosion leather producing process condition, the first step adopts low temperature and high concentration acid making herbs into wool, at-10 DEG C-20 DEG C, pressure is 0.1Mpa, pass under nitrogen carries out the condition of disturbance in oxytropism treatment solution, with high-concentration acidic wastewater treatment solution, surface damage layer is carried out to polysilicon chip and remove and elementary making herbs into wool; Second step then adopts normal temperature lower concentration acid making herbs into wool, and at normal temperature, pressure is 0.1Mpa, passes under nitrogen carries out the condition of disturbance, carry out two changes strengthening making herbs into wool with lower concentration acidic treatment liquid to polysilicon chip surface in oxytropism treatment solution; The present invention is that polycrystalline silicon texturing provides more suitable acidic treatment liquid and corrosion leather producing process condition, make the mechanical damage layer of silicon chip surface remove and making herbs into wool more easy to control, accurately can control the Reducing thickness of silicon chip surface making herbs into wool texturing degree and silicon chip, the making herbs into wool time can be shortened, improve the making herbs into wool yield rate of cell piece; Adopt polycrystalline etching method of the present invention can improve even concentration and the solution temperature homogeneity of acid solution, overcome the drawback that existing leather producing process exists, can obtain without flower basket mark, corrosion matte without serious grain boundary corrosion, surface uniform; Adopt polycrystalline etching method of the present invention can obtain the effect of desirable " having little corrosion pit in large corrosion pit ", increase the order of reflection of light at silicon chip surface, reflectivity is made to be reduced to 20% (see in Fig. 6 4) by 28% of existing groove type etching technology, increase the absorption of light, thus cell conversion efficiency is up to 16.5%.Adopt the etching method of polysilicon chip of the present invention, existing etching device can use, and the composition of acidic treatment liquid is determined, compounding process is ripe, without the need to adding other auxiliary agent and refrigerator, the acidic treatment liquid that the first step uses can be mixed with the strengthening making herbs into wool acidic treatment liquid of second step.Greatly reduce and change liquid frequency, decrease the usage quantity of chemical reagent, reduce production cost.The spent acid produced in production can effectively be processed by neutralization reaction, eliminates Pollution by Chemicals.
[accompanying drawing explanation]
Fig. 1 is the technical process frame diagram of a kind of polycrystalline silicon texturing method of the present invention.
Fig. 2 is the first step of the present invention acid making herbs into wool side pattern schematic diagram.
Fig. 3 is second step of the present invention acid making herbs into wool side pattern schematic diagram.
Fig. 4 is SEM (scanning electron microscope) figure of the first step acid making herbs into wool in embodiment one.
Fig. 5 is SEM (scanning electron microscope) figure of second step acid making herbs into wool in embodiment one.
Fig. 6 is that (wherein curve 1 is the reflectance curve in embodiment one after second step making herbs into wool to reflectance test comparison diagram in the present invention; Curve 2 is the reflectance curve in embodiment one after the first step making herbs into wool; Curve 3 is the reflectance curve in embodiment two after second step making herbs into wool; Curve 4 for reflectivity be the reflectance curve of 20%).
[embodiment]
Consult Fig. 1 below, illustrate the specific embodiment of the present invention:
A kind of polycrystalline silicon texturing method, comprise the following steps: low temperature and high concentration acid making herbs into wool, normal temperature lower concentration acid making herbs into wool acid making herbs into wool, diluted alkaline are washed, removed ion and passivation, and described low temperature and high concentration acid making herbs into wool and normal temperature lower concentration acid making herbs into wool acidic treatment liquid used are the mixed acid solution of nitric acid, hydrofluoric acid and pure water.
The first step, low temperature and high concentration acid making herbs into wool, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein, nitric acid (HNO
3) volume fraction be 40%-60%, the volume fraction of hydrofluoric acid (HF) is 10%-25%, pure water (H
2o) volume fraction is 15%-50%, under 0.1MPa air pressure, circulating cooling condition, controls liquid temperature at-10 DEG C-20 DEG C, and pass into 0.1-1.0m in mixed acid solution
3/ h nitrogen carries out disturbance, corrosion treatment 20 seconds-240 seconds, removes polysilicon chip surface mechanical damage layer, and realizes elementary making herbs into wool, while removing silicon chip surface mechanical damage layer rapidly, form shallow corrosion pit (effect of idealized formation Fig. 2) at silicon chip surface.
Second step, normal temperature lower concentration acid making herbs into wool, being washed through pure water by silicon chip after the first step process immerses in making herbs into wool acidic treatment liquid again, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively in the sour mixed solution of 10%-20%, 2%-8% and 72%-89%, under the condition of liquid temperature room temperature, 0.1MPa air pressure, 0.1-1.0m
3corrode making herbs into wool 100 seconds-360 seconds under the nitrogen disturbance of/h, secondary hardening making herbs into wool is carried out to silicon chip surface, shallow corrosion pit basis is carried out degree of depth making herbs into wool (effect of idealized formation Fig. 3), and then reduce surface albedo.
Acid making herbs into wool after, then carry out diluted alkaline wash, remove ion, passivation processing, its working method is prior art, does not repeat them here.
Embodiment one:
In low temperature and high concentration acid making herbs into wool process, nitric acid (HNO in described acidic treatment liquid
3) and hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 46.5%, 18.6%, 34.9%, and polysilicon chip being immersed temperature is in the above-mentioned mixed acid solution of 15 DEG C, under 0.1MPa air pressure conditions, in mixed acid solution, passes into 0.2m
3the nitrogen of/h carries out disturbance, corrosion treatment 80 seconds, form slightly wide shallow corrosion pit (width is at about 5um) at silicon chip surface, (see Fig. 4), grain boundary corrosion is shallow, intercrystalline is without obvious aberration, without flower basket mark, can obtain reflectivity is 28.01% (shown in curve in Fig. 6 2), effectively removes surface damage layer, reduce battery surface compound, surface light absorbs less.
In normal temperature lower concentration acid making herbs into wool process, nitric acid (HNO in described acidic treatment liquid
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 18.2%, 6.5%, 75.3%, at room temperature, 0.1MPa air pressure, 0.5m
3the 120 second time of making herbs into wool is corroded under the nitrogen disturbed conditions of/h, silicon chip surface formed little, width is narrow and uniform corrosion pit (width is about about 3um) (see Fig. 5), there is no obvious grain boundary corrosion, intercrystalline is without obvious aberration, silicon chip everywhere reflectivity is even, and silicon chip surface order of reflection increases, add the absorption of light.Can obtain reflectivity is 24.76% (shown in curve in Fig. 6 1).
Embodiment two:
The first step, low temperature and high concentration acid making herbs into wool.Nitric acid (HNO in described acidic treatment liquid
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 56.9%, 20.3%, 22.8%, and polysilicon chip being immersed temperature is in the above-mentioned acidic treatment liquid of 8 DEG C, at 0.1MPa air pressure, 0.1m
3corrode the 50 second time of making herbs into wool under the condition that the nitrogen disturbance of/h and refrigerating unit are opened, silicon chip surface corrosion pit is more shallow, and grain boundary corrosion is shallow, and intercrystalline, without obvious aberration, without flower basket mark, effectively removes surface damage layer, reduces battery surface compound.
Second step, normal temperature lower concentration acid making herbs into wool.Being washed through pure water by silicon chip after the first step process immerses in making herbs into wool acidic treatment liquid, wherein nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 15.5%, 5.5%, 79%, at room temperature, 0.1MPa normal atmosphere, 0.8m
3the 150 second time of making herbs into wool is corroded under the condition of/h nitrogen disturbance, described silicon chip surface forms little and uniform corrosion pit, and does not have obvious grain boundary corrosion, and intercrystalline is without obvious aberration, silicon chip everywhere reflectivity is even, and can obtain reflectivity is 23.40% (shown in curve in Fig. 6 3).
Embodiments of the invention are a lot, but making herbs into wool principle is identical, difference is: the parameter of low temperature and high concentration acid making herbs into wool and the normal temperature lower concentration acid concrete technology condition of making herbs into wool and acidic treatment liquid is different, such as: the concentration configuration of mixed acid solution, the temperature of sour making herbs into wool, pressure, the type of cooling, nitrogen disturbance flow are different, as long as select the concentration configuration span of mixed acid solution disclosed in this invention, adopt corresponding etching process condition, expection object of the present invention can be reached.According to instruction of the present invention and the requirement to polysilicon design parameter after corrosion, suitable adjustment can be carried out to parameters such as involved concentration, temperature, times.
The present invention, by the combination of two step making herbs into wool, improves the homogeneity of silicon chip surface corrosion pit, increases the absorption of light, reduce reflectivity, increase short-circuit current, improve the electricity conversion of battery while realizing removing affected layer.Meanwhile, do not give wastewater treatment build-up of pressure, can effectively be processed by general neutralization reaction; And the transformation for groove type etching machine requires simple, without the need to adding other refrigerating unit, only need add a common cell body, being applicable to the scale operation of operate continuously.
Claims (5)
1. a polycrystalline silicon texturing method, it comprises the following steps: sour making herbs into wool, diluted alkaline is washed, remove ion and passivation, it is characterized in that: described sour making herbs into wool comprises the low temperature and high concentration acid making herbs into wool and normal temperature lower concentration acid making herbs into wool two steps implemented successively, and two step acid making herbs into wool acidic treatment liquid used is the mixed acid solution of nitric acid, hydrofluoric acid and pure water;
In low temperature and high concentration acid making herbs into wool process, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein, and nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 40%-60%, 10%-25%, 15%-50%, polysilicon chip is put into above-mentioned mixed acid solution, and passes into 0.1-1.0m
3/ h nitrogen carries out disturbance, and liquid temperature-10 DEG C-20 DEG C, pressure 0.1Mpa, corrodes 20 seconds-240 seconds under circulating cooling condition, removes the mechanical damage layer on polysilicon chip surface, and realizes preliminary making herbs into wool;
In normal temperature lower concentration acid making herbs into wool process, nitric acid, the massfraction of acidic treatment liquid used to be massfraction be 55%-65% are the hydrofluoric acid of 40%-55% and the mixed acid solution of pure water, wherein nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 10%-20%, 1%-8% and 72%-89%, polysilicon chip is put into above-mentioned mixed acid solution, and passes into 0.1-1.0m
3/ h nitrogen carries out disturbance, is room temperature in liquid temperature, and pressure is corrode 100 seconds-360 seconds under the condition of 0.1Mpa, carries out strengthening making herbs into wool to polysilicon chip surface.
2. polycrystalline silicon texturing method as claimed in claim 1, is characterized in that: in low temperature and high concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 46.5%, 18.6%, 34.9%, is put by polysilicon chip and states in mixed acid solution, in mixed acid solution, pass into 0.2m
3the nitrogen of/h carries out disturbance, and liquid temperature 15 DEG C, pressure is 0.1Mpa, under circulating cooling condition, corrodes 80 seconds.
3. polycrystalline silicon texturing method as claimed in claim 1, is characterized in that: in low temperature and high concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 56.9%, 20.3%, 22.8%, polysilicon chip is put and states in mixed acid solution, in mixed acid solution, pass into 0.1m
3the nitrogen of/h carries out disturbance, and liquid temperature 8 DEG C, pressure is 0.1Mpa, and circulating cooling condition corrodes 50 seconds.
4. polycrystalline silicon texturing method as claimed in claim 1, is characterized in that: in normal temperature lower concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 18.2%, 6.5%, 75.3%, at room temperature, 0.1MPa, passes into 0.5m
3under the nitrogen of/h carries out disturbed conditions, corrosion making herbs into wool 120 seconds.
5. polycrystalline silicon texturing method as claimed in claim 1, is characterized in that: in normal temperature lower concentration acid making herbs into wool process, in described acidic treatment liquid, nitric acid (HNO
3), hydrofluoric acid (HF) and pure water (H
2o) volume fraction is respectively 15.5%, 5.5%, 79%, at room temperature, 0.1MPa, passes into 0.8m
3under/h nitrogen carries out disturbed conditions, corrosion making herbs into wool 150 seconds.
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| CN102634799A (en) * | 2011-02-15 | 2012-08-15 | 中山大学 | Solar cell emitting electrode corroding method |
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| CN102181940B (en) * | 2011-04-08 | 2012-07-18 | 光为绿色新能源股份有限公司 | Preparation method of multicrystalline silicon texture |
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| CN102254992A (en) * | 2011-07-04 | 2011-11-23 | 南昌航空大学 | Novel polycrystalline silicon etching process |
| CN102296369B (en) * | 2011-09-13 | 2013-02-06 | 江阴鑫辉太阳能有限公司 | Polycrystalline silicon acid texturing process |
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| CN102851743B (en) * | 2012-09-05 | 2016-12-21 | 浙江鸿禧能源股份有限公司 | A kind of method reducing polysilicon making herbs into wool surface reflectivity |
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| CN103346204B (en) * | 2013-06-07 | 2016-08-10 | 中利腾晖光伏科技有限公司 | A kind of polycrystalline chain type multistep process for etching |
| CN103394484B (en) * | 2013-08-02 | 2016-08-10 | 常州时创能源科技有限公司 | Cleaning after polysilicon solar cell silicon chip processed with acid floss |
| CN104746146A (en) * | 2013-12-25 | 2015-07-01 | 新奥光伏能源有限公司 | Monocrystalline silicon slice texturing method |
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