CN103184523B - The preparation method of a kind of silicon single crystal Wool-making agent and textured mono-crystalline silicon - Google Patents
The preparation method of a kind of silicon single crystal Wool-making agent and textured mono-crystalline silicon Download PDFInfo
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Abstract
The invention provides a kind of silicon single crystal Wool-making agent, comprise basic cpd and etching reagent; Described etching reagent comprises following component: the urea of 5wt% ~ 20wt%; The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%; Surplus is water.Silicon single crystal is placed in Wool-making agent provided by the invention, after heating, obtains textured mono-crystalline silicon.Adopt silicon single crystal Wool-making agent provided by the invention, the urea wherein comprised can be hydrolyzed and produce ammonia and carbonic acid gas, and the gas being conducive to producing in making herbs into wool process successfully overflows, and avoids the impact of gas on matte quality; And etching reagent provided by the invention can control the erosion rate of basic cpd to silicon face effectively; Etching reagent provided by the invention also has stronger soil removability, therefore, Wool-making agent provided by the invention can effectively reduce silicon chip surface occur bright piece, hickie, raindrop probability, make the type of pyramid matte little and evenly, thus the qualification rate of textured mono-crystalline silicon is significantly improved.
Description
Technical field
The present invention relates to silicon single crystal making herbs into wool technical field, particularly relate to the preparation method of a kind of silicon single crystal Wool-making agent and textured mono-crystalline silicon.
Background technology
Under the background of energy dilemma, the renewable energy sources such as sun power are more and more subject to people's attention.Sun power is a kind of primary energy source, is again renewable energy source, its aboundresources, both without the need to transport, again to environment without any pollution, for the mankind create a kind of new lifestyle, make society enter the epoch of a save energy less contamination.To in the utilizing of sun power, the research and development of solar cell obtains the great attention of people, and wherein monocrystaline silicon solar cell receives much concern due to its relatively high efficiency and low cost.
One of important step in monocrystaline silicon solar cell preparation process is exactly silicon single crystal making herbs into wool, by the surface wool manufacturing to silicon single crystal, the suede structure of similar pyramid can be formed at silicon chip surface, this suede structure can reduce silicon chip surface effectively to incident light reflectance, reduce the reflection of incident light, improve solar cell to the absorption of incident light, thus greatly can improve the efficiency of conversion of battery.Current existing method for making single crystal silicon into wool has: chemical corrosion method, reactive ion etching method, photolithography and mechanical carving groove method etc., wherein chemical corrosion method is because cost is low, productivity is high and method is simple, is widely used in monocrystaline silicon solar cell industry always.
Chemical corrosion method making herbs into wool normally adopts basic solution to corrode silicon chip surface.The different crystal faces of basic solution to silicon chip have different erosion rates, 100 crystal faces of silicon single crystal and other crystal faces are as compared with 111 crystal faces or 110 crystal faces, there is corrosion speed faster, due to this anisotropic corrosive property, the suede structure of similar pyramid can be formed at silicon chip surface.Monocrystalline silicon etching solution conventional in prior art comprises sodium hydroxide and Virahol, and wherein sodium hydroxide meeting and pasc reaction, erodes the silicon of plane of crystal, forms pyramid pyramid structure; In the process of sodium hydroxide and pasc reaction, there is hydrogen to produce, the effect of making herbs into wool can be affected, Virahol add the bubble can getting rid of generation, and Virahol also can reduce the surface tension of silicon chip, be conducive to the contact of sodium hydroxide and silicon chip surface, be beneficial to the formation of suede structure.But in making herbs into wool process, also there will be the phenomenon of caving in causing suede structure because the erosion rate of sodium hydroxide to silicon chip surface is too fast, therefore need to add additive in Wool-making agent, to suppress hydroxide ion to the erosion rate of silicon face, additive conventional in prior art comprises lactic acid, Sodium.alpha.-hydroxypropionate, vitamins B and water, additive can reduce the concentration of hydroxide ion effectively, slow down the corrosion of sodium hydroxide to silicon chip surface to a certain extent, be conducive to formation and the maintenance of pyramid matte.But the pyramid matte of the textured mono-crystalline silicon adopting this Wool-making agent comprising sodium hydroxide, Virahol and above-mentioned additive to obtain is uneven, causes the qualification rate of monocrystalline silicon suede lower.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of silicon single crystal Wool-making agent and textured mono-crystalline silicon, the type of the pyramid matte of the textured mono-crystalline silicon adopting silicon single crystal Wool-making agent provided by the invention to obtain is little and even, improves the qualification rate of textured mono-crystalline silicon.
The invention provides a kind of silicon single crystal Wool-making agent, comprise basic cpd and etching reagent;
Described etching reagent comprises following component:
The urea of 5wt% ~ 20wt%;
The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%;
Surplus is water.
Preferably, described etching reagent comprises the urea of 10wt% ~ 15wt%.
Preferably, described etching reagent comprises the Sodium.alpha.-hydroxypropionate of 3wt% ~ 6wt%.
Preferably, described basic cpd accounts for the mass percent of Wool-making agent is 0.5% ~ 3%.
Preferably, described basic cpd accounts for the mass percent of Wool-making agent is 1.5% ~ 2.5%.
Preferably, described basic cpd is sodium hydroxide, potassium hydroxide or sodium carbonate.
Preferably, described basic cpd is sodium hydroxide.
The invention provides a kind of preparation method of textured mono-crystalline silicon, comprise the following steps:
Silicon single crystal is placed in the silicon single crystal Wool-making agent described in technique scheme, after heating, obtains textured mono-crystalline silicon.
Preferably, the temperature of described heating is 70 DEG C ~ 90 DEG C.
Preferably, the time of described heating is 1000s ~ 1500s.
The invention provides a kind of silicon single crystal Wool-making agent, comprise basic cpd and etching reagent; Described etching reagent comprises following component: the urea of 5wt% ~ 20wt%; The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%; Surplus is water.Etching reagent in silicon single crystal Wool-making agent provided by the invention is the aqueous solution of urea and Sodium.alpha.-hydroxypropionate, wherein urea can be hydrolyzed and produce ammonia and carbonic acid gas, add the buoyancy of gas in Wool-making agent, be conducive to the surface tension overcoming silicon chip surface, thus the gas produced in making herbs into wool process is successfully overflowed, avoid the impact of gas on matte quality, and etching reagent provided by the invention can make hydroxide ion in Wool-making agent maintain the state of balance, thus effectively can control the erosion rate of basic cpd to silicon face, etching reagent provided by the invention also has stronger soil removability, therefore, Wool-making agent provided by the invention effectively can reduce silicon chip surface and occur bright piece, hickie, the probability of raindrop, make the type of the pyramid matte obtained little and evenly, thus reduce silicon chip to light reflectance, improve short-circuit current and efficiency of conversion, the qualification rate of textured mono-crystalline silicon is improved significantly.Experimental result shows, the qualification rate of the textured mono-crystalline silicon that silicon single crystal Wool-making agent provided by the invention obtains is 97% ~ 100%.In addition, not containing Virahol in silicon single crystal Wool-making agent provided by the invention, reduce production cost, and can not pollute operating environment due to the volatilization of Virahol, be conducive to the chemical oxygen demand (COD) reducing water body, reduce the pollution of leather producing process wastewater in waters.
Embodiment
The invention provides a kind of silicon single crystal Wool-making agent, comprise basic cpd and etching reagent;
Described etching reagent comprises following component:
The urea of 5wt% ~ 20wt%;
The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%;
Surplus is water.
Silicon single crystal Wool-making agent provided by the invention comprises basic cpd.Basic cpd can corrode the surface of monocrystalline silicon piece, and to silicon face, there is anisotropic corrosive property due to basic cpd, make silicon single crystal 100 crystal face and other crystal faces as compared with 111 crystal faces or 110 crystal faces, there is corrosion speed faster, therefore, it is possible to form the suede structure of pyramid shape on the surface of monocrystalline silicon piece.This suede structure formed can reduce monocrystalline silicon surface to incident light reflectance, increases monocrystalline silicon piece to the absorption of incident light, effectively improves the transformation efficiency of monocrystalline silicon battery.The reaction equation of basic cpd and silicon is:
In the present invention, described basic cpd is preferably sodium hydroxide, potassium hydroxide or sodium carbonate, is more preferably sodium hydroxide; The mass percent that described basic cpd accounts for Wool-making agent is preferably 0.5% ~ 3%, is more preferably 1.5% ~ 2.5%.
Comprise etching reagent in silicon single crystal Wool-making agent provided by the invention, described etching reagent comprises following component:
The urea of 5wt% ~ 20wt%;
The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%;
Surplus is water.
In the present invention, comprise urea in described etching reagent, urea has formula (I) structure, in weakly alkaline, hydrolysis reaction can occur in the solution, and produce ammonia and carbonic acid gas, the hydrolysis reaction equation of uric acid is:
NH
2CONH
2+H
2O＝2NH
3↑+CO
2↑。
The ammonia that hydrolysis of urea produces and carbonic acid gas can increase the buoyancy of silicon chip surface gas, make the buoyancy of gas be greater than the sticking power of silicon chip surface, thus the hydrogen that basic cpd and pasc reaction are produced easily depart from silicon chip surface.Gas can hinder the contact of basic cpd and silicon face in the gathering of silicon chip surface, adding of urea can make the gas of generation easily depart from silicon face, Wool-making agent is contacted with silicon face again corrode, thus make silicon chip surface corrode completely, avoid occurring bright piece, the underproof phenomenon such as raindrop at silicon chip surface, improve the quality of monocrystalline silicon piece texture, thus improve the qualification rate of textured mono-crystalline silicon.The present invention is not particularly limited described urea, adopts urea well known to those skilled in the art.In the present invention, in described etching reagent, the content of urea is 5wt% ~ 20wt%, is preferably 10wt% ~ 15wt%.
Etching reagent of the present invention comprises Sodium.alpha.-hydroxypropionate, and Sodium.alpha.-hydroxypropionate can be used as water retention agent, acidity regulator, antioxidant, raising agent, thickening material and stablizer.The present invention utilizes the character of the acidity adjustment of Sodium.alpha.-hydroxypropionate, to maintain the balance of hydroxide ion concentration in Wool-making agent, effectively controls basic cpd to the corrosion speed of monocrystalline silicon sheet surface.Sodium.alpha.-hydroxypropionate is a kind of salt of weak acid, easily hydrolysis reaction occurs in the solution, and its hydrolysis equation is:
When the excessive concentration of hydroxide ion in solution, the pyramid in the matte of formation can cave on top, causes occurring large-area bright piece, affects the performance of Monocrystalline silicon cell piece, the qualification rate of textured mono-crystalline silicon is declined.In the present invention, when the excessive concentration of hydroxide ion in solution, the hydrolysising balance of Sodium.alpha.-hydroxypropionate can carry out left, significantly reduce the concentration of hydroxide ion in Wool-making agent, avoid the phenomenon that the pyramid top of causing because hydroxide ion concentration is too high caves in, improve the qualification rate of textured mono-crystalline silicon; Along with the carrying out of corrosion process, in Wool-making agent, the concentration of hydroxide ion can reduce, and at this moment the hydrolysising balance of Sodium.alpha.-hydroxypropionate can carry out to the right, produces hydroxide ion, supplements the hydroxide ion consumed, making herbs into wool can be proceeded.Sodium.alpha.-hydroxypropionate in etching reagent of the present invention can make the concentration of hydroxide ion in Wool-making agent keep equilibrium state, effectively controls basic cpd to the erosion rate of silicon chip surface.The present invention does not have special restriction to described Sodium.alpha.-hydroxypropionate, adopts Sodium.alpha.-hydroxypropionate well known to those skilled in the art.In the present invention, in described etching reagent, the content of Sodium.alpha.-hydroxypropionate is 1wt% ~ 10wt%, is preferably 3wt% ~ 6wt%.
In the present invention, comprise water in described etching reagent, the present invention is not particularly limited described water, adopts water well known to those skilled in the art.In the present invention, the amount of described water can make the content of described basic cpd, urea and Sodium.alpha.-hydroxypropionate meet the content of the basic cpd described in technique scheme, urea and Sodium.alpha.-hydroxypropionate.
The preparation method of the present invention to described etching reagent is not particularly limited, and first can prepare the aqueous solution of urea described in technique scheme, then in described aqueous solution of urea, add Sodium.alpha.-hydroxypropionate, obtain etching reagent.
First the preparation method of described etching reagent also can prepare the sodium lactate aqueous solution described in technique scheme, then in described sodium lactate aqueous solution, adds urea, obtains etching reagent.
The preparation method of described etching reagent first by urea and Sodium.alpha.-hydroxypropionate mixing, can also obtain the mixture of urea and Sodium.alpha.-hydroxypropionate; Then in the mixture of described urea and Sodium.alpha.-hydroxypropionate, add water, obtain the etching reagent described in technique scheme.
After obtaining etching reagent, basic cpd in technique scheme preferably mixes with described etching reagent by the present invention, obtain the mixture of basic cpd and etching reagent, then water is added wherein, the mass percent making described basic cpd account for Wool-making agent meets the mass percent that basic cpd described in technique scheme accounts for Wool-making agent, can obtain Wool-making agent; The volume of described etching reagent and the mass ratio of basic cpd are preferably (5 ~ 40) mL: (1 ~ 10) g, are more preferably (10 ~ 30) mL: (3 ~ 8) g.
The invention provides a kind of preparation method of textured mono-crystalline silicon, comprise the following steps:
Silicon single crystal is placed in the Wool-making agent described in technique scheme, after heating, obtains textured mono-crystalline silicon.
Due in the production of monocrystalline silicon piece, transport, storage process, inevitably there will be physical abuse, monocrystalline silicon piece also can be subject to the organic contamination of grease, rosin-cerate etc., in order to avoid these pollutents and physical abuse are on the impact of making herbs into wool, the present invention preferably carries out pre-treatment to silicon single crystal, comprises ultrasonic cleaning, washes and go to damage.The present invention to described ultrasonic cleaning, wash and go the technical scheme of damaging there is no special restriction, silicon single crystal ultrasonic cleaning well known to those skilled in the art, wash and remove damage method.
In the present invention, preferably in accordance with the following methods pre-treatment is carried out to monocrystalline silicon piece:
In order to remove the Organic pollutants of monocrystalline silicon surface, the present invention is preferably at 80 DEG C ~ 90 DEG C, and carry out first ultrasonic to monocrystalline silicon piece, described first ultrasonic time is preferably 2 minutes ~ 5 minutes; Then preferred at 60 DEG C ~ 70 DEG C, carry out second ultrasonic to the monocrystalline silicon piece obtained, described second ultrasonic time is preferably 2 minutes ~ 5 minutes, the organic pollutant such as grease, rosin, wax of removing monocrystalline silicon surface.To complete ultrasonic monocrystalline silicon piece water cleaning, described cleaning temperature is preferably 25 DEG C ~ 35 DEG C, and described scavenging period is preferably 2 minutes ~ 5 minutes.
In order to remove the mechanical damage layer of monocrystalline silicon sheet surface, the present invention is preferably at 75 DEG C ~ 85 DEG C, the silicon single crystal obtained preferably is placed in mass concentration be 2% ~ 8% sodium hydroxide solution clean, described scavenging period is preferably 1 minute ~ 3 minutes, removes the mechanical damage layer that silicon single crystal shows; Then preferably the silicon single crystal obtained is placed in water cleans, described cleaning temperature is preferably 40 DEG C ~ 50 DEG C, and described scavenging period is preferably 1 minute ~ 3 minutes, obtains the silicon single crystal removing mechanical damage layer.
After completing the pre-treatment to silicon single crystal, the present invention carries out making herbs into wool to the silicon single crystal obtained, and obtains textured mono-crystalline silicon.The preparation method of the present invention to described textured mono-crystalline silicon is not particularly limited, and adopts the preparation method of textured mono-crystalline silicon well known to those skilled in the art.Pretreated silicon single crystal is placed in the Wool-making agent described in technique scheme by the present invention, obtains textured mono-crystalline silicon after heating.Heating temperature of the present invention is preferably 70 DEG C ~ 90 DEG C, is more preferably 75 DEG C ~ 85 DEG C; Described heat-up time is preferably 1000s ~ 1500s, is more preferably 1100s ~ 1350s.
In order to adapt to industrialized continuous seepage, the present invention adds basic cpd and etching reagent continuously in making herbs into wool process in Wool-making agent, add-on preferably (80 ~ 150) g/L that described basic cpd is each, is more preferably (100 ~ 125) g/L; Add-on preferably (10 ~ 30) ml/L that described etching reagent is each, is more preferably (15 ~ 20) ml/L.
After obtaining textured mono-crystalline silicon, in order to remove the metal ion of silicon chip surface, residual basic cpd and oxide compound, the present invention preferably carries out aftertreatment to described textured mono-crystalline silicon, is specially:
In order to remove the metal ion of monocrystalline silicon surface and residual basic cpd, the present invention preferably carries out hydrochloric acid cleaning to the textured mono-crystalline silicon obtained, the present invention is not particularly limited the concentration, scavenging period, cleaning temperature etc. of hydrochloric acid in described hydrochloric acid cleaning, adopts the hydrochloric acid cleaning in silicon single crystal making herbs into wool process well known to those skilled in the art.In the present invention, the concentration of described hydrochloric acid is preferably 5% ~ 50%, is more preferably 15% ~ 30%, the described hydrochloric acid cleaning time is preferably 2 minutes ~ 8 minutes, be more preferably 3 minutes ~ 5 minutes, described hydrochloric acid cleaning temperature is preferably 20 DEG C ~ 40 DEG C, is more preferably 25 DEG C ~ 35 DEG C.
In order to remove the oxide compound of silicon chip surface, the present invention preferably carries out hydrofluoric acid clean to textured mono-crystalline silicon, the present invention is not particularly limited the concentration, scavenging period, cleaning temperature etc. of hydrofluoric acid in described hydrofluoric acid clean, adopts the hydrofluoric acid clean in silicon single crystal making herbs into wool process well known to those skilled in the art.In the present invention, the concentration of described hydrofluoric acid is preferably 1% ~ 30%, be more preferably 5% ~ 20%, most preferably be 10% ~ 15%, the time of described hydrofluoric acid clean is preferably 2 minutes ~ 8 minutes, be more preferably 3 minutes ~ 5 minutes, the temperature of described hydrofluoric acid clean is preferably 20 DEG C ~ 40 DEG C, is more preferably 25 DEG C ~ 35 DEG C.
After completing the aftertreatment to described textured mono-crystalline silicon, the textured mono-crystalline silicon obtained preferably is dried by the present invention, obtain textured mono-crystalline silicon, the present invention does not have particular requirement to described oven dry, adopts the oven dry in silicon single crystal making herbs into wool process well known to those skilled in the art.
The obvious raising that the qualification rate of the textured mono-crystalline silicon that the present invention obtains obtains is 97% ~ 100%.The performance of the present invention to the textured mono-crystalline silicon obtained measures, result shows, Wool-making agent provided by the invention improves short-circuit current and the efficiency of conversion of textured mono-crystalline silicon, reduces the reflectivity of textured mono-crystalline silicon, and the performance of the textured mono-crystalline silicon that the present invention obtains is improved.
The invention provides a kind of silicon single crystal Wool-making agent, comprise basic cpd and etching reagent; Described etching reagent comprises following component: the urea of 5wt% ~ 20wt%; The Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt%; Surplus is water.Wool-making agent provided by the invention effectively can control the corrosion speed of basic cpd to silicon face, get rid of gas to the interference of making herbs into wool process, make the type of the pyramid matte obtained little and evenly, thus reduce the reflectivity of silicon single crystal, improve the short-circuit current of silicon single crystal, improve the transformation efficiency of cell piece, and Wool-making agent provided by the invention has stronger soil removability, therefore make the qualification rate of the textured mono-crystalline silicon obtained be improved significantly.
In order to further illustrate the present invention, below in conjunction with embodiment, the preparation method to silicon single crystal Wool-making agent provided by the invention and textured mono-crystalline silicon is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
In 22.2g urea, add 200mL water, obtain the urea soln that mass concentration is 10%, then add 6.87g Sodium.alpha.-hydroxypropionate wherein, obtain etching reagent, wherein the mass concentration of Sodium.alpha.-hydroxypropionate is 3%.Get 4.5g sodium hydroxide and the above-mentioned etching reagent of 26.7mL, add 200mL water wherein, obtain Wool-making agent, wherein the mass concentration of sodium hydroxide is 2%, and in etching reagent, urea and the total mass concentration of Sodium.alpha.-hydroxypropionate are 1.5%.
Comparative example 1
In 10.5g lactic acid, add 200mL water, obtain the lactic acid solution that mass concentration is 5%, then add 23.8g Sodium.alpha.-hydroxypropionate and 8.9g vitamins B wherein, obtain additive, wherein the mass concentration of Sodium.alpha.-hydroxypropionate is 8%, and the mass concentration of vitamins B is 3%.Get 1.76g sodium hydroxide, 10.89mL Virahol and the above-mentioned additive of 5.02mL, add 200mL water wherein, obtain Wool-making agent, wherein the mass concentration of sodium hydroxide is 0.8%, the mass concentration of Virahol is 5%, and the mass concentration that in additive, lactic acid, Sodium.alpha.-hydroxypropionate and vitamins B are total is 0.3%.
Embodiment 2
In 10.5g Sodium.alpha.-hydroxypropionate, add 200mL water, obtain the sodium lactate solution that mass concentration is 5%, then add 28.7g urea wherein, obtain etching reagent, wherein the mass concentration of urea is 12%.Get 5.85g sodium hydroxide and the above-mentioned etching reagent of 24.38mL, add 200mL water wherein, obtain Wool-making agent, wherein the mass concentration of sodium hydroxide is 2.5%, and in etching reagent, urea and the total mass concentration of Sodium.alpha.-hydroxypropionate are 1.8%.
Comparative example 2
In 12.7g lactic acid, add 200mL water, obtain the lactic acid solution that mass concentration is 6%, then add 34.6g Sodium.alpha.-hydroxypropionate and 12.1g vitamins B wherein, obtain additive, wherein the mass concentration of Sodium.alpha.-hydroxypropionate is 10%, and the mass concentration of vitamins B is 3.5%.Get 2.2g sodium hydroxide, 13.2mL Virahol and the above-mentioned additive of 4.51mL, add 200mL water wherein, obtain Wool-making agent, wherein the massfraction of sodium hydroxide is 1%, the mass concentration of Virahol is 6%, and the mass concentration that in additive, lactic acid, Sodium.alpha.-hydroxypropionate and vitamins B are total is 0.4%.
Embodiment 3
In 11.28g Sodium.alpha.-hydroxypropionate, add 200mL water, obtain the sodium lactate solution that mass concentration is 6%, then add 37.28g urea wherein, obtain corrosive fluid, wherein the mass concentration of urea is 15%.Get 6.86g sodium hydroxide and the above-mentioned etching reagent of 21.77mL, add 200mL water wherein, obtain Wool-making agent, wherein the mass concentration of sodium hydroxide is 3%, and in etching reagent, urea and the total mass concentration of Sodium.alpha.-hydroxypropionate are 2%.
Comparative example 3
In 17.4g lactic acid, add 200mL water, obtain the lactic acid solution that mass concentration is 8%, then add 31.05g Sodium.alpha.-hydroxypropionate and 10.35g vitamins B wherein, obtain additive, wherein the mass concentration of Sodium.alpha.-hydroxypropionate is 12%, and the mass concentration of vitamins B is 4%.Get 2.93g sodium hydroxide, 18.06mL Virahol and the above-mentioned additive of 18.06mL, add 200mL water wherein, obtain Wool-making agent, wherein the massfraction of sodium hydroxide is 1.3%, the mass concentration of Virahol is 8%, and the mass concentration that in additive, lactic acid, Sodium.alpha.-hydroxypropionate and Mierocrystalline cellulose B are total is 0.5%.
Embodiment 4 ~ 6
Select the monocrystalline silicon piece 100 of same batch respectively, 150 and 200, it is carried out ultrasonic cleaning 3 minutes at 85 DEG C, then the monocrystalline silicon piece obtained is carried out ultrasonic cleaning 3 minutes at 65 DEG C, again the monocrystalline silicon piece obtained is cleaned 3 minutes with water at 25 DEG C, then at 80 DEG C, the sodium hydroxide solution monocrystalline silicon piece obtained being placed in mass concentration 5% cleans 1 minute, again the monocrystalline silicon piece obtained is cleaned 1 minute with water at 45 DEG C, then the monocrystalline silicon piece obtained is placed in the Wool-making agent that embodiment 1 obtains, heating 1200s, Heating temperature is 80 DEG C, obtain textured mono-crystalline silicon.The textured mono-crystalline silicon obtained is cleaned 1 minute with water at 45 DEG C, and then 1 minute is cleaned with water at 30 DEG C, then the textured mono-crystalline silicon obtained is placed at 25 DEG C mass concentration be 10% hydrochloric acid soln cleaning 4 minutes, again the textured mono-crystalline silicon obtained is placed at 25 DEG C mass concentration be 5% hydrofluoric acid solution cleaning 4 minutes, then textured mono-crystalline silicon complete for hydrofluoric acid clean is cleaned 4 minutes with water at 30 DEG C, after oven dry, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that embodiment 4 ~ 6 obtains is respectively 100,148 and 200, and qualification rate is respectively 100%, 99% and 100%.The present invention measures the reflectivity of the textured mono-crystalline silicon obtained, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and efficiency of conversion, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
Comparative example 4 ~ 6
Select respectively with embodiment 4 ~ 6 with batch monocrystalline silicon piece 100,150 and 200, adopt the Wool-making agent that obtains of comparative example 1, according to the technical scheme described in embodiment 4 ~ 6, making herbs into wool carried out to monocrystalline silicon piece, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that comparative example 4 ~ 6 obtains is respectively 94,145 and 190, qualification rate is respectively 94%, 97% and 95%, the present invention measures the reflectivity of the textured mono-crystalline silicon obtained, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and efficiency of conversion, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
Embodiment 7 ~ 9
Select the monocrystalline silicon piece 100 of same batch respectively, 200 and 300, it is carried out ultrasonic cleaning 2 minutes at 90 DEG C, then the monocrystalline silicon piece obtained is carried out ultrasonic cleaning 3 minutes at 70 DEG C, again the monocrystalline silicon piece obtained is cleaned 3 minutes with water at 30 DEG C, then at 83 DEG C, the sodium hydroxide solution monocrystalline silicon piece obtained being placed in mass concentration 8% cleans 1 minute, again the monocrystalline silicon piece obtained is cleaned 2 minutes with water at 40 DEG C, then the monocrystalline silicon piece obtained is placed in the Wool-making agent that embodiment 2 obtains, heating 1100s, Heating temperature is 85 DEG C, obtain textured mono-crystalline silicon.The textured mono-crystalline silicon obtained is cleaned 1 minute with water at 45 DEG C, and then 1 minute is cleaned with water at 28 DEG C, then the textured mono-crystalline silicon obtained is placed at 30 DEG C mass concentration be 10% hydrochloric acid soln cleaning 4 minutes, again the textured mono-crystalline silicon obtained is placed at 25 DEG C mass concentration be 5% hydrofluoric acid solution cleaning 4 minutes, then textured mono-crystalline silicon complete for hydrofluoric acid clean is cleaned 4 minutes with water at 30 DEG C, after oven dry, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that embodiment 7 ~ 9 obtains is respectively 98,200 and 294, qualification rate is respectively 98%, 100% and 98%, the present invention measures the reflectivity of the textured mono-crystalline silicon obtained, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and efficiency of conversion, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
Comparative example 7 ~ 9
Select respectively with embodiment 7 ~ 9 with batch monocrystalline silicon piece 100,200 and 300, adopt the Wool-making agent that obtains of comparative example 2, according to the technical scheme described in embodiment 7 ~ 9, making herbs into wool carried out to monocrystalline silicon piece, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that comparative example 7 ~ 9 obtains is respectively 98,186 and 273, qualification rate is respectively 98%, 93% and 91%, the present invention measures the reflectivity of the textured mono-crystalline silicon obtained, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and efficiency of conversion, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
Embodiment 10 ~ 13
Select the monocrystalline silicon piece 150 of same batch respectively, 250, 350 and 400, it is carried out ultrasonic cleaning 3 minutes at 80 DEG C, then the monocrystalline silicon piece obtained is carried out ultrasonic cleaning 5 minutes at 60 DEG C, again the monocrystalline silicon piece obtained is cleaned 2 minutes with water at 35 DEG C, then at 85 DEG C, the sodium hydroxide solution monocrystalline silicon piece obtained being placed in mass concentration 10% cleans 1 minute, again the monocrystalline silicon piece obtained is cleaned 2 minutes with water at 45 DEG C, then the monocrystalline silicon piece obtained is placed in the Wool-making agent that embodiment 3 obtains, heating 1300s, Heating temperature is 83 DEG C, obtain textured mono-crystalline silicon.The textured mono-crystalline silicon obtained is cleaned 2 minutes with water at 40 DEG C, and then 1 minute is cleaned with water at 30 DEG C, then the textured mono-crystalline silicon obtained is placed at 25 DEG C mass concentration be 12% hydrochloric acid soln cleaning 4 minutes, again the textured mono-crystalline silicon obtained is placed at 25 DEG C mass concentration be 10% hydrofluoric acid solution cleaning 3 minutes, then textured mono-crystalline silicon complete for hydrofluoric acid clean is cleaned 4 minutes with water at 30 DEG C, after oven dry, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that embodiment 10 ~ 13 obtains is respectively 145,250,346 and 392, qualification rate is respectively 97%, 100%, 99% and 98%, the present invention measures the reflectivity of the textured mono-crystalline silicon obtained, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and efficiency of conversion, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
Comparative example 10 ~ 13
Select respectively with embodiment 10 ~ 13 with batch monocrystalline silicon piece 150,250,350 and 400, adopt the Wool-making agent that obtains of comparative example 3, according to the technical scheme described in embodiment 10 ~ 13, making herbs into wool carried out to monocrystalline silicon piece, obtain textured mono-crystalline silicon.
The qualified textured mono-crystalline silicon that comparative example 10 ~ 13 obtains is respectively 142,242,322 and 360, qualification rate is respectively 95%, 97%, 92% and 90%, the present invention measures the textured mono-crystalline silicon reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion that obtain, result is as shown in table 1, and table 1 is qualification rate and the performance test results of the textured mono-crystalline silicon that the embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain.
The qualification rate of the textured mono-crystalline silicon that table 1 embodiment of the present invention 4 ~ 13 and comparative example 4 ~ 13 obtain and the performance test results
As can be seen from Table 1, the qualification rate of the textured mono-crystalline silicon adopting Wool-making agent provided by the invention to prepare is 97% ~ 100%, be significantly improved, and Wool-making agent provided by the invention reduces the reflectivity of textured mono-crystalline silicon, improve its short-circuit current, improve the efficiency of conversion of textured mono-crystalline silicon sheet.
As seen from the above embodiment, Wool-making agent provided by the invention can improve the qualification rate of textured mono-crystalline silicon, and can improve the performance of textured mono-crystalline silicon, reduces the reflectivity of textured mono-crystalline silicon, improves its short-circuit current and efficiency of conversion.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (9)
1. a silicon single crystal Wool-making agent, is made up of basic cpd, etching reagent and water;
Described etching reagent is made up of the urea of 5wt% ~ 20wt%, the Sodium.alpha.-hydroxypropionate of 1wt% ~ 10wt% and water;
The volume of described etching reagent and the mass ratio of described basic cpd are (5 ~ 40) mL:(1 ~ 10) g;
The mass percent that described basic cpd accounts for silicon single crystal Wool-making agent is 0.5% ~ 3%.
2. silicon single crystal Wool-making agent according to claim 1, is characterized in that, described etching reagent comprises the urea of 10wt% ~ 15wt%.
3. silicon single crystal Wool-making agent according to claim 1, is characterized in that, described etching reagent comprises the Sodium.alpha.-hydroxypropionate of 3wt% ~ 6wt%.
4. silicon single crystal Wool-making agent according to claim 1, is characterized in that, the mass percent that described basic cpd accounts for silicon single crystal Wool-making agent is 1.5% ~ 2.5%.
5. silicon single crystal Wool-making agent according to claim 1, is characterized in that, described basic cpd is sodium hydroxide, potassium hydroxide or sodium carbonate.
6. silicon single crystal Wool-making agent according to claim 5, is characterized in that, described basic cpd is sodium hydroxide.
7. a preparation method for textured mono-crystalline silicon, comprises the following steps:
Silicon single crystal is placed in the silicon single crystal Wool-making agent described in claim 1 ~ 6 any one, after heating, obtains textured mono-crystalline silicon.
8. preparation method according to claim 7, is characterized in that, the temperature of described heating is 70 DEG C ~ 90 DEG C.
9. preparation method according to claim 7, is characterized in that, the time of described heating is 1000s ~ 1500s.
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| WO2016152228A1 (en) * | 2015-03-24 | 2016-09-29 | 株式会社カネカ | Method for manufacturing crystalline silicon substrate for solar cell, method for manufacturing crystalline silicon solar cell, and method for manufacturing crystalline silicon solar cell module |
| CN105206687A (en) * | 2015-08-21 | 2015-12-30 | 合肥中南光电有限公司 | Efficient and rapid monocrystalline silicon wafer texturing solution and preparation method thereof |
| CN107858752A (en) * | 2017-11-03 | 2018-03-30 | 通威太阳能（安徽）有限公司 | A kind of crystal silicon Woolen-making liquid and preparation method thereof |
| CN108004598A (en) * | 2017-12-01 | 2018-05-08 | 绍兴拓邦电子科技有限公司 | A kind of crystalline silicon etching edge additive and its application method |
| CN111024596A (en) * | 2019-12-20 | 2020-04-17 | 苏州纳格检测科技有限公司 | Alkali resistance test method for metal parts for toilet |
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