CN103184523A - Monocrystalline silicon texturing agent and preparation method of texture monocrystalline silicon - Google Patents
Monocrystalline silicon texturing agent and preparation method of texture monocrystalline silicon Download PDFInfo
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- CN103184523A CN103184523A CN2011104447947A CN201110444794A CN103184523A CN 103184523 A CN103184523 A CN 103184523A CN 2011104447947 A CN2011104447947 A CN 2011104447947A CN 201110444794 A CN201110444794 A CN 201110444794A CN 103184523 A CN103184523 A CN 103184523A
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Abstract
The invention provides a monocrystalline silicon texturing agent, comprising an alkaline compound and a corrodent; wherein the corrodent includes the following components: 5wt%-20wt% of urea, 1wt%-10wt% of sodium lactate, and the balance water. The texture monocrystalline silicon is prepared by placing monocrystalline silicon into the texturing agent provided by the present invention and heating. The urea in the monocrystalline silicon texturing agent can hydrolyze to produce ammonia and carbon dioxide, being conducive to the smooth overflow of gases generated during texturing process, and preventing the effects of gas on texture quality. The corrodent of the present invention can effectively control the etching rate of the alkali compound for the silicon surface, and also has a strong decontamination capacity, therefore the texturing agent provided by the present invention can effectively reduce the probability of appearing bright pieces, hickies and rain drops, so that the pyramid type suede is small and uniform, and the qualified rate of suede monocrystalline silicon has been markedly improved.
Description
Technical field
The present invention relates to silicon single crystal making herbs into wool technical field, relate in particular 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, renewable energy sources such as sun power more and more are subject to people's attention.Sun power is a kind of primary energy source, is again renewable energy source, and its aboundresources both need not transportation, again environment was not had any pollution, for the mankind have created a kind of new lifestyle, made society enter the epoch of a save energy less contamination.Aspect the utilizing of sun power, the research and development of solar cell has obtained people's great attention, and wherein monocrystaline silicon solar cell receives much concern owing to its high relatively efficient and low cost.
One of important step in the monocrystaline silicon solar cell preparation process is exactly silicon single crystal making herbs into wool, by the surface wool manufacturing to silicon single crystal, can form the suede structure of similar pyramid at silicon chip surface, this suede structure can reduce silicon chip surface effectively to the reflection of incident light rate, reduce reflection of incident light, improve solar cell to absorption of incident light, thereby can improve the efficiency of conversion of battery greatly.Present existing silicon single crystal etching method has: chemical corrosion method, reactive ion etching method, photolithography and mechanical carving groove method etc., wherein chemical corrosion method is low because of cost, productivity is high and method is simple, is widely used in the monocrystaline silicon solar cell industry always.
Chemical corrosion method making herbs into wool normally adopts basic solution that silicon chip surface is corroded.Basic solution has different erosion rates to the different crystal faces of silicon chip, 100 crystal faces of silicon single crystal are compared as 111 crystal faces or 110 crystal faces with other crystal faces, have corrosion speed faster, because this anisotropic corrosive property, meeting form the suede structure of similar pyramid at silicon chip surface.Silicon single crystal Woolen-making liquid commonly used in the prior art comprises sodium hydroxide and Virahol, and wherein sodium hydroxide meeting and pasc reaction erode the silicon of plane of crystal, formation pyramid pyramid structure; In the process of sodium hydroxide and pasc reaction, there is hydrogen to produce, can influence the effect of making herbs into wool, the adding of Virahol can be got rid of the bubble of generation, and Virahol also can reduce the surface tension of silicon chip, be conducive to contacting of sodium hydroxide and silicon chip surface, be beneficial to the formation of suede structure.Yet in the making herbs into wool process, also can occur because of sodium hydroxide to the too fast phenomenon of caving in that causes suede structure of the erosion rate of silicon chip surface, therefore need in Wool-making agent, add additive, to suppress hydroxide ion to the erosion rate of silicon face, additive commonly used in the prior art comprises lactic acid, Sodium.alpha.-hydroxypropionate, vitamins B and water, additive can reduce the concentration of hydroxide ion effectively, slow down sodium hydroxide to a certain extent to the corrosion of silicon chip surface, be conducive to formation and the maintenance of pyramid matte.But adopt the pyramid matte of the textured mono-crystalline silicon that this Wool-making agent that comprises sodium hydroxide, Virahol and above-mentioned additive obtains inhomogeneous, cause 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, adopt the type of pyramid matte of the textured mono-crystalline silicon that silicon single crystal Wool-making agent provided by the invention makes little and even, improved 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, to account for the mass percent of Wool-making agent be 0.5%～3% to described basic cpd.
Preferably, to account for the mass percent of Wool-making agent be 1.5%～2.5% to described basic cpd.
Preferably, described basic cpd is sodium hydroxide, potassium hydroxide or yellow soda ash.
Preferably, described basic cpd is sodium hydroxide.
The invention provides a kind of preparation method of textured mono-crystalline silicon, may further comprise the steps:
Silicon single crystal is placed the described silicon single crystal Wool-making agent of technique scheme, obtain textured mono-crystalline silicon after the heating.
Preferably, the temperature of described heating is 70 ℃～90 ℃.
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 the urea of following component: 5wt%～20wt%; The Sodium.alpha.-hydroxypropionate of 1wt%～10wt%; Surplus is water.Etching reagent in the silicon single crystal Wool-making agent provided by the invention is the aqueous solution of urea and Sodium.alpha.-hydroxypropionate, wherein urea can hydrolysis produce ammonia and carbonic acid gas, increased the buoyancy of gas in the Wool-making agent, be conducive to overcome the surface tension of silicon chip surface, thereby the gas that produces in the making herbs into wool process is successfully overflowed, avoided the influence of gas to the matte quality; And etching reagent provided by the invention can make hydroxide ion in the Wool-making agent maintain the state of balance, thereby can control basic cpd effectively to the erosion rate of silicon face, etching reagent provided by the invention also has stronger soil removability, therefore, Wool-making agent provided by the invention can reduce the probability of bright of silicon chip surface appearance, hickie, raindrop effectively, make the type of the pyramid matte that obtains little and even, thereby reduced silicon chip to the reflection of light rate, improved short-circuit current and efficiency of conversion, made that the qualification rate of textured mono-crystalline silicon is improved significantly.Experimental result shows that the qualification rate of the textured mono-crystalline silicon that silicon single crystal Wool-making agent provided by the invention makes is 97%～100%.In addition, do not contain Virahol in the silicon single crystal Wool-making agent provided by the invention, reduced production cost, and can operating environment not polluted owing to the volatilization of Virahol, be conducive to reduce the chemical oxygen demand (COD) of water body, reduce leather producing process waste water to the pollution of water body.
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.
Comprise basic cpd in the silicon single crystal Wool-making agent provided by the invention.Basic cpd can corrode the surface of monocrystalline silicon piece, and because basic cpd has anisotropic corrosive property to silicon face, make silicon single crystal 100 crystal faces compare as 111 crystal faces or 110 crystal faces with other crystal faces, have corrosion speed faster, therefore can form the suede structure of pyramid shape on the surface of monocrystalline silicon piece.This suede structure that forms can reduce monocrystalline silicon surface to the reflection of incident light rate, increases monocrystalline silicon piece to absorption of incident light, improves the transformation efficiency of monocrystalline silicon battery effectively.The reaction equation of basic cpd and silicon is:
In the present invention, described basic cpd is preferably sodium hydroxide, potassium hydroxide or yellow soda ash, more preferably sodium hydroxide; The mass percent that described basic cpd accounts for Wool-making agent is preferably 0.5%～3%, and more preferably 1.5%～2.5%.
Comprise etching reagent in the 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 the described etching reagent, urea has formula (I) structure, is weakly alkaline, in solution hydrolysis reaction can take place, and produces ammonia and carbonic acid gas, and the hydrolysis reaction equation of uric acid is:
NH
2CONH
2+H
2O＝2NH
3↑+CO
2↑。
The buoyancy that the ammonia that hydrolysis of urea produces and carbonic acid gas can increase silicon chip surface gas makes the buoyancy of gas greater than the sticking power of silicon chip surface, thereby makes basic cpd and the hydrogen of pasc reaction generation easily break away from silicon chip surface.Gas can hinder contacting of basic cpd and silicon face in the gathering of silicon chip surface, the adding of urea can make the gas of generation easily break away from silicon face, Wool-making agent is contacted with silicon face again to be corroded, thereby make the silicon chip surface corrosion fully, avoid in underproof phenomenons such as bright of silicon chip surface appearance, raindrops, improve the quality of monocrystalline silicon piece texture, thereby improved the qualification rate of textured mono-crystalline silicon.The present invention does not have particular restriction to described urea, adopts urea well known to those skilled in the art to get final product.In the present invention, content of urea is 5wt%～20wt% in the described etching reagent, is preferably 10wt%～15wt%.
Comprise Sodium.alpha.-hydroxypropionate in the etching reagent of the present invention, 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 keep the balance of hydroxide ion concentration in the Wool-making agent, controls basic cpd effectively to the corrosion speed of monocrystalline silicon sheet surface.Sodium.alpha.-hydroxypropionate is a kind of salt of weak acid, and hydrolysis reaction takes place in solution easily, and its hydrolysis equation is:
When the excessive concentration of hydroxide ion in the solution, the pyramid in the matte of formation can cave on the top, causes occurring large-area bright, influences the performance of monocrystalline silicon battery sheet, makes the qualification rate of textured mono-crystalline silicon descend.In the present invention, when the excessive concentration of hydroxide ion in the solution, the hydrolysising balance of Sodium.alpha.-hydroxypropionate can carry out left, reduced the concentration of hydroxide ion in the Wool-making agent effectively, avoided because the phenomenon that hydroxide ion concentration too high pyramid top of causing caves in, improved the qualification rate of textured mono-crystalline silicon; Along with the carrying out of corrosion process, the concentration of hydroxide ion can reduce in the Wool-making agent, and at this moment the hydrolysising balance of Sodium.alpha.-hydroxypropionate can carry out to the right, produces hydroxide ion, and the hydroxide ion of supplement consumed makes making herbs into wool to proceed.Sodium.alpha.-hydroxypropionate in the etching reagent of the present invention can make the concentration of hydroxide ion in the Wool-making agent keep equilibrium state, controls basic cpd effectively 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 to get final product.In the present invention, the content of Sodium.alpha.-hydroxypropionate is 1wt%～10wt% in the described etching reagent, is preferably 3wt%～6wt%.
In the present invention, comprise water in the described etching reagent, the present invention does not have particular restriction to described water, adopts water well known to those skilled in the art to get final product.In the present invention, the amount of the described water content that can make the content of described basic cpd, urea and Sodium.alpha.-hydroxypropionate meet the basic cpd described in the technique scheme, urea and Sodium.alpha.-hydroxypropionate gets final product.
The present invention does not have particular restriction to the preparation method of described etching reagent, can at first prepare the described aqueous solution of urea of technique scheme, adds Sodium.alpha.-hydroxypropionate then in described aqueous solution of urea, obtains etching reagent.
The preparation method of described etching reagent also can at first prepare the described sodium lactate aqueous solution of technique scheme, adds urea then in described sodium lactate aqueous solution, obtains etching reagent.
The preparation method of described etching reagent can also at first mix urea and Sodium.alpha.-hydroxypropionate, obtains the mixture of urea and Sodium.alpha.-hydroxypropionate; In the mixture of described urea and Sodium.alpha.-hydroxypropionate, add water then, obtain the described etching reagent of technique scheme.
Obtain after the etching reagent, the present invention preferably mixes the basic cpd in the technique scheme with described etching reagent, obtain the mixture of basic cpd and etching reagent, then to wherein adding water, the mass percent that makes described basic cpd account for Wool-making agent meets the mass percent that basic cpd described in the 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, more preferably (10～30) mL: (3～8) g.
The invention provides a kind of preparation method of textured mono-crystalline silicon, may further comprise the steps:
Silicon single crystal is placed the described Wool-making agent of technique scheme, obtain textured mono-crystalline silicon after the heating.
Because in the production of monocrystalline silicon piece, transportation, storage process, inevitably physical abuse can appear, monocrystalline silicon piece also can be subjected to the organic contamination of grease, rosin-cerate etc., for fear of the influence to making herbs into wool of these pollutents and physical abuse, the present invention preferably carries out pre-treatment to silicon single crystal, comprises ultrasonic cleaning, washes and go decreasing.The present invention does not have special restriction to described ultrasonic cleaning, the technical scheme of washing and going to decrease, and silicon single crystal ultrasonic cleaning well known to those skilled in the art, washes and goes damage method to get final product.
In the present invention, preferably in accordance with the following methods monocrystalline silicon piece is carried out pre-treatment:
In order to remove the Organic pollutants of monocrystalline silicon surface, the present invention carries out first ultrasonicly preferably under 80 ℃～90 ℃ to monocrystalline silicon piece, and described first ultrasonic time is preferably 2 minutes～and 5 minutes; Then preferably under 60 ℃～70 ℃, the monocrystalline silicon piece that obtains is carried out second ultrasonic, described second ultrasonic time is preferably 2 minutes～5 minutes, removes the organic pollutant such as grease, rosin, wax of monocrystalline silicon surface.Will finish ultrasonic monocrystalline silicon piece water cleans, and described cleaning temperature is preferably 25 ℃～35 ℃, and described scavenging period is preferably 2 minutes～and 5 minutes.
In order to remove the mechanical damage layer of monocrystalline silicon sheet surface, the present invention is preferably under 75 ℃～85 ℃, it is that 2%～8% sodium hydroxide solution cleans that the silicon single crystal that obtains is preferably placed mass concentration, described scavenging period is preferably 1 minute～and 3 minutes, remove the mechanical damage layer that silicon single crystal shows; Preferably place water to clean the silicon single crystal that obtains then, described cleaning temperature is preferably 40 ℃～50 ℃, and described scavenging period is preferably 1 minute～3 minutes, obtains removing the silicon single crystal of mechanical damage layer.
After finishing the pre-treatment to silicon single crystal, the present invention carries out making herbs into wool to the silicon single crystal that obtains, and obtains textured mono-crystalline silicon.The present invention does not have particular restriction to the preparation method of described textured mono-crystalline silicon, adopts the preparation method of textured mono-crystalline silicon well known to those skilled in the art to get final product.The present invention places the described Wool-making agent of technique scheme with pretreated silicon single crystal, obtains textured mono-crystalline silicon after the heating.Heating temperature of the present invention is preferably 70 ℃～90 ℃, more preferably 75 ℃～85 ℃; Be preferably 1000s～1500s, more preferably 1100s～1350s described heat-up time.
In order to adapt to industrialized continuous production, the present invention adds basic cpd and etching reagent continuously in Wool-making agent in the making herbs into wool process, and the each add-on of described basic cpd is preferably (80～150) g/L, more preferably (100～125) g/L; The each add-on of described etching reagent is preferably (10～30) ml/L, more preferably (15～20) ml/L.
After obtaining textured mono-crystalline silicon, for the metal ion of removing silicon chip surface, residual basic cpd and oxide compound, the present invention preferably carries out aftertreatment to described textured mono-crystalline silicon, is specially:
For the metal ion of removing monocrystalline silicon surface and residual basic cpd, the present invention preferably carries out hydrochloric acid to the textured mono-crystalline silicon that obtains and cleans, the concentration of hydrochloric acid, scavenging period, cleaning temperature etc. did not have particular restriction during the present invention cleaned described hydrochloric acid, adopted the hydrochloric acid cleaning in the silicon single crystal making herbs into wool process well known to those skilled in the art to get final product.In the present invention, the concentration of described hydrochloric acid is preferably 5%～50%, and more preferably 15%～30%, described hydrochloric acid scavenging period is preferably 2 minutes～and 8 minutes, more preferably 3 minutes～5 minutes, described hydrochloric acid cleaning temperature was preferably 20 ℃～40 ℃, more preferably 25 ℃～35 ℃.
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 does not have particular restriction to the concentration of hydrofluoric acid in the described hydrofluoric acid clean, scavenging period, cleaning temperature etc., adopts the hydrofluoric acid clean in the silicon single crystal making herbs into wool process well known to those skilled in the art to get final product.In the present invention, the concentration of described hydrofluoric acid is preferably 1%～30%, more preferably 5%～20%, most preferably be 10%～15%, the time of described hydrofluoric acid clean is preferably 2 minutes～and 8 minutes, more preferably 3 minutes～5 minutes, the temperature of described hydrofluoric acid clean was preferably 20 ℃～40 ℃, more preferably 25 ℃～35 ℃.
After finishing the aftertreatment to described textured mono-crystalline silicon, the present invention is preferably with the textured mono-crystalline silicon oven dry that obtains, obtain textured mono-crystalline silicon, the present invention does not have particular requirement to described oven dry, adopts the oven dry in the silicon single crystal making herbs into wool process well known to those skilled in the art to get final product.
The tangible raising that the qualification rate of the textured mono-crystalline silicon that the present invention obtains obtains is 97%～100%.The present invention measures the performance of the textured mono-crystalline silicon that obtains, the result shows, Wool-making agent provided by the invention has improved short-circuit current and the efficiency of conversion of textured mono-crystalline silicon, has reduced 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 the urea of following component: 5wt%～20wt%; The Sodium.alpha.-hydroxypropionate of 1wt%～10wt%; Surplus is water.Wool-making agent provided by the invention can effectively be controlled basic cpd to the corrosion speed of silicon face, get rid of gas to the interference of making herbs into wool process, make the type of the pyramid matte that obtains little and even, thereby reduced the reflectivity of silicon single crystal, improved the short-circuit current of silicon single crystal, improved the transformation efficiency of battery sheet, and Wool-making agent provided by the invention has stronger soil removability, therefore the qualification rate of the textured mono-crystalline silicon that obtains is improved significantly.
In order to further specify the present invention, below in conjunction with embodiment the preparation method of 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 restriction to protection domain of the present invention.
Embodiment 1
Add 200mL water in the 22.2g urea, obtain mass concentration and be 10% urea soln, to wherein adding the 6.87g Sodium.alpha.-hydroxypropionate, obtain etching reagent then, wherein the mass concentration of Sodium.alpha.-hydroxypropionate is 3%.Get the above-mentioned etching reagent of 4.5g sodium hydroxide and 26.7mL, to wherein adding 200mL water, obtain Wool-making agent, wherein sodium hydroxide concentration is 2%, and the total mass concentration of urea and Sodium.alpha.-hydroxypropionate is 1.5% in the etching reagent.
Comparative example 1
Add 200mL water in the 10.5g lactic acid, obtain mass concentration and be 5% lactic acid solution, to wherein adding 23.8g Sodium.alpha.-hydroxypropionate and 8.9g vitamins B, obtain additive then, 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, to wherein adding 200mL water, obtain Wool-making agent, wherein sodium hydroxide concentration is 0.8%, the mass concentration of Virahol is 5%, and the total mass concentration of lactic acid, Sodium.alpha.-hydroxypropionate and vitamins B is 0.3% in the additive.
Embodiment 2
Add 200mL water in the 10.5g Sodium.alpha.-hydroxypropionate, obtain mass concentration and be 5% sodium lactate solution, to wherein adding 28.7g urea, obtain etching reagent then, wherein the mass concentration of urea is 12%.Get the above-mentioned etching reagent of 5.85g sodium hydroxide and 24.38mL, to wherein adding 200mL water, obtain Wool-making agent, wherein sodium hydroxide concentration is 2.5%, and the total mass concentration of urea and Sodium.alpha.-hydroxypropionate is 1.8% in the etching reagent.
Comparative example 2
Add 200mL water in the 12.7g lactic acid, obtain mass concentration and be 6% lactic acid solution, to wherein adding 34.6g Sodium.alpha.-hydroxypropionate and 12.1g vitamins B, obtain additive then, 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, to wherein adding 200mL water, obtain Wool-making agent, wherein the massfraction of sodium hydroxide is 1%, the mass concentration of Virahol is 6%, and the total mass concentration of lactic acid, Sodium.alpha.-hydroxypropionate and vitamins B is 0.4% in the additive.
Embodiment 3
Add 200mL water in the 11.28g Sodium.alpha.-hydroxypropionate, obtain mass concentration and be 6% sodium lactate solution, to wherein adding 37.28g urea, obtain corrosive fluid then, wherein the mass concentration of urea is 15%.Get the above-mentioned etching reagent of 6.86g sodium hydroxide and 21.77mL, to wherein adding 200mL water, obtain Wool-making agent, wherein sodium hydroxide concentration is 3%, and the total mass concentration of urea and Sodium.alpha.-hydroxypropionate is 2% in the etching reagent.
Comparative example 3
Add 200mL water in the 17.4g lactic acid, obtain mass concentration and be 8% lactic acid solution, to wherein adding 31.05g Sodium.alpha.-hydroxypropionate and 10.35g vitamins B, obtain additive then, 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, to wherein adding 200mL water, obtain Wool-making agent, wherein the massfraction of sodium hydroxide is 1.3%, the mass concentration of Virahol is 8%, and the total mass concentration of lactic acid, Sodium.alpha.-hydroxypropionate and Mierocrystalline cellulose B is 0.5% in the additive.
Embodiment 4～6
Select respectively with batch 100 of monocrystalline silicon pieces, 150 and 200, it is carried out ultrasonic cleaning 3 minutes under 85 ℃, then the monocrystalline silicon piece that obtains is carried out ultrasonic cleaning 3 minutes under 65 ℃, again the monocrystalline silicon piece that obtains was cleaned 3 minutes at 25 ℃ of following waters, then under 80 ℃, place the sodium hydroxide solution of mass concentration 5% to clean 1 minute the monocrystalline silicon piece that obtains, again the monocrystalline silicon piece that obtains was cleaned 1 minute at 45 ℃ of following waters, the Wool-making agent that places embodiment 1 to obtain the monocrystalline silicon piece that obtains then, heating 1200s, Heating temperature is 80 ℃, obtains textured mono-crystalline silicon.The textured mono-crystalline silicon that obtains was cleaned 1 minute at 45 ℃ of following waters, and then 30 ℃ of following waters cleanings 1 minute, then the textured mono-crystalline silicon that obtains being placed mass concentration under 25 ℃ is that 10% hydrochloric acid soln cleaned 4 minutes, the textured mono-crystalline silicon that obtains being placed mass concentration under 25 ℃ is that 5% hydrofluoric acid solution cleaned 4 minutes again, then that hydrofluoric acid clean is intact textured mono-crystalline silicon cleaned 4 minutes at 30 ℃ of following waters, obtained textured mono-crystalline silicon after the oven dry.
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 reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion of the textured mono-crystalline silicon that obtains, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Comparative example 4～6
Select respectively with embodiment 4～6 with batch 100,150 and 200 of monocrystalline silicon pieces, the Wool-making agent that adopts comparative example 1 to obtain carries out making herbs into wool according to embodiment 4～6 described technical schemes to monocrystalline silicon piece, obtains 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 reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion of the textured mono-crystalline silicon that obtains, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Embodiment 7～9
Select respectively with batch 100 of monocrystalline silicon pieces, 200 and 300, it is carried out ultrasonic cleaning 2 minutes under 90 ℃, then the monocrystalline silicon piece that obtains is carried out ultrasonic cleaning 3 minutes under 70 ℃, again the monocrystalline silicon piece that obtains was cleaned 3 minutes at 30 ℃ of following waters, then under 83 ℃, place the sodium hydroxide solution of mass concentration 8% to clean 1 minute the monocrystalline silicon piece that obtains, again the monocrystalline silicon piece that obtains was cleaned 2 minutes at 40 ℃ of following waters, the Wool-making agent that places embodiment 2 to obtain the monocrystalline silicon piece that obtains then, heating 1100s, Heating temperature is 85 ℃, obtains textured mono-crystalline silicon.The textured mono-crystalline silicon that obtains was cleaned 1 minute at 45 ℃ of following waters, and then 28 ℃ of following waters cleanings 1 minute, then the textured mono-crystalline silicon that obtains being placed mass concentration under 30 ℃ is that 10% hydrochloric acid soln cleaned 4 minutes, the textured mono-crystalline silicon that obtains being placed mass concentration under 25 ℃ is that 5% hydrofluoric acid solution cleaned 4 minutes again, then that hydrofluoric acid clean is intact textured mono-crystalline silicon cleaned 4 minutes at 30 ℃ of following waters, obtained textured mono-crystalline silicon after the oven dry.
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 reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion of the textured mono-crystalline silicon that obtains, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Comparative example 7～9
Select respectively with embodiment 7～9 with batch 100,200 and 300 of monocrystalline silicon pieces, the Wool-making agent that adopts comparative example 2 to obtain carries out making herbs into wool according to embodiment 7～9 described technical schemes to monocrystalline silicon piece, obtains 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 reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion of the textured mono-crystalline silicon that obtains, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Embodiment 10～13
Select respectively with batch 150 of monocrystalline silicon pieces, 250,350 and 400, it is carried out ultrasonic cleaning 3 minutes under 80 ℃, then the monocrystalline silicon piece that obtains is carried out ultrasonic cleaning 5 minutes under 60 ℃, again the monocrystalline silicon piece that obtains was cleaned 2 minutes at 35 ℃ of following waters, then under 85 ℃, place the sodium hydroxide solution of mass concentration 10% to clean 1 minute the monocrystalline silicon piece that obtains, again the monocrystalline silicon piece that obtains was cleaned 2 minutes at 45 ℃ of following waters, the Wool-making agent that places embodiment 3 to obtain the monocrystalline silicon piece that obtains then, heating 1300s, Heating temperature is 83 ℃, obtains textured mono-crystalline silicon.The textured mono-crystalline silicon that obtains was cleaned 2 minutes at 40 ℃ of following waters, and then 30 ℃ of following waters cleanings 1 minute, then the textured mono-crystalline silicon that obtains being placed mass concentration under 25 ℃ is that 12% hydrochloric acid soln cleaned 4 minutes, the textured mono-crystalline silicon that obtains being placed mass concentration under 25 ℃ is that 10% hydrofluoric acid solution cleaned 3 minutes again, then that hydrofluoric acid clean is intact textured mono-crystalline silicon cleaned 4 minutes at 30 ℃ of following waters, obtained textured mono-crystalline silicon after the oven dry.
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 reflectivity, open circuit voltage, short-circuit current, series resistance, shunting resistance, packing factor and the efficiency of conversion of the textured mono-crystalline silicon that obtains, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Comparative example 10～13
Select respectively with embodiment 10～13 with batch 150,250,350 and 400 of monocrystalline silicon pieces, the Wool-making agent that adopts comparative example 3 to obtain carries out making herbs into wool according to embodiment 10～13 described technical schemes to monocrystalline silicon piece, obtains 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, the result is as shown in table 1, qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 obtains for the embodiment of the invention 4～13 and comparative example 4～13.
Qualification rate and the The performance test results of the textured mono-crystalline silicon that table 1 embodiment of the invention 4～13 and comparative example 4～13 obtain
As can be seen from Table 1, adopting the qualification rate of the textured mono-crystalline silicon of Wool-making agent preparation provided by the invention is 97%～100%, be significantly improved, and Wool-making agent provided by the invention has reduced the reflectivity of textured mono-crystalline silicon, improve its short-circuit current, improved 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, has reduced the reflectivity of textured mono-crystalline silicon, has improved its short-circuit current and efficiency of conversion.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle 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 (10)
1. a silicon single crystal Wool-making agent comprises 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.
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 the silicon single crystal Wool-making agent is 0.5%～3%.
5. silicon single crystal Wool-making agent according to claim 4 is characterized in that, the mass percent that described basic cpd accounts for the silicon single crystal Wool-making agent is 1.5%～2.5%.
6. silicon single crystal Wool-making agent according to claim 1 is characterized in that, described basic cpd is sodium hydroxide, potassium hydroxide or yellow soda ash.
7. silicon single crystal Wool-making agent according to claim 6 is characterized in that, described basic cpd is sodium hydroxide.
8. the preparation method of a textured mono-crystalline silicon may further comprise the steps:
Silicon single crystal is placed any described silicon single crystal Wool-making agent of claim 1～7, obtain textured mono-crystalline silicon after the heating.
9. preparation method according to claim 8 is characterized in that, the temperature of described heating is 70 ℃～90 ℃.
10. preparation method according to claim 8 is characterized in that, the time of described heating is 1000s～1500s.
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