CN103882528A - Method for preparing polycrystalline silicon wafer texture surface - Google Patents
Method for preparing polycrystalline silicon wafer texture surface Download PDFInfo
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- CN103882528A CN103882528A CN201410123902.4A CN201410123902A CN103882528A CN 103882528 A CN103882528 A CN 103882528A CN 201410123902 A CN201410123902 A CN 201410123902A CN 103882528 A CN103882528 A CN 103882528A
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Abstract
The invention discloses a method for preparing a polycrystalline silicon water texture surface. The method comprises the following steps: (1) polycrystalline silicon wafers to be treated are put in a first texture making groove for first texture making, and the texture making mixed liquid stays in the circulating state; (2) the polycrystalline silicon wafers to be treated are put in a second texture making groove for second texture making, and the texture making mixed liquid stays in the circulating state and bubbling condition; and (3) the polycrystalline silicon wafers to be treated are put in a third texture making groove for third texture making, and the texture making mixed liquid stays in the circulating state and bubbling condition. Experiments obtained from the production lines prove that only 80 of 150000 silicon wafers which are subjected to texture making according to the method of the invention produce water marks, and the removal of water marks is greatly improved compared with the existing technologies; in addition, after the texture is made by using the method of the invention, the silicon wafers almost have no basket marks on the surface, so that the appearance of a battery slice is greatly improved based on the method, and the technical problems to be solved in the field are solved.
Description
Technical field
The present invention relates to a kind of preparation method of polysilicon chip matte, belong to solar cell field.
Background technology
In prior art, in the preparation process of solar battery sheet, in order to improve performance and the efficiency of solar cell, generally all can be in silicon chip surface making herbs into wool.Effectively suede structure can make the sunlight of incident carry out multiple reflections and refraction at silicon chip surface, changes the working direction of incident light in silicon chip.Increase the absorption of silicon chip to infrared light, improve photoelectric transformation efficiency.
At present, the etching method of polysilicon chip is all generally to adopt chromic acid making herbs into wool, its equipment is all to adopt cheap and groove type etching equipment that process window is wide, and concrete mode is in single texturing slot, to add chromic acid mixing solutions, then polysilicon chip is immersed in and in chromic acid mixing solutions, carries out making herbs into wool.
But, practical application is found, because making herbs into wool reaction is violent, easily produces amount of heat, temperature controllability is low, cause silicon chip surface crystalline substance to be spent obviously, and negative and positive sheet is more, loss of weight is difficult to be controlled, especially producing serious flower basket mark and water wave prints, and this flower basket mark and water wave seal are obvious especially, have a strong impact on the outward appearance of cell piece, participate in the silicon chip surface figure after the making herbs into wool shown in accompanying drawing 1.
On the other hand, the cell piece overwhelming majority that China produces is at present that outlet is sold, and abroad the outward appearance of cell piece is valued very much.For example, selling in Japanese process, first the other side can assess the outward appearance of product, if having obvious flower basket mark on cell piece and water wave prints, can be judged as defectively, had a strong impact on sale.
For the problems referred to above, the staff of this area has carried out a large amount of research experiments, finds simple adjusting process parameter, and as corrosion temperature, etching time etc., all cannot obtain breakthrough.Thereby this problem becomes this area but insurmountable technical barrier all the time urgently to be resolved hurrily.
Therefore, develop a kind of preparation method of polysilicon chip matte, print with the flower basket mark and the water wave that reduce silicon chip surface, there is positive realistic meaning.
Summary of the invention
The object of the invention is to provide a kind of preparation method of polysilicon chip matte.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of polysilicon chip matte, comprises the steps:
(1) pending polysilicon chip is put into the first texturing slot and carry out making herbs into wool for the first time;
The component of the making herbs into wool mixing solutions in described the first texturing slot, by mass, comprising: 0.5% ~ 1.5% CrO
3, 40% ~ 50% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 10 ~ 30 DEG C, and etching time is 250 ~ 350 seconds;
Making herbs into wool mixing solutions is in recurrent state;
(2) pending polysilicon chip is put into the second texturing slot and carry out making herbs into wool for the second time;
The component of the making herbs into wool mixing solutions in described the second texturing slot, by mass, comprising: 0.3% ~ 1% CrO
3, 45% ~ 60% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 15 ~ 25 DEG C, and etching time is 230 ~ 270 seconds;
Making herbs into wool mixing solutions is in recurrent state and bubbling state;
(3) pending polysilicon chip is put into the 3rd texturing slot and carried out making herbs into wool for the third time;
The component of the making herbs into wool mixing solutions in described the 3rd texturing slot, by mass, comprising: 0.3% ~ 1% CrO
3, 45% ~ 60% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 15 ~ 25 DEG C, and etching time is 230 ~ 270 seconds;
Making herbs into wool mixing solutions is in recurrent state and bubbling state.
Above, the water-soluble chromic acid that obtains of chromium trioxide.Be chromic acid making herbs into wool.
In the described HF aqueous solution, contain mass percent and be 49% HF, can certainly adopt the HF aqueous solution of other concentration, as long as the total mass percentage composition in mixing solutions unanimously.
In technique scheme, described step (3) afterwards, is also provided with at least 1 texturing slot and carries out making herbs into wool, and making herbs into wool mixing solutions, corrosion temperature, etching time and the state in texturing slot is all identical with step (3).
In technique scheme, in described step (1), the component of the making herbs into wool mixing solutions in the first texturing slot, by mass, comprising: 0.9% ~ 1.1% CrO
3, 43% ~ 45% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF; Etching time is 270 ~ 320 seconds.
In technique scheme, in described step (3), the component of the making herbs into wool mixing solutions in the 3rd texturing slot, by mass, comprising: 0.3% ~ 0.8% CrO
3, 46% ~ 58% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF; Etching time is 230 ~ 270 seconds.
Working mechanism of the present invention is as follows:
The first step: the first texturing slot, as principal reaction district, by the corrosion of Woolen-making liquid, can effectively be removed damaged layer on surface of silicon slice, and loss of weight is controlled at 0.2g-0.3g, then form the default corrosion matte that reaches the first step making herbs into wool by texturing slot circulatory function; If (multiparity line experiment showed, that described the first non-ON cycle of texturing slot function can make Woolen-making liquid insufficient in silicon chip surface reaction, makes the silicon chip surface after making herbs into wool can form big area dead color, affects unified appearance; And if the first texturing slot ON cycle function is also opened bubbling function, can make the silicon chip surface after making herbs into wool produce light and shade striped, affect Si wafer quality and outward appearance) therefore the first texturing slot ON cycle function, silicon chip can reach best effect after Woolen-making liquid corrosion.
Second step: the in the situation that the second texturing slot being removed at damaged layer on surface of silicon slice, it is violent that making herbs into wool process is no longer reacted, and reacting phase is to evenly, by further corrosion and modification of Woolen-making liquid, brilliant flower obtains further fuzzy, simultaneously owing to having opened circulation and bubbling function, can make silicon chip and gaily decorated basket contact part suitably pine from, continue fully reaction, the flower basket mark water wave seal of silicon chip surface is further improved, and silicon chip loss of weight is controlled to 0.1g left and right.
The 3rd step: the reaction of the 3rd texturing slot is progressively slow, by the corrosive nature for the third time of Woolen-making liquid, formation reaches default crystalline substance and spends fuzzy matte, the 3rd texturing slot has been opened circulation and bubbling function in the lump, make silicon chip and solution continue fully reaction, reach the effect of removing water wave seal and flower basket mark, the 3rd texturing slot silicon chip loss of weight is controlled at 0.05g left and right.
The present invention is directed to chromic acid making herbs into wool, divide three steps to carry out making herbs into wool by three grooves, with respect to single groove making herbs into wool, it is advantageous that: sufficient reacting, corrosion evenly, can produce the brilliant flower of fuzzy polycrystalline, can improve and produce line production capacity.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the present invention has developed a kind of preparation method of new polysilicon chip matte, the experiment of multiparity line confirms: 150,000 silicon chips are after method making herbs into wool of the present invention, only have 80 to produce water wave seal, had and significantly improve removing water wave India side face (in prior art solution later stage water wave print off existing probability be roughly 90% left and right) compared to conventional art; In addition, adopt after method making herbs into wool of the present invention, the flower basket mark of silicon chip surface exists hardly; As can be seen here, the present invention has greatly improved the outward appearance of cell piece, has solved this area technical barrier urgently to be resolved hurrily, creative.
2. the present invention can obtain the cell piece of better outward appearance, and can not affect electrical property and the efficiency of conversion of cell piece, and this has created fabulous condition to for export, has positive realistic meaning.
3. method of the present invention has been widened the process window of polysilicon chip chromic acid making herbs into wool, effectively reduces the reflectivity of silicon chip, has improved quality and the production capacity of polysilicon chip chromic acid making herbs into wool.
Brief description of the drawings
Fig. 1 is the silicon chip surface figure after single texturing slot making herbs into wool in background technology;
Fig. 2 is the silicon chip surface figure after the embodiment of the present invention one making herbs into wool.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment mono-
Shown in Figure 2, a kind of preparation method of polysilicon chip matte, comprises the steps:
The first step: the circulatory function of opening the first texturing slot is carried out acidic solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution, deionized water massfraction be respectively 1%, 44.7%, 52%, also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.024%, 0.028%, 0.04%, 2.208%; Etching time is 300s, and Woolen-making liquid temperature is 23.5 DEG C;
Second step: circulation and the bubbling function of opening the second texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.6%, 51.7%, 45.4%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.024%, 0.028%, 0.04%, 2.208%; Etching time is 250s, and Woolen-making liquid temperature is 23.5 DEG C;
The 3rd step: circulation and the bubbling function of opening the 3rd texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.6%, 51.7%, 45.4%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.024%, 0.028%, 0.04%, 2.208%; Etching time is 250s, and Woolen-making liquid temperature is 23.5 DEG C.
The silicon chip surface figure of the polysilicon solar cell of preparing as shown in Figure 2.Can see, the water wave in Fig. 2 prints obviously and improves, and flower basket mark does not exist.
This making herbs into wool silicon chip loss of weight is at 0.41g, and water wave prints and reduces to 0.05%.
Compare with single-channel type making herbs into wool, open circuit voltage promotes 0.0006V, and short-circuit current promotes 0.06A, and packing factor promotes 0.44%, and photoelectric transformation efficiency promotes 0.1%.
Embodiment bis-
A preparation method for polysilicon chip matte, comprises the steps:
The first step: the circulatory function of opening the first texturing slot is carried out acidic solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution, deionized water massfraction be respectively 0.5%, 40%, 57.5%, also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 350s, and Woolen-making liquid temperature is 10 DEG C;
Second step: circulation and the bubbling function of opening the second texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.3%, 45%, 52.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 300s, and Woolen-making liquid temperature is 10 DEG C;
The 3rd step: circulation and the bubbling function of opening the 3rd texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.3%, 45%, 52.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 300s, and Woolen-making liquid temperature is 10 DEG C.
This making herbs into wool silicon chip loss of weight is at 0.35g, and water wave prints and reduces to 0.1%.
The open circuit voltage of comparing with single-channel type making herbs into wool promotes 0.0004V, and short-circuit current promotes 0.05A, and packing factor promotes 0.36%, and photoelectric transformation efficiency promotes 0.04%.
Embodiment tri-
A preparation method for polysilicon chip matte, comprises the steps:
The first step: the circulatory function of opening the first texturing slot is carried out acidic solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution, deionized water massfraction be respectively 1.5%, 50%, 45.5%, also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.03%, 0.03%, 0.15%, 2.79%; Etching time is 250s, and Woolen-making liquid temperature is 30 DEG C;
Second step: circulation and the bubbling function of opening the second texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 1%, 60%, 36%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.03%, 0.03%, 0.15%, 2.79%; Etching time is 200s, and Woolen-making liquid temperature is 30 DEG C;
The 3rd step: circulation and the bubbling function of opening the 3rd texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 1%, 60%, 36%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.03%, 0.03%, 0.15%, 2.79%; Etching time is 200s, and Woolen-making liquid temperature is 30 DEG C.
This making herbs into wool silicon chip loss of weight is at 0.44g, and water wave prints and reduces to 0.09%.
Compare with single-channel type making herbs into wool, open circuit voltage promotes 0.0005V, and short-circuit current promotes 0.05A, and packing factor promotes 0.21%, and photoelectric transformation efficiency promotes 0.04%.
Embodiment tetra-
A preparation method for polysilicon chip matte, comprises the steps:
The first step: the circulatory function of opening the first texturing slot is carried out acidic solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution, deionized water massfraction be respectively 0.9%, 43%, 54.1%, also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 320s, and Woolen-making liquid temperature is 15 DEG C;
Second step: circulation and the bubbling function of opening the second texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.3%, 46%, 51.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 270s, and Woolen-making liquid temperature is 15 DEG C;
The 3rd step: circulation and the bubbling function of opening the 3rd texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.3%, 46%, 51.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.004%, 0.01%, 0.04%, 1.946%; Etching time is 270s, and Woolen-making liquid temperature is 15 DEG C.
Compare with single-channel type making herbs into wool, open circuit voltage promotes 0.0006V, and short-circuit current promotes 0.05A, and packing factor promotes 0.23%, and photoelectric transformation efficiency promotes 0.06%.
Embodiment five
A preparation method for polysilicon chip matte, comprises the steps:
The first step: the circulatory function of opening the first texturing slot is carried out acidic solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution, deionized water massfraction be respectively 1.1%, 45%, 51.4%, also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.025%, 0.025%, 0.125%, 2.325%; Etching time is 270s, and Woolen-making liquid temperature is 25 DEG C;
Second step: circulation and the bubbling function of opening the second texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.8%, 58%, 38.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.025%, 0.025%, 0.125%, 2.325%; Etching time is 230s, and Woolen-making liquid temperature is 25 DEG C;
The 3rd step: circulation and the bubbling function of opening the 3rd texturing slot are carried out acid solution making herbs into wool, the component of the making herbs into wool mixing solutions in texturing slot: CrO
3, the HF aqueous solution and deionized water massfraction be respectively 0.8%, 58%, 38.7%; Also comprise polyoxyethylene glycol, polyacrylamide, vinylformic acid, deionized water, its massfraction is respectively 0.025%, 0.025%, 0.125%, 2.325%; Etching time is 230s, and Woolen-making liquid temperature is 25 DEG C.
Compare with single-channel type making herbs into wool, open circuit voltage promotes 0.0004V, and short-circuit current promotes 0.04A, and packing factor promotes 0.2%, and photoelectric transformation efficiency promotes 0.05%.
The content that above-described embodiment is illustrated should be understood to these embodiment only for being illustrated more clearly in the present invention, limit the scope of the invention and be not used in, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the amendment of the various equivalent form of values of the present invention.
Claims (4)
1. a preparation method for polysilicon chip matte, is characterized in that, comprises the steps:
(1) pending polysilicon chip is put into the first texturing slot and carry out making herbs into wool for the first time;
The component of the making herbs into wool mixing solutions in described the first texturing slot, by mass, comprising: 0.5% ~ 1.5% CrO
3, 40% ~ 50% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 10 ~ 30 DEG C, and etching time is 250 ~ 350 seconds;
Making herbs into wool mixing solutions is in recurrent state;
(2) pending polysilicon chip is put into the second texturing slot and carry out making herbs into wool for the second time;
The component of the making herbs into wool mixing solutions in described the second texturing slot, by mass, comprising: 0.3% ~ 1% CrO
3, 45% ~ 60% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 15 ~ 25 DEG C, and etching time is 230 ~ 270 seconds;
Making herbs into wool mixing solutions is in recurrent state and bubbling state;
(3) pending polysilicon chip is put into the 3rd texturing slot and carried out making herbs into wool for the third time;
The component of the making herbs into wool mixing solutions in described the 3rd texturing slot, by mass, comprising: 0.3% ~ 1% CrO
3, 45% ~ 60% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF;
Corrosion temperature is 15 ~ 25 DEG C, and etching time is 230 ~ 270 seconds;
Making herbs into wool mixing solutions is in recurrent state and bubbling state.
2. method according to claim 1, it is characterized in that: described step (3) afterwards, also be provided with at least 1 texturing slot and carry out making herbs into wool, making herbs into wool mixing solutions, corrosion temperature, etching time and the state in texturing slot is all identical with step (3).
3. method according to claim 1, is characterized in that: in described step (1), the component of the making herbs into wool mixing solutions in the first texturing slot, by mass, comprising: 0.9% ~ 1.1% CrO
3, 43% ~ 45% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF; Etching time is 270 ~ 320 seconds.
4. method according to claim 1, is characterized in that: in described step (3), the component of the making herbs into wool mixing solutions in the 3rd texturing slot, by mass, comprising: 0.3% ~ 0.8% CrO
3, 46% ~ 58% the HF aqueous solution, 0.004% ~ 0.03% polyoxyethylene glycol, 0.01% ~ 0.03% polyacrylamide, 0.04% ~ 0.15% vinylformic acid, surplus is water; In the described HF aqueous solution, contain mass percent and be 49% HF; Etching time is 230 ~ 270 seconds.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107201518A (en) * | 2017-05-04 | 2017-09-26 | 中国第汽车股份有限公司 | A kind of coat of metal corrosive liquid |
| CN115020548A (en) * | 2022-07-14 | 2022-09-06 | 通威太阳能(金堂)有限公司 | Silicon wafer texturing device and texturing process |
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| CN103681974A (en) * | 2013-12-27 | 2014-03-26 | 常州时创能源科技有限公司 | Dual-slot polycrystalline silicon chip texturing method |
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| CN107201518A (en) * | 2017-05-04 | 2017-09-26 | 中国第汽车股份有限公司 | A kind of coat of metal corrosive liquid |
| CN115020548A (en) * | 2022-07-14 | 2022-09-06 | 通威太阳能(金堂)有限公司 | Silicon wafer texturing device and texturing process |
| CN115020548B (en) * | 2022-07-14 | 2023-07-25 | 通威太阳能(金堂)有限公司 | Silicon wafer texturing device and texturing process |
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