CN106119976B - Additive and its application of the black silicon making herbs into wool of polycrystalline with reaming acid solution - Google Patents
Additive and its application of the black silicon making herbs into wool of polycrystalline with reaming acid solution Download PDFInfo
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- CN106119976B CN106119976B CN201610688156.2A CN201610688156A CN106119976B CN 106119976 B CN106119976 B CN 106119976B CN 201610688156 A CN201610688156 A CN 201610688156A CN 106119976 B CN106119976 B CN 106119976B
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- polycrystalline
- black silicon
- acid solution
- reaming
- acid
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The present invention provides a kind of additive of the black silicon making herbs into wool reaming acid solution of polycrystalline, and the mass percentage of each component is：Polyvinyl alcohol 0.5%~2%, triethanolamine 1%~5%, tartaric acid 1%~3%, silane coupling agent 0.5%~2%, surplus are water.The present invention also provides the reaming acid solutions and the black silicon etching method of polycrystalline of the above-mentioned additive of application.The additive of the present invention is added in reaming acid solution, it can be so that the reaction of expanding treatment be slack-off and then controllable, reaction rate of the reaming acid solution on each crystal face of the black silicon of polycrystalline can be made farthest to be consistent, to which anisotropic etch is inhibited, the final crystalline substance flower for making the black silicon of polycrystalline be improved significantly, the appearance advantage and performance advantage of black silicon are embodied.
Description
Technical field
The additive with reaming acid solution and its application the present invention relates to the black silicon making herbs into wool of polycrystalline.
Background technology
Currently, in the technological process of the black silicon making herbs into wool of polycrystalline, the method for metal Aided Wet chemical etching is increasingly wider
It uses generally, the black silicon of the polycrystalline with nano aperture can be prepared using metal Aided Wet chemical etching.
Metal Aided Wet chemical etching generally uses metal ion, since metallic particles is all smaller, only several nanometers
To tens nanometers, the nano aperture accordingly generated on the black silicon of polycrystalline, aperture also only has several nanometers to tens nanometers.In order to carry
The coverage rate of high matte is compound with reduction silicon chip surface, promotes the electrical property of cell piece, needs to metal Aided Wet chemistry
The black silicon of polycrystalline for etching gained carries out expanding treatment, so that the aperture of nano aperture is reached hundreds of nanometers, also can be thorough in this way
The condition that metal in cleaning cavity provides.
It is the mixing of one-component acid solution or several acid that expanding treatment, which generally uses reaming acid solution, currently used reaming acid solution,
Liquid（Such as the mixed liquor of nitric acid and hydrofluoric acid）Although reaming purpose can be completed to a certain extent using these reaming acid solutions, expand
The reaction of hole processing is too fast, is difficult to control, the uniformity of nanometer suede is caused to be affected；Meanwhile reaming acid solution is each to different
Property corrosion black silicon face crystalline substance can be allowed to spend the appearance for seriously having seriously affected the black silicon of polycrystalline, allow user to the degree of recognition of black silicon making herbs into wool
It is greatly reduced.
Invention content
The additive with reaming acid solution and its application the purpose of the present invention is to provide a kind of black silicon making herbs into wool of polycrystalline, in reaming
The additive of the present invention is added in acid solution, the reaction of expanding treatment can be made slack-off and then controllable, reaming acid solution can be made in polycrystalline
Reaction rate on the black each crystal face of silicon is farthest consistent, and to which anisotropic etch is inhibited, is finally made
The black silicon of polycrystalline crystalline substance flower be improved significantly, the appearance advantage and performance advantage of black silicon are embodied.
To achieve the above object, the present invention provides a kind of additive of the black silicon making herbs into wool reaming acid solution of polycrystalline, each component
Mass percentage be：Polyvinyl alcohol 0.5%~2%, triethanolamine 1%~5%, tartaric acid 1%~3%, silane coupling agent 0.5%
~2%, surplus is water.
Preferably, the silane coupling agent is selected from one or more of KH550, KH560 and KH570.
Preferably, the water is deionized water.
The present invention also provides a kind of black silicon making herbs into wool reaming acid solutions of polycrystalline, contain acid solution and above-mentioned additive；Institute
The mass ratio for stating additive and acid solution is 0.5~5:100；5%~40% HNO has been incorporated in the acid solution3Aqueous solution and
10%~50% HF aqueous solutions；Containing 49% HF in the HF aqueous solutions, contain 69% HNO in the HNO3 aqueous solutions3；Its
In, percentage is mass percent.
The present invention also provides a kind of black silicon etching methods of polycrystalline, and band nano-pore is prepared in metal Aided Wet chemical etching
It is black to polycrystalline using above-mentioned reaming acid solution after the black silicon of polycrystalline in hole, and before pickling removal surface metal particle residual
Silicon carries out expanding treatment, and the aperture of nano aperture is made to reach 100~500nm.
Preferably, the black silicon etching method of above-mentioned polycrystalline prepares the black silicon of polycrystalline, the polycrystalline using polysilicon chip as raw material
Silicon chip is that Buddha's warrior attendant wire cutting polysilicon chip or mortar cut polysilicon chip or class monocrystalline silicon piece.
Preferably, the black silicon etching method of above-mentioned polycrystalline, includes the following steps：
1）Polycrystalline silicon texturing or polishing；The making herbs into wool uses nitric hydrofluoric acid mixed solution making herbs into wool；It is described to be finished to alkali
Polishing or acid polishing；The alkali polishing is polished using NaOH, KOH or TMAH solution；The acid polishing is mixed using nitric hydrofluoric acid
Close solution polishing；
2）The black silicon of polycrystalline with nano aperture is prepared using metal Aided Wet chemical etching；
3）Using the reaming acid solution described in claim 4, expanding treatment is carried out to the black silicon of polycrystalline, treatment temperature is 6~35
DEG C, processing time is 30~200s, and the aperture of nano aperture is made to reach 100~500nm；
4）Pickling removes surface metal particle residual：The metallic of polysilicon chip remained on surface is removed with concentrated nitric acid；
5）Alkali cleaning：With lye neutralization procedure 4）Concentrated nitric acid, and cleaning silicon chip surface removes undesired impurities；The lye
For NaOH, KOH or TMAH solution.
Preferably, step 2）In, metal Aided Wet chemical etching uses metal ion and acid solution, which is
Hydrogen peroxide hydrofluoric acid mixed solution or nitric hydrofluoric acid mixed solution, the metal ion are selected from gold, silver, iron, copper, nickel, zinc, tin
One or more of ion.
Preferably, step 2）In, the black silicon of polycrystalline that metal Aided Wet chemical etching is prepared, the aperture of nano aperture
For 5~50nm, and the reflectivity of the black silicon of polycrystalline is below 10%.
Preferably, step 3）In, the reflectivity of the black silicon of polycrystalline is 17%~22% after expanding treatment.
The advantages of the present invention are：There is provided a kind of black silicon making herbs into wool reaming acid solution of polycrystalline additive and its
Using, added in reaming acid solution the present invention additive, can make expanding treatment reaction it is slack-off and then controllable, reaming can be made
Reaction rate of the acid solution on each crystal face of the black silicon of polycrystalline is farthest consistent, to which anisotropic etch is pressed down
System, finally make the black silicon of polycrystalline crystalline substance flower be improved significantly, the appearance advantage and performance advantage of black silicon are embodied.
In more detail, the present invention has following features：
1, it during polycrystalline black silicon making herbs into wool, is especially prepared with nano aperture in metal Aided Wet chemical etching
After the black silicon of polycrystalline, and pickling removal surface metal particle residual before, using addition additive of the present invention reaming acid solution,
Expanding treatment is carried out to the black silicon of polycrystalline, the aperture of nano aperture can be made to reach 100~500nm, the reflectivity control of the black silicon of polycrystalline
17%~22%.
2, the additive of the present invention is added in reaming acid solution, the reaction of expanding treatment can be made slack-off and then controllable, energy
Reaction rate of the reaming acid solution on each crystal face of the black silicon of polycrystalline is set farthest to be consistent, you can to make reaming acid solution to each
The oxidation rate of a crystal face reaches consistent as possible, to which anisotropic etch is inhibited, keeps the silicon chip surface after corrosion brilliant
Flower color reaches unanimity, and reaches that brilliant embossing die paste, appearance be uniform, the uniform effect of matte；And the matte hole after corroding（Nano-pore
Hole）Size uniformity, opening direction utmostly tend to that unanimously, battery efficiency can be improved.
3, using the reaming acid solution of addition additive of the present invention, expanding treatment is carried out to the black silicon of polycrystalline, expanding treatment can be made
The reflectivity control of the black silicon of polycrystalline is 17%~22% afterwards, and good in full band range invagination light effect, surface recombination is low, can improve electricity
The transfer efficiency in pond.
4, the black silicon etching method of polycrystalline of the present invention is suitable for Buddha's warrior attendant wire cutting polysilicon chip and mortar cuts polysilicon chip.
5, the black silicon etching method of polycrystalline of the present invention is simple for process, at low cost, is suitble to industrialized production.
Description of the drawings
Fig. 1 is the final gained polysilicon chip of the black silicon etching method of polycrystalline of the present invention（The black silicon of polycrystalline）Appearance photo；
Fig. 2 is the final gained polysilicon chip of the black silicon etching method of polycrystalline of the present invention（The black silicon of polycrystalline）Stereoscan photograph.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is further described.Following embodiment is only
For clearly illustrating technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
The technical solution that the present invention embodies is：
The present invention provides a kind of additive of the black silicon making herbs into wool reaming acid solution of polycrystalline, the mass percentage of each component
For：Polyvinyl alcohol 0.5%~2%, triethanolamine 1%~5%, tartaric acid 1%~3%, silane coupling agent 0.5%~2%, surplus are water.
Preferably, the silane coupling agent is selected from one or more of KH550, KH560 and KH570.
Preferably, the water is deionized water.
The present invention also provides a kind of black silicon making herbs into wool reaming acid solutions of polycrystalline, contain acid solution and above-mentioned additive；Institute
The mass ratio for stating additive and acid solution is 0.5~5:100；5%~40% HNO has been incorporated in the acid solution3Aqueous solution and
10%~50% HF aqueous solutions；Containing 49% HF in the HF aqueous solutions, contain 69% HNO in the HNO3 aqueous solutions3；Its
In, percentage is mass percent.
The present invention also provides a kind of black silicon etching methods of polycrystalline, and band nano-pore is prepared in metal Aided Wet chemical etching
It is black to polycrystalline using above-mentioned reaming acid solution after the black silicon of polycrystalline in hole, and before pickling removal surface metal particle residual
Silicon carries out expanding treatment, and the aperture of nano aperture is made to reach 100~500nm.
Preferably, the black silicon etching method of above-mentioned polycrystalline prepares the black silicon of polycrystalline, the polycrystalline using polysilicon chip as raw material
Silicon chip is that Buddha's warrior attendant wire cutting polysilicon chip or mortar cut polysilicon chip or class monocrystalline silicon piece.
Preferably, the black silicon etching method of above-mentioned polycrystalline, includes the following steps：
1）Polycrystalline silicon texturing or polishing；The making herbs into wool uses nitric hydrofluoric acid mixed solution making herbs into wool；It is described to be finished to alkali
Polishing or acid polishing；The alkali polishing is polished using NaOH, KOH or TMAH solution；The acid polishing is mixed using nitric hydrofluoric acid
Close solution polishing；
2）The black silicon of polycrystalline with nano aperture is prepared using metal Aided Wet chemical etching, the aperture of nano aperture is
5~50nm, and the reflectivity of the black silicon of polycrystalline is below 10%；
Metal Aided Wet chemical etching uses metal ion and acid solution, which mixes for hydrogen peroxide hydrofluoric acid
Solution or nitric hydrofluoric acid mixed solution, the one kind or several of the metal ion in gold, silver, iron, copper, nickel, zinc, tin ion
Kind；
3）Using the reaming acid solution described in claim 4, expanding treatment is carried out to the black silicon of polycrystalline, treatment temperature is 6~35
DEG C, processing time is 30~200s, and the aperture of nano aperture is made to reach 100~500nm；The reflectivity of the black silicon of polycrystalline 17%~
22%；
4）Pickling removes surface metal particle residual：The metallic of polysilicon chip remained on surface is removed with concentrated nitric acid；
5）Alkali cleaning：With lye neutralization procedure 4）Concentrated nitric acid, and cleaning silicon chip surface removes undesired impurities；The lye
For NaOH, KOH or TMAH solution.
The above-mentioned black silicon etching method of polycrystalline, final gained polysilicon chip（The black silicon of polycrystalline）Appearance photo it is as shown in Figure 1；
The above-mentioned black silicon etching method of polycrystalline, final gained polysilicon chip（The black silicon of polycrystalline）Stereoscan photograph such as Fig. 2 institutes
Show.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (9)
1. the additive of the black silicon making herbs into wool reaming acid solution of polycrystalline, which is characterized in that the mass percentage of its each component is：Poly- second
Enol 0.5%~2%, triethanolamine 1%~5%, tartaric acid 1%~3%, silane coupling agent 0.5%~2%, surplus are water；The silane
Coupling agent is selected from one or more of KH550, KH560 and KH570.
2. additive according to claim 1, which is characterized in that the water is deionized water.
3. the black silicon making herbs into wool reaming acid solution of polycrystalline, which is characterized in that it contains acid solution and addition as claimed in claim 1 or 2
Agent；The mass ratio of the additive and acid solution is 0.5~5:100；5%~40% HNO has been incorporated in the acid solution3It is water-soluble
Liquid and 10%~50% HF aqueous solutions；Contain 49% HF, the HNO in the HF aqueous solutions3Contain 69% in aqueous solution
HNO3；Wherein, percentage is mass percent.
4. the black silicon etching method of polycrystalline, which is characterized in that prepared with the more of nano aperture in metal Aided Wet chemical etching
After brilliant black silicon, and before pickling removal surface metal particle residual, using the reaming acid solution described in claim 3, to more
Brilliant black silicon carries out expanding treatment, and the aperture of nano aperture is made to reach 100~500nm.
5. the black silicon etching method of polycrystalline according to claim 4, which is characterized in that prepared as raw material using polysilicon chip more
Brilliant black silicon, the polysilicon chip are Buddha's warrior attendant wire cutting polysilicon chip, mortar cutting polysilicon chip or class monocrystalline silicon piece.
6. the black silicon etching method of polycrystalline according to claim 5, which is characterized in that include the following steps：
1）Polycrystalline silicon texturing or polishing；The making herbs into wool uses nitric hydrofluoric acid mixed solution making herbs into wool；It is described to be finished to alkali polishing
Or acid polishing；The alkali polishing is polished using NaOH, KOH or TMAH solution；The acid polishing is mixed molten using nitric hydrofluoric acid
Liquid polishes；
2）The black silicon of polycrystalline with nano aperture is prepared using metal Aided Wet chemical etching；
3）Using the reaming acid solution described in claim 3, expanding treatment is carried out to the black silicon of polycrystalline, treatment temperature is 6~35 DEG C, place
The reason time is 30~200s, and the aperture of nano aperture is made to reach 100~500nm；
4）Pickling removes surface metal particle residual：The metallic of polysilicon chip remained on surface is removed with concentrated nitric acid；
5）Alkali cleaning：With lye neutralization procedure 4）Concentrated nitric acid, and cleaning silicon chip surface removes undesired impurities；The lye is
NaOH, KOH or TMAH solution.
7. the black silicon etching method of polycrystalline according to claim 6, which is characterized in that step 2）In, metal Aided Wet
It learns etching and uses metal ion and acid solution, which is that hydrogen peroxide hydrofluoric acid mixed solution or nitric hydrofluoric acid mixing are molten
Liquid, the metal ion are selected from one or more of gold, silver, iron, copper, nickel, zinc, tin ion.
8. the black silicon etching method of polycrystalline according to claim 7, which is characterized in that step 2）In, metal Aided Wet
The black silicon of polycrystalline that etching is prepared is learned, the aperture of nano aperture is 5~50nm, and the reflectivity of the black silicon of polycrystalline is below 10%.
9. the black silicon etching method of polycrystalline according to claim 8, which is characterized in that step 3）In, polycrystalline after expanding treatment
The reflectivity of black silicon is 17%~22%.
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| WO2019013706A1 (en) * | 2017-07-11 | 2019-01-17 | National University Of Singapore | A method of texturing photovoltaic silicon wafers |
| CN107742660B (en) * | 2017-09-25 | 2019-06-11 | 江西展宇新能源股份有限公司 | It is a kind of improve the black silicon solar cell crystal orientation of polycrystalline between difference process |
| CN107805845B (en) * | 2017-10-23 | 2020-06-09 | 常州时创能源股份有限公司 | Reaming process of polycrystalline black silicon |
| CN108179478A (en) * | 2017-12-27 | 2018-06-19 | 无锡尚德太阳能电力有限公司 | The method that metal catalytic chemical corrosion method single side prepares the black silicon matte of polycrystalline |
| CN108193281B (en) * | 2018-03-09 | 2020-06-09 | 常州时创能源股份有限公司 | Polycrystalline black silicon texturing process |
| TWI665344B (en) * | 2018-03-26 | 2019-07-11 | 中國大陸商常州時創能源科技有限公司 | Polish and texture method for polycrystalline black silicon perc battery |
| CN108807568A (en) * | 2018-06-14 | 2018-11-13 | 浙江晶科能源有限公司 | A kind of processing method of the black silicon silicon chip of wet method and the preparation method of the black silicon silicon chip of wet method |
| CN109244178B (en) * | 2018-08-09 | 2020-10-27 | 江苏辉伦太阳能科技有限公司 | Preparation method of metal-free catalytic black silicon |
| CN110872729B (en) * | 2018-08-30 | 2021-07-20 | 比亚迪股份有限公司 | Texturing and hole digging additive, texturing and silver sinking hole digging liquid, silicon wafer and solar cell of diamond wire cutting polycrystalline silicon wafer |
| CN109750353B (en) * | 2019-03-14 | 2020-12-29 | 常州时创能源股份有限公司 | Auxiliary agent for inverted pyramid texturing of monocrystalline silicon wafer and application thereof |
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| JP2009141165A (en) * | 2007-12-07 | 2009-06-25 | Siltronic Japan Corp | Method of etching silicon wafer |
| CN103132079B (en) * | 2013-02-07 | 2015-07-08 | 睿纳能源科技（上海）有限公司 | Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof |
| CN103409808B (en) * | 2013-09-04 | 2015-10-21 | 常州时创能源科技有限公司 | Polycrystalline silicon texturing additive and using method thereof |
| CN103668467B (en) * | 2013-12-20 | 2016-08-31 | 常州时创能源科技有限公司 | A kind of polycrystalline silicon texturing additive and application thereof |
| CN103993360B (en) * | 2014-06-09 | 2016-08-24 | 常州时创能源科技有限公司 | Polycrystalline silicon texturing adjuvant and application thereof |
| CN104294369A (en) * | 2014-11-13 | 2015-01-21 | 苏州润阳光伏科技有限公司 | Acid texturing additive for polysilicon film and use method thereof |
| CN104651949B (en) * | 2015-02-11 | 2017-09-29 | 常州君合科技股份有限公司 | A kind of polycrystalline silicon texturing additive |
| CN105040108B (en) * | 2015-08-21 | 2017-11-17 | 浙江启鑫新能源科技股份有限公司 | The etching method of polysilicon solar cell |
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Address after: Liyang City, Jiangsu province 213300 Li Cheng Zhen Wu Changzhou city Tandu Road No. 8 Patentee after: Changzhou Shichuang Energy Co., Ltd Address before: Liyang City, Jiangsu province 213300 Li Cheng Zhen Wu Changzhou city Tandu Road No. 8 Patentee before: CHANGZHOU SHICHUANG ENERGY TECHNOLOGY Co.,Ltd. |