CN113981543B - Texturing additive with liquid crystal structure and preparation method and application thereof - Google Patents

Texturing additive with liquid crystal structure and preparation method and application thereof Download PDF

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CN113981543B
CN113981543B CN202111288788.7A CN202111288788A CN113981543B CN 113981543 B CN113981543 B CN 113981543B CN 202111288788 A CN202111288788 A CN 202111288788A CN 113981543 B CN113981543 B CN 113981543B
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liquid crystal
texturing
solution
polyethylene glycol
additive
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CN113981543A (en
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陆由东
毛科人
吴伟峰
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Changzhou Junhe Technology Stock Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08Etching
    • C30B33/10Etching in solutions or melts
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
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  • Photovoltaic Devices (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to the technical field of monocrystalline silicon texturing, in particular to a texturing additive with a liquid crystal structure, which comprises the following components in percentage by weight: sucrose ester 0.01-1.0%, liquid crystal emulsifier 0.02-1.2%, polyethylene glycol 0.5-3.0%, sodium lignin sulfonate 0.01-2%, tetra sodium ethylenediamine tetraacetate 0.5-1.5%, triethanolamine 0.01-1.0% and deionized water 96-99%. The sucrose ester serving as the main nucleating agent has strong polar groups, forms strong hydrogen bond with Si-H bonds on the surface of the silicon wafer, can be well adsorbed on the surface of the silicon wafer, generates rich nucleation points, and has good velvet-out performance. The liquid crystal emulsifier can self-emulsify in water phase or oil phase, and forms micelle in water, and the emulsifier molecule micelle tends to form a multilayer film structure, so that a liquid crystal structure is formed, the reflectivity of the upper and lower parts of the silicon wafer after texturing reaches good identity, and the in-wafer uniformity of the silicon wafer after texturing is improved.

Description

Texturing additive with liquid crystal structure and preparation method and application thereof
Technical Field
The invention relates to the technical field of monocrystalline silicon texturing, in particular to a texturing additive with a liquid crystal structure, and a preparation method and application thereof.
Background
The texturing is a process for producing monocrystalline silicon pieces, and is realized by adopting a mode of chemically etching to remove a damaged layer and forming an antireflection textured structure in the texturing process of the monocrystalline silicon pieces cut by diamond wires. The conventional texturing process generally adopts sodium hydroxide or potassium hydroxide solution to corrode the surface of a single crystal, and utilizes the characteristics of different corrosion rates of crystalline silicon in different crystal orientations to form uniformly-densely-distributed pyramid morphology (namely pyramid) on the surface of a silicon wafer so as to achieve the purposes of reducing the reflection of the silicon wafer on sunlight and improving the photoelectric conversion efficiency of a solar cell.
The prior texturing additive can only control the size of the pyramid within the range of 2-4 mu m, can not further improve the density of the pyramid, and has the reflectivity of the surface of only 10-14%, which is not beneficial to further improving the photoelectric conversion rate of the solar cell.
Therefore, various additive components in the texturing agent are continuously improved, the texturing additive with special structure and special function is developed, the size of the textured pyramid can be controlled below 1um, lower reflectivity is obtained, the reflectivity is reduced to below 10%, the photoelectric conversion efficiency is greatly improved, and the development of the photovoltaic industry is promoted.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a wool making additive with a liquid crystal structure, and a preparation method and application thereof.
The texture-making additive with the liquid crystal structure comprises the following components in percentage by weight: sucrose ester 0.01-1.0%, liquid crystal emulsifier 0.02-1.2%, polyethylene glycol 0.5-3.0%, sodium lignin sulfonate 0.01-2%, tetra sodium ethylenediamine tetraacetate 0.5-1.5%, triethanolamine 0.01-1.0% and deionized water 96-99%.
Preferably, the sucrose ester is one or a mixture of several of HLB values between 5 and 14.
Preferably, the liquid crystal emulsifier is one or a mixture of several of C16-18 alkyl glucoside, C16 alkanol coco glucoside, C14-22 alkanol glucoside, sorbitol stearate and sucrose cocoate.
Preferably, the polyethylene glycol is one or a mixture of several of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and polyethylene glycol 800.
The preparation method of the texturing additive with the liquid crystal structure comprises the following steps:
s1, adding sucrose ester and a liquid crystal emulsifier into a container according to parts by weight, mixing with deionized water, heating to 45-75 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignin sulfonate, ethylene diamine tetraacetic acid tetrasodium salt and triethanolamine into a container according to parts by weight, mixing with deionized water, and heating to 75-85 ℃ to obtain a solution B;
and S3, centrifugally stirring the solution B at the stirring speed of 1000r/min, adding the solution A into the solution B, stirring for 30min, and rapidly cooling to room temperature to obtain the wool making additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a wool making solution: adding the texturing additive with a liquid crystal structure into an alkali solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkali solution is 0.5-2.0% and the concentration of the additive is 0.5-2.0%;
s2, surface texturing of monocrystalline silicon: immersing monocrystalline silicon slice into the texturing solution prepared in the step S1, wherein the texturing temperature is 75-85 ℃ and the reaction time is 300-500S.
Preferably, the alkali solution is sodium hydroxide or potassium hydroxide solution.
The beneficial effects of the invention are as follows:
1. the sucrose ester serving as the main nucleating agent has strong polar groups, forms strong hydrogen bond with Si-H bonds on the surface of the silicon wafer, can be well adsorbed on the surface of the silicon wafer, generates rich nucleation points, and has good velvet-out performance.
2. Liquid crystal emulsifiers are capable of self-emulsifying in either the aqueous or oil phase, forming micelles in water, the emulsifier molecular micelles tending to form a multilayer film structure, thereby forming a liquid crystal structure. In the liquid crystal structure, gel-like crystal phases of the liquid crystal are inserted into the interface film, so that the system obtains enough hardness, fluctuation of interlayer substances is reduced, and the system obtains enough high stability. The liquid crystal structure is similar to a layered network structure, when the liquid crystal is adsorbed on the surface of a silicon wafer, the layered crystalline phase network structure is broken, polar groups are gradually released, so that nucleation points can be distributed on the surface of the silicon wafer more fully and uniformly, and therefore good uniformity is maintained after pyramid growth, reflectivity of upper and lower parts of the silicon wafer after texturing is good, and uniformity of the silicon wafer in the silicon wafer after texturing is improved.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Embodiment one:
the texture-making additive with the liquid crystal structure comprises the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.3%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5% and deionized water 96.5%.
In this example, the sucrose ester has an HLB of 11, the liquid crystal emulsifier is C16-18 alkyl glucoside, and the polyethylene glycol is polyethylene glycol 400.
The preparation method of the texturing additive with the liquid crystal structure comprises the following steps:
s1, adding sucrose ester and a liquid crystal emulsifier into a container according to parts by weight, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignin sulfonate, ethylene diamine tetraacetic acid tetrasodium salt and triethanolamine into a container according to parts by weight, mixing with deionized water, and heating to 80 ℃ to obtain a solution B;
and S3, centrifugally stirring the solution B at the stirring speed of 1000r/min, adding the solution A into the solution B, stirring for 30min, and rapidly cooling to room temperature to obtain the wool making additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a wool making solution: adding the texturing additive with a liquid crystal structure into an alkali solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkali solution is 1.0% and the concentration of the additive is 1.0%;
s2, surface texturing of monocrystalline silicon: immersing the monocrystalline silicon wafer into the texturing solution prepared in the step S1, wherein the texturing temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is sodium hydroxide solution.
Embodiment two:
the texture-making additive with the liquid crystal structure comprises the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.4%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5% and deionized water 96.4%.
In this example, the sucrose ester has HLB of 11, the liquid crystal emulsifier is C14-22 alkanol glucoside, and the polyethylene glycol is polyethylene glycol 200.
The preparation method of the texturing additive with the liquid crystal structure comprises the following steps:
s1, adding sucrose ester and a liquid crystal emulsifier into a container according to parts by weight, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignin sulfonate, ethylene diamine tetraacetic acid tetrasodium salt and triethanolamine into a container according to parts by weight, mixing with deionized water, and heating to 80 ℃ to obtain a solution B;
and S3, centrifugally stirring the solution B at the stirring speed of 1000r/min, adding the solution A into the solution B, stirring for 30min, and rapidly cooling to room temperature to obtain the wool making additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a wool making solution: adding the texturing additive with a liquid crystal structure into an alkali solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkali solution is 1.0% and the concentration of the additive is 1.0%;
s2, surface texturing of monocrystalline silicon: immersing the monocrystalline silicon wafer into the texturing solution prepared in the step S1, wherein the texturing temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is sodium hydroxide solution.
Embodiment III:
the texture-making additive with the liquid crystal structure comprises the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.2%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5% and deionized water 96.6%.
In this example, sucrose ester has HLB of 9, liquid crystal emulsifier is sorbitol stearate, and polyethylene glycol is polyethylene glycol 600.
The preparation method of the texturing additive with the liquid crystal structure comprises the following steps:
s1, adding sucrose ester and a liquid crystal emulsifier into a container according to parts by weight, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignin sulfonate, ethylene diamine tetraacetic acid tetrasodium salt and triethanolamine into a container according to parts by weight, mixing with deionized water, and heating to 80 ℃ to obtain a solution B;
and S3, centrifugally stirring the solution B at the stirring speed of 1000r/min, adding the solution A into the solution B, stirring for 30min, and rapidly cooling to room temperature to obtain the wool making additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a wool making solution: adding the texturing additive with a liquid crystal structure into an alkali solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkali solution is 1.0% and the concentration of the additive is 1.0%;
s2, surface texturing of monocrystalline silicon: immersing the monocrystalline silicon wafer into the texturing solution prepared in the step S1, wherein the texturing temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is potassium hydroxide solution.
The monocrystalline silicon is subjected to surface treatment by using the texturing additive in the first to third embodiments and adopting the monocrystalline silicon surface texturing method in the first to third embodiments, and the experimental results are as follows:
the foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (5)

1. The texture-making additive with the liquid crystal structure is characterized by comprising the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.3%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5%, deionized water 96.5%;
wherein the HLB of the sucrose ester is 11, the liquid crystal emulsifier is C16-18 alkyl glucoside, and the polyethylene glycol is polyethylene glycol 400.
2. The texture-making additive with the liquid crystal structure is characterized by comprising the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.4%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5%, deionized water 96.4%;
wherein the HLB of the sucrose ester is 11, the liquid crystal emulsifier is C14-22 alkanol glucoside, and the polyethylene glycol is polyethylene glycol 200.
3. The texture-making additive with the liquid crystal structure is characterized by comprising the following components in percentage by weight: sucrose ester 0.4%, liquid crystal emulsifier 0.3%, polyethylene glycol 1.0%, sodium lignin sulfonate 0.2%, tetra sodium ethylenediamine tetraacetate 1.0%, triethanolamine 0.5%, deionized water 96.6%;
wherein the HLB of sucrose ester is 9, the liquid crystal emulsifier is sorbitol stearate, and the polyethylene glycol is polyethylene glycol 600.
4. A method for preparing a texture-making additive having a liquid crystal structure according to any one of claims 1 to 3, comprising the steps of:
s1, adding sucrose ester and a liquid crystal emulsifier into a container according to parts by weight, mixing with deionized water, heating to 45-75 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignin sulfonate, ethylene diamine tetraacetic acid tetrasodium salt and triethanolamine into a container according to parts by weight, mixing with deionized water, and heating to 75-85 ℃ to obtain a solution B;
and S3, centrifugally stirring the solution B at the stirring speed of 1000r/min, adding the solution A into the solution B, stirring for 30min, and rapidly cooling to room temperature to obtain the wool making additive with the liquid crystal structure.
5. A single crystal silicon surface texturing method using a texturing additive having a liquid crystal structure according to any one of claims 1 to 3 or a texturing additive prepared by a method for preparing a texturing additive having a liquid crystal structure according to claim 4, comprising the steps of:
s1, preparing a wool making solution: adding the texturing additive with the liquid crystal structure into an alkali solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkali solution is 1.0% and the concentration of the additive is 1.0%;
s2, surface texturing of monocrystalline silicon: immersing the monocrystalline silicon wafer into the texturing solution prepared in the step S1, wherein the texturing temperature is 75-85 ℃, and the reaction time is 300-500S;
the alkali solution is sodium hydroxide or potassium hydroxide solution.
CN202111288788.7A 2021-11-02 2021-11-02 Texturing additive with liquid crystal structure and preparation method and application thereof Active CN113981543B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943307A (en) * 2012-11-27 2013-02-27 韩华新能源(启东)有限公司 Single crystal silicon alcohol-free wool making additive
CN103710179A (en) * 2013-12-09 2014-04-09 长沙艾森设备维护技术有限公司 Cleaning agent for solar energy monocrystalline silicon wafer
CN105113013A (en) * 2015-08-21 2015-12-02 合肥中南光电有限公司 Efficient and environment-friendly monocrystalline silicon piece texture surface making liquid and preparation method thereof
CN105113015A (en) * 2015-08-21 2015-12-02 合肥中南光电有限公司 Low-reflectivity monocrystalline silicon piece texture surface making liquid and preparation method thereof
CN110644057A (en) * 2019-10-12 2020-01-03 湖南理工学院 Monocrystalline silicon texturing additive formula containing alkyl glycoside and use method
CN110644053A (en) * 2019-10-12 2020-01-03 湖南理工学院 Formula and using method for preparing corn-shaped monocrystalline silicon suede composite texturing additive
CN111663186A (en) * 2020-06-30 2020-09-15 常州时创能源股份有限公司 Additive for texturing of diamond wire cut monocrystalline silicon wafer and application thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943307A (en) * 2012-11-27 2013-02-27 韩华新能源(启东)有限公司 Single crystal silicon alcohol-free wool making additive
CN103710179A (en) * 2013-12-09 2014-04-09 长沙艾森设备维护技术有限公司 Cleaning agent for solar energy monocrystalline silicon wafer
CN105113013A (en) * 2015-08-21 2015-12-02 合肥中南光电有限公司 Efficient and environment-friendly monocrystalline silicon piece texture surface making liquid and preparation method thereof
CN105113015A (en) * 2015-08-21 2015-12-02 合肥中南光电有限公司 Low-reflectivity monocrystalline silicon piece texture surface making liquid and preparation method thereof
CN110644057A (en) * 2019-10-12 2020-01-03 湖南理工学院 Monocrystalline silicon texturing additive formula containing alkyl glycoside and use method
CN110644053A (en) * 2019-10-12 2020-01-03 湖南理工学院 Formula and using method for preparing corn-shaped monocrystalline silicon suede composite texturing additive
CN111663186A (en) * 2020-06-30 2020-09-15 常州时创能源股份有限公司 Additive for texturing of diamond wire cut monocrystalline silicon wafer and application thereof

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