CN113981543A - 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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CN113981543A
CN113981543A CN202111288788.7A CN202111288788A CN113981543A CN 113981543 A CN113981543 A CN 113981543A CN 202111288788 A CN202111288788 A CN 202111288788A CN 113981543 A CN113981543 A CN 113981543A
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liquid crystal
texturing
solution
crystal structure
additive
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CN113981543B (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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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: 0.01-1.0% of sucrose ester, 0.02-1.2% of liquid crystal emulsifier, 0.5-3.0% of polyethylene glycol, 0.01-2% of sodium lignosulfonate, 0.5-1.5% of tetrasodium ethylenediamine tetraacetate, 0.01-1.0% of triethanolamine and 96-99% of deionized water. The sucrose ester as the main nucleating agent has strong polar groups, forms strong hydrogen bond action with Si-H bonds on the surface of a silicon wafer, can be well adsorbed on the surface of the silicon wafer to generate abundant nucleation points, and has good down production performance. The liquid crystal emulsifier can be self-emulsified in a water phase or an oil phase to form micelles in water, and molecular micelles of the emulsifier tend to form a multilayer thin film structure, so that a liquid crystal structure is formed, the reflectivity of the upper part and the lower part of a textured silicon wafer can reach good identity, and the uniformity in the textured silicon wafer 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 procedure of monocrystalline silicon wafer production, and is realized by adopting a mode of chemically corroding a damage layer and forming an anti-reflection textured structure in the texturing process of the diamond wire cut monocrystalline silicon wafer. In a conventional texturing process, sodium hydroxide or potassium hydroxide solution is generally adopted to corrode the surface of a single crystal, and the characteristics that crystalline silicon has different corrosion rates in different crystal orientations are utilized to form a uniform and dense pyramid shape (namely, a 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 size of the pyramid can only be controlled within the range of 2-4 μm by the texturing additive used at present, the density of the pyramid cannot be further improved, the reflectivity of the surface only reaches 10-14%, and the further improvement of the photoelectric conversion rate of the solar cell is not facilitated.
Therefore, various additive components in the texturing agent are continuously improved, a texturing additive with a special structure and special functions is developed, the size of a 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 texturing additive with a liquid crystal structure, and a preparation method and application thereof.
The texture-making additive with the liquid crystal structure consists of the following components in percentage by weight: 0.01-1.0% of sucrose ester, 0.02-1.2% of liquid crystal emulsifier, 0.5-3.0% of polyethylene glycol, 0.01-2% of sodium lignosulfonate, 0.5-1.5% of tetrasodium ethylenediamine tetraacetate, 0.01-1.0% of triethanolamine and 96-99% of deionized water.
Preferably, the sucrose ester is one or a mixture of more of HLB value between 5 and 14.
Preferably, the liquid crystal emulsifier is one or a mixture of more of C16-18 alkyl glucoside, C16 alkanol cocoyl glucoside, C14-22 alkanol glucoside, sorbitol stearate and sucrose cocoate.
Preferably, the polyethylene glycol is one or a mixture 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 in parts by weight into a container, mixing with deionized water, heating to 45-75 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignosulfonate, 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 texturing additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a texturing solution: adding a texturing additive with a liquid crystal structure into an alkaline solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkaline solution is 0.5-2.0%, and the concentration of the additive is 0.5-2.0%;
s2, texturing on the surface of the monocrystalline silicon: and (3) immersing the monocrystalline silicon piece 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 a sodium hydroxide or potassium hydroxide solution.
The invention has the beneficial effects that:
1. the sucrose ester as the main nucleating agent has strong polar groups, forms strong hydrogen bond action with Si-H bonds on the surface of a silicon wafer, can be well adsorbed on the surface of the silicon wafer to generate abundant nucleation points, and has good down production performance.
2. The liquid crystal emulsifier can be self-emulsified in an aqueous phase or an oil phase to form micelles in water, and molecular micelles of the emulsifier tend to form a multilayer thin film structure, so that a liquid crystal structure is formed. In the liquid crystal structure, gel-like crystal phase of liquid crystal is inserted into an interface film, so that the system obtains enough hardness, fluctuation of substances among layers is reduced, and the system obtains enough high stability. The liquid crystal structure is similar to a layered network structure, when liquid crystal is adsorbed on the surface of a silicon wafer, the structure in a multilayer crystalline phase network shape is broken, and polar groups are gradually released, so that nucleation points can be more fully and uniformly distributed on the surface of the silicon wafer, the pyramid still has good uniformity after growing up, the reflectivity of the upper part and the lower part of the silicon wafer after texturing achieves good identity, and the in-chip uniformity of the silicon wafer after texturing is improved.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The first embodiment is as follows:
the texture-making additive with the liquid crystal structure consists of the following components in percentage by weight: 0.4% of sucrose ester, 0.3% of liquid crystal emulsifier, 1.0% of polyethylene glycol, 0.3% of sodium lignosulfonate, 1.0% of tetrasodium ethylenediamine tetraacetate, 0.5% of triethanolamine and 96.5% of deionized water.
In the embodiment, 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.
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 in parts by weight into a container, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignosulfonate, 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 texturing additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a texturing solution: adding a texturing additive with a liquid crystal structure into an alkaline solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkaline solution is 1.0%, and the concentration of the additive is 1.0%;
s2, texturing on the surface of the monocrystalline silicon: and (3) immersing the monocrystalline silicon piece into the wool making liquid prepared in the step S1, wherein the wool making temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is sodium hydroxide solution.
Example two:
the texture-making additive with the liquid crystal structure consists of the following components in percentage by weight: 0.4% of sucrose ester, 0.3% of liquid crystal emulsifier, 1.0% of polyethylene glycol, 0.4% of sodium lignosulfonate, 1.0% of tetrasodium ethylenediamine tetraacetate, 0.5% of triethanolamine and 96.4% of deionized water.
In the embodiment, 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.
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 in parts by weight into a container, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignosulfonate, 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 texturing additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a texturing solution: adding a texturing additive with a liquid crystal structure into an alkaline solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkaline solution is 1.0%, and the concentration of the additive is 1.0%;
s2, texturing on the surface of the monocrystalline silicon: and (3) immersing the monocrystalline silicon piece into the wool making liquid prepared in the step S1, wherein the wool making temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is sodium hydroxide solution.
Example three:
the texture-making additive with the liquid crystal structure consists of the following components in percentage by weight: 0.4% of sucrose ester, 0.3% of liquid crystal emulsifier, 1.0% of polyethylene glycol, 0.2% of sodium lignosulfonate, 1.0% of tetrasodium ethylenediamine tetraacetate, 0.5% of triethanolamine and 96.6% of deionized water.
In this example, the HLB of sucrose ester is 9, the liquid crystal emulsifier is sorbitol stearate, and the 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 in parts by weight into a container, mixing with deionized water, heating to 60 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignosulfonate, 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 texturing additive with the liquid crystal structure.
The monocrystalline silicon surface texturing method comprises the following steps:
s1, preparing a texturing solution: adding a texturing additive with a liquid crystal structure into an alkaline solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkaline solution is 1.0%, and the concentration of the additive is 1.0%;
s2, texturing on the surface of the monocrystalline silicon: and (3) immersing the monocrystalline silicon piece into the wool making liquid prepared in the step S1, wherein the wool making temperature is 80 ℃, and the reaction time is 400S.
Wherein the alkali solution is potassium hydroxide solution.
The texturing additive in the first to third embodiments is used, and the monocrystalline silicon surface texturing method in the first to third embodiments is used to perform surface treatment on monocrystalline silicon, and the experimental results are as follows:
Figure BDA0003333849260000061
Figure BDA0003333849260000071
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (7)

1. The texture-making additive with the liquid crystal structure is characterized by comprising the following components in percentage by weight: 0.01-1.0% of sucrose ester, 0.02-1.2% of liquid crystal emulsifier, 0.5-3.0% of polyethylene glycol, 0.01-2% of sodium lignosulfonate, 0.5-1.5% of tetrasodium ethylenediamine tetraacetate, 0.01-1.0% of triethanolamine and 96-99% of deionized water.
2. The texture-making additive with a liquid crystal structure as claimed in claim 1, wherein the sucrose ester is one or a mixture of several having HLB value of 5-14.
3. The texture surface making additive with the liquid crystal structure as claimed in claim 1, and the preparation method and the application thereof, wherein the liquid crystal emulsifier is one or a mixture of more of C16-18 alkyl glucoside, C16 alkanol cocoyl glucoside, C14-22 alkanol glucoside, sorbitol stearate and sucrose cocoate.
4. The additive for making herbs into wool with liquid crystal structure, the preparation method and the application thereof according to claim 1, wherein the polyethylene glycol is one or a mixture of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and polyethylene glycol 800.
5. The preparation method of the texturing additive with the liquid crystal structure is characterized by comprising the following steps:
s1, adding sucrose ester and a liquid crystal emulsifier in parts by weight into a container, mixing with deionized water, heating to 45-75 ℃, and continuously stirring to obtain a solution A;
s2, adding polyethylene glycol, sodium lignosulfonate, 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 texturing additive with the liquid crystal structure.
6. The monocrystalline silicon surface texturing method is characterized by comprising the following steps:
s1, preparing a texturing solution: adding a texturing additive with a liquid crystal structure into an alkaline solution, and uniformly mixing to prepare a texturing solution, wherein the concentration of the alkaline solution is 0.5-2.0%, and the concentration of the additive is 0.5-2.0%;
s2, texturing on the surface of the monocrystalline silicon: and (3) immersing the monocrystalline silicon piece into the texturing solution prepared in the step S1, wherein the texturing temperature is 75-85 ℃, and the reaction time is 300-500S.
7. The method of claim 6, wherein the alkali solution is a sodium hydroxide or potassium hydroxide solution.
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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
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
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
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
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
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
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
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
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
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
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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