Alcohol-free amphiphilic texturing additive and preparation method thereof

An additive and amphiphilic technology, which is applied in the field of alcohol-free amphiphilic texturing additive and its preparation, can solve the problems of weak silicon adsorption, achieve high-efficiency texturing performance, good application prospects, and good large-scale industrialization promotion potential effect

Active Publication Date: 2022-02-25
ZHEJIANG AUFIRST MATERIAL TECH CO LTD
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AI-Extracted Technical Summary

Problems solved by technology

[0004] In order to solve the problem of alcohols and other low-boiling volatile substances in the prior art, it is necessary to continuously replenish volatile substances and have weak adsorption to silicon. The invention provides a novel, alcohol-free, amphiphilic, texturing additive for treati...
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Method used

Fig. 3 is the texturing liquid of the amphiphilic texturing additive prepared by embodiment 1, the microscope picture of the texturing silicon chip suede surface after placing 50h at 85 DEG C, and the magnification is 1000 times, as can be seen clearly, The suede coverage is complete and the pyramids are evenly distributed. Comparing Figure 3 with Figure 2, it proves that the ...
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Abstract

The invention discloses an alcohol-free amphiphilic texturing additive and a preparation method thereof, and belongs to the technical field of monocrystalline silicon surface treatment. The additive comprises polysaccharide, a surfactant and inorganic base, but does not contain alcohols, and is an alcohol-free amphiphilic texturing additive. Polysaccharide is adsorbed on the surface of monocrystalline silicon, can effectively reduce surface tension in a solution, is adsorbed on the surface of a silicon wafer as a starting point of a corrosion reaction, and provides a nucleation site for texturing corrosion. The polysaccharide is adsorbed on the surface of the silicon wafer, so that hydrogen generated in the texturing process is enabled to be timely separated from the surface of the silicon wafer, and uneven texturing caused by wafer floating or bubble mark generation is avoided. The surfactant is associated with the polysaccharide to solve the problem of high-temperature precipitation of the polysaccharide, and the additive with good adsorbability and solution stability is obtained. The additive assists the growth of a pyramid on the surface of a silicon wafer, enhances anisotropic factors of anisotropic corrosion, forms a good light trapping structure on the surface of the silicon, increases the optical path of light on the surface of the silicon, and reduces the reflectivity of the silicon wafer.

Application Domain

Polycrystalline material growthAfter-treatment details +3

Technology Topic

Optical pathChemistry +13

Image

  • Alcohol-free amphiphilic texturing additive and preparation method thereof
  • Alcohol-free amphiphilic texturing additive and preparation method thereof
  • Alcohol-free amphiphilic texturing additive and preparation method thereof

Examples

  • Experimental program(3)
  • Comparison scheme(1)

Example Embodiment

[0031] Example 1-10
[0032] According to the amount of the components in each of the following table, it is called, and the polysaccharide is added to the inorganic base solution, and the mixture is dissolved in the inorganic base solution, and the mixture is dissolved in the inorganic base solution. .
[0033] Table 1 Embodiment 1-10 of the components
[0034]
[0035]

Example Embodiment

[0040] Example 11 Test when used in failure
[0041] Test methods for failure, including the following steps:
[0042](1) The obtained an aqueous solution prepared by the prepared formulation of an example is 0.1%, and then the NaOH solid of 2% of the NaOH mass concentration is added;
[0043] (2) Preparation of a solution of a concentration of a concentration of a concentration of a concentration of a concentration of 0.1%, and then a NaOH solid having a NaOH mass concentration of 2%;
[0044] (3) Eleged liquid prepared by heating step (1) and (2) at 85 ° C, and the falling liquid temperature reached at 85 ° C, and placed in a single crystal silicon wafer to the reaction tank, and the reaction was 360s Silicon wafer, rinse the front and negative surface with pure water 15s, add N 2 Dry under the atmosphere. Since then, a phenotypy is performed every 2h, and the appearance of the four flavor flake appearance is obviously deteriorated.

Example Embodiment

[0045] Example 12 Silicon wafer weight loss test
[0046] Test methods for wafers weight loss, including the following steps:
[0047] (1) The obtained an aqueous solution prepared by the prepared formulation of an example is 0.1%, and then the NaOH solid of 2% of the NaOH mass concentration is added;
[0048] (2) Preparation of a solution of a concentration of a concentration of a concentration of a concentration of a concentration of 0.1%, and then a NaOH solid having a NaOH mass concentration of 2%;
[0049] (3) Heating steps (1) and (2) prepared from the flavor to 85 ° C; 2 sets of single crystal silicon wafers, 10 pieces per group, recorded in group I and II; use the preparation of the present invention The pile of the velvet additive was continuously velvet in group I, and the set of silicon wafers containing the II group silicon containing the existing product. The silicon wafer was dried. The weight changes before and after the reaction of the silicon film, thereby examining the weight loss stability of the silicon wafers with different velvet hydraulic velvet.
[0050] Table 3 Performance test results of embodiment
[0051]
[0052]
[0053] In terms of weight loss, use of additives containing simultaneous polysaccharide and surfactant, the wafer has a stable value before and after the reaction, fluctuating in a range of 0.2 g ± 0.02g; the use of polysaccharide materials in ratio 1 without surface When an additive of the active agent, since the effective ingredients in the pile is gradually precipitated, the weight loss of the silicon wafer not only has a high start value, but also has significantly increased over time; contained in ratio 2 contains a surfactant without containing polysaccharides, the velvet There is no substance that can be supplied into a nuclear sites in the liquid, and the silicon wafer is severely corroded by the alkali, which is highly reduced, and there is no significant change due to time growth. The contrast extension 3 reduction is slightly higher than the contrast 1, because the alkali promotes the solubility of the polysaccharide, and when the additive does not contain the inorganic base, the polysaccharide content in the ulcerous solution may be slightly lower than the inorganic base additive velvet The content in the liquid results in a reduction in nuclear sites, and the degree of etching in the direction perpendicular to the plane of the silicon wafer makes weight loss slightly. The contrast of isopropyl alcohol was added to the phenoliol using the decanol of the present invention, and the initial weight loss (0.22 g) was slightly higher than that of the embodiment, and the failure weight loss (0.30 g) was significantly higher than the initial weight loss. This may be because isopropyl alcohol is attached to a partial surface region of the silicon wafer as a nucleation agent, and its adsorption force is weaker so that the mask is insufficient, and the silicon wafer is highly etched and thus weight loss; in subsequent heating In the process, isopropyl alcohol is gradually volatilized, and the number of nucleation sites has caused weight loss to increase until it is exposed.
[0054] During single crystal silicon, the polysaccharide can effectively reduce the surface tension of the solution, adsorb the surface of the silicon film to provide the starting point, while effectively facilitating the desorption of the generated gas, ensuring uniform system Silicone. However, when a separate polysaccharide is used in the velvet conditions, the polysaccharide substance adsorbed on the silicon wafer is precipitated with time, and the number of nucleation sites is reduced. The silicon is gradually exposed to the alkali environment, so the number of pyramids is reduced, and the shape is deteriorated, at 1000 Under the multiplication microscope, it can be seen that the pyramid is sparse after the initial arrangement is tight into heating for a period of time. The addition of surfactants in polysaccharide can be used to stably dissolve polysaccharides by association, even if it is heated, it can maintain a furproof, to obtain a silicon wafer surface, under 1000 times microscope, pyramid, pyramid in initial and There was no significant change after heating for a period of time. If the surfactant in the present invention is used alone under the decancing conditions, the surfactant cannot be provided into a nuclear bit point in the surface of the silicon wafer, so that the reaction thereof is alkalite. Under 1000 times of microscope, you can see that there is only a little pyramid on the surface of the silicon.
[0055] The specific result is: figure 1 It is a set of pyrocollenesia-produced velvet additives prepared by Example 1, and the SEM picture of the silicon velvet surface was placed at 85 ° C, and the magnification was 80,000 times, and it could be clearly seen that the silicon suede is A four-square cone pyramid composition, the pyramid is closely arranged, and it is wrong. figure 2 It is a result of a knocked microscope picture of the amphiphilic velvet, which is produced at 85 ° C for 0 h, and the magnification is 1000 times. surface.
[0056] image 3 It is a result of a buffalnamer, and the microscope picture of the silicon flannel was produced at 85 ° C for 50 hours, and the magnification was 1000 times, and it could be clearly seen that the suede covered is complete. The pyramid is evenly distributed. image 3 and figure 2 Compared, it is proved that the addition of surfactants in polysaccharide can be combined to stably dissolve polysaccharide in solution, even if it is heated, it can maintain a wonderful silicon film, under 1000 times microscope There is no significant change in the initial and heated for a while.
[0057] Figure 4 It is a microscope picture of the silicon flannel, the magnification is 1000 times, which can be clearly seen that the pyrolysis is uniform, and the pyramid is uniform, indicating that the pyramid is evenly distributed. The corrosion site is provided for suede formation. Figure 5 It is a microscope picture of the silicon blade, and the magnification is 1000 times, which can be clearly seen that there is no complete suede cover of the surface of the silicon surface, indicating that the surface of the silicon surface is lost at this time. Effective polysaccharide adsorption, prove that polysaccharide is significantly reduced in solution.
[0058] Image 6 It is the use of the anti-velvet containing the surfactant in the present invention, and the microscope picture of the silicon velvet surface is placed at 85 ° C, and the magnification is 1000 times, which can be clearly seen that the surface of the silicon is obvious. Corrosion, proves that the surfactant is not adsorbed on the silicon wafer to provide a nuclear bit. Comparative Example 2 The surfactant in the present invention was separately used under the decancing conditions, and the surfactant was unable to adhere to the surface of the silicon substance due to lack of adsorbed polyhydroxy structures. The surface of the silicon wafer lacks a nuclear bit to make it completely Alkali corrosion, under 1000 times microscope, you can see that there is only a little pyramid on the surface of the silicon.
[0059] Figure 7 It is a decancing of the velvet additive of the ratio 1, and the microscope picture of the silicon velvet surface after 6 h is placed at 85 ° C, and the magnification is 1000 times, which can be clearly seen that the suede ratio image 3 The pyramid distribution is dispersed after 50 h, which is demonstrated that the pyramidal effect is not as prepared in the same conditions as in the same conditions. When the polysaccharide is used alone, the polysaccharide substance adsorbed on the silicon wafer is precipitated with time, and the number of nucleate sites is gradually exposed to the alkali environment, so the number of pyramids is reduced. Deternection, under 1000 times microscope, it can be seen that the pyramid is sparsely dispersed by the initial arrangement to be heated for a period of time. Compared Figure 7 and Figure 4 It can be seen that the pyramid density containing no tablet additive is less than 0 h, indicating that the nucleating agent concentration is reduced, and the nucleation site is reduced, so the pyramid is sparse.
[0060] Figure 8 It is a decancing of the velvet additive of the ratio 2, and the microscope picture of the velvet, the microscope of the silicon, and 1000 times, can clearly see that the silicon wafer is severely corroded. Further demonstrate additives without polysaccharide unable to provide a nucleation site of silicon surface.
[0061] Figure 9 It is a pixel using Example 1 and a decision additive of the adjusted additive of the Comparative Example 5, and the picture of the appearance of the silicon wafer is placed at 85 ° C, and the left side is a film of the formula 1, and the right side is the ratio 5 The silicon wafer can clearly see that the appearance of the left silicon wafer is uniform, the upper silicon appearance is uneven, and the appearance of the radiation, the appearance means that the problem of micro pyramids, indicating that the contrast 5 is clearly weak. In Example 1.

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