CN109786501B - Texturing method of polycrystalline black silicon wafer - Google Patents
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Abstract
The invention provides a polycrystalline black silicon texturing method, which comprises the steps of firstly placing a silicon wafer subjected to hole digging into a mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer; and then carrying out subsequent treatment on the desilverized and chambered silicon wafer according to the prior art to obtain the textured polycrystalline black silicon wafer. The method comprises the following steps of selecting a mixed solution as a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid, a mixed solution composed of ammonium nitrite and hydrofluoric acid or a solution composed of ammonium nitrite and ammonium fluoride; furthermore, the texturing method can simultaneously realize two process steps of silver removal and hole expansion in one reaction system, and the obtained textured surface of the textured silicon wafer is good; not only shortens the process flow of the reaction, but also reduces the cost of silicon wafer texturing.
Description
Technical Field
The invention relates to the field of silicon solar cells, in particular to a texturing method for a polycrystalline black silicon wafer.
Background
The silicon solar cell is developed relatively mature in the field of solar cells, has strong practicability and is commercialized for many years now. With the continuous development of the technology, the photoelectric conversion rate is correspondingly improved, and the cost is also continuously reduced. Today, the ratio of solar cells to energy consumed by society is increasing year by year due to the exhaustion of fossil energy.
The production process of the wet black silicon solar cell mainly comprises the following steps: texturing, diffusion, etching, coating, printing, sintering and the like. Texturing is the first step in the preparation of silicon solar cells and is also very importantAn important step. At present, the texturing process of the silicon solar cell mainly comprises a reactive ion etching method (RIE), a mechanical grooving technology, a laser etching technology, a honeycomb texturing technology, metal induced wet black silicon (MCCE) and the like. The MCCE process is currently the most common process used in the industry. The main process of the process comprises alkali washing, acid washing, silver precipitation, hole digging, silver removal, acid washing, hole expanding, alkali washing, acid washing, drying and the like, wherein a plurality of water washing steps are also doped. Wherein, the acid washing is to neutralize residual alkali liquor, organic matters and the like, so as to avoid influencing the next silver plating; the silver plating step is undoubtedly one of the key steps, with the aim of forming reaction sites; then, digging holes on the silver sites, desilvering by using hydrogen peroxide and ammonia water solution after digging the holes, and adopting HF/HNO after desilvering3To ream the hole. Residual acid solution is KOH + H2O2+NH4OH is used for washing, and burrs and small structures on the surface of the silicon wafer are removed simultaneously. Then acid washing is carried out to remove residual alkali liquor, and finally water washing and drying are carried out. The process flow is numerous and complicated, and each step affects the final efficiency. HF/HNO, especially in the reaction scheme for pore expansion3The chemical reaction in the system mainly consists of oxidation reaction and dissolution reaction. Nitric acid as a strong oxidant to oxidize Si to SiO2，SiO2Again, the formation of nitric acid can be prevented. While hydrofluoric acid will dissolve SiO2Corroded and thereby dissolved in water. The reaction occurs first at the fault or recombination center of the wafer, i.e., the reaction site with lower activation energy. The reaction will progress both laterally and longitudinally. However, after a while, the longitudinal excitation energy becomes high, and thus the reaction speed becomes slow, and eventually lower than the transverse speed. The silver nanoparticles in the system act as reaction sites, where the reaction rate is much higher than where no silver nanoparticles are attached, and thus a void-like nanostructure is created. This structure can reduce the reflectivity, thereby improving the efficiency of the battery. However, the two-step etching process of desilvering and pore-expanding is long, and the cost is inevitably increased. Moreover, the increase of the process steps also increases the risk of contamination, such as oil stains and impurities. Therefore, how to improve the texturing efficiency of the texturing process has important significance.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a texturing method for a polycrystalline black silicon wafer, in which the desilvering and hole expanding processes are performed in the same system, so that the texturing efficiency is improved, and the obtained textured surface of the textured silicon wafer is good.
The invention provides a texturing method of a polycrystalline black silicon wafer, which comprises the following steps:
1) placing the silicon wafer with the hole into the mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer;
the mixed solution is a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid, a mixed solution composed of ammonium nitrite and hydrofluoric acid, a mixed solution composed of ammonium nitrate and ammonium fluoride, a solution composed of ammonium nitrite and ammonium fluoride or a solution composed of ammonium ceric nitrate and ammonium fluoride;
2) and carrying out subsequent treatment on the desilverized and chambered silicon wafer to obtain the textured polycrystalline black silicon wafer.
Preferably, the temperature of the treatment in the step 1) is 6-30 ℃.
Preferably, the temperature of the treatment in the step 1) is 10-25 ℃.
Preferably, the mass fraction of the solute in the mixed solution is 15% to 45%.
Preferably, the mass fraction of the solute in the mixed solution is 20% to 30%.
Preferably, in the mixed solution, the molar ratio of the primary fluorine ions to the primary nitrate ions is 1: (1-5);
in the mixed solution, the molar ratio of the primary complex fluoride ions to the primary complex nitrite ions is 1: (1-5).
Preferably, in the mixed solution, the molar ratio of fluoride ions, nitrate ions and ammonium ions is 1: (2-3);
in the mixed solution, the molar ratio of the primary complex fluoride ions to the primary complex nitrite ions is 1: (2-3).
Preferably, the time for the treatment in the step 1) is 60-600 seconds.
Preferably, the silicon wafer with the holes is prepared according to the following method: and sequentially carrying out alkali washing, acid washing, silver precipitation and hole digging treatment on the silicon wafer to be subjected to texturing to obtain the hole-dug silicon wafer.
Preferably, the step 2) is to sequentially perform alkali washing, acid washing, water washing, drying and the like on the reamed silicon wafer to obtain the textured silicon wafer.
Compared with the prior art, the invention provides a texturing method of a polycrystalline black silicon wafer, which comprises the steps of firstly putting a silicon wafer with a hole into a mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer; and then, further processing the expanded silicon wafer to obtain the textured polycrystalline black silicon wafer. The method comprises the following steps of selecting a mixed solution as a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid or a mixed solution composed of ammonium nitrite and hydrofluoric acid, a mixed solution composed of ammonium nitrate and ammonium fluoride, a solution composed of ammonium nitrite and ammonium fluoride or a solution composed of ammonium ceric nitrate and ammonium fluoride; furthermore, the texturing method can simultaneously realize two process steps of silver removal and hole expansion in one reaction system, and the obtained textured surface of the textured silicon wafer is good; the technological process of the reaction is not shortened, and the silicon wafer texturing cost is reduced.
Drawings
FIG. 1 is a digital image of an enlarged appearance of a textured silicon wafer prepared in example 1;
FIG. 2 is a digital image of the appearance of the textured silicon wafer prepared in example 1;
FIG. 3 is a scanning electron micrograph of a textured silicon wafer prepared according to example 1;
FIG. 4 is a numerical chart showing the appearance of the textured silicon wafer prepared in comparative example 1;
FIG. 5 is a flow chart under a standard process;
FIG. 6 is a process flow diagram of a method of making the present invention.
Detailed Description
The invention provides a texturing method of a polycrystalline black silicon wafer, which comprises the following steps:
1) placing the silicon wafer with the hole into the mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer;
the mixed solution is a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid or a mixed solution composed of ammonium nitrite and hydrofluoric acid;
2) and further processing the reamed silicon wafer to obtain the textured polycrystalline black silicon wafer.
According to the invention, the silicon wafer with the hole dug is placed into a mixed solution for desilvering and reaming treatment to obtain a reamed silicon wafer; wherein the treatment temperature is preferably 6-30 ℃, more preferably 10-25 ℃, and most preferably 15-20 ℃; the treatment time is preferably 60 to 600 seconds, more preferably 100 to 400 seconds, and most preferably 150 to 300 seconds; the mixed solution is preferably a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid, a mixed solution composed of ammonium nitrite and hydrofluoric acid, a mixed solution composed of ammonium nitrate and ammonium fluoride, a solution composed of ammonium nitrite and ammonium fluoride or a solution composed of ammonium ceric nitrate and ammonium fluoride, and more preferably a mixed solution composed of ammonium fluoride and ammonium nitrate; in the mixed solution, the molar ratio of the primary fluorine ions to the primary nitrate ions is 1: (1-5), wherein the amount of the substance of ammonium ion varies depending on the kinds of the two solutes and the amount of the substance. In the mixed solution, the molar ratio of the primary complex fluoride ions to the primary complex nitrite ions is 1: (1-5), wherein the amount of the substance of ammonium ion varies with the kinds of the two solutes and the amounts of the substances, and more specifically, the molar ratio of the initially coordinated fluoride ion, the initially coordinated nitrate ion and the initially coordinated ammonium ion in the mixed solution is preferably 1: (1-5): (1-6); more preferably 1: (2-3): (2-4), most preferably 1:3: 4; or in the mixed solution, the molar ratio of the primary complex fluoride ions, the primary complex nitrite ions and the primary complex ammonium ions is preferably 1: (1-5): (1-6); more preferably 1: (2-3): (2-4), most preferably 1:3: 4; the mass fraction of the solute in the mixed solution is preferably 15% to 45%, and more preferably 20% to 30%.
In the invention, the source of the silicon wafer with holes dug in the invention is not particularly required, and the silicon wafer with holes dug prepared by the preparation method known in the field can be used, and the silicon wafer with holes dug in the invention can be prepared by the following method conventionally: sequentially carrying out alkali washing, acid washing, silver precipitation and hole digging treatment on a silicon wafer to be subjected to texturing to obtain a hole-dug silicon wafer; the silicon wafer to be subjected to texturing has no special requirement and can be black silicon or a common silicon wafer; the invention has no special requirements on the processes of acid washing, alkali washing, silver precipitation and hole digging treatment, and can adopt methods known in the field.
According to the invention, the reamed silicon wafer is subjected to subsequent treatment according to a conventional process to obtain a textured polycrystalline black silicon wafer; the silicon wafer after desilvering and reaming is preferably subjected to alkali washing, acid washing, water washing, drying and the like in sequence to obtain the textured silicon wafer, wherein the alkali washing or acid washing process has no special requirements, and the processes which can be used for alkali washing and acid washing of the silicon wafer after reaming are known by the technical personnel in the field.
The polycrystalline black silicon wafer texturing method provided by the invention comprises the steps of firstly placing a silicon wafer with holes into a mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer; and then carrying out subsequent treatment on the reamed silicon wafer according to a conventional process to obtain the textured polycrystalline black silicon wafer. The method comprises the following steps of selecting a mixed solution as a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid, a mixed solution composed of ammonium nitrite and hydrofluoric acid, a mixed solution composed of ammonium nitrate and ammonium fluoride, a solution composed of ammonium nitrite and ammonium fluoride or a solution composed of ceric ammonium nitrate and ammonium fluoride; furthermore, the texturing method can simultaneously realize two process steps of silver removal and hole expansion in a solution system, and the obtained textured surface of the textured silicon wafer is good; not only shortens the process flow of the reaction, but also reduces the cost of silicon wafer texturing.
Specifically, the process flow diagrams of the texturing silicon wafer prepared by the method and the prior art are shown in fig. 5-6; FIG. 5 is a flow chart of a prior art standard process; FIG. 6 is a process flow diagram of a preparation method provided by the present invention.
In addition, in the present application, the mole numbers of the initially prepared fluoride ion, the initially prepared nitrite ion and the initially prepared nitrate ion refer to the mole number of the fluoride ion, the mole number of the nitrite ion and the mole number of the nitrate ion added when the mixed solution is prepared, and if 1mol of ammonium fluoride and 1mol of ammonium nitrate are added to the mixed solution to obtain the mixed solution, the mole number of the initially prepared fluoride ion is 1mol, and the mole number of the initially prepared nitrate ion is 1 mol.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The polycrystalline black silicon texturing process comprises the following steps:
treating the polycrystalline black silicon wafer by adopting a standard cleaning process, wherein the specific process parameters are as follows: the solution is 14% KOH + 0.5% Naxin additive A, the percentage is volume fraction, the temperature is 78 ℃, the reaction time is 210 s. The mass fraction of KOH was 48%.
And depositing a layer of silver nanoparticles on the surface of the silicon wafer subjected to the cleaning process. The specific process parameters are as follows: the solution is 1.5 percent of HF +0.3 percent of Naxin additive B, the percentage is volume fraction, the temperature is 25 ℃, and the reaction time is 120 s. The HF mass fraction was 49%.
And (4) digging holes in the silicon wafer on which the silver nanoparticles are deposited. The specific process parameters are as follows: the solution was 11.4% HF + 32% H2O2+ 0.5% of Naxin additive C + 0.16% of Naxin additive D, the percentage being volume fraction, the temperature being 34-36 ℃, the reaction time being 210 s. HF mass fraction of 48 percent and 30 percent of hydrogen peroxide by mass.
And carrying out desilvering and reaming integrated treatment on the silicon wafer with the hole. The specific process comprises the following steps: putting the silicon chip with the hole into solution with the composition of NH4F+NH4NO3In the mixed aqueous solution of (a), (wherein: NH (NH)4F and NH4NO3Has a molar ratio of 1:3 and a solute mass concentration of 30% (i.e., NH)4F+NH4NO3The sum of the two types of silicon chips) at the reaction temperature of 10 ℃ for 100s to obtain the desilverized chambered silicon chip.
Sequentially carrying out alkaline washing (NaOH + NH) on the desilvered and chambered silicon wafer3·H2O+H2O2120s-180 s; room temperature), acid wash (NaOH + NH)3·H2O+H2O2120s-180 s; room temperature), water washing and drying (nitrogen/clean compressed air; heating) to obtain a textured silicon wafer.
The analysis results of the obtained textured silicon wafer are shown in fig. 1 to 3, fig. 1 is an enlarged appearance digital diagram of the textured silicon wafer prepared in example 1, fig. 2 is an appearance digital diagram of the textured silicon wafer prepared in example 1, and fig. 3 is a scanning electron microscope image of the textured silicon wafer prepared in example 1. As can be seen from the three figures, the polycrystalline black silicon obtained by the method has a frosted effect macroscopically, and holes are uniform and compact microscopically.
Example 2
Preparing a hole-digging silicon wafer in the same way as in example 1;
and carrying out desilvering and reaming integrated treatment on the silicon wafer with the hole. The specific process comprises the following steps: putting the silicon chip with the hole into solution with the composition of NH4F+NH4NO3In the mixed aqueous solution of (a), (wherein: NH (NH)4F and NH4NO3Has a molar ratio of 1:3 and a solute mass concentration of 20% (i.e., NH)4F+NH4NO3The sum of the two types of silicon chips) at the reaction temperature of 25 ℃ for 100s to obtain the desilverized chambered silicon chip.
The polycrystalline black silicon is in a porous structure in appearance and the holes are uniform and compact through the detection of a scanning electron microscope.
Can be dissolved in a specific solvent by the above experimentThe one-step pore expansion is realized under liquid, and the reaction mechanism is supposed to be as follows: NH is produced by hydrolysis of ammonium salts in water4OH, the solution is acidic, nitrate/nitrite is reduced after contacting with silver nano particles under the acidic condition, a large number of holes are generated in the silver nano particles, the holes in the silver nano particles are injected into Si through contact, the Si in the contact part can be oxidized into silicon dioxide, and the silicon dioxide can be oxidized into silicon dioxide by F-Corroding to generate fluosilicic acid, when the hole injection rate of the silver nanoparticles is greater than the corroded rate of the silicon dioxide, complexing the silver nanoparticles by a large amount of ammonia water to leave the surface of the silicon wafer to achieve the effect of desilvering, and when the silver nanoparticles are not used as reaction sites, oxidizing the silicon wafer by nitric acid to generate the silicon dioxide directly to be F-doped-Corroding to achieve the effect of reaming.
Comparative example 1:
preparing a hole-digging silicon wafer in the same way as in example 1;
and carrying out desilvering and reaming integrated treatment on the silicon wafer with the hole. The specific process comprises the following steps: putting the silicon chip with the hole into solution with the composition of NH4F+KNO3In the mixed aqueous solution of (a), (wherein: NH (NH)4F and NH4NO3Has a molar ratio of 1:5 and a solute mass concentration of 15% (i.e., NH)4F+NH4NO3The sum of the two types of silicon chips) at the reaction temperature of 10 ℃ for 100s to obtain the desilverized chambered silicon chip.
The reaction was very slow and the resulting dug silicon wafer was examined, the results are shown in figure 4,
FIG. 4 is a numerical chart showing the appearance of the textured silicon wafer prepared in comparative example 1; as can be seen from the figure, the difference between the suede and the suede after hole digging is not large, the suede is dark and is yellow, and crystal grains obviously do not form a frosting effect.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. A texturing method of a polycrystalline black silicon wafer comprises the following steps:
1) placing the silicon wafer with the hole into the mixed solution for desilvering and chambering treatment to obtain a chambered silicon wafer;
the mixed solution is a mixed solution composed of ammonium fluoride and nitric acid, a mixed solution composed of ammonium fluoride and nitrate, a mixed solution composed of ammonium fluoride and nitrous acid, a mixed solution composed of ammonium nitrate and hydrofluoric acid, a solution composed of ammonium nitrite and ammonium fluoride or a mixed solution composed of ammonium nitrite and hydrofluoric acid;
2) and carrying out subsequent treatment on the reamed silicon wafer to obtain the textured polycrystalline black silicon wafer.
2. The texturing method according to claim 1, wherein the temperature of the step 1) treatment is 6 to 30 ℃.
3. The texturing method according to claim 1, wherein the temperature of the step 1) treatment is 10 to 25 ℃.
4. The texturing method according to claim 1, wherein the mass fraction of the solute in the mixed solution is 15% to 45%.
5. The texturing method according to claim 1, wherein the mass fraction of the solute in the mixed solution is 20% to 30%.
6. The wool making method according to claim 1, wherein the molar ratio of the initially-mixed fluoride ions to the initially-mixed nitrate ions in the mixed solution is 1: 1 to 5;
in the mixed solution, the molar ratio of the primary fluorine ions to the primary nitrite ions is 1: 1-5.
7. The wool making method according to claim 1, wherein the molar ratio of the initially-mixed fluoride ions to the initially-mixed nitrate ions in the mixed solution is 1: 2-3;
in the mixed solution, the molar ratio of the primary fluorine ions to the primary nitrite ions is 1: 2-3.
8. The texturing method according to claim 1, wherein the time for the step 1) is 60 to 600 seconds.
9. The texturing method according to claim 1, wherein the silicon wafer with holes is prepared according to the following method:
and sequentially carrying out alkali washing, acid washing, silver precipitation and hole digging treatment on the silicon wafer to be subjected to texturing to obtain the hole-dug silicon wafer.
10. The texturing method according to claim 1, wherein the step 2) is specifically to sequentially perform alkali washing, acid washing, water washing and drying on the silicon wafer after hole expanding to obtain the textured silicon wafer.
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| WO2010042209A1 (en) * | 2008-10-09 | 2010-04-15 | Bandgap Engineering, Inc. | Process for structuring silicon |
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