CN111650022A - Method for determining silicon nitride film in HIT solar cell - Google Patents
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- CN111650022A CN111650022A CN202010696977.7A CN202010696977A CN111650022A CN 111650022 A CN111650022 A CN 111650022A CN 202010696977 A CN202010696977 A CN 202010696977A CN 111650022 A CN111650022 A CN 111650022A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 32
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 61
- 238000002386 leaching Methods 0.000 claims abstract description 56
- 229910052738 indium Inorganic materials 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 54
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 49
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910001449 indium ion Inorganic materials 0.000 claims abstract description 17
- 239000012634 fragment Substances 0.000 claims abstract description 16
- 238000002835 absorbance Methods 0.000 claims abstract description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 150000002471 indium Chemical class 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 24
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 235000021110 pickles Nutrition 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
The invention discloses a method for determining a silicon nitride film in an HIT (heterojunction with intrinsic thin layer) solar cell, which comprises the following steps: selecting two HIT battery pieces, weighing and crushing; acid leaching the first battery fragment to obtain a first acid leaching solution, and measuring the volume of the first acid leaching solution; placing the second battery fragments in hydrofluoric acid solution for reaction, then carrying out acid leaching to obtain a second acid leaching solution, and measuring the volume of the second acid leaching solution; preparing an indium standard solution, measuring the absorbance of the indium standard solution, and drawing a standard curve of the absorbance and the indium concentration; respectively measuring the absorbance of the first acid leaching solution and the second acid leaching solution, and then calculating to obtain the concentration of the indium ions in the first acid leaching solution and the second acid leaching solution; calculating to obtain the mass fraction of indium in the first HIT battery piece and the second HIT battery piece; judging a silicon nitride film in the HIT battery; according to the invention, the recovery rate of the metal indium in the HIT cell is improved by determining whether the silicon nitride film exists in the HIT cell.
Description
Technical Field
The invention relates to the technical field of photovoltaic material recycling, in particular to a method for determining a silicon nitride film in an HIT (heterojunction with intrinsic thin-film) solar cell.
Background
Common HIT (heterojunction with intrinsic thin) solar cells include single-sided HIT solar cells, double-sided HIT solar cells, and back-contact HIT solar cells. The most typical HIT solar cell is a double-sided HIT solar cell which is developed in the Sanyo Japan and is based on an N-type substrate, and the structure of the HIT solar cell is that an N-type monocrystalline silicon wafer is used as the substrate, and an N-type intrinsic amorphous silicon film, a P-type amorphous silicon film, a TCO (transparent conductive oxide) transparent conductive oxide film and a silver gate electrode are symmetrically distributed on two sides of the substrate.
In recent years, the structure of the HIT solar cell is continuously improved, and the efficiency is continuously improved. However, for HIT solar cells of different structures, it cannot be determined whether the surface of the TCO layer is covered with a silicon nitride film.
Disclosure of Invention
The invention aims to provide a method for determining a silicon nitride film in an HIT (heterojunction with intrinsic thin film) solar cell, which aims to solve the problem that whether a layer of silicon nitride film covers the surface of a TCO (transparent conducting oxide) layer or not cannot be determined for HIT solar cells with different structures in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for determining a silicon nitride film in an HIT (heterojunction with intrinsic thin layer) solar cell, which comprises the following steps:
selecting two HIT solar cells, namely a first HIT solar cell and a second HIT solar cell, weighing and crushing the two HIT solar cells respectively to obtain a first cell fragment and a second cell fragment;
placing the first battery fragments in excessive concentrated nitric acid for acid leaching and filtering to obtain a first acid leaching solution, and measuring the volume of the first acid leaching solution;
placing the second battery fragments into a hydrofluoric acid solution for reaction, cleaning, air-drying, placing into excessive concentrated nitric acid for acid leaching, filtering to obtain a second acid leaching solution, and measuring the volume of the second acid leaching solution;
preparing a series of indium standard solutions with different concentrations, and then measuring and drawing a standard curve of the absorbance and the indium concentration by using a spectrophotometer;
respectively measuring the absorbance of the first acid leaching solution and the second acid leaching solution by using a spectrophotometer, and respectively calculating the concentration of indium ions in the first acid leaching solution and the concentration of indium ions in the second acid leaching solution according to the standard curve;
calculating the mass fraction of indium in the first HIT solar cell piece according to the mass of the first HIT solar cell piece, the volume of the first acid leaching solution and the concentration of indium ions in the first acid leaching solution;
calculating the mass fraction of indium in the second HIT solar cell piece according to the mass of the second HIT solar cell piece, the volume of the second acid immersion liquid and the concentration of indium ions in the second acid immersion liquid;
and judging the silicon nitride film in the HIT solar cell according to the magnitude relation between the mass fraction of the indium in the first HIT solar cell and the mass fraction of the indium in the second HIT solar cell.
Further, according to the magnitude relation between the mass fraction of indium in the first HIT solar cell piece and the mass fraction of indium in the second HIT solar cell piece, the specific method for judging the silicon nitride film in the HIT solar cell comprises the following steps: when the mass fraction of indium in the first HIT solar cell sheet is smaller than the mass fraction of indium in the second HIT solar cell sheet, a silicon nitride film is present in the HIT solar cell for the following reasons: if the HIT solar cell has a silicon nitride film, the HIT solar cell is firstly placed in hydrofluoric acid solution for reaction, the silicon nitride film covered on the TCO layer is removed by hydrofluoric acid, indium tin oxide in the TCO layer is exposed, and then the HIT solar cell is placed in excessive concentrated nitric acid for acid leaching, so that the concentrated nitric acid can sufficiently react with the indium tin oxide, and the mass fraction of the leached indium is higher than that of the indium which is not treated by the hydrofluoric acid solution and is directly placed in the excessive concentrated nitric acid for acid leaching;
when the mass fraction of indium in the first HIT solar cell sheet is greater than the mass fraction of indium in the second HIT solar cell sheet, the silicon nitride thin film is not present in the HIT solar cell for the following reasons: if the HIT solar cell does not have the silicon nitride film, the HIT solar cell is firstly placed in hydrofluoric acid solution and then placed in excessive concentrated nitric acid for acid leaching, hydrofluoric acid reacts with leached indium, so that the content of indium is reduced, and the mass fraction of indium is lower than that of indium which is not treated by the hydrofluoric acid solution and directly placed in the excessive concentrated nitric acid for acid leaching.
Further, the temperature for acid leaching is controlled between 70 and 120 ℃.
Furthermore, the mass fraction of hydrofluoric acid in the hydrofluoric acid solution is 10-25%.
Further, the second cell fragment is placed in a hydrofluoric acid solution for reaction for 3-5 min.
Further, the concentration of a series of indium standard solutions was 2, 5, 10, 20, 40 and 100ug/ml, respectively.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for determining the silicon nitride film in the HIT solar cell, whether the silicon nitride film exists in the HIT solar cell or not is determined, so that preparation can be made for pretreatment of the problem of recycling a large number of scrapped HIT solar cells in the future, the leaching rate and the recycling rate of indium are improved, and the method is suitable for determining whether the silicon nitride film exists in different HIT solar cell structures or not.
Drawings
Fig. 1 is a flowchart illustrating a method for determining a silicon nitride film in an HIT solar cell according to an embodiment of the present invention;
fig. 2 is a standard curve diagram of an indium standard solution provided by an embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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 of the 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.
The embodiment of the invention provides a method for determining a silicon nitride film in an HIT (heterojunction with intrinsic thin layer) solar cell, which comprises the following steps:
(1) selecting two HIT solar cells, namely a first HIT solar cell and a second HIT solar cell, weighing the first HIT solar cell and the second HIT solar cell respectively by using laboratory nonmetal special balance, wherein the mass of the first HIT solar cell and the mass of the second HIT solar cell are 5.263g and 2.8g respectively, and then crushing the first HIT solar cell and the second HIT solar cell to obtain first cell fragments and second cell fragments respectively;
(2) placing the first battery fragments in excessive concentrated nitric acid, carrying out acid leaching under the constant-temperature heating condition of 90 ℃ to leach out indium ions, filtering to obtain a first acid leaching solution, and measuring the volume of the first acid leaching solution to be 73 ml; the chemical reactions that occur during the acid leaching process are:
In2O3+6H+＝2In3++3H2O，
2InO+6H+＝2In3++2H2O+H2↑，
SnO2+4H+＝Sn4++2H2↑；
(3) placing the second battery fragment in a hydrofluoric acid solution with the mass fraction of 15% for reacting for 5min, wherein the main reaction equation is as follows: si3N4+HF+9H2O＝3H2SiO3↓+4NH4F; washing with deionized water, air drying, placing in excessive concentrated nitric acid, performing acid leaching at constant temperature of 90 deg.C to leach indium ions, filtering to obtain second acid leaching solution, and measuring the volume of the second acid leaching solution to be 79 ml;
(4) preparing a series of indium standard solutions with different concentrations, wherein the concentration of the indium standard solutions is 2, 5, 10, 20, 40 and 100ug/ml, and then measuring and drawing a standard curve of the absorbance of the indium standard solutions at a wavelength of 230nm and the indium concentration by using a spectrophotometer;
the regression equation of the standard curve is that Y is 0.0025X +2.0863,
wherein: y is absorbance, X is the concentration of indium ions in the solution, and the unit is ug/ml;
(5) measuring the absorbances of the first acid leaching solution and the second acid leaching solution at the wavelength of 230nm by using a spectrophotometer to be 2.461 and 2.432 respectively, and then calculating according to the standard curve to obtain the concentration of the indium ions in the first acid leaching solution to be 149.9ug/ml and the concentration of the indium ions in the second acid leaching solution to be 138.3ug/ml respectively;
(6) the calculation formula of the mass fraction of indium in the HIT solar cell sheet is as follows:
wherein: w is the mass fraction of indium in the HIT solar cell slice, C0M is the measured concentration of indium ions in the pickle liquor0The mass of the HIT solar cell is shown, and V is the volume of the pickle liquor;
(7) the mass fraction of indium in the first HIT solar cell piece is 0.21% calculated according to 5.263g of the mass of the first HIT solar cell piece, 73ml of the first acid leaching solution and 149.9ug/ml of the concentration of indium ions in the first acid leaching solution, and is shown in Table 1;
(8) the mass fraction of indium in the second HIT solar cell piece is 0.39% calculated according to the mass of the second HIT solar cell piece, the volume of the second acid immersion liquid is 79ml, and the concentration of indium ions in the second acid immersion liquid is 138.3ug/ml, and is shown in Table 1;
(9) and if the mass fraction of indium in the first HIT solar cell is smaller than that of indium in the second HIT solar cell, the silicon nitride film exists in the HIT solar cell.
TABLE 1
As can be seen from table 1, the HIT solar cell is first placed in the hydrofluoric acid solution to react, the hydrofluoric acid removes the silicon nitride film covering the TCO layer, the indium tin oxide in the TCO layer is exposed, and then placed in the excess concentrated nitric acid to perform acid leaching, so that the concentrated nitric acid can sufficiently react with the indium tin oxide, the mass fraction of the leached indium is higher than that of the indium which is not treated by the hydrofluoric acid solution and directly placed in the excess concentrated nitric acid to perform acid leaching, and the mass fraction of the indium in the first HIT solar cell piece is smaller than that of the indium in the second HIT solar cell piece, so that the HIT solar cell has the silicon nitride film. According to the invention, the recovery rate of the metal indium in the HIT solar cell is improved by determining whether the silicon nitride film exists in the HIT solar cell.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A method for determining a silicon nitride film in an HIT solar cell is characterized by comprising the following steps:
selecting two HIT solar cells, namely a first HIT solar cell and a second HIT solar cell, weighing and crushing the two HIT solar cells respectively to obtain a first cell fragment and a second cell fragment;
placing the first battery fragments in excessive concentrated nitric acid for acid leaching and filtering to obtain a first acid leaching solution, and measuring the volume of the first acid leaching solution;
placing the second battery fragments into a hydrofluoric acid solution for reaction, cleaning, air-drying, placing into excessive concentrated nitric acid for acid leaching, filtering to obtain a second acid leaching solution, and measuring the volume of the second acid leaching solution;
preparing a series of indium standard solutions with different concentrations, and then measuring and drawing a standard curve of the absorbance and the indium concentration by using a spectrophotometer;
respectively measuring the absorbance of the first acid leaching solution and the second acid leaching solution by using a spectrophotometer, and respectively calculating the concentration of indium ions in the first acid leaching solution and the concentration of indium ions in the second acid leaching solution according to the standard curve;
calculating the mass fraction of indium in the first HIT solar cell piece according to the mass of the first HIT solar cell piece, the volume of the first acid leaching solution and the concentration of indium ions in the first acid leaching solution;
calculating the mass fraction of indium in the second HIT solar cell piece according to the mass of the second HIT solar cell piece, the volume of the second acid immersion liquid and the concentration of indium ions in the second acid immersion liquid;
and judging the silicon nitride film in the HIT solar cell according to the magnitude relation between the mass fraction of the indium in the first HIT solar cell and the mass fraction of the indium in the second HIT solar cell.
2. The method for determining the silicon nitride film in the HIT solar cell according to claim 1, wherein the specific method for determining the silicon nitride film in the HIT solar cell according to the magnitude relationship between the mass fraction of indium in the first HIT solar cell and the mass fraction of indium in the second HIT solar cell comprises: when the mass fraction of indium in the first HIT solar cell piece is smaller than that of indium in the second HIT solar cell piece, a silicon nitride film exists in the HIT solar cell; when the mass fraction of indium in the first HIT solar cell slice is larger than that of indium in the second HIT solar cell slice, the silicon nitride film is not present in the HIT solar cell.
3. The method of claim 1, wherein the method comprises the following steps: the temperature for acid leaching is controlled between 70 and 120 ℃.
4. The method of claim 1, wherein the method comprises the following steps: the mass fraction of hydrofluoric acid in the hydrofluoric acid solution is 10-25%.
5. The method of claim 1, wherein the method comprises the following steps: and placing the second battery fragment in a hydrofluoric acid solution for reaction for 3-5 min.
6. The method of claim 1, wherein the method comprises the following steps: the concentrations of a series of indium standard solutions were 2, 5, 10, 20, 40 and 100ug/ml, respectively.
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| CN115117184A (en) * | 2022-06-28 | 2022-09-27 | 河海大学 | Method for determining structure of heterojunction solar cell to be recovered |
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| CN110016566A (en) * | 2019-05-17 | 2019-07-16 | 河海大学常州校区 | A method of recycling indium in discarded photovoltaic module |
| CN110273069A (en) * | 2019-07-23 | 2019-09-24 | 河海大学常州校区 | A kind of HIT solar cell recycling preprocess method |
| CN110306070A (en) * | 2019-07-31 | 2019-10-08 | 河海大学常州校区 | A kind of extracting process of indium |
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| CN103107212A (en) * | 2013-02-01 | 2013-05-15 | 中国科学院上海微系统与信息技术研究所 | Heterojunction solar battery with electroplate electrodes and preparation method |
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| CN110016566A (en) * | 2019-05-17 | 2019-07-16 | 河海大学常州校区 | A method of recycling indium in discarded photovoltaic module |
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| CN115117184B (en) * | 2022-06-28 | 2024-04-30 | 河海大学 | Method for determining heterojunction solar cell structure to be recovered |
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