Preparation process of bottom-coated perovskite layer
By adopting the lower coating preparation process and equipment during the perovskite battery preparation process, the cleanliness and cost problems caused by the flip of the TCO base film surface are solved, and the manufacturing efficiency and product quality of the perovskite battery are improved.
Patent Information
- Application Number
- CN202411661810.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-03-04
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
During the preparation of perovskite batteries, the TCO base film surface needs to be frequently flipped, resulting in high cleanliness requirements in the production environment, increased equipment costs and production line complexity, and dust falling on the substrate will lead to perovskite film formation defects.
The lower coating preparation process is used to identify the status valid value of the FTO glass film surface. If the preset requirements are met, the subsequent process will be carried out, otherwise the pre-order process will be processed in cycles. The lower coating preparation equipment is used to prepare the lower interface layer, perovskite layer and upper interface layer, and the film surface is always facing downward to reduce the impact of dust and reduce the cost of the equipment.
Effectively prevent dust from affecting the quality of perovskite film layer, reduce equipment costs and production line complexity, and improve the manufacturing efficiency and product quality of perovskite batteries.
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Figure CN119562738A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of photovoltaic cell preparation, and in particular to a process for preparing a bottom-coated perovskite layer. Background Art
[0002] During the preparation process of perovskite cells, due to the different preparation processes involved, the perovskite cell base needs to be flipped back and forth according to different processes to meet the needs of different processes.
[0003] In the conventional perovskite cell preparation process, the TCO glass substrate needs to go through the processes of cleaning, hole transport layer preparation, P1 laser scribing, lower interface layer preparation, perovskite layer preparation, upper interface layer preparation, vapor deposition of C60 layer, SnO2 layer preparation, P2 laser scribing, back electrode layer preparation, P3 laser scribing, edge cleaning, testing and sorting, and then laminated into components. Among them, the cleaning process, lower interface layer preparation, perovskite layer preparation, upper interface layer preparation and other processes require the TCO substrate film to face up according to process requirements, and the vapor deposition of C60 layer requires the TCO substrate film to face down according to equipment requirements. In other processes, the TCO substrate film surface can be facing up, down or vertical, which is determined by the equipment requirements.
[0004] In the prior art, the three processes of preparing the lower interface layer, the perovskite layer, and the upper interface layer require the TCO substrate to be prepared upwards, which places very high demands on the cleanliness of the production environment. During the preparation process, if dust falls on the substrate, it will cause defects in the perovskite film formation, affecting the appearance and performance of the device.
[0005] In addition, since the TCO substrate has its membrane facing upward, downward, or vertical in different processes, it is necessary to flip the TCO substrate back and forth, which not only increases the complexity of the production line and the equipment cost, but also is not conducive to the smoothness of the substrate positioning process. Summary of the invention
[0006] The purpose of the present invention is to provide a process for preparing a lower film-coated perovskite layer. Combined with the "lower film-coating (transfer, coating, printing) preparation equipment" technology, a process for preparing a perovskite layer by lower film-coating is proposed to reduce the impact of dust on the quality of the perovskite film layer. In addition, the lower film-coating preparation of the perovskite layer can also reduce equipment costs, reduce the complexity of the production line, reduce the difficulty of manufacturing perovskite batteries, and promote the development of industrialization.
[0007] The purpose of the present invention can be achieved by the following technical solutions:
[0008] A process for preparing a bottom-coated perovskite layer comprises the following steps:
[0009] Before preparing the lower interface layer, the perovskite layer, and the upper interface layer, obtaining the effective value of the state of the FTO glass film surface;
[0010] Identify the effective value of the state of the FTO glass film surface. If the effective value of the state of the FTO glass film surface meets the preset requirements, proceed to the subsequent process of preparing the lower coating perovskite layer.
[0011] Subsequent processes include evaporation of C60 layer, preparation of SnO2 layer, P2 scribing, preparation of back electrode layer, P3 scribing and edge cleaning;
[0012] If the effective value of the state of the FTO glass film surface does not meet the preset requirements, the previous process of preparing the lower coating perovskite layer is cyclically processed;
[0013] The pre-process includes glass cleaning, hole transport layer preparation, and P1 scribing and Mark dot scribing;
[0014] Among them, the preparation of the lower interface layer, the preparation of the perovskite layer, and the preparation of the upper interface layer are all prepared using lower film coating preparation equipment.
[0015] As a further solution of the present invention: the FTO glass film faces downward during the preparation of the lower interface layer, the perovskite layer, and the upper interface layer.
[0016] As a further solution of the present invention: the process of obtaining the effective value of the state of the FTO glass film surface is:
[0017] Capturing an image of the FTO glass film surface to obtain an FTO surface image, preprocessing the FTO surface image, and extracting features from the preprocessed FTO surface image to obtain an FTO surface feature image;
[0018] And obtaining the encapsulation layer base value of the FTO surface feature image and the smoothness characterization value of the FTO surface feature image according to the FTO surface feature image;
[0019] The encapsulation layer base value of the FTO surface feature image is recorded as Ftf;
[0020] The smoothness characterization value of the FTO surface feature image is recorded as Ftg;
[0021] By the formula Ft i = e -θ×(Hy+Hg) The effective value Ft i of the state of the FTO glass film surface is calculated, where θ is the preset proportional coefficient.
[0022] As a further solution of the present invention: comparing the effective value Ft i of the state of the FTO glass film surface with the effective value threshold Fty of the state of the FTO glass film surface;
[0023] If the effective value Ft i of the state of the FTO glass film surface is less than or equal to the effective value threshold Fty of the state of the FTO glass film surface, it indicates that the state of the FTO glass film surface is abnormal, and an abnormal state signal of the FTO glass film surface is obtained;
[0024] Based on the abnormal signal of the FTO glass film surface state, the pre-process cycle treatment of the lower coating perovskite layer preparation is carried out;
[0025] If the effective value Ft i of the state of the FTO glass film surface is greater than the effective value threshold of the state of the FTO glass film surface, it indicates that the state of the FTO glass film surface is normal, and a signal indicating that the state of the FTO glass film surface is normal is obtained;
[0026] Based on the abnormal signal of the FTO glass film surface state, the subsequent process of preparing the lower coating perovskite layer is carried out.
[0027] As a further solution of the present invention: the process of obtaining the base value of the encapsulation layer of the FTO surface feature image is as follows:
[0028] Perform image segmentation on the FTO surface feature image to obtain a number of FTO surface image sub-units of the same area;
[0029] Obtaining the number of foreign body encapsulation FTO surface image subunits, calculating the ratio of the number of foreign body encapsulation FTO surface image subunits to the total number of FTO surface image subunits, and obtaining the foreign body encapsulation unit number ratio;
[0030] The ratio of the foreign body scribe line area to the area of the foreign body encapsulation FTO surface image sub-unit is calculated to obtain the foreign body encapsulation FTO unit surface ratio;
[0031] The encapsulation layer base value of the FTO surface feature image is obtained by multiplying the foreign matter encapsulation unit number ratio corresponding to the FTO surface image subunit and the foreign matter encapsulation unit surface ratio corresponding to the FTO surface image subunit.
[0032] As a further solution of the present invention: the process of obtaining the area of the foreign body line in the foreign body encapsulation FTO surface image subunit is:
[0033] If there are less than three foreign objects in the foreign object encapsulation FTO surface image subunit, a minimum circumscribed circle around the edge of each foreign object is made to completely place the foreign object in the circle, and the areas of all circumscribed circles are summed to obtain the foreign object line area in the foreign object encapsulation FTO surface image subunit;
[0034] If there are more than or equal to three foreign objects in the foreign object encapsulation FTO surface image subunit, all foreign objects are connected end to end in a clockwise direction to obtain a foreign object connection circle, and the area of the foreign object connection circle is obtained, that is, the foreign object marking area in the foreign object encapsulation FTO surface image subunit is obtained.
[0035] As a further solution of the present invention: the acquisition process of the foreign body encapsulation FTO surface image subunit is:
[0036] Obtain the number of FTO surface image subunits corresponding to the foreign matter encapsulated in the inner hole transport layer of each FTO surface image subunit, and record the FTO surface image subunit as a foreign matter encapsulated FTO surface image subunit;
[0037] Among them, there are foreign matters in the hole transport layer, including uncleaned dust and oil on the surface of the FTO surface image subunit and bubbles in the hole transport layer.
[0038] As a further solution of the present invention: the process of obtaining the smoothness characterization value of the FTO surface feature image is as follows:
[0039] Use deep learning frameworks to build convolutional neural network models;
[0040] Collect a large number of FTO surface images with different smoothness, and annotate the actual smoothness value corresponding to each FTO surface image to form a data set, and use the data set to train the model;
[0041] In the training process, the error between the predicted smoothness value and the true value is minimized by continuously adjusting the parameters of the model;
[0042] Apply the trained model to each FTO surface image subunit to obtain the smoothness value corresponding to each FTO surface image subunit;
[0043] The smoothness values corresponding to all FTO surface image sub-units are summed and averaged to obtain the total smoothness value of the FTO surface;
[0044] The smoothness deviation value of the FTO surface image subunit is calculated by ratio with the total smoothness value of the FTO surface to obtain the smoothness characterization value of the FTO surface feature image.
[0045] As a further solution of the present invention: the process of obtaining the smoothness deviation value of the FTO surface image subunit is:
[0046] Identify the smoothness values corresponding to all FTO surface image sub-units;
[0047] Sum the smoothness values of all image subunits on the positive FTO surface to obtain the positive smoothness value;
[0048] The smoothness values of all image subunits located on the reverse FTO surface are summed to obtain the reverse smoothness value;
[0049] The absolute value of the difference between the forward smoothness value and the reverse smoothness value is obtained to obtain a smoothness deviation value, and the smoothness deviation value is calculated by ratio calculation with the smoothness threshold of the FTO surface image subunit to obtain the smoothness deviation value of the FTO surface image subunit.
[0050] As a further solution of the present invention: the process of distinguishing the FTO surface image subunit is:
[0051] If the smoothness value corresponding to the FTO surface image subunit is greater than or equal to the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a positive FTO surface image subunit;
[0052] If the smoothness value corresponding to the FTO surface image subunit is less than the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a reverse FTO surface image subunit.
[0053] Beneficial effects of the present invention:
[0054] (1) In the preparation process of the perovskite battery of the present invention, if dust particles fall into the effective area, it will cause coating defects and affect the appearance and quality of the product. In this patent, since the perovskite layer is prepared using the bottom coating process, the film surface is located at the bottom, which can effectively prevent the impact of falling dust;
[0055] (2) The present invention uses the "lower coating (transfer, coating, printing) preparation equipment" technology in the three processes of lower interface layer preparation, perovskite layer preparation, and upper interface layer preparation. Compared with conventional slit coating technology or vacuum evaporation technology, its equipment cost can be reduced to less than 1 / 3 of the original, greatly reducing the equipment cost;
[0056] (3) The three processes of preparing the lower interface layer, the perovskite layer, and the upper interface layer of the present invention use the "lower coating (transfer, coating, printing) preparation equipment" technology. During the process, the TCO substrate film faces downward. After the preparation is completed, the subsequent C60 vapor deposition process is directly carried out. The TCO substrate does not need to be turned over, which is conducive to the automated design of the production line. Further, the subsequent SnO2 layer preparation, P2 laser scribing, back electrode layer preparation, P3 laser scribing, edge cleaning, testing and sorting processes can be designed with the TCO substrate film facing downward, further reducing the difficulty of automated production lines.
[0057] (4) Before preparing the lower interface layer, the perovskite layer, and the upper interface layer, the present invention monitors the state of the FTO substrate film surface, collects images of the FTO glass film surface through a camera or a scanner, and obtains a characteristic image of the FTO surface. The characteristic image of the FTO surface is then processed to obtain a smoothness characterization value of the FTO surface characteristic image and a base value of the encapsulation layer of the FTO surface characteristic image. Based on the smoothness characterization value of the FTO surface characteristic image and the base value of the encapsulation layer of the FTO surface characteristic image, an effective value of the state of the FTO glass film surface is obtained. Through the effective value of the state of the FTO glass film surface, online monitoring of whether the FTO substrate film surface meets the requirements for the preparation of the lower interface layer, the perovskite layer, and the upper interface layer is completed, thereby effectively ensuring the yield rate of the preparation of the lower coated perovskite layer. BRIEF DESCRIPTION OF THE DRAWINGS
[0058] The present invention will be further described below in conjunction with the accompanying drawings.
[0059] Figure 1 It is a flow chart of a process for preparing a bottom-coated perovskite layer according to an embodiment of the present invention;
[0060] Figure 2 This is a flow chart of FTO glass film surface state identification in a bottom-coated perovskite layer preparation process according to an embodiment of the present invention. DETAILED DESCRIPTION
[0061] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0062] Example 1
[0063] See also Figure 1 As shown, the present invention is a process for preparing a bottom-coated perovskite layer, comprising the following steps:
[0064] S1, glass cleaning;
[0065] Among them, the substrate is a 450mm×650mm×3.2mm FTO glass, which is cleaned by an automatic cleaning machine, washed with a cleaning machine, washed with pure water, washed with a wind knife, and treated with UV / O3, and the FTO glass film is facing upward during the cleaning process;
[0066] S2, preparation of hole transport layer;
[0067] Among them, a 20nm NiOx layer was prepared using a magnetron sputtering device, and the FTO glass film was facing upward during the preparation process;
[0068] S3, P1 marking and Mark dot marking;
[0069] Use a laser with a wavelength of 1064nm to draw 61 equally spaced lines along the long side of the FTO layer. The distance between any two adjacent lines is 7mm. The 60 areas distinguished are the number of sub-cells.
[0070] Use a laser with a wavelength of 1064nm to draw two lines along the two short sides to define the effective area. The two lines along the short sides are 12mm away from the short sides.
[0071] Use a laser with a wavelength of 1064nm to scratch MaK points outside the effective area for positioning in the P2 and P3 processes;
[0072] During the preparation process, the FTO glass film faces upward;
[0073] S4, preparation of lower interface layer;
[0074] A layer of ethanol solution of SAMs material was prepared using "bottom coating (transfer, coating, printing) preparation equipment, and annealed at 100 ° C × 5 min. During the preparation process, the FTO glass film faced downwards.
[0075] Among them, the annealing equipment is upper radiation heating;
[0076] S5, preparation of perovskite layer;
[0077] The perovskite material is composed of one or more materials with a general chemical formula of ABX3 type crystal structure, wherein A is CH3NH3, C4H9NH3, NH2=CHNH2 or Cs, B is Pb or Sn, and X is Cl, Br or I;
[0078] A mixed solvent of DMF and DMSO with a volume ratio of 4:1 is used to dissolve the perovskite material into a precursor, and the perovskite precursor is coated on the substrate using a "lower coating (transfer, coating, printing) preparation device". After coating, the substrate is transferred to a VCD device for vacuum treatment to remove the solvent, and then annealed. The annealing equipment is irradiated from above and the annealing conditions are 120°C×15min. During the preparation process, the FTO glass film faces downward;
[0079] S6, preparation of upper interface layer;
[0080] Among them, a layer of isopropanol solution of PEA I material is prepared by using a bottom coating (transfer, coating, printing) preparation equipment, and annealing treatment is performed. The annealing equipment is irradiated from above and the annealing conditions are 100°C×2min. During the preparation process, the FTO glass film faces downward;
[0081] S7, evaporation of C60 layer;
[0082] Use a line source evaporation device to evaporate 15nm of C60, and the FTO glass film faces downward during the preparation process;
[0083] S8, SnO2 layer preparation;
[0084] Among them, 20nm SnO2 was deposited using RPD equipment, and the FTO glass film faced downward during the preparation process.
[0085] S9, P2 line drawing;
[0086] Use a laser with a wavelength of 532nm to scribe on the left side of the P1 line after positioning at the Mark point to form the P2 line;
[0087] The spacing between P1 and P2 scribe lines is 100 μm, and P2 scribes the SnO2 layer, C60 layer, upper interface layer, perovskite layer, lower interface layer and hole transport layer. During the preparation process, the FTO glass film faces downward;
[0088] S10, preparation of back electrode layer;
[0089] Magnetron sputtering was used to sequentially prepare 30nmn ITO, 100nm Cu, and 50nm ITO materials as the back electrode layer. The back electrode layer was filled into P2 and contacted with the FTO layer. During the preparation process, the FTO glass film faced downwards.
[0090] S11, P3 line drawing;
[0091] Use a laser with a wavelength of 532nm to scribe on the left side of the P2 line after positioning at the Mark point to form the P3 line;
[0092] The distance between P2 and P3 scribe lines is 100 μm;
[0093] P3 cuts the back electrode layer, SnO2 layer, C60 layer, upper interface layer, perovskite layer, lower interface layer and hole transport layer. At this time, each sub-cell forms a series structure, and the FTO glass film faces downward during the preparation process;
[0094] S12, clear edge;
[0095] Use laser edge removal equipment to remove all film layers within 11mm from the edge of the glass substrate to ensure the insulation effect of the component. During the preparation process, the FTO glass film faces downward;
[0096] S13. Use an ultrasonic welding gun to weld the tinned copper tape to the two outermost sub-cells as a lead to lead out the current. The width of the tinned copper tape is 2 mm. Lay the encapsulation film and the back glass to laminate them into a perovskite component.
[0097] Example 2
[0098] In S4, when preparing a lower interface layer on the FTO glass film surface using a lower coating (transfer, coating, printing) preparation device, an effective value of the state of the FTO glass film surface is obtained;
[0099] Among them, the process of obtaining the effective value of the state of the FTO glass film surface is:
[0100] Capturing an image of the FTO glass film surface by a camera or a scanner to obtain an FTO surface image, preprocessing the FTO surface image, and extracting features from the preprocessed FTO surface image to obtain an FTO surface feature image;
[0101] Preprocessing: Preprocessing is the first step in image processing. Its goal is to improve image quality, remove noise, enhance useful information in the image, and lay a good foundation for subsequent feature extraction and classification recognition; perform denoising operations on printed product images to eliminate noise in the printed product images. The denoising operation uses filters and other methods to make the image smoother and clearer; in order to highlight key information in the image, such as texture and color, image enhancement is required. Image enhancement operations are performed on printed product images through methods such as histogram equalization and contrast stretching; and in order to simplify the image processing process, grayscale images are converted into binary images. By setting appropriate thresholds, the pixels in the printed product images are divided into foreground and background categories, which is convenient for subsequent feature extraction;
[0102] Feature extraction: Feature extraction is the core step of image processing. It aims to extract key features that can represent the quality of printed products from preprocessed images. The texture of printed products is an important basis for judging their quality. By calculating the grayscale co-occurrence matrix and Fourier transform of the image, the texture features of printed products, such as texture direction and texture period, can be extracted. Color is also an important manifestation of the quality of printed products. The color features of printed products, such as color distribution and color saturation, can be extracted through methods such as color histogram and color moment. For defects in printed products, such as holes and stains, the shape features of the defects, such as area and perimeter, can be extracted through methods such as edge detection and morphological operations.
[0103] Performing image segmentation on the FTO surface feature image to obtain a number of FTO surface image sub-units of the same area;
[0104] Obtain the number of FTO surface image subunits corresponding to the foreign matter encapsulated in the inner hole transport layer of each FTO surface image subunit, and record the FTO surface image subunit as a foreign matter encapsulated FTO surface image subunit;
[0105] Among them, foreign matter in the hole transport layer includes uncleaned dust and oil on the surface of the FTO surface image subunit and bubbles in the hole transport layer;
[0106] Obtaining the number of foreign body encapsulation FTO surface image subunits, calculating the ratio of the number of foreign body encapsulation FTO surface image subunits to the total number of FTO surface image subunits, and obtaining the foreign body encapsulation unit number ratio;
[0107] The area of the foreign matter encapsulated FTO surface image subunit is calculated by dividing the area of the foreign matter encapsulated FTO surface image subunit, and the area of the foreign matter encapsulated FTO surface image subunit is calculated by ratio calculation to obtain the foreign matter encapsulated FTO unit surface ratio;
[0108] The foreign body encapsulation FTO unit surface ratios corresponding to all foreign body encapsulation FTO surface image sub-units are summed to obtain the foreign body encapsulation unit surface ratio;
[0109] Among them, the process of obtaining the foreign matter line area in the foreign matter encapsulation FTO surface image subunit is:
[0110] If there are less than three foreign objects in the foreign object encapsulation FTO surface image subunit, a minimum circumscribed circle around the edge of each foreign object is made to completely place the foreign object in the circle, and the areas of all circumscribed circles are summed to obtain the foreign object line area in the foreign object encapsulation FTO surface image subunit;
[0111] If there are more than or equal to three foreign objects in the foreign object encapsulation FTO surface image subunit, connect all foreign objects end to end in a clockwise direction to obtain a foreign object connection circle, and obtain the area of the foreign object connection circle, that is, the foreign object line area in the foreign object encapsulation FTO surface image subunit;
[0112] The encapsulation layer base value of the FTO surface feature image is obtained by multiplying the foreign matter encapsulation unit number ratio corresponding to the FTO surface image subunit and the foreign matter encapsulation unit surface ratio corresponding to the FTO surface image subunit;
[0113] Use deep learning frameworks to build convolutional neural network models;
[0114] Collect a large number of FTO surface images with different smoothness, and annotate the actual smoothness value corresponding to each FTO surface image to form a data set, and use the data set to train the model;
[0115] In the training process, the error between the predicted smoothness value and the true value is minimized by continuously adjusting the parameters of the model;
[0116] Apply the trained model to each FTO surface image subunit to obtain the smoothness value corresponding to each FTO surface image subunit;
[0117] Compare the smoothness value corresponding to the FTO surface image subunit with the smoothness threshold corresponding to the FTO surface image subunit;
[0118] If the smoothness value corresponding to the FTO surface image subunit is greater than or equal to the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a positive FTO surface image subunit;
[0119] If the smoothness value corresponding to the FTO surface image subunit is less than the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a reverse FTO surface image subunit;
[0120] The smoothness values of all the positive FTO surface image sub-units are summed to obtain the positive smoothness value;
[0121] Sum the smoothness values of all reverse FTO surface image sub-units to obtain the reverse smoothness value;
[0122] Obtaining the absolute value of the difference between the forward smoothness value and the reverse smoothness value to obtain a smoothness deviation value, performing ratio calculation on the smoothness deviation value and the smoothness threshold of the FTO surface image subunit to obtain a smoothness deviation value of the FTO surface image subunit;
[0123] The smoothness values corresponding to all FTO surface image sub-units are summed and averaged to obtain the total smoothness value of the FTO surface;
[0124] The smoothness deviation value of the FTO surface image subunit is calculated by ratio with the total smoothness value of the FTO surface to obtain the smoothness representation value of the FTO surface feature image;
[0125] The encapsulation layer base value of the FTO surface feature image is recorded as Ftf;
[0126] The smoothness characterization value of the FTO surface feature image is recorded as Ftg;
[0127] By the formula Ft i = e -θ×(Hy+Hg) The effective value Ft i of the state of the FTO glass film surface is calculated, where θ is the preset proportional coefficient;
[0128] See also Figure 2 , presetting the effective value threshold of the state of the FTO glass film surface as Fty, and comparing the effective value Ft i of the state of the FTO glass film surface with the effective value threshold Fty of the state of the FTO glass film surface;
[0129] If the effective value Ft i of the state of the FTO glass film surface is less than or equal to the effective value threshold Fty of the state of the FTO glass film surface, it means that the surface layer of the FTO glass film does not meet the preset requirements in terms of the hole transport layer or the smoothness, indicating that the state of the FTO glass film surface is abnormal, and an abnormal state signal of the FTO glass film surface is obtained;
[0130] Repeat steps S1-S3 on the FTO glass film surface based on the abnormal state signal of the FTO glass film surface until the effective state value Ft i of the FTO glass film surface is greater than the effective state value threshold of the FTO glass film surface;
[0131] If the effective value Ft i of the state of the FTO glass film surface is greater than the effective value threshold of the state of the FTO glass film surface, it means that the surface layer of the FTO glass film meets the preset requirements in terms of the hole transport layer or the smoothness, indicating that the state of the FTO glass film surface is normal, and a signal of the normal state of the FTO glass film surface is obtained;
[0132] Based on the normal signal of the FTO glass film surface state, enter S4 to prepare the interface layer under the FTO layer.
[0133] Comparative Example
[0134] W1, glass cleaning;
[0135] Among them, the substrate is a 450mm×650mm×3.2mm FTO glass, which is cleaned by an automatic cleaning machine, washed with a cleaning machine, washed with pure water, washed with a wind knife, and treated with UV / O3, and the FTO glass film is facing upward during the cleaning process;
[0136] W2, preparation of hole transport layer;
[0137] Among them, a magnetron sputtering device was used to prepare a 20nm NiOx layer, and the FTO glass film surface was facing upward during the preparation process;
[0138] W3, P1 line and Mark dot marking;
[0139] Use a laser with a wavelength of 1064nm to draw 61 equally spaced lines along the long side of the FTO layer. The distance between any two adjacent lines is 7mm. The 60 areas distinguished are the number of sub-cells.
[0140] Use a laser with a wavelength of 1064nm to draw two lines along the two short sides to define the effective area. The two lines along the short sides are 12mm away from the short sides.
[0141] Use a laser with a wavelength of 1064nm to scratch MaK points outside the effective area for positioning in the P2 and P3 processes;
[0142] The FTO glass film was facing upward during the preparation process.
[0143] W4, preparation of lower interface layer;
[0144] A layer of ethanol solution of SAMs material was prepared by slit coating and annealed at 100°C for 5 min. The FTO glass film was facing upward during the preparation process.
[0145] W5, perovskite layer preparation;
[0146] The perovskite material is composed of one or more materials with a general chemical formula of ABX3 type crystal structure, wherein A is CH3NH3, C4H9NH3, NH2=CHNH2 or Cs, B is Pb or Sn, and X is Cl, Br or I;
[0147] The perovskite material was dissolved into a precursor using a mixed solvent of DMF and DMSO in a volume ratio of 4:1. The perovskite precursor was coated on the substrate using slit coating, and vacuum treatment was performed to remove the solvent. The substrate was then annealed at 120°C for 15 min. The FTO glass film was facing upward during the preparation process.
[0148] W6, preparation of upper interface layer;
[0149] Among them, a layer of isopropanol solution of PEA I material was prepared by slit coating and annealed at 100°C × 2min. During the preparation process, the FTO glass film was facing upward.
[0150] W7, evaporation C60 layer;
[0151] Use a line source evaporation device to evaporate 15nm of C60, and the FTO glass film faces downward during the preparation process;
[0152] W8, SnO2 layer preparation;
[0153] Among them, 20nm SnO2 was deposited using RPD equipment, and the FTO glass film faced downward during the preparation process.
[0154] W9, P2 line drawing;
[0155] Use a laser with a wavelength of 532nm to scribe on the left side of the P1 line after positioning at the Mark point to form the P2 line;
[0156] The spacing between the P1 and P2 lines is 100 μm. P2 cuts through the SnO2 layer, C60 layer, upper interface layer, perovskite layer, lower interface layer and hole transport layer. The FTO glass film faces downward during the preparation process.
[0157] W10, preparation of back electrode layer;
[0158] Magnetron sputtering was used to sequentially prepare 30nmn ITO, 100nm Cu, and 50nm ITO materials as the back electrode layer. The back electrode layer was filled into P2 and contacted with the FTO layer. During the preparation process, the FTO glass film faced upwards.
[0159] W11, P3 line drawing;
[0160] Use a laser with a wavelength of 532nm to scribe on the left side of the P2 line after positioning at the Mark point to form the P3 line;
[0161] The distance between P2 and P3 scribe lines is 100 μm;
[0162] P3 cuts through the back electrode layer, SnO2 layer, C60 layer, upper interface layer, perovskite layer, lower interface layer and hole transport layer. At this time, each sub-cell forms a series structure, and the FTO glass film faces downward during the preparation process.
[0163] W12, clear edge;
[0164] Use laser edge removal equipment to remove all film layers within 11mm from the edge of the glass substrate to ensure the insulation effect of the component. During the preparation process, the FTO glass film faces downward.
[0165] W13. Use an ultrasonic welding gun to weld the tinned copper tape to the two outermost sub-cells as a lead to lead out the current. The width of the tinned copper tape is 2mm. Lay the encapsulation film and the back glass to laminate them into a perovskite component.
[0166] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.
Claims
1. A process for preparing a bottom-coated perovskite layer, characterized in that: The following steps are involved: Before preparing the lower interface layer, the perovskite layer, and the upper interface layer, obtaining the effective value of the state of the FTO glass film surface; Identify the effective value of the state of the FTO glass film surface. If the effective value of the state of the FTO glass film surface meets the preset requirements, proceed to the subsequent process of preparing the lower coating perovskite layer. Subsequent processes include evaporation of C60 layer, preparation of SnO2 layer, P2 scribing, preparation of back electrode layer, P3 scribing and edge cleaning; If the effective value of the state of the FTO glass film surface does not meet the preset requirements, the previous process of preparing the lower coating perovskite layer is cyclically processed; The pre-process includes glass cleaning, hole transport layer preparation, and P1 scribing and Mark dot scribing; Among them, the preparation of the lower interface layer, the preparation of the perovskite layer, and the preparation of the upper interface layer are all prepared using lower film coating preparation equipment.
2. A process for preparing a bottom-coated perovskite layer according to claim 1, characterized in that: The FTO glass film faces downward during the preparation of the lower interface layer, the perovskite layer, and the upper interface layer.
3. The process for preparing a bottom-coated perovskite layer according to claim 1, characterized in that: The process of obtaining the effective value of the state of the FTO glass film surface is as follows: Capturing an image of the FTO glass film surface to obtain an FTO surface image, preprocessing the FTO surface image, and extracting features from the preprocessed FTO surface image to obtain an FTO surface feature image; And obtaining the encapsulation layer base value of the FTO surface feature image and the smoothness characterization value of the FTO surface feature image according to the FTO surface feature image; The encapsulation layer base value of the FTO surface feature image is recorded as Ftf; The smoothness characterization value of the FTO surface feature image is recorded as Ftg; By the formula Fti = e -θ×(Hy+Hg) The effective value Fti of the state of the FTO glass film surface is calculated, where θ is the preset proportional coefficient.
4. A process for preparing a bottom-coated perovskite layer according to claim 3, characterized in that: Compare the effective value Fti of the state of the FTO glass film surface with the effective value threshold Fty of the state of the FTO glass film surface; If the effective value Ft i of the state of the FTO glass film surface is less than or equal to the effective value threshold Fty of the state of the FTO glass film surface, it indicates that the state of the FTO glass film surface is abnormal, and an abnormal state signal of the FTO glass film surface is obtained; Based on the abnormal signal of the FTO glass film surface state, the pre-process cycle treatment of the lower coating perovskite layer preparation is carried out; If the effective value Ft i of the state of the FTO glass film surface is greater than the effective value threshold of the state of the FTO glass film surface, it indicates that the state of the FTO glass film surface is normal, and a signal indicating that the state of the FTO glass film surface is normal is obtained; Based on the abnormal signal of the FTO glass film surface state, the subsequent process of preparing the lower coating perovskite layer is carried out.
5. A process for preparing a bottom-coated perovskite layer according to claim 4, characterized in that: The process of obtaining the base value of the encapsulation layer of the FTO surface feature image is as follows: Perform image segmentation on the FTO surface feature image to obtain a number of FTO surface image sub-units of the same area; Obtaining the number of foreign body encapsulation FTO surface image subunits, calculating the ratio of the number of foreign body encapsulation FTO surface image subunits to the total number of FTO surface image subunits, and obtaining the foreign body encapsulation unit number ratio; The ratio of the foreign body scribe line area to the area of the foreign body encapsulation FTO surface image sub-unit is calculated to obtain the foreign body encapsulation FTO unit surface ratio; The encapsulation layer base value of the FTO surface feature image is obtained by multiplying the foreign matter encapsulation unit number ratio corresponding to the FTO surface image subunit and the foreign matter encapsulation unit surface ratio corresponding to the FTO surface image subunit.
6. A process for preparing a bottom-coated perovskite layer according to claim 5, characterized in that: The process of obtaining the foreign matter scribe line area in the foreign matter encapsulation FTO surface image subunit is as follows: If there are less than three foreign objects in the foreign object encapsulation FTO surface image subunit, a minimum circumscribed circle around the edge of each foreign object is made to completely place the foreign object in the circle, and the areas of all circumscribed circles are summed to obtain the foreign object line area in the foreign object encapsulation FTO surface image subunit; If there are more than or equal to three foreign objects in the foreign object encapsulation FTO surface image subunit, all foreign objects are connected end to end in a clockwise direction to obtain a foreign object connection circle, and the area of the foreign object connection circle is obtained, that is, the foreign object marking area in the foreign object encapsulation FTO surface image subunit is obtained.
7. A process for preparing a bottom-coated perovskite layer according to claim 5, characterized in that: The acquisition process of the FTO surface image subunit of foreign body encapsulation is as follows: Obtain the number of FTO surface image subunits corresponding to the foreign matter encapsulated in the inner hole transport layer of each FTO surface image subunit, and record the FTO surface image subunit as a foreign matter encapsulated FTO surface image subunit; Among them, there are foreign matters in the hole transport layer, including uncleaned dust and oil on the surface of the FTO surface image subunit and bubbles in the hole transport layer.
8. A process for preparing a bottom-coated perovskite layer according to claim 4, characterized in that: The process of obtaining the smoothness characterization value of the FTO surface feature image is as follows: Use deep learning frameworks to build convolutional neural network models; Collect a large number of FTO surface images with different smoothness, and annotate the actual smoothness value corresponding to each FTO surface image to form a data set, and use the data set to train the model; In the training process, the error between the predicted smoothness value and the true value is minimized by continuously adjusting the parameters of the model; Apply the trained model to each FTO surface image subunit to obtain the smoothness value corresponding to each FTO surface image subunit; The smoothness values corresponding to all FTO surface image sub-units are summed and averaged to obtain the total smoothness value of the FTO surface; The smoothness deviation value of the FTO surface image subunit is calculated by ratio with the total smoothness value of the FTO surface to obtain the smoothness characterization value of the FTO surface feature image.
9. A process for preparing a bottom-coated perovskite layer according to claim 8, characterized in that: The process of obtaining the smoothness deviation value of the FTO surface image subunit is as follows: Identify the smoothness values corresponding to all FTO surface image sub-units; Sum the smoothness values of all image subunits on the positive FTO surface to obtain the positive smoothness value; The smoothness values of all image subunits located on the reverse FTO surface are summed to obtain the reverse smoothness value; The absolute value of the difference between the forward smoothness value and the reverse smoothness value is obtained to obtain a smoothness deviation value, and the smoothness deviation value is calculated by ratio calculation with the smoothness threshold of the FTO surface image subunit to obtain the smoothness deviation value of the FTO surface image subunit.
10. A process for preparing a bottom-coated perovskite layer according to claim 1, characterized in that: The process of distinguishing the FTO surface image subunits is as follows: If the smoothness value corresponding to the FTO surface image subunit is greater than or equal to the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a positive FTO surface image subunit; If the smoothness value corresponding to the FTO surface image subunit is less than the smoothness threshold corresponding to the FTO surface image subunit, the FTO surface image subunit is recorded as a reverse FTO surface image subunit.
Citation Information
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