CN110624789A - Method for preparing large-area film by inversion type sticking coating method - Google Patents
Method for preparing large-area film by inversion type sticking coating method Download PDFInfo
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- CN110624789A CN110624789A CN201910826215.1A CN201910826215A CN110624789A CN 110624789 A CN110624789 A CN 110624789A CN 201910826215 A CN201910826215 A CN 201910826215A CN 110624789 A CN110624789 A CN 110624789A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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Abstract
The invention relates to a method for preparing a large-area device by an inverted bonding method, which is suitable for preparing an electronic device, in particular to a large-area solar cell device, and belongs to the field of device preparation. The process mainly comprises three stages of adsorption, transmission and film forming of the precursor liquid. The precursor liquid adsorption mainly comprises the adsorption of the drum on the precursor liquid in a solution tank below the drum, so that the precursor liquid is adhered to the surface of the drum; the transfer refers to transferring the precursor liquid to the surface of the substrate above, and the surface of the substrate is acted by surface tension to transfer the precursor liquid on the roller to the surface of the substrate in a sticking way; finally, a film is formed by post-treatment processes such as photocuring or thermal annealing. Compared with the prior art of roll-to-roll, screen printing, spin coating and the like, the invention adopts an inverted substrate to adhere the solution, and the substrate and the liquid are adhered under the action of surface tension, thereby avoiding the defects of difficult solution amount control, uneven coating and the like caused by front contact.
Description
Technical Field
The invention belongs to the field of large-area device preparation, and relates to a method for preparing a large-area film by an inverted bonding method, which can be applied to the preparation of information electronics or photoelectronic devices, and is particularly suitable for preparing a large-area solar cell device system.
Background
With the rapid development of the electronic and photovoltaic industries, the fast, large-area and low-cost device fabrication becomes an urgent problem. The traditional preparation process mainly comprises spin coating, such as the photoetching process in the semiconductor industry, wherein photoresist is spin-coated on the surface of a silicon substrate with the thickness of 300 mm. The spin coating process produces a uniform film, but has the major disadvantages of not being able to operate continuously and wasting around 90% of the solution [ Energy environ. sci.,2015,7,2642 ].
With the development of technology, other solution deposition methods have received much attention, such as knife coating, slot-die extrusion coating, spray coating, ink-jet printing, and screen printing. Blade coating is the process of diffusing a precursor solution onto the surface of a substrate to form a wet film. The film thickness is generally controlled by several factors, including the concentration of the precursor solution, the distance between the substrate surface and the blade, and the speed of the substrate motion. Compared with spin coating, blade coating can be operated continuously, with less solution waste, but is not suitable for preparing ultra-thin films [ CN201510447759.9 ]. Slit extrusion coating is a method more similar to knife coating, where the precursor liquid can be better controlled in the slot die, but this method requires more ink to fill the cartridge, and is also not as applicable to the preparation of the ultra-thin coating as knife coating [ nat. The spraying process is to disperse small liquid drops on the surface of the substrate uniformly by a nozzle and then to carry out a post-treatment process. The methods for producing droplets in spray coating are classified into pneumatic spray coating (by a rapid air flow), ultrasonic spray coating (ultrasonic vibration) or electric spray coating (by electric repulsion). Spraying is greatly influenced by the process conditions, such as pneumatic spraying, and is influenced by factors such as air flow, jet distance, droplet size, nozzle size and the like [ CN207533459U ]. In an inkjet printing process, nozzles are used to disperse the precursor ink and control droplet size and trajectory. When a small nozzle is used and the distance between the nozzle and the substrate is short, the resolution is good. However, whether ink jet printing is suitable for mass production and large area production depends on the printing speed and the apparatus structure. The silk-screen printing operation is convenient, the cost is low, the application range is wide, but the printing precision is lower [ CN201310358425.5 ].
The dip-coating method is also a method for preparing a film in a large area and can be divided into two modes of manual coating and mechanical coating. The manual pulling operation is easy, but the manual pulling operation has strong influence of human factors, and the shaking caused by unstable operation easily causes the unevenness of the prepared film. The mechanical pulling speed is relatively stable, and the prepared film has better quality [ CN201610405835.4 ]. However, the film prepared by the pulling method is prepared by the combined action of the gravity and the surface tension of the solution. The problem that the large-area film is not uniform up and down is easy to be irradiated, and the like, and the large-area preparation application of the ultrathin film is difficult.
At present, electronic and optoelectronic devices have high preparation precision, and a more precise and rapid preparation process is needed to achieve the purpose of production.
Disclosure of Invention
Aiming at the problem of poor quality of the existing prepared high-precision large-area film, the invention provides a method for preparing the large-area film by an inverted bonding coating method so as to prepare a device, and the method is particularly suitable for organic and inorganic film photovoltaic and electronic devices with higher development speed at present.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing a large-area film by an inversion type sticking coating method comprises the following specific steps:
(1) adsorption of precursor liquid by drum
The front surface of the substrate faces downwards, the roller is positioned below the substrate, the solution tank is positioned below the roller, and the surface of the roller is in contact with the precursor solution in the solution tank; the roller rotates to adsorb the precursor liquid in the solution tank and adsorb the precursor liquid to the surface of the roller; the baffle plates are arranged on two sides of the notch of the solution tank, so that the precursor liquid dripped in the rotation process of the roller falls back to the solution tank to play a role in recovery.
The substrate is a rigid substrate or a flexible substrate; the rigid substrate is quartz, glass, ITO glass, FTO glass, metal, silicon wafer, silicon oxide or alloy and the like; the flexible substrate is PEN, PDMS, polytetrafluoroethylene material, colloid material, resin material or fiber material.
The precursor solution is a polymer solution, a nanoparticle solution or a micromolecular solution; the concentration of the precursor solution is 0.01M-10M.
The solvent used in the precursor solution comprises water, aromatic hydrocarbon solvent, aliphatic hydrocarbon solvent, alicyclic hydrocarbon solvent, halogenated hydrocarbon solvent, alcohol solvent, ether solvent, ester solvent, ketone solvent, glycol derivative solvent and other solvents; aromatic hydrocarbon solvents include benzene, toluene, xylene, etc.; aliphatic hydrocarbon solvents include pentane, hexane, octane, and the like; alicyclic hydrocarbon solvents include cyclohexane, cyclohexanone, toluene cyclohexanone, and the like; halogenated hydrocarbon solvents include chlorobenzene, dichlorobenzene, dichloromethane, and the like; the alcohol solvent comprises methanol, ethanol, isopropanol, etc.; ether solvents include diethyl ether, propylene oxide, and the like; the ester solvent comprises methyl acetate, ethyl acetate, propyl acetate, etc.; the ketone solvent comprises acetone, methyl butanone, methyl isobutyl ketone, etc.; the glycol derivative solvent comprises ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, etc.; other solvents include acetonitrile, pyridine, phenol, thionyl chloride, dimethyl sulfoxide, and the like.
In the polymer solution, the polymer is one or more than two of polymethyl methacrylate, polystyrene, polyurethane, polyethylene, polypropylene, polyvinyl chloride, polybutylene, polyvinyl alcohol, polystyrene-butadiene copolymer, poly-styrene-polyoxyethylene copolymer, ABS resin, MEH-PPV, BEH-PPV, BuEH-PPV or PPP.
The material of the roller is metal, silicon material, polytetrafluoroethylene material, resin material, glass material, plastic or mixed material, wherein the mixed material comprises gum material and other mixed material loaded on the surface of the metal; the edge linear velocity of the roller is 8-80000mm/min, the diameter of the roller is 10-10000mm, the movement speed of the substrate is 2-100000mm/min, and the rotation speed of the roller is 1-5000 r/min.
(2) Precursor liquid transfer between a platen and a substrate
The precursor liquid on the roller is coated on the front surface of the substrate in a spin mode through rotation of the roller, and the surface of the substrate is attached and transferred to the surface of the substrate through the action of surface tension to form a liquid film.
(3) Post-treatment film formation
And carrying out post-treatment process on the liquid film formed on the front surface of the substrate to form a film so as to obtain the required film.
The post-treatment process comprises heat treatment, photocuring treatment, ultrasonic treatment, anti-solvent treatment, drying, roasting, ironing and the like, and different post-treatment processes are selected according to the types of the precursor liquid.
When the large-area device needs to be cut in the preparation process, a groove structure corresponding to the cutting can be carved on the surface of the roller so as to divide the film once in the sticking and coating process.
The rollers are arranged side by side, and are selected according to specific conditions.
The invention has the beneficial effects that: the method of the invention can form film quickly with low cost, the number of the rollers can be increased, and the latter roller can correct and supplement the former step of film forming; the method can be operated continuously and is suitable for preparing large-area optoelectronic devices; can be directly connected with a post-treatment process to form a continuous production line. Compared with the prior art of roll-to-roll, screen printing, spin coating and the like, the invention adopts an inverted substrate to adhere the solution, and the substrate and the liquid are adhered under the action of surface tension, thereby avoiding the defects of difficult solution amount control, uneven coating and the like caused by front contact.
Drawings
FIG. 1 is a schematic diagram of the inverted pasting process of a rigid substrate to produce a large area film.
FIG. 2 is a schematic view of a solution tank using baffles.
Fig. 3 is a schematic view of a cutting cylinder.
FIG. 4 is a schematic view of a rigid substrate multi-roll continuous film formation.
FIG. 5 is a schematic representation of the efficiency of a large area perovskite device for producing perovskite films by the inverted bond coating method of the present invention.
FIG. 6 is a schematic representation of the preparation of multilayer (TiO) by the inverted bond coating method of the present invention2(CL)、TiO2(ML), perovskite, hole transport layer, carbon electrode) are largeSchematic of the efficiency of an area perovskite device.
FIG. 7 is a PMMA film prepared by the inverted bonding method of the present invention.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
A method for preparing a large-area film by an inversion-type adhesion method comprises a precursor liquid adsorption stage, a precursor liquid transfer stage and a film forming stage, and is shown in figure 1. The substrate shown in fig. 1 is a rigid substrate, and the precursor liquid is transported to the surface of the substrate by the rotation of the drum after the drum adsorbs the solution in the solution tank below and adsorbs the precursor liquid to the surface of the drum. The surface of the substrate is acted upon by surface tension to adhesively transfer the liquid on the roller to the surface of the substrate. In the whole process, the front surface of the substrate faces downwards, and the precursor liquid is completely adsorbed by surface tension to overcome the action of gravity. During the rotation of the rotating shaft, if the liquid drops from the roller, baffles may be added to the two ends of the solution tank to return the precursor to the solution tank, as shown in fig. 2. Finally, the formed liquid film is subjected to a post-treatment process to form a film. The post-treatment process may be a heat treatment, a photo-curing treatment, or the like. Most of the large-area device manufacturing processes require a cutting process, and the inverted bonding method of the present invention can directly etch a groove structure on the surface of the roller, as shown in fig. 3, and the groove structure can divide the film once during the coating process.
To prevent the precursor solution from not completely covering the rigid substrate surface, the rollers should be a corrosion resistant, compliant material compatible with the precursor solution. If the substrate surface is not completely smoothed at one time, multiple roll coating may be performed, as shown in FIG. 4, which is not possible with other methods in which the front surface of the substrate faces upward.
The method of the invention is also applicable to flexible substrate surfaces, except that the method can be used for sticking and coating on rigid substrate surfaces. When the surface of the flexible substrate is coated, the roller can be made of rigid material or flexible material.
Example 1, application in the preparation of perovskite solar cell devices:
firstly, preparing a substrate: on FTO substrateThe surface is spin-coated with 50 mu L of dense layer TiO2Organic sol, spin coating at 5000rpm for 60s, and high temperature sintering. 75 μ L of porous layer slurry was dropped on TiO2And spin-coating the dense layer at 5000rpm for 30s, and sintering at high temperature to obtain the substrate.
The perovskite layer is prepared by an inverted adhesion coating method, the prepared perovskite solution is placed in a solution tank, and the formula of the solution is a small molecular solution with the concentration of 1.1M. The formula is as follows: FAI (1M), CsI (1.5M), PbI2(1.1M), MABr (0.2M) and PbBr2(0.2M) was dissolved in DMF: DMSO ═ 4:1(v: v). The perovskite solution is pasted on the FTO/TiO by the inversion pasting method2(CL)/TiO2(ML) the surface of the substrate, the movement speed of the substrate being 1000mm/min, the edge line speed being 1000mm/min, the diameter of the roller being 20mm, the rotation speed of the roller being 50 revolutions/min. The post-treatment process comprises annealing at 125 ℃ for 40min on a hot plate, dripping 75 mu L of prepared Spiro-MeOTAD chlorobenzene solution on a perovskite layer thin film, spin-coating at 3500rpm for 30s, and preparing the perovskite solar cell by taking C as a back electrode, wherein the efficiency is shown in figure 5. Sequentially adding TiO2(CL)、TiO2(ML), a perovskite layer, a hole transport layer (Spiro-MeOTAD chlorobenzene solution) and a precursor solution of a carbon back electrode, and the efficiency of the perovskite solar cell with multiple layers prepared by the inverted bonding method is shown in FIG. 6.
Example 2 application in polymer film formation:
the method is applied to a polymer material capable of being spin-coated to form a film, wherein the polymer material can be polymethyl methacrylate (PMMA), Polystyrene (PS), Polyurethane (PU), Polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polybutylene, polyvinyl alcohol (PVA), polystyrene-butadiene copolymer (SBS), poly (p-styrene-poly (ethylene oxide) copolymer (PPVPE), ABS resin, mr-NIL6000 photo-curing adhesive and the like.
After a solution of a 0.5M xylene organic solvent is directly prepared from a PMMA polymer, a film is prepared by adopting the inverted sticking method, the edge linear velocity is 1000mm/min, the diameter of a roller is 200mm, the movement speed of a substrate is 1000mm/min, and the rotation speed of the roller is 50 revolutions/min. The finally prepared film has the thickness of 200nm and uniform and smooth surface, as shown in FIG. 7.
Claims (10)
1. A method for preparing a large-area film by an inversion type sticking coating method is characterized by comprising the following specific steps:
(1) adsorption of precursor liquid by drum
The front surface of the substrate faces downwards, the roller is positioned below the substrate, the solution tank is positioned below the roller, and the surface of the roller is in contact with the precursor solution in the solution tank; the roller rotates to adsorb the precursor liquid in the solution tank and adsorb the precursor liquid to the surface of the roller;
(2) precursor liquid transfer between a platen and a substrate
The precursor liquid on the roller is spin-coated on the front surface of the substrate through the rotation of the roller, and the surface of the substrate is adhered and transferred to the surface of the substrate under the action of surface tension to form a liquid film;
(3) post-treatment film formation
And carrying out post-treatment process on the liquid film formed on the front surface of the substrate to form a film so as to obtain the required film.
2. The method of claim 1, wherein the step of preparing the large area film by the inverted bonding method,
the substrate is a rigid substrate or a flexible substrate; the rigid substrate is quartz, glass, ITO glass, FTO glass, metal, silicon wafer, silicon oxide or alloy; the flexible substrate is PEN, PDMS, polytetrafluoroethylene material, colloid material, resin material or fiber material;
the material of the roller is metal, silicon material, polytetrafluoroethylene material, resin material, glass material, plastic or mixed material, wherein the mixed material comprises gum material and other mixed material loaded on the surface of the metal;
the edge linear velocity of the roller is 8-80000mm/min, the diameter of the roller is 10-10000mm, the movement speed of the substrate is 2-100000mm/min, and the rotation speed of the roller is 1-5000 r/min;
the precursor solution is a polymer solution, a nanoparticle solution or a micromolecular solution; the concentration of the precursor solution is 0.01M-10M;
the solvent used in the precursor solution comprises water, aromatic hydrocarbon solvent, aliphatic hydrocarbon solvent, alicyclic hydrocarbon solvent, halogenated hydrocarbon solvent, alcohol solvent, ether solvent, ester solvent, ketone solvent, glycol derivative solvent and other solvents; aromatic hydrocarbon solvents include benzene, toluene and xylene; aliphatic hydrocarbon solvents include pentane, hexane and octane; alicyclic hydrocarbon solvents include cyclohexane, cyclohexanone and toluene cyclohexanone; halogenated hydrocarbon solvents include chlorobenzene, dichlorobenzene, and dichloromethane; alcohol solvents include methanol, ethanol and isopropanol; ether solvents include diethyl ether and propylene oxide; the ester solvent comprises methyl acetate, ethyl acetate and propyl acetate; ketone solvents include acetone, methyl butanone and methyl isobutyl ketone; the glycol derivative solvent comprises ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and ethylene glycol monobutyl ether; other solvents include acetonitrile, pyridine, phenol, thionyl chloride and dimethylsulfoxide;
in the polymer solution, the polymer is one or more than two of polymethyl methacrylate, polystyrene, polyurethane, polyethylene, polypropylene, polyvinyl chloride, polybutylene, polyvinyl alcohol, polystyrene-butadiene copolymer, poly-styrene-polyoxyethylene copolymer, ABS resin, MEH-PPV, BEH-PPV, BuEH-PPV or PPP.
3. The method of claim 1 or 2, wherein the post-treatment process comprises heat treatment, photo-curing, ultrasonic treatment, anti-solvent treatment, drying, baking and ironing, and the post-treatment process is selected according to the type of the precursor solution.
4. The method of claim 1 or 2, wherein the rollers are arranged side by side in one or more rows, as the case may be.
5. The method of claim 3, wherein the rollers are arranged side by side in one or more rows, as the case may be.
6. The method for preparing a large-area thin film by the inverted bonding method according to claim 1, 2 or 5, wherein when the large-area device preparation process requires cutting, a groove structure corresponding to the cutting is engraved on the surface of the roller to divide the thin film once during the bonding process.
7. The method of claim 3, wherein when the large-area device is required to be cut in the manufacturing process, the groove structure corresponding to the cutting is engraved on the surface of the roller to divide the film once in the pasting process.
8. The method of claim 4, wherein when the large-area device is required to be cut in the manufacturing process, the groove structure corresponding to the cutting is first engraved on the surface of the roller to divide the film once in the pasting process.
9. The method for preparing a large-area film by the inverted bonding method according to claim 1, 2, 5,7 or 8, wherein the two sides of the notch of the solution tank are provided with baffle plates, so that the precursor liquid dripped during the rotation of the roller falls back into the solution tank.
10. The method of claim 3, wherein the solution tank is provided with baffles on both sides of the opening to allow the precursor solution dripping during the rotation of the drum to fall back into the solution tank.
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| CN201910826215.1A CN110624789A (en) | 2019-09-03 | 2019-09-03 | Method for preparing large-area film by inversion type sticking coating method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112691558A (en) * | 2020-12-02 | 2021-04-23 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Preparation method and system of membrane material |
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Application publication date: 20191231 |