Single-layer liquid crystal reflective liquid crystal color display material and its preparation method
By employing a single-layer liquid crystal reflective liquid crystal color display material preparation method and utilizing photolithography and micro-area filling techniques, the high cost problem of reflective liquid crystal display technology in the field of color display has been solved, achieving efficient RGB independent display and bistable display effects.
Patent Information
- Application Number
- CN202411316817.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2025-12-02
- Estimated Expiration
- 2044-09-20
AI Technical Summary
Existing reflective liquid crystal display technology suffers from high costs and the need for polarizers in the field of color display, which limits its application.
A method for preparing single-layer liquid crystal reflective liquid crystal color display materials was adopted. By combining photolithography and micro-area filling techniques with high-precision photolithography and high-throughput printing techniques, RGB pixels were prepared to achieve single-layer micro-pixel color reflective display.
It achieves ultra-high reflectivity, independent display of red, green and blue colors, and bistable display controllable by electric field, reducing costs and improving display effect.
Smart Images

Figure CN118981130B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of liquid crystal display technology, specifically relating to single-layer liquid crystal reflective liquid crystal color display materials and their preparation methods. Background Technology
[0002] Bistable liquid crystal display (BLCD) technology, a type of reflective liquid crystal display, boasts significant advantages such as full-color flexible display, high reflective brightness, high contrast, and low power consumption. However, its high cost limits its application in the color display field. Existing display technologies achieve color display through three-layer grayscale stacking, which requires substantial costs and addresses issues such as polarizers. Summary of the Invention
[0003] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: a method for preparing a single-layer liquid crystal reflective liquid crystal color display material, comprising the following steps:
[0004] Step 1: Spin-coat the photoresist onto the TFT conductive glass, then dry it to remove the solvent from the photoresist, and then polymerize it under ultraviolet light with the help of a mask to obtain TFT substrate I containing photolithographic walls.
[0005] Step 2: Develop TFT substrate I for a period of time, and then transfer it to the rinsing solution to remove the solvent, to obtain TFT substrate II with a pixel photolithography wall with uniform and highly regular morphology. The three adjacent pixels are called red pixel, green pixel and blue pixel, respectively.
[0006] Step 3: Mix 1-30 parts by weight of chiral agent, 70-98 parts by weight of organic solvent, 3-30 parts by weight of polymer and 0-2 parts by weight of photoinitiator, and stir evenly to obtain mixture 1. Take a portion of mixture 1 and spin coat it onto TFT substrate II under a spin coater. Then polymerize it under ultraviolet light to form a polymer-loaded chiral agent film A on TFT substrate II, and obtain TFT substrate III with a pixel photolithography wall with uniform and highly regular morphology and a first layer of polymer-loaded chiral agent film.
[0007] Step 4: Under the etching machine, the excess polymer-loaded chiral agent film A in the red and green pixels of TFT substrate Ⅲ is etched away to obtain TFT substrate Ⅳ with a pixel photolithography wall with uniform and highly regular morphology and only the blue pixels contain the polymer-loaded chiral agent film A.
[0008] Step 5: Take a portion of mixture 1 and spin coat it onto TFT substrate IV using a spin coater. Then, use ultraviolet light to irradiate and polymerize it to form a thin film B with a high molecular weight loaded with a chiral agent on TFT substrate IV. Use an etching machine to remove the excess thin film B in the red pixels to obtain a TFT substrate V with a pixel photolithography wall with uniform and highly regular morphology and red pixels without thin films A and B, green pixels containing thin film B, and blue pixels containing thin films A and B.
[0009] Step 6: Mix 2-30 parts by weight of chiral agent, 5-15 parts by weight of UV polymerizable monomer, 0.5-2 parts by weight of photoinitiator, and 70-95 parts by weight of phase-phase liquid crystal to obtain a red-reflective parent liquid crystal mixture 2. Roll the parent liquid crystal mixture 2 between a PET substrate with an ITO conductive surface and a TFT substrate V. After diffusion for a period of time, irradiate with ultraviolet light for a period of time to obtain a single-layer liquid crystal reflective liquid crystal color display material.
[0010] As a preferred embodiment of the above technical solution, the height of the photolithography wall in step 2 is 1-3 μm, the width is 1-15 μm, and the area of a single photolithography wall is 100 μm. 2 -10000μm 2 .
[0011] As a preferred embodiment of the above technical solution, the chiral agent comprises any one or more of the following compounds:
[0012]
[0013]
[0014]
[0015] As a preferred embodiment of the above technical solution, the organic solvent is one or more of N,N-dimethylformamide, dimethyl sulfoxide, methanol, ethanol, isopropanol, dichloromethane, tetrahydrofuran, ethyl acetate, acetonitrile, toluene, phenol, and anisole; the photoinitiator is one or more of (2,4,6-trimethylbenzoyl)diphenylphosphine oxide, bis(1-(2,4-difluorophenyl)-3-pyrrolidone)dicenoctane, 2-isopropylthioxanthone, methyl o-benzoylbenzoate, or ethyl 2,4,6-trimethylbenzoylphenylphosphonate; and the polymer is one or more of polyvinylpyrrolidone, polyvinyl alcohol, ribomeric polysaccharide, polylactic acid, polycaprolactone, polymethyl methacrylate, and dipentaerythritol hexaacrylate.
[0016] As a preferred embodiment of the above technical solution, the thickness of the polymer-loaded chiral agent film A in step 3 is 25-400 nm.
[0017] As a preferred embodiment of the above technical solution, the ultraviolet polymerizable monomer is one or more of the following: isobornyl methacrylate, butyl acrylate, 1,6-hexanediol acrylate, 1,4-butanediol acrylate, phenyl acrylate, pentaerythritol tetrakis(3-mercaptopropionic acid) ester, cyclohexyl acrylate, and hydroxypropyl methacrylate.
[0018] As a preferred embodiment of the above technical solution, step 1 involves placing 0.3-1 ml / cm at 25-45°C. 2 Photoresist is dropped onto TFT conductive glass and spin-coated for 5-120 seconds at 500-1000 rpm. Then, it is pre-baked at 90-180℃ for 1-10 minutes to remove the solvent. Finally, using a mask, it is coated with 365nm ultraviolet light at 25-45℃ with an intensity of 30-800 mw / cm². 2 Polymerization under light intensity for 3-60s yields TFT substrate I containing photolithographic walls;
[0019] Step 2: Develop the TFT substrate I containing the photolithography wall at 25-35℃ for 1-5 minutes, and then transfer it to the rinsing solution at 25-35℃ to remove the solvent, to obtain the TFT substrate II with a pixel photolithography wall with uniform and highly regular morphology. The three adjacent pixels are called red pixel, green pixel and blue pixel, respectively.
[0020] Step 3: At 25-45℃, mix 1-30 parts by weight of chiral agent, 70-98 parts by weight of organic solvent, 3-30 parts by weight of polymer, and 0-2 parts by weight of photoinitiator. After stirring evenly, obtain mixture 1. At 20-45℃, spin coat mixture 1 at a speed of 500-10000 r / min for 5-120 s. Then, at 20-45℃, apply 365 nm ultraviolet light with a light intensity of 30-800 mw / cm². 2 Polymerization under light intensity for 0-300s forms a polymer-loaded chiral agent film A on TFT substrate II, resulting in a TFT substrate III with a pixel photolithography wall of uniform and highly regular morphology and a first layer of polymer-loaded chiral agent film.
[0021] Step 4: At 25-45℃, the TFT substrate Ⅲ is etched in an etching machine to remove the excess thin film A in the red and green pixels, resulting in a TFT substrate Ⅳ with a pixel photolithography wall with uniform and highly regular morphology and a TFT substrate Ⅳ containing only the blue pixels with a polymer-loaded chiral agent thin film A.
[0022] Step 5: Take a portion of mixture 1 and spin coat it onto TFT substrate IV at 500-10000 r / min for 5-120 s using a spin coater. Then, at 25-45℃, use 365 nm ultraviolet light with a light intensity of 30-800 mw / cm². 2 Polymerization under light intensity for 0-300s yields a polymer-loaded chiral agent film B with a thickness of 25-400nm. The excess film B in the red pixels is removed using an etching machine, resulting in a TFT substrate V with a highly uniform and orderly pixel lithography wall and red pixels containing no films A and B, green pixels containing film B, and blue pixels containing films A and B.
[0023] Step 6: At 25-45℃, 2-30 parts by weight of chiral agent, 5-15 parts by weight of UV polymerizable monomer, 0.5-2 parts by weight of photoinitiator, and 70-95 parts by weight of phase-phase liquid crystal are uniformly mixed to obtain a red-reflective parent liquid crystal mixture 2. The parent liquid crystal mixture 2 is rolled between a PET substrate with an ITO conductive surface and a TFT substrate V. After diffusion at 10-45℃ for 1-60 minutes, it is irradiated with ultraviolet light for 5-30 minutes to obtain a single-layer liquid crystal reflective liquid crystal color display material.
[0024] A single-layer liquid crystal reflective liquid crystal color display material was prepared using the above-described preparation method.
[0025] The beneficial effects of this invention are as follows: This invention utilizes nano-doping technology to improve the photoelectric properties of liquid crystals. Simultaneously, it employs diffusion control of initiators, chiral compounds, and ultraviolet absorbers, along with a polymer network to anchor the liquid crystal pitch, to develop a single-layer liquid crystal material with ultra-high reflectivity, independent red, green, and blue (RGB) display, and bistable display controllable by an electric field. It innovatively combines high-precision photolithography to fabricate micro-regions with high-throughput printing technology to create RGB pixels through a differential filling method within the micro-regions. Utilizing the lateral superposition of RGB pixels for reflective display, it revolutionarily achieves single-layer micro-pixel color reflective display technology, overcoming the cost and yield drawbacks of traditional RGB three-layer liquid crystal superposition systems. It also creates the simulation models and fundamental theories required for this technology, thus providing theoretical guidance for next-generation reflective display technology. Attached Figure Description
[0026] Figure 1 This is a schematic diagram of the structure of the single-layer liquid crystal reflective liquid crystal color display material of the present invention;
[0027] Figure 2 This is a schematic diagram of the preparation process of the single-layer liquid crystal reflective liquid crystal color display material of the present invention;
[0028] Figure 3Polarized microscope texture images of the single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 of this invention;
[0029] Figure 4 Transmittance curves of the single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 of this invention;
[0030] Figure 5 The reflection spectra of the single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 of this invention;
[0031] Figure 6 Images of the driving voltages of the single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 of this invention;
[0032] Figure 7 Contrast images of the single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 of this invention. Detailed Implementation
[0033] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0034] The photoresist selected in Examples 1-7 of this invention has the following characteristics: flash point 20-35℃, boiling point 90-180℃, saturated vapor pressure 1.16 / 25℃, density 0.1-5g / cm3, and explosion limit 1.1-7.0%.
[0035] The polymer mixture solutions used in Examples 1-7 of this invention are mixtures of organic polymers and chiral molecules or polymerizable monomers of organic polymers, photoinitiators, chiral molecules, and other materials, with a concentration of 0.1-5%. For example, PMMA, dichloromethane, and chiral molecules are mixed in a ratio of 3:1:400, and then spin-coated to obtain a polymer-loaded film. The photoresist used in Examples 1-7 of this invention is a negative photoresist, which can rapidly polymerize under ultraviolet light irradiation and remains stable after polymerization.
[0036] Example 1
[0037] Step 1: At 20-35℃, RFJ-220-60 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at a speed of 800 r / min to obtain TFT substrate I containing photolithographic walls. Then, a mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer, and the light intensity is 400mW / cm². 2Polymerize under ultraviolet light for 3 seconds. Then, the TFT substrate after mask polymerization is placed in dichloromethane for development. After immersion in dichloromethane for 5 minutes, it is removed and placed in a special rinsing solution matching RFJ-220-60 photoresist to wash away excess solvent and unpolymerized photoresist. Then, the TFT substrate after development and rinsing is baked at 165°C for 5 minutes to obtain TFT substrate I with photolithographic walls (e.g., Figure 1 (As shown).
[0038] Step 2: At 20-35℃, a uniformly mixed solution of 1 part S5011, 3 parts polymethyl methacrylate, and 96 parts dichloromethane is dropped onto TFT substrate I containing the photolithographic wall, according to weight. Spin-coating is performed for 30 seconds at a speed of 10000 r / min, followed by drying at 60℃ for 10 minutes to obtain TFT substrate II containing a polymer-loaded chiral molecular film and the photolithographic wall. Figure 1 As shown.
[0039] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine, and etch away the polymethyl methacrylate-loaded chiral molecule S5011 film in the red and green pixel areas to obtain the TFT substrate III with a pixel photolithography wall and the first polymer-loaded chiral agent film with uniform and highly regular morphology.
[0040] Step 4: At 20-35℃, a mixed solution of ethanol, dichloromethane, polyvinylpyrrolidone and S5011 in a mass ratio of 100:20:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed for 30s at a speed of 10000r / min to obtain TFT substrate IV containing polyvinylpyrrolidone loaded with S5011 in the red and green pixels.
[0041] Step 5: At 20-35℃, place the TFT substrate Ⅳ from step 4 in the etching area of the etching machine, and etch away the thin film of PMMA loaded with chiral molecules in the red pixel area to obtain the TFT substrate Ⅴ for diffusion of RGB pixels.
[0042] Step 6: At 20-35℃, mix 90.3 parts by weight of liquid crystal SLC-1717, 2.2 parts by weight of chiral molecule S5011, 2 parts by weight of acryloyloxypropionic acid, 2 parts by weight of isobornyl methacrylate, 2.2 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, 0.9 parts by weight of phenyl acrylate, and 0.4 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0043] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, polymerize for 10 minutes under ultraviolet light irradiation at a wavelength of 365nm and an intensity of 6mW / cm2 to obtain a single-layer liquid crystal reflective liquid crystal color display material.
[0044] Example 2
[0045] Step 1: At 20-35℃, SU-82025 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 800 r / min. Then, it is pre-baked at 135℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer and polymerized under ultraviolet light with an intensity of 400mW / cm² for 3 seconds. The polymerized TFT substrate is then immersed in a special developer for development. After immersion in the developer for 5 minutes, it is removed and placed in a special rinsing solution compatible with SU-82025 to wash away excess solvent and unpolymerized photoresist. Finally, the TFT substrate after development and rinsing is baked at 135℃ for 5 minutes to obtain TFT substrate I with photolithographic walls.
[0046] Step 2: At 20-35℃, a uniformly mixed solution of 1 part R5011, 3 parts polyvinylpyrrolidone, and 110 parts dichloromethane is dropped onto TFT substrate I containing a photolithographic wall. Spin-coating is performed for 10 seconds at a speed of 8000 r / min, and then dried at 60℃ for 10 min to obtain TFT substrate II containing a polymer-loaded chiral molecular film and a photolithographic wall.
[0047] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, the polyvinylpyrrolidone-loaded R5011 film in the red pixel and green pixel areas is etched away to obtain the TFT substrate III with a pixel photolithography wall with uniform and highly regular morphology and the first layer of polymer-loaded chiral agent film.
[0048] Step 4: At 20-35℃, a mixed solution of ethanol, polyvinylpyrrolidone and R5011 in a mass ratio of 100:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed for 10s at a speed of 5000r / min to obtain TFT substrate IV containing polyvinylpyrrolidone loaded with R5011 in red and green pixels. The blue pixel film has the highest R5011 content.
[0049] Step 5: At 20-35℃, place the TFT substrate IV from step four in the etching area of the etching machine and etch away the polyvinylpyrrolidone-loaded chiral molecule film in the red pixel area to obtain the TFT substrate V for diffusion of RGB pixels.
[0050] Step 6: At 20-35℃, mix 90.3 parts by weight of liquid crystal SLC1717, 2.2 parts by weight of chiral molecule S5011, 2 parts by weight of acryloyloxypropionic acid, 2 parts by weight of isobornyl methacrylate, 2.2 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, 0.9 parts by weight of phenyl acrylate, and 0.4 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0051] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, expose it to ultraviolet light at a wavelength of 365nm and an intensity of 6mW / cm². 2 Polymerization under irradiation for 10 minutes yields a single-layer liquid crystal reflective liquid crystal color display material.
[0052] Example 3
[0053] Step 1: At 20-35℃, AZ4620 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 800 r / min. Then, it is pre-baked at 150℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer and polymerized under ultraviolet light with a wavelength of 365nm and an intensity of 400mW / cm² for 3 seconds. The polymerized TFT substrate is then immersed in a developer for 5 minutes, removed, and placed in a special rinsing solution compatible with AZ4620 to wash away excess solvent and unpolymerized photoresist. Finally, the TFT substrate after development and rinsing is baked at 150℃ for 5 minutes to obtain a TFT substrate with photolithographic walls (e.g., ...). Figure 1 (As shown).
[0054] Step 2: At 20-35℃, a uniform mixed solution of 1 part S811, 3 parts polymethyl methacrylate, and 90 parts dichloromethane is dropped onto TFT substrate I containing a photolithography wall according to the weight ratio. Spin-coating is performed for 30s at a speed of 10000r / min, and then dried at 60℃ for 10min to obtain TFT substrate II containing a polymer-loaded chiral molecular film and a photolithography wall.
[0055] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, the polymethyl methacrylate-loaded R5011 film in the red pixel area is etched away to obtain the TFT substrate III with a pixel photolithography wall and the first layer of polymer-loaded chiral agent film with uniform and highly regular morphology.
[0056] Step 4: At 20-35℃, a mixed solution of ethanol, dichloromethane, polyvinylpyrrolidone, polymethyl methacrylate, and S5011 in a mass ratio of 100:1.5:1.5:1 is dropped onto the TFT substrate from Step 3. Then, the solution is spin-coated for 30 seconds at a speed of 10000 r / min to obtain TFT substrate IV containing polymethyl methacrylate and polyvinylpyrrolidone loaded with S5011 in the red and green pixels. The blue pixel film has the highest S5011 content.
[0057] Step 5: At 20-35℃, place the TFT substrate IV from step four in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, etch away the thin film of polymethyl methacrylate and polyvinylpyrrolidone loaded with chiral molecules in the red pixel area to obtain the TFT substrate V for diffusion of RGB pixels.
[0058] Step 6: At 20-35℃, mix 75 parts by weight of liquid crystal E7, 25 parts by weight of chiral molecule S811, 5 parts by weight of butyl acrylate, 1 part by weight of 1,6-butanediol acrylate, 0.5 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, and 0.5 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0059] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, expose it to ultraviolet light at a wavelength of 365nm and an intensity of 6mW / cm². 2 Polymerization under irradiation for 10 minutes yields a single-layer liquid crystal reflective liquid crystal color display material.
[0060] Example 4
[0061] Step 1: At 20-35℃, AZ9260 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 1000 r / min. Then, it is pre-baked at 110℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer. The substrate is then exposed to ultraviolet light at a wavelength of 365nm and an intensity of 400mW / cm². 2 Polymerize under ultraviolet light for 3 seconds. Then, the TFT substrate after mask polymerization is placed in the developer for development. After soaking in the special developer for 5 minutes, it is taken out and placed in the special rinsing solution matched with AZ9260 to wash away excess solvent and unpolymerized photoresist. Then, the TFT substrate after development and rinsing is baked at 110°C for 5 minutes to obtain TFT substrate I with photolithography walls.
[0062] Step 2: At 20-35℃, a homogeneous mixture of 5 parts by weight of R6N, 25 parts by weight of RFJ-200-60 solution, and 60 parts by weight of dichloromethane is dropped onto TFT substrate I containing the photolithography wall. Spin-coating is performed for 30 seconds at a rotation speed of 10000 r / min, followed by drying at 60℃ for 10 minutes, and then exposure to ultraviolet light at a wavelength of 365 nm and an intensity of 400 mW / cm². 2 Polymerization under ultraviolet light for 120 s yields TFT substrate II containing a polymer-loaded chiral molecular film and a photolithographic wall.
[0063] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine, and etch away the polymethyl methacrylate-loaded R6N film in the red and green pixel areas to obtain the TFT substrate III with a pixel photolithography wall and the first layer of polymer-loaded chiral agent film with uniform and highly regular morphology.
[0064] Step 4: At 20-35℃, a mixed solution of ethanol, dichloromethane, polymethyl methacrylate, and R6N in a mass ratio of 60:10:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed at a speed of 10000 r / min for 30 s to obtain TFT substrate IV containing polymethyl methacrylate loaded with R6N in red and green pixels. The blue pixel film has the highest R6N content.
[0065] Step 5: At 20-35℃, place the TFT substrate IV from step four in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, etch away the thin film of polymethyl methacrylate loaded with chiral molecule R6N in the red pixel area to obtain the TFT substrate V for diffusion of RGB pixels.
[0066] Step 6: At 20-35℃, mix 96.6 parts by weight of liquid crystal E8, 3.4 parts by weight of chiral molecule R6N, 2 parts by weight of hydroxypropyl methacrylate, 6 parts by weight of 1,4-butanediol acrylate, 0.5 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, 5 parts by weight of pentaerythritol tetra-3-mercaptopropionate, and 0.5 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0067] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, polymerize for 10 minutes under ultraviolet light irradiation at a wavelength of 365nm and an intensity of 6mW / cm2 to obtain a single-layer liquid crystal reflective liquid crystal color display material.
[0068] Example 5
[0069] Step 1: At 20-35℃, AZ4330 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 1000 r / min. Then, it is pre-baked at 130℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer and polymerized under ultraviolet light with a wavelength of 365nm and an intensity of 400mW / cm² for 3 seconds. The polymerized TFT substrate is then immersed in a developer solution for development. After immersion in the dedicated developer solution for 5 minutes, it is removed and placed in a dedicated rinsing solution compatible with AZ4330 to wash away excess solvent and unpolymerized photoresist. Finally, the TFT substrate after development and rinsing is baked at 130℃ for 5 minutes to obtain TFT substrate I with photolithographic walls.
[0070] Step 2: At 20-35℃, a homogeneous mixture of 5 parts by weight of R6N, 25 parts by weight of RFJ-200-60 solution, and 60 parts by weight of dichloromethane is dropped onto TFT substrate I containing the photolithography wall. Spin-coating is performed for 30 seconds at a rotation speed of 10000 r / min, followed by drying at 60℃ for 10 minutes, and then exposure to ultraviolet light at a wavelength of 365 nm and an intensity of 400 mW / cm². 2 TFT substrate II containing a polymer-loaded chiral molecular film and a photolithographic wall was obtained by polymerization under ultraviolet light for 120 s.
[0071] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine, and etch away the polymethyl methacrylate-loaded R6N film in the red and green pixel areas to obtain the TFT substrate III with a pixel photolithography wall and the first layer of polymer-loaded chiral agent film with uniform and highly regular morphology.
[0072] Step 4: At 20-35℃, a mixed solution of ethanol, dichloromethane, polymethyl methacrylate, and R6N in a mass ratio of 60:10:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed at a speed of 10000 r / min for 30 s to obtain TFT substrate IV containing polymethyl methacrylate loaded with R6N in red and green pixels. The blue pixel film has the highest R6N content.
[0073] Step 5: At 20-35℃, place the TFT substrate IV from step four in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, etch away the thin film of polymethyl methacrylate loaded with chiral molecule R6N in the red pixel area to obtain the TFT substrate V for diffusion of RGB pixels.
[0074] Step 6: At 20-35℃, mix 96.6 parts by weight of liquid crystal SLC1717, 3.4 parts by weight of chiral molecule R6N, 2 parts by weight of hydroxypropyl methacrylate, 6 parts by weight of 1,4-butanediol acrylate, 0.5 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, 5 parts by weight of pentaerythritol tetra-3-mercaptopropionate, and 0.5 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0075] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another flexible PET film with an ITO coating with substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, the film is then subjected to ultraviolet light at a wavelength of 365nm and an intensity of 6mW / cm². 2 Polymerization under irradiation for 10 minutes yields a single-layer liquid crystal reflective liquid crystal color display material.
[0076] Example 6
[0077] Step 1: At 20-35℃, AZ1500 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 800 r / min. Then, it is pre-baked at 150℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer. The substrate is then exposed to ultraviolet light at a wavelength of 365nm and an intensity of 400mW / cm². 2 The TFT substrate was polymerized under ultraviolet light for 3 seconds. Then, the TFT substrate after mask polymerization was placed in the developer for development. After soaking in the special developer for 5 minutes, it was taken out and placed in the special rinsing solution matched with AZ1500 to wash away excess solvent and unpolymerized photoresist. Then, the TFT substrate after development and rinsing was baked at 150°C for 5 minutes to obtain TFT substrate I with photolithography walls.
[0078] Step 2: At 20-35℃, a uniform mixed solution of 3 parts R6N, 9 parts polylactic acid and 90 parts dichloromethane is dropped onto TFT substrate I containing a photolithography wall according to the weight ratio. Spin-coating is performed for 30s at a speed of 5000r / min, and then dried at 60℃ for 10min to obtain TFT substrate II containing a polymer-loaded chiral molecular film and a photolithography wall.
[0079] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine, and etch away the polymethyl methacrylate-loaded R6N film in the red and green pixel areas to obtain the TFT substrate III with a pixel photolithography wall and the first layer of polymer-loaded chiral agent film with uniform and highly regular morphology.
[0080] Step 4: At 20-35℃, a mixed solution of ethanol, dichloromethane, polylactic acid, and R6N in a mass ratio of 80:10:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed at a speed of 5000 r / min for 30 s to obtain TFT substrate IV containing polylactic acid-loaded R6N in red and green pixels, with the blue pixel film having the highest R6N content.
[0081] Step 5: At 20-35℃, place the TFT substrate Ⅳ from step 4 in the etching area of the etching machine, and under the conditions of etching energy of 50% and frequency of 300Hz, etch away the thin film of polylactic acid loaded chiral molecule R6N in the red pixel area to obtain the TFT substrate Ⅴ for diffusion of RGB pixels.
[0082] Step 6: At 20-35℃, mix 96.6 parts by weight of liquid crystal SLC1717, 3.4 parts by weight of chiral molecule R6N, 2 parts by weight of isobutyl methacrylate, 6 parts by weight of 1,6-pentanediol acrylate, 0.5 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, and 0.5 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0083] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, expose it to ultraviolet light at a wavelength of 365nm and an intensity of 6mW / cm². 2 Polymerization under irradiation for 10 minutes yields a single-layer liquid crystal reflective liquid crystal color display material.
[0084] Example 7
[0085] Step 1: At 20-35℃, AZ5214 photoresist is dropped onto the TFT substrate and spin-coated for 30 seconds at 850 r / min. Then, it is pre-baked at 145℃ for 10 minutes on a constant-temperature heating stage, and then cooled to room temperature to obtain a TFT substrate with a photolithographic layer. A mask with pixel size of 100μm × 100μm and pixel pitch of 3μm is placed on the TFT substrate containing the photolithographic layer. The substrate is then exposed to ultraviolet light at a wavelength of 365nm and an intensity of 400mW / cm². 2 The TFT substrate was polymerized under ultraviolet light for 5 seconds. Then, the TFT substrate after mask polymerization was placed in the developer for development. After soaking in the special developer for 5 minutes, it was taken out and placed in the special rinsing solution matched with AZ5214 to wash away excess solvent and unpolymerized photoresist. Then, the TFT substrate after development and rinsing was baked at 145°C for 5 minutes to obtain TFT substrate I with photolithography walls.
[0086] Step 2: At 20-35℃, a homogeneous mixture of 2 parts by weight of R5011, 50 parts by weight of RFJ-200-60 solution, and 350 parts by weight of dichloromethane is dropped onto TFT substrate I containing the photolithography wall. Spin-coating is performed for 30 seconds at a rotation speed of 10000 r / min, followed by drying at 60℃ for 10 minutes, and then exposure to ultraviolet light at a wavelength of 365 nm and an intensity of 400 mW / cm². 2 TFT substrate II containing a polymer-loaded chiral molecular film and a photolithographic wall was obtained by polymerization under ultraviolet light for 120 s.
[0087] Step 3: At 20-35℃, place the TFT substrate II containing the polymer-loaded chiral molecular film and photolithography wall in the etching area of the etching machine. Under the conditions of etching energy of 50% and frequency of 300Hz, the polymethyl methacrylate-loaded R5011 film in the red pixel area is etched away to obtain the TFT substrate III with a pixel photolithography wall and the first layer of polymer-loaded chiral agent film with uniform and highly regular morphology.
[0088] Step 4: At 20-35℃, a mixed solution of ethanol, anisole, polymethyl methacrylate, and R5011 in a mass ratio of 60:10:3:1 is dropped onto TFT substrate III from step 3. Then, spin-coating is performed at a speed of 10000 r / min for 30s to obtain TFT substrate IV containing polymethyl methacrylate loaded with R5011 in red and green pixels. The blue pixel film has the highest R5011 content.
[0089] Step 5: At 20-35℃, place the TFT substrate from step 4 in the etching area of the etching machine, and etch away the polymethyl methacrylate film loaded with chiral molecules R5011 in the red pixel area to obtain TFT substrate V for diffusion of RGB pixels.
[0090] Step 6: At 20-35℃, mix 96.6 parts by weight of liquid crystal SLC1717, 8 parts by weight of chiral molecule R6N, 2 parts by weight of hydroxypropyl methacrylate, 6 parts by weight of 1,4-butanediol acrylate, 0.5 parts by weight of 1,4-bis[4-(6-acryloyloxyhexyloxy)benzoyloxy]-2-methylbenzene, 5 parts by weight of pentaerythritol tetra-3-mercaptopropionate, and 0.5 parts by weight of benzoyl dimethyl ether in an ultrasonic bath for 4 hours, and then stir for 6 hours under a magnetic stirrer to obtain a uniformly mixed red parent liquid crystal.
[0091] Step 7: Drop red parent liquid crystal onto the TFT substrate V from step 5. Then, align another PET flexible film with an ITO coating with the TFT substrate V from step 5 and perform encapsulation. After diffusion for 5 minutes, polymerize for 10 minutes under ultraviolet light irradiation at a wavelength of 365nm and an intensity of 6mW / cm2 to obtain a single-layer liquid crystal reflective liquid crystal color display material.
[0092] The single-layer liquid crystal reflective liquid crystal color display materials prepared in Examples 1-7 were subjected to performance tests, and the test results are shown in the appendix of the instruction manual. Figure 3-7 and the table below.
[0093]
[0094]
[0095] It is worth mentioning that the technical features of the rotary coating machine, etching machine, etc. involved in this patent application should be regarded as prior art. The specific structure, working principle, and possible control methods and spatial arrangement of these technical features can be adopted using conventional choices in the field, and should not be regarded as the inventive point of this patent. This patent will not be further elaborated in detail.
[0096] The preferred embodiments of the present invention have been described in detail above. It should be understood that those skilled in the art can make many modifications and variations based on the concept of the present invention without creative effort. Therefore, all technical solutions that can be obtained by those skilled in the art based on the concept of the present invention through logical analysis, reasoning or limited experimentation on the basis of the prior art should be within the scope of protection defined by the claims.
Claims
1. A method for preparing a single-layer liquid crystal reflective liquid crystal color display material, characterized in that, Includes the following steps: Step 1: Spin-coat the photoresist onto the TFT conductive glass, then dry it to remove the solvent from the photoresist, and then polymerize it under ultraviolet light with the help of a mask to obtain TFT substrate I containing photolithographic walls. Step 2: Develop TFT substrate I for a period of time, and then transfer it to the rinsing solution to remove the solvent, to obtain TFT substrate II with a pixel photolithography wall with uniform and highly regular morphology. The three adjacent pixels are called red pixel, green pixel and blue pixel, respectively. Step 3: Mix 1-30 parts by weight of chiral agent, 70-98 parts by weight of organic solvent, 3-30 parts by weight of polymer and 0-2 parts by weight of photoinitiator, and stir evenly to obtain mixture 1. Take a portion of mixture 1 and spin coat it onto TFT substrate II under a spin coater. Then, polymerize it under ultraviolet light to form a polymer-loaded chiral agent film A on TFT substrate II, and obtain TFT substrate III with a pixel photolithography wall with uniform and highly regular morphology and a first layer of polymer-loaded chiral agent film. Step 4: Under the etching machine, the excess polymer-loaded chiral agent film A in the red and green pixels of TFT substrate Ⅲ is etched away to obtain TFT substrate Ⅳ with a pixel photolithography wall with uniform and highly regular morphology and only the blue pixels contain the polymer-loaded chiral agent film A. Step 5: Take a portion of mixture 1 and spin coat it onto TFT substrate IV using a spin coater. Then, use ultraviolet light to irradiate and polymerize it to form a thin film B with a high molecular weight loaded with a chiral agent on TFT substrate IV. Use an etching machine to remove the excess thin film B in the red pixels to obtain a TFT substrate V with a pixel photolithography wall with uniform and highly regular morphology and red pixels without thin films A and B, green pixels containing thin film B, and blue pixels containing thin films A and B. Step 6: Mix 2-30 parts by weight of chiral agent, 5-15 parts by weight of UV polymerizable monomer, 0.5-2 parts by weight of photoinitiator, and 70-95 parts by weight of phase-phase liquid crystal to obtain a red-reflective parent liquid crystal mixture 2. Roll the parent liquid crystal mixture 2 between a PET substrate with an ITO conductive surface and a TFT substrate V. After diffusion for a period of time, irradiate with ultraviolet light for a period of time to obtain a single-layer liquid crystal reflective liquid crystal color display material.
2. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to claim 1, characterized in that, The height of the photolithography wall in step 2 is 1-3 μm, the width is 1-15 μm, and the area of a single photolithography wall is 100 μm. 2 -10000μm 2 .
3. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to claim 1, characterized in that, The chiral agent includes any one or more of the following compounds:
4. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to claim 1, characterized in that, The organic solvent is one or more of N,N-dimethylformamide, dimethyl sulfoxide, methanol, ethanol, isopropanol, dichloromethane, tetrahydrofuran, ethyl acetate, acetonitrile, toluene, phenol, and anisole; the photoinitiator is one or more of (2,4,6-trimethylbenzoyl)diphenylphosphine oxide, bis(1-(2,4-difluorophenyl)-3-pyrrolidone)dicenoctane, 2-isopropylthioxanthone, methyl o-benzoylbenzoate, or ethyl 2,4,6-trimethylbenzoylphenylphosphonate; the polymer is one or more of polyvinylpyrrolidone, polyvinyl alcohol, riboglycolic acid, polylactic acid, polycaprolactone, polymethyl methacrylate, and dipentaerythritol hexaacrylate.
5. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to claim 1, characterized in that, The thickness of the polymer-loaded chiral agent film A in step 3 is 25-400 nm.
6. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to claim 1, characterized in that, The UV-polymerizable monomer is one or more of the following: isobornyl methacrylate, butyl acrylate, 1,6-hexanediol acrylate, 1,4-butanediol acrylate, phenyl acrylate, pentaerythritol tetrakis(3-mercaptopropionic acid) ester, cyclohexyl acrylate, and hydroxypropyl methacrylate.
7. The method for preparing a single-layer liquid crystal reflective liquid crystal color display material according to any one of claims 1-6, characterized in that, Step 1: At 25-45℃, add 0.3-1 ml / cm 2 Photoresist is dropped onto TFT conductive glass and spin-coated for 5-120 seconds at 500-1000 rpm. Then, it is pre-baked at 90-180℃ for 1-10 minutes to remove the solvent. Finally, using a mask, it is coated with 365nm ultraviolet light at 25-45℃ with an intensity of 30-800 mw / cm². 2 Polymerization under light intensity for 3-60s yields TFT substrate I containing photolithographic walls; Step 2: Develop the TFT substrate I containing the photolithography wall at 25-35℃ for 1-5 minutes, and then transfer it to the rinsing solution at 25-35℃ to remove the solvent, to obtain the TFT substrate II with a pixel photolithography wall with uniform and highly regular morphology. The three adjacent pixels are called red pixel, green pixel and blue pixel, respectively. Step 3: At 25-45℃, mix 1-30 parts by weight of chiral agent, 70-98 parts by weight of organic solvent, 3-30 parts by weight of polymer, and 0-2 parts by weight of photoinitiator. After stirring evenly, obtain mixture 1. At 20-45℃, spin coat mixture 1 at a speed of 500-10000 r / min for 5-120 s. Then, at 20-45℃, apply 365 nm ultraviolet light with a light intensity of 30-800 mw / cm². 2 Polymerization under light intensity for 0-300s forms a polymer-loaded chiral agent film A on TFT substrate II, resulting in a TFT substrate III with a pixel photolithography wall of uniform and highly regular morphology and a first layer of polymer-loaded chiral agent film. Step 4: At 25-45℃, the TFT substrate Ⅲ is etched in an etching machine to remove the excess thin film A in the red and green pixels, resulting in a TFT substrate Ⅳ with a pixel photolithography wall with uniform and highly regular morphology and a TFT substrate Ⅳ containing only the blue pixels with a polymer-loaded chiral agent thin film A. Step 5: Take a portion of mixture 1 and spin coat it onto TFT substrate IV at 500-10000 r / min for 5-120 s using a spin coater. Then, at 25-45℃, use 365 nm ultraviolet light with a light intensity of 30-800 mw / cm². 2 Polymerize under light intensity for 0-300s to obtain a thin film B with a thickness of 25-400nm loaded with a chiral agent. Use an etching machine to remove excess thin film B in the red pixels to obtain a pixel lithography wall with uniform and highly regular morphology and a TFT substrate V with no thin films A and B in the red pixels, thin film B in the green pixels, and thin films A and B in the blue pixels. Step 6: At 25-45℃, 2-30 parts by weight of chiral agent, 5-15 parts by weight of UV polymerizable monomer, 0.5-2 parts by weight of photoinitiator, and 70-95 parts by weight of phase-phase liquid crystal are uniformly mixed to obtain a red-reflective parent liquid crystal mixture 2. The parent liquid crystal mixture 2 is rolled between a PET substrate with an ITO conductive surface and a TFT substrate V. After diffusion at 10-45℃ for 1-60 minutes, it is irradiated with ultraviolet light for 5-30 minutes to obtain a single-layer liquid crystal reflective liquid crystal color display material.
8. A single-layer liquid crystal reflective liquid crystal color display material, characterized in that, It is prepared using the preparation method described in any one of claims 1-7.
Citation Information
Patent Citations
Single-layer liquid crystal reflection type liquid crystal color display module and preparation method thereof
CN120652701A