Pouring and laminating method for flat plate with large area, high optical quality and uniform thickness

By employing a process of small-angle injection, vertical degassing, and flat curing, combined with a backplate mold design, the problems of bubble removal, curing shrinkage, and deformation control in the manufacturing of large-area transparent parts have been solved, achieving high optical quality and uniform thickness in flat plate injection lamination.

CN121848682APending Publication Date: 2026-04-14AVIC BEIJING AERONAUTICAL MFG TECH RES INST
View PDF 0 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-01-21
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

Existing infusion lamination processes have difficulty controlling air bubble removal, uniform curing shrinkage of adhesive, and deformation of transparent materials in the manufacture of large-area transparent parts, leading to problems with optical quality and thickness uniformity.

Method used

By employing a method of small-angle injection, vertical degassing, and flat curing, combined with the design of a bottom edge inlet and an top overflow outlet, the height difference of the liquid adhesive is reduced and deformation is limited by a rigid back plate mold. With the assistance of gradient temperature curing, uniform degassing and thickness uniformity of the adhesive are ensured.

Benefits of technology

High optical quality and thickness uniformity of large-area transparent parts were achieved, and the problems of bubble marks and structural deformation were solved, resulting in the preparation of high-quality flat plate infusion laminated parts.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN121848682A_ABST
    Figure CN121848682A_ABST
Patent Text Reader

Abstract

The invention relates to a large-area, high-optical-quality and uniform-thickness flat plate pouring and laminating method which comprises the following steps: assembling a lower cover plate and a pre-pouring flat plate piece, then placing a cushion block along the edge of an inorganic glass back plate, and placing an upper cover plate on the pre-pouring flat plate piece to finish integral assembly; the overflow port is slightly higher than the glue inlet, meanwhile, the filling pressure of the glue inlet cylinder is controlled, the glue is filled into the laminating channel, and the pressure gradient is increased in the filling process; after the whole laminated structure is filled with the sizing material and the sizing material overflows from the overflow port, continuously curing the sizing material for a certain time, and then erecting the laminating tool to a certain angle to carry out bubble removal treatment; after all bubbles in the laminated structure are discharged, the laminated structure is integrally laid flat, later curing is carried out, and curing is carried out in a gradient temperature rising mode. The optical problems of bubbles, marks and the like in the rubber material in the large-area flat plate pouring lamination process and the structural deformation control problem of the laminated transparent material can be effectively solved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This application relates to the field of transparent component injection lamination manufacturing technology, and in particular to a method for large-area, high-optical-quality, and uniformly thick flat plate injection lamination. Background Technology

[0002] Lamination of transparent components is a crucial method for improving their bird strike resistance. Infusion lamination is an important process for preparing laminated transparent components. It typically involves injecting a reactive liquid adhesive between two transparent materials under pressure. As the adhesive cures, the transparent materials bond together, resulting in the laminated transparent component. Compared to traditional hot-press lamination, infusion lamination is generally performed under milder temperature and pressure conditions. This avoids the surface quality defects, localized internal structural deformation, and residual thermal stress problems caused by high-temperature and high-pressure lamination of transparent laminates such as PMMA and polycarbonate (PC) in traditional hot-press processes, thus improving the stability of the laminated structure to some extent. However, the process is relatively complex and cumbersome, and the difficulty increases significantly with the size of the laminated component.

[0003] The development of large-area flat laminated transparent components with high optical quality and uniform thickness control through a potting lamination process requires addressing the following technical challenges: First, controlling and removing air bubbles during the potting process of the interlayer adhesive. Adhesive potting generates air bubbles, and due to the rapid reaction and curing of the adhesive, the system viscosity increases dramatically, reducing the rate of bubble removal and significantly increasing the difficulty of removal. Furthermore, at high viscosity, the interaction between bubbles and the adhesive easily generates optical problems such as flow marks. Moreover, as the lamination area increases, the difficulty of bubble removal becomes even greater, making process control more challenging. Second, controlling the uniformity of curing shrinkage of the interlayer potting adhesive. Reactive interlayer adhesives continuously produce uneven volume shrinkage during the curing reaction. The larger the lamination area, the more difficult it is to control the uniformity of adhesive shrinkage, making the laminated component more prone to optical distortion. Finally, controlling the deformation of the potted laminated transparent material. During the injection process, the injection pressure and the gravity of the intermediate layer adhesive will cause structural deformation of the transparent laminate. Controlling the structural deformation of the transparent laminate is an important guarantee for ensuring the overall thickness and dimensional accuracy of the laminated transparent part. Summary of the Invention

[0004] This application provides a method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination to solve the problems mentioned in the background art.

[0005] The method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination includes: Assemble the lower cover plate with the pre-filled flat plate, then place pads along the edge of the inorganic glass back plate, and place the upper cover plate on the pre-filled flat plate to complete the overall assembly. Make the overflow port slightly higher than the glue inlet, and at the same time control the injection pressure of the glue inlet cylinder to inject the glue into the lamination channel. The pressure gradient increases during the injection process. After the adhesive has filled the entire laminate structure and overflowed from the overflow port, continue to cure for a certain period of time, and then stand the laminating fixture upright at a certain angle to perform de-bubbling treatment; After removing all air bubbles from the laminated structure, the laminated structure is laid flat and then cured using a gradient heating method.

[0006] Furthermore, before assembling the lower cover plate with the pre-filled flat plate, placing a pad along the edge of the inorganic glass backing plate, and placing the upper cover plate on the pre-filled flat plate to complete the overall assembly, the process further includes: Choose one of two pre-laminated transparent materials to set the positions of the inlet and overflow ports. After drilling, use fast-curing adhesive to connect the inlet and overflow ports.

[0007] Furthermore, the size of the glue inlet is 5-20mm, the size of the overflow outlet is 5-20mm, the length of the glue inlet tube is 1-3m, and the length of the overflow tube is 0.2-1m.

[0008] Furthermore, after selecting one of two pre-laminated transparent materials to set the positions of the inlet and overflow ports, and connecting the inlet and overflow pipes with fast-curing adhesive after drilling, the method further includes: Use a suitable width of elastic sealing material to arrange the sealing strip along the edge of another pre-laminated transparent material, align the position, and leave the gate inside the injection channel; The processed laminated transparent materials are stacked face-up and compressed to form injection channels, resulting in a pre-injected flat plate.

[0009] Furthermore, the width of the sealing strip is 2-20mm.

[0010] Furthermore, the process of slightly raising the overflow port above the glue inlet while controlling the injection pressure of the glue inlet cylinder to inject the glue into the lamination channel, before the pressure gradient increases during the injection process, also includes: The injection compound is pre-treated by heating, weighed and mixed, and then degassed. After the air bubbles in the mixed compound are removed, it is placed in the injection pressure tank and ready for injection.

[0011] Furthermore, the potting compound is a polyurethane potting compound, which includes components A and B. Component A is left to stand at room temperature, and component B is heated at 40°C for 4 hours before use. The mass ratio of components A to B is 170-180mg:290-300mg.

[0012] Furthermore, the angle between the overflow port and the glue inlet is 5-30°, and the pressure gradient during the injection process is 0.5-1.5atm→1.5-2atm→2-3atm.

[0013] Furthermore, the continued curing time is 0.5h-2h, and the lamination fixture is erected at a certain angle of 50°-90°.

[0014] Furthermore, the gradient heating method involves curing at room temperature (20℃-25℃) for 5-7 days, followed by curing at 30℃ for 1 day, 40℃ for 1 day, and 50℃ for 1 day.

[0015] The above-mentioned technical solution of this application has the following advantages: This application provides a method for large-area, high-optical-quality, and uniform-thickness flat plate lamination. It addresses technical challenges in the lamination process by employing three dynamic processes: small-angle injection, vertical degassing, and flat curing. The small-angle injection method reduces pressure on the laminated glass by minimizing the overall height difference of the liquid adhesive. A rigid backing mold (inorganic glass + metal mold) further restricts large structural deformations of the laminated plate. Simultaneously, a vertical degassing process, combined with an optimal degassing design at the bottom edge and top overflow outlet, maximizes the degassing of the intermediate layer adhesive. Finally, the laminated specimen is placed flat, and the gravity compression of the backing mold allows the adhesive to self-level. This gravity compression also compensates for curing shrinkage to some extent, ensuring overall thickness uniformity and guaranteeing the overall optical performance of the laminated sample. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram showing the locations of the glue inlet and overflow outlet provided in an embodiment of this application; Figure 2 This is a schematic diagram of a pre-set infusion channel provided in an embodiment of this application; Figure 3 An assembly diagram of the pre-filled flat plate and the lamination tooling provided in the embodiments of this application; Figure 4 This is a schematic diagram illustrating the small-angle injection, vertical degassing, and horizontal curing processes provided in the embodiments of this application. Figure 5This is a schematic diagram of the thickness distribution of the sample in Embodiment 1 of this application; Figure 6 This is a schematic diagram of the sample thickness distribution in Embodiment 2 of this application. Detailed Implementation

[0018] In the following description, specific details such as particular system architectures and techniques are set forth for illustrative purposes and not for limitation, in order to provide a thorough understanding of the embodiments of this application. However, those skilled in the art will understand that this application may also be implemented in other embodiments without these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of this application with unnecessary detail.

[0019] It should be understood that, when used in this application specification and the appended claims, the term "comprising" indicates the presence of the described features, integrals, steps, operations, elements and / or components, but does not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or a collection thereof.

[0020] Furthermore, in the description of this application and the appended claims, the terms "first," "second," "third," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0021] References to "one embodiment" or "some embodiments" in this specification mean that one or more embodiments of this application include a specific feature, structure, or characteristic described in connection with that embodiment. Therefore, the phrases "in one embodiment," "in some embodiments," "in other embodiments," "in still other embodiments," etc., appearing in different parts of this specification do not necessarily refer to the same embodiment, but rather mean "one or more, but not all, embodiments," unless otherwise specifically emphasized. The terms "comprising," "including," "having," and variations thereof mean "including but not limited to," unless otherwise specifically emphasized. "A plurality" means "two or more."

[0022] The specific embodiments of this application will be described in further detail below with reference to the accompanying drawings and examples. The following examples are used to illustrate this application, but are not intended to limit the scope of this application.

[0023] This application provides a method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination, including: 1) Setting and treatment of the injection gate: Select one of the two pre-laminated transparent materials to set the positions of the glue inlet and overflow outlet, and connect the glue inlet and overflow pipelines after opening the hole.

[0024] 2) Pre-setting of the injection channel: Use an elastic sealing material of appropriate width to arrange the sealing strip along the edge of another pre-laminated transparent material, align the position, reserve the gate inside the injection channel, and then stack the treated laminated transparent materials face to face and compress to form the injection channel, thus obtaining the pre-injected flat plate.

[0025] 3) Assembly of the pre-filled flat plate and the lamination fixture: The lamination fixture includes upper and lower cover plates, which are made of metal and inorganic glass. The cover plates are slightly larger than the pre-filled flat plate and are used to place spacers to control the thickness of the poured laminated sample. After adjusting the lamination fixture, stack the lower back plate, the pre-filled flat plate, and the upper back plate in sequence, align them, insert the rigid spacers, and finally tighten the locking nuts to complete the assembly.

[0026] 4) Pretreatment of intermediate layer injection compound: The injection compound is pretreated by heating, weighed and mixed, and then degassed. After the air bubbles in the mixed compound are removed, it is placed in the injection pressure tank and ready for injection.

[0027] 5) Small-angle injection: Make the overflow port slightly higher than the injection port, and at the same time control the injection pressure of the injection cylinder to inject the adhesive into the lamination channel.

[0028] 6) Vertical degassing: After the adhesive has filled the entire laminated structure and overflowed from the overflow port, let it stand for a while, and then stand the laminating fixture upright at a certain angle to carry out the degassing process.

[0029] 7) Flat curing: After removing all air bubbles from the laminated structure, lay the laminated structure flat as a whole for subsequent curing.

[0030] This application provides a method for large-area, high-optical-quality, and uniform-thickness flat plate casting lamination. Through three dynamic processes—small-angle casting, vertical degassing, and horizontal curing—it can effectively solve optical problems such as air bubbles and marks inside the adhesive material and control the structural deformation of the laminated transparent material during the large-area flat plate casting lamination process, thus preparing a large-area, high-optical-quality, and uniform-thickness flat plate casting laminate sample.

[0031] Specifically, the steps include: 1) Setting and treatment of the injection gate: Select one of two pre-laminated transparent materials to set the positions of the inlet and overflow gate. The location diagram can be attached. Figure 1 One of the methods is as follows: the specific distance between the gate and the overflow port and the edge is not required (a sealing width must be left); the size of the inlet is preferably 5-20mm, and the size of the overflow port is preferably 5-20mm; after drilling, use fast-curing adhesive to connect the inlet tube and the overflow tube, the length of the inlet tube is preferably 1-3m, and the length of the overflow tube is preferably 0.2-1m.

[0032] 2) Pre-set injection channels: as shown in the attached document Figure 2As shown, first, select one of two pre-laminated transparent materials and arrange a sealing strip along the edge of the material. The width of the strip is preferably 2-20mm. After aligning the positions, reserve the gate inside the injection channel. Then, close and seal the two pre-laminated transparent materials to form the injection channel.

[0033] 3) Assembly of pre-filled flat parts with lamination tooling: such as Figure 3 As shown, first, the lower cover plate and the pre-filled flat plate are assembled. Then, pads are placed along the edge of the inorganic glass back plate. Finally, the upper cover plate is placed on the pre-filled flat plate to complete the overall assembly. 4) Pretreatment of intermediate layer potting compound: In this embodiment, reactive polyurethane potting compound is used as the intermediate adhesive layer material. The polyurethane potting compound consists of components A and B. Component A is left to stand at room temperature, and component B is heated at 40°C for 4 hours before use. The preferred mass ratio of components A and B is 170-180mg:290-300mg. After weighing and mixing, vacuum degassing is performed. After the compound is completely degassed, it is placed in the potting pressure tank and ready for injection.

[0034] 5) Small-angle injection: as shown in the attached document Figure 4 As shown, the overflow port is positioned higher than the glue inlet, with an angle preferably between 5-30°. The injection pressure of the glue inlet cylinder is controlled to inject the glue into the lamination channel. During the injection process, the pressure gradient increases: preferably 0.5-1.5 atm → 1.5-2 atm → 2-3 atm.

[0035] 6) Vertical degassing: After the adhesive has filled the entire laminated structure and overflowed from the overflow port, continue to cure for a certain period of time, preferably 0.5h-2h. Then, stand the laminating fixture upright at a certain angle, preferably 50°-90°, to perform degassing treatment.

[0036] 7) Flat Curing: After removing all air bubbles from the laminated structure, lay the entire laminated structure flat for post-curing using a gradient temperature increase method. Preferred temperature increase method: cure at room temperature (20℃-25℃) for 5-7 days, then at 30℃ for 1 day, 40℃ for 1 day, and 50℃ for 1 day.

[0037] The following is a description through specific embodiments.

[0038] Example 1 The infusion lamination method of this embodiment is used for the high-quality lamination of plexiglass (PMMA) and polycarbonate (PC). The specific steps are as follows: Setting and treatment of the injection gate: The opening is made on the PMMA with a single inlet gate in the middle of the bottom and double outlet gates on both sides of the top. The gates are all 10mm in size. After the opening is made, the glue inlet pipe and the overflow pipe are connected. The glue inlet pipe is 1m long and the overflow pipe is 0.3m long.

[0039] Pre-set injection channel: Arrange elastic butyl tape with a width of 10mm along the edge of PC, then position PMMA and PC together to close the mold, leaving the gate open and forming a sealed channel.

[0040] Assembly of pre-filled flat plate parts and laminated tooling: Place the PMMA and PC composite structure on the lower back plate, place 18mm limit blocks along the edge of the inorganic glass back plate, determine the relative positions of all materials, cover with the upper back plate, tighten the nuts, and complete the assembly.

[0041] Intermediate layer potting compound pretreatment: The intermediate layer uses polyurethane potting compound, which consists of components A and B. Component A is left to stand at room temperature, while component B is heated at 40°C for 4 hours before use. The components A and B are weighed and mixed according to a mass ratio of 179.5mg:292.8mg, and then subjected to vacuum degassing treatment. After degassing for 30 minutes using a vacuum stirring degassing device, the mixture is placed in a potting pressure tank and prepared for injection.

[0042] Small-angle injection: Injection is performed at a 10° angle, controlling the injection pressure of the injection cylinder to inject the adhesive into the lamination channel. The pressure gradient increases during injection: 1 atm → 1.5 atm → 2 atm.

[0043] Vertical degassing: Degassing is performed at an 85° angle, and degassing is completed in about 30 minutes.

[0044] Flat curing: The laminated structure was laid flat and cured at room temperature (25℃) for 5 days. After curing in an oven at 30℃, 40℃, and 50℃ for 24 hours each, the laminated flat pieces were removed. The thickness distribution of the samples is as follows: Figure 5 As shown.

[0045] Example 2 The infusion lamination method of this embodiment is used for the high-quality lamination of plexiglass (PMMA) and polycarbonate (PC). The specific steps are as follows: Setting and treatment of the injection gate: The opening is made on the PC, adopting a single gate in the middle of the bottom and a double gate on both sides of the top. The gate size is uniformly 10mm. After the opening is made, the glue inlet pipe and the overflow pipe are connected. The glue inlet pipe is 1m long and the overflow pipe is 0.3m long.

[0046] Pre-set injection channel: Arrange elastic butyl tape with a width of 10mm along the edge of PMMA, then position PMMA and PC together to close the mold, leaving the gate open and forming a sealed channel.

[0047] Assembly of pre-filled flat plate parts and laminated tooling: Place the PMMA and PC composite structure on the lower back plate, place 18mm limit blocks along the edge of the inorganic glass back plate, determine the relative positions of all materials, cover with the upper back plate, tighten the nuts, and complete the assembly.

[0048] Intermediate layer potting compound pretreatment: The intermediate layer uses polyurethane potting compound, which consists of components A and B. Component A is left to stand at room temperature, while component B is heated at 40°C for 4 hours before use. The components A and B are weighed and mixed according to a mass ratio of 179.5mg:292.8mg, and then subjected to vacuum degassing treatment. After degassing for 30 minutes using a vacuum stirring degassing device, the mixture is placed in a potting pressure tank and prepared for injection.

[0049] Small-angle injection: Injection is performed at a 10° angle, controlling the injection pressure of the injection cylinder to inject the adhesive into the lamination channel. The pressure gradient increases during injection: 1 atm → 1.5 atm → 2 atm.

[0050] Vertical degassing: Degassing is performed at an 85° angle, and degassing is completed in about 30 minutes.

[0051] Flat curing: The laminated structure was laid flat and cured at room temperature (25℃) for 5 days. After curing in an oven at 30℃, 40℃, and 50℃ for 24 hours each, the laminated flat pieces were removed. The thickness distribution of the samples is as follows: Figure 6 As shown.

[0052] The large-area flat plate infusion laminated sample prepared by the infusion lamination process proposed in this application has good overall thickness uniformity, with a thickness tolerance within 0.5 mm. Furthermore, the laminated sample is free of obvious optical defects such as bubbles and marks, and exhibits excellent overall optical performance.

[0053] It should be clarified that the various embodiments in this specification are described in a progressive manner, and the same or similar parts between the various embodiments can be referred to mutually. Each embodiment focuses on describing the differences from other embodiments. This application is not limited to the specific structures described above and shown in the figures. Furthermore, for the sake of brevity, detailed descriptions of known methods and techniques are omitted here.

[0054] The above-described embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application, and should all be included within the protection scope of this application.

Claims

1. A method for large-area, high-optical-quality, and uniformly thick flat plate infusion lamination, characterized in that, include: Assemble the lower cover plate with the pre-filled flat plate, then place pads along the edge of the inorganic glass back plate, and place the upper cover plate on the pre-filled flat plate to complete the overall assembly. Make the overflow port slightly higher than the glue inlet, and at the same time control the injection pressure of the glue inlet cylinder to inject the glue into the lamination channel. The pressure gradient increases during the injection process. After the adhesive has filled the entire laminate structure and overflowed from the overflow port, continue to cure for a certain period of time, and then stand the laminating fixture upright at a certain angle to perform de-bubbling treatment; After removing all air bubbles from the laminated structure, the laminated structure is laid flat and then cured using a gradient heating method.

2. The method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination as described in claim 1, characterized in that, Before assembling the lower cover plate with the pre-filled flat plate, placing a pad along the edge of the inorganic glass back plate, and placing the upper cover plate on the pre-filled flat plate to complete the overall assembly, the process also includes: Choose one of two pre-laminated transparent materials to set the positions of the inlet and overflow ports. After drilling, use fast-curing adhesive to connect the inlet and overflow ports.

3. The method for large-area, high-optical-quality, and uniformly thick flat plate infusion lamination as described in claim 2, characterized in that, The size of the glue inlet is 5-20mm, and the size of the overflow outlet is 5-20mm; the length of the glue inlet tube is 1-3m, and the length of the overflow tube is 0.2-1m.

4. The method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination as described in claim 2, characterized in that, The process of selecting one of two pre-laminated transparent materials to set the inlet and overflow positions, and after drilling the holes, connecting the inlet and overflow tubes with fast-curing adhesive, further includes: Use a suitable width of elastic sealing material to arrange the sealing strip along the edge of another pre-laminated transparent material, align the position, and leave the gate inside the injection channel; The processed laminated transparent materials are stacked face-up and compressed to form injection channels, resulting in a pre-injected flat plate.

5. The method for large-area, high-optical-quality, and uniform-thickness flat plate infusion lamination as described in claim 4, characterized in that, The width of the sealing strip is 2-20mm.

6. The method for large-area, high-optical-quality, and uniform-thickness plate infusion lamination as described in claim 1, characterized in that, The process of slightly raising the overflow port above the glue inlet while controlling the injection pressure of the glue inlet cylinder to inject the glue into the lamination channel, before the pressure gradient increases during injection, also includes: The injection compound is pre-treated by heating, weighed and mixed, and then degassed. After the air bubbles in the mixed compound are removed, it is placed in the injection pressure tank and ready for injection.

7. The method for large-area, high-optical-quality, and uniformly thick flat plate infusion lamination as described in claim 6, characterized in that, The potting compound used is a polyurethane potting compound, which includes components A and B. Component A is left to stand at room temperature, and component B is heated at 40°C for 4 hours before use. The mass ratio of components A and B is 170-180mg:290-300mg.

8. The method for large-area, high-optical-quality, and uniformly thick flat plate infusion lamination as described in claim 1, characterized in that, The angle between the overflow port and the glue inlet is 5-30°, and the pressure gradient during the injection process is 0.5-1.5atm→1.5-2atm→2-3atm.

9. The method for large-area, high-optical-quality, and uniformly thick flat plate infusion lamination as described in claim 1, characterized in that, The curing time is 0.5h-2h, and the lamination fixture is erected at an angle of 50°-90°.

10. The method for large-area, high-optical-quality, and uniform-thickness plate infusion lamination as described in claim 1, characterized in that, The gradient heating method involves curing at room temperature (20℃-25℃) for 5-7 days, followed by curing at 30℃ for 1 day, 40℃ for 1 day, and 50℃ for 1 day.