A process for template passivation

Abstract

This application belongs to the field of nanoimprint technology, and particularly relates to a process for passivating a template. This application provides a process for passivating a template, which includes the following steps: placing the template in a passivation device, continuously introducing vaporized fluorochlorosilane into the passivation device, and performing a passivation reaction on the template to obtain a passivated template; wherein, the gas flow rate of the fluorochlorosilane is 1 μL / min to 5 μL / min. Among them, by means of isothermal control of the gas flow rate of fluorochlorosilane, the vaporized fluorochlorosilane in the passivation chamber can continuously and stably perform moderate passivation on the template, making the passivation on the template surface uniform and dense. This application provides a process for passivating a template, effectively solving the technical problems of non-uniform and non-dense passivation on the template surface existing in the existing passivation process.

Description

Technical Field

[0001] This application belongs to the field of nanoimprint technology, and particularly relates to a process for passivating a template. Background Art

[0002] Nanoimprint technology is considered to be one of the most promising micro-nano manufacturing technologies. It can break through the limitations of the diffraction effect of optical lithography and process nano-structures. It is most likely to become the main technology in the future micro-nano photonics and electronics industries. It can be applied to the low-cost and large-scale production of micro-nano structure functional devices, especially in the preparation of optical devices, where it has unique technical advantages and is also the most widely used field currently. The basic process of nanoimprint technology includes three stages: pattern imprinting, pattern transfer, and demolding of the imprint template. According to the pattern transfer method, there are mainly two methods: hot embossing and ultraviolet imprinting. Regardless of the imprinting method used, the imprinting process is to faithfully replicate the micro-nano pattern on the template onto the substrate. The commonly used template materials for nanoimprint master templates are mainly silicon and quartz, which have the characteristics of long processing time, high cost, and expensive price. In order to enable smooth demolding after imprinting, usually when making the master template, after the pattern on the master template is made, the master template is passivated to make the surface tension of the master template meet the requirements for demolding.

[0003] The existing method for passivating the master template is as follows: First, the master template is placed in an incubator at 250°C, and then a passivation reagent is injected into the incubator and maintained for 2 hours. Taking out the sample completes the passivation. However, this application has found that there is a problem during the passivation process. When passivating, as soon as the passivation reagent is dropped into the incubator at 250°C, it will quickly vaporize and simultaneously passivate the template. However, due to the too fast vaporization process of the passivation reagent, the vaporized passivation reagent in this closed space of the incubator quickly reaches a saturated state. After reaching the saturated state, the vaporized passivation reagent has poor fluidity, resulting in uneven and non-dense passivation on the surface of the template, affecting demolding. Summary of the Invention

[0004] In view of this, this application provides a process for passivating a template, effectively solving the technical problems of uneven and non-dense passivation on the surface of the template existing in the existing passivation process.

[0005] This application provides a process for passivating a template, including the following steps:

[0006] Place the template in a passivation device, continuously introduce vaporized fluorochlorosilane into the passivation device, and perform a passivation reaction on the template to obtain a passivated template;

[0007] Wherein, the gas flow rate of the fluorochlorosilane is 1 μL / min to 5 μL / min.

[0008] In another embodiment, the passivation reaction specifically includes: placing the template in the passivation device, heating the passivation device at a preset heating rate, and continuously introducing vaporized fluorochlorosilane into the passivation device while heating, so that the template undergoes a passivation reaction.

[0009] Specifically, in this application, the passivation device is a cavity with a containing space and a cover body with an opening covering the cavity. The template is placed in the cavity, and then the cover body is covered. After the opening of the cover body is hermetically connected to a delivery pipe for inputting vaporized fluorochlorosilane to form a sealed space, the cavity is heated at a preset heating rate, and at the same time, vaporized fluorochlorosilane is continuously introduced into the passivation device, and then the template undergoes a passivation reaction.

[0010] In another embodiment, heating the passivation device at a preset heating rate and continuously introducing vaporized fluorochlorosilane into the passivation device specifically means: dropping fluorochlorosilane into the passivation device, and then heating the passivation device at a preset heating rate, so that the fluorochlorosilane located in the passivation device is continuously vaporized, and then the template undergoes a passivation reaction; wherein, the fluorochlorosilane does not contact the template.

[0011] It should be noted that the preset heating rate is a heating rate that can control the vaporization of fluorochlorosilane and control the gas flow rate of fluorochlorosilane within 1 μL / min to 5 μL / min. This application does not make specific limitations.

[0012] Specifically, in this application, the passivation device is a cavity with a containing space and a cover body with an opening. The membrane plate is placed in the cavity, and then the cover body is covered. Fluorochlorosilane liquid is added through the opening of the cover body, and then the opening is sealed with a sealing plug. Then the device is heated at a preset heating rate, so that the fluorochlorosilane liquid is vaporized, and the vaporized fluorochlorosilane reacts with the template to undergo a passivation reaction.

[0013] In another embodiment, the passivation device includes a passivation chamber, and the passivation reaction specifically includes: placing the template in the passivation chamber, heating the passivation chamber so that the temperature in the passivation chamber reaches a temperature capable of vaporizing fluorochlorosilane;

[0014] Then continuously introduce vaporized fluorochlorosilane into the passivation chamber, so that the template undergoes a passivation reaction.

[0015] In another embodiment, the passivation device further includes a vaporization chamber communicated with the passivation chamber. Continuously introducing vaporized fluorochlorosilane into the passivation chamber, the passivation reaction of the template is specifically as follows: dropping fluorochlorosilane into the vaporization chamber, heating the vaporization chamber to continuously vaporize the fluorochlorosilane located in the vaporization chamber, and flowing it into the passivation chamber that has reached the temperature capable of vaporizing the fluorochlorosilane, so that the template located in the passivation chamber undergoes a passivation reaction.

[0016] Specifically, the passivation device includes a passivation chamber and a vaporization chamber communicated with the passivation chamber (the passivation chamber and the vaporization chamber are hermetically connected to form a closed reaction vessel). The template is placed in the passivation chamber. An opening is provided at the top of the vaporization chamber. The liquid fluorochlorosilane is dropped into the vaporization chamber from the opening of the vaporization chamber, and then the passivation device is heated at a preset heating rate (that is, heating the passivation chamber and the vaporization chamber simultaneously), so that the liquid fluorochlorosilane in the vaporization chamber is continuously vaporized and flows into the passivation chamber, and the vaporized fluorochlorosilane reacts with the template for passivation.

[0017] In some embodiments, the passivation device can be an inverted concave-shaped closed reaction vessel. The inverted concave-shaped closed reaction vessel is divided into a passivation chamber and a vaporization chamber directly communicated with the passivation chamber (not communicated through a pipeline). In this case, first use a heating device to heat the passivation chamber to make the passivation chamber reach the temperature for vaporizing fluorochlorosilane, and then heat the vaporization chamber at a preset heating rate to continuously vaporize the liquid fluorochlorosilane located in the vaporization chamber and flow it into the delivery passivation chamber, and the vaporized fluorochlorosilane reacts with the template for passivation.

[0018] In some embodiments, the passivation device can include a passivation chamber, a vaporization chamber, and a pipeline. The passivation chamber and the vaporization chamber are connected through the pipeline to form a closed reaction vessel. There are two passivation methods using this passivation device. The first one: heating the vaporization chamber at a preset heating rate to continuously vaporize the fluorochlorosilane, and the vaporized fluorochlorosilane flows into the passivation chamber through the pipeline for passivation reaction. The second one: there is a flow valve in the pipeline connecting the passivation chamber and the vaporization chamber. First, heat the passivation chamber to make it reach the temperature for vaporizing fluorochlorosilane and keep it, then heat the vaporization chamber to vaporize the fluorochlorosilane in the vaporization chamber (any heating method as long as it can vaporize the fluorochlorosilane), and then adjust the flow valve to make the vaporized fluorochlorosilane in the vaporization chamber flow into the passivation chamber at a preset flow rate for passivation reaction.

[0019] In another embodiment, the fluorochlorosilane is selected from fluorotrichlorosilane or / and fluoromonochlorosilane.

[0020] In another embodiment, the fluorinated trichlorosilane is selected from one or more of (trichloro(1H,1H,2H,2H-tridecafluorooctyl)silane, (1H,1H,2H,2H-perfluorodecyl)trichlorosilane, 1H,1H,2H,2H-perfluorohexyltrichlorosilane, 1H,1H,2H,2H-perfluorododecyltrichlorosilane, trichloro(12,12,13,13,14,14,15,15,15-nonafluoropentadecyl)silane, trichloro(12,12,13,13,14,14,15,15,16,16,17,18,18,19,19,19-heptadecafluorononadecyl)silane, trichloro(1,1,2,2,3,3-hexafluoropropyl)silane, trichloro(1,1,2,2,3,3,4,4-octafluorobutyl)silane, trichloro(1,3,3,4,4,5,5,6,6,7,8,8-tetrafluorooctyl)silane, and trichloro(12,12,13,13,14,14,15,15,16,16,17,17,17-tridecafluoroheptadecyl)silane; the fluorinated monochlorosilane is selected from one or more of 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane, 1H,1H,2H,2H-perfluorodecyldimethylchlorosilane, nonafluorohexyldimethylchlorosilane, chlorodimethyl-3,3,3-fluoropropylsilane, chlorodimethyl-[4,4,4-trifluoro-3,3-bis(trifluoromethyl)butyl]silane, chlorodimethyl-(1,1,3,3,3-pentafluoropropyl)silane, and chlorodimethyl-(1,1,2,3,3,3-hexafluoropropyl)silane.

[0021] Specifically, when the passivation process of the present application uses two passivation reagents (two different fluorinated chlorosilanes) for passivation, the passivation process is carried out by a staged passivation method of vaporizing the fluorinated chlorosilane at a preset heating rate. The passivation reaction in the first stage is to passivate the template by vaporizing the fluorinated trichlorosilane, and the passivation reaction in the second stage is to passivate the template by vaporizing the fluorinated monochlorosilane.

[0022] In another embodiment, the fluorinated chlorosilane is selected from fluorinated trichlorosilane and fluorinated monochlorosilane, and the passivation reaction specifically includes:

[0023] Place the template in the passivation device, then inject the fluorinated trichlorosilane into the passivation device, and then heat the passivation device at a first heating rate to continuously vaporize the fluorinated trichlorosilane, so that the template undergoes the passivation reaction in the first stage; then inject the fluorinated monochlorosilane into the passivation device, and then heat the passivation device at a second heating rate to continuously vaporize the fluorinated monochlorosilane, thereby enabling the template to undergo the passivation reaction in the second stage to obtain a passivated template.

[0024] In another embodiment, the fluorochlorosilane is selected from fluorotrichlorosilane and fluoro-monochlorosilane. The passivation device includes a passivation chamber, and the passivation reaction specifically includes:

[0025] Place the template into the passivation chamber, then heat the passivation chamber to the first vaporization temperature. Next, continuously introduce the vaporized fluorotrichlorosilane into the passivation chamber to carry out the passivation reaction in the first stage. Then, heat the passivation chamber to the second vaporization temperature, and then continuously introduce the vaporized fluoro-monochlorosilane into the passivation chamber to carry out the passivation reaction in the second stage, obtaining a passivated template.

[0026] Specifically, the temperature of the first heating rate is the temperature at which the fluorotrichlorosilane can be vaporized, and the rate of the first heating rate is such that the gas flow rate of the fluorotrichlorosilane is 1 μL / min to 5 μL / min; the temperature of the second heating rate is the temperature at which the fluoro-monochlorosilane can be vaporized, and the rate of the second heating rate is such that the gas flow rate of the fluoro-monochlorosilane is 1 μL / min to 5 μL / min.

[0027] Specifically, the time of the passivation reaction in the first stage is 15 to 30 min, and the time of the passivation reaction in the second stage is 15 to 30 min.

[0028] Specifically, the first heating rate is to heat from 5 °C / min to 20 °C / min to 160 °C to 250 °C; the second heating rate is to heat from 5 °C / min to 20 °C / min to 160 °C to 250 °C.

[0029] In another embodiment, the passivation device includes: a cavity, a cover body matching with the cavity, a heat conducting plate, and an injection hole seal;

[0030] The interior of the cavity is divided into a template placement area and a fluorochlorosilane dropping area. An injection hole is opened on the cover body, and the projection of the injection hole is located in the fluorochlorosilane dropping area. The injection hole seal is used to seal the injection hole so that the cavity and the cover body covered on the cavity can form a closed space;

[0031] The heat conducting plate is in contact connection with the bottom of the cavity, and the heat conducting plate is used to heat the cavity so that the fluorochlorosilane in the fluorochlorosilane dropping area of the cavity can be continuously vaporized, and then the template in the template placement area can carry out the passivation reaction.

[0032] Specifically, the cavity and the cover body can be watch glasses. Two watch glasses are covered to form a closed space, and the material of the watch glass can be a material such as glass that does not react with fluorochlorosilane and the template.

[0033] Specifically, fluorotrichlorosilane is first dropped into the gasification chamber. After the fluorotrichlorosilane is heated and gasified, the gasified fluorotrichlorosilane can react with the template to form a relatively high surface coverage rate on the template surface, forming a relatively dense passivation layer. However, fluorotrichlorosilane has a tendency to polymerize into massive deposits. Therefore, fluoromonochlorosilane is dropped into the gasification chamber again. After the fluoromonochlorosilane is heated and gasified, the gasified fluoromonochlorosilane has a very fast capping speed, which can inhibit the formation of massive deposits and further improve the surface coverage rate of fluorine elements. Therefore, better passivation effects can be achieved by first passivating with gasified fluorotrichlorosilane and then passivating with gasified fluoromonochlorosilane, which is convenient for better peeling of the template and the resin layer in the subsequent imprinting process, achieving a good demolding effect.

[0034] In another embodiment, the template is a template that has been sequentially etched and plasma-treated.

[0035] Specifically, the plasma treatment time is 5 min.

[0036] Specifically, the dropping amount of the fluorochlorosilane is 10 μL to 80 μL.

[0037] This application uses a specific passivation device. After placing the template in the passivation chamber, gasified fluorochlorosilane is continuously introduced into the passivation chamber. By controlling the flow rate of the gasified fluorochlorosilane and adopting an isothermal specific-rate fluorochlorosilane gas introduction method to passivate the template, the gasified fluorochlorosilane in the passivation chamber can continuously and stably passivate the template moderately, making the passivation on the template surface uniform and dense. This application effectively avoids the phenomenon of uneven and non-dense passivation caused by the strong gasification of fluorochlorosilane at too high a temperature and the too fast passivation of the template. In addition, it is found in the passivation process of this application that better passivation effects can be achieved by first passivating the template with gasified fluorotrichlorosilane and then passivating the template with gasified fluoromonochlorosilane, which is convenient for better peeling of the template and the resin layer in the subsequent imprinting process, achieving a good demolding effect. Description of the Drawings

[0038] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for description in the embodiments or the prior art.

[0039] Figure 1 It is a schematic structural diagram of the passivation device used in the embodiment of the present application;

[0040] Figure 2 It is the measurement result of the water contact angle at the test site A of the passivated template provided in Embodiment 1 of the present application;

[0041] Figure 3Measurement results of the water contact angle of the passivated template test site A provided in Example 2 of this application;

[0042] Figure 4 Measurement results of the water contact angle of the passivated template test site A provided in Example 3 of this application;

[0043] Figure 5 Measurement results of the water contact angle of the passivated template test site A provided in Example 4 of this application;

[0044] Figure 6 Appearance diagram of the passivated template provided in Comparative Example 1 of this application;

[0045] Figure 7 Measurement results of the water contact angle of the passivated template test site A and test site D provided in Comparative Example 2 of this application. Detailed implementation manners

[0046] This application provides a process for template passivation to solve the technical defects of uneven and non-dense passivation on the template surface in existing passivation technologies.

[0047] The technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of this application, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in this application without creative efforts shall fall within the protection scope of this application.

[0048] Among them, the raw materials or reagents used in the following embodiments are all commercially available or self-made.

[0049] The reagent F13-TCS used below is (trichloro(1H,1H,2H,2H-tridecafluorooctyl)silane), and its molecular formula: C8H4Cl3F 13 Si), and the structural formula is as follows:

[0050]

[0051] The structural formula of 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane is as follows:

[0052]

[0053] FDTS is (1H,1H,2H,2H-perfluorodecyltrichlorosilane), and its molecular formula: C 10 H4Cl3F 17 Si), and the structural formula is as follows:

[0054]

[0055] Please refer to Figure 1 , Figure 1 which is a schematic structural diagram of the passivation device adopted in the embodiment of the present application. The structure of the passivation device includes:

[0056] A lower surface dish 1, an upper surface dish 2, and a heat conducting plate 3; the heat conducting plate 3 is in surface contact connection with the bottom plate surface of the lower surface dish 1, so that the heat conducting plate 3 heats the bottom plate of the lower surface dish 1;

[0057] The interior of the lower surface dish 1 is divided into a template placement area and a fluorochlorosilane dropping area;

[0058] The lower surface dish 1 and the upper surface dish 2 are matched in shape and size, and the upper surface dish 2 covers the lower surface dish 1, so that the upper surface dish 1 and the lower surface dish 2 form a sealed atmosphere space, and the atmosphere space includes a template placement area and a fluorochlorosilane dropping area that communicate with each other; an injection hole 4 is provided on the upper surface, and the projection of the injection hole 4 is located in the fluorochlorosilane dropping area.

[0059] Specifically, the heat conducting plate 3 heats the bottom plate of the lower surface dish 1, thereby heating the template placed in the template placement area of the lower surface dish 1.

[0060] Specifically, the heat conducting plate 3 heats the bottom plate of the lower surface dish 1, thereby heating the fluorochlorosilane dropped in the fluorochlorosilane dropping area of the lower surface dish 1.

[0061] Specifically, the materials of the lower surface dish 1 and the upper surface dish 2 are materials that do not have a thermal conductivity reaction with the template and fluorochlorosilane and are heat-resistant, such as glass, etc.

[0062] Specifically, the heat conducting plate 3 is a metal flat plate with strong thermal conductivity, such as an iron plate, a copper plate, etc.

[0063] Specifically, the bottom plate of the lower surface dish 1 is partitioned so that the template and the fluorochlorosilane do not directly contact; the mutually communicating template placement area and fluorochlorosilane dropping area are used to bring the vaporized fluorochlorosilane into contact with the surface of the template, and uniformly passivate the surface of the template located in the template placement area.

[0064] The passivation process of the template in the embodiment of the present application includes the following steps:

[0065] Place the template 5 on the bottom plate of the passivation chamber of the passivation device, heat the fluorochlorosilane to vaporize it, and continuously introduce the fluorochlorosilane gas into the passivation chamber. The fluorochlorosilane gas with a preset flow rate reacts with the template to obtain a passivated template.

[0066] Example 1

[0067] The embodiment of the present application provides a passivation process for a template, including the following steps:

[0068] 1. Plasma process the etched template for 5 minutes. Place the processed template in the passivation chamber of the lower petri dish, and cover the upper petri dish on the lower petri dish so that the upper and lower petri dishes form a sealed atmosphere space. The atmosphere space includes a passivation chamber and a vaporization chamber that communicate with each other.

[0069] 2. Use a pipette to transfer 25 μL of F13-TCS (trichloro(1H,1H,2H,2H-tridecafluorooctyl)silane) and inject it into the vaporization chamber through the injection hole. Seal the injection hole with a stopper. The F13-TCS drips onto the bottom plate of the vaporization chamber.

[0070] 3. Start the heating plate. The heating plate heats the bottom plate of the lower petri dish at a heating rate of 10 °C / min, so that the bottom plate temperatures of both the passivation chamber and the vaporization chamber reach 160 °C. The F13-TCS in the vaporization chamber is continuously heated and vaporized, and the vaporized F13-TCS is introduced into the passivation chamber to passivate the template. The passivation time is 20 minutes.

[0071] 4. Remove the stopper. Use a pipette to transfer 25 μL of 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane and inject it into the vaporization chamber through the injection hole. Seal the injection hole with a stopper. The heating plate heats the bottom plate of the lower petri dish at a heating rate of 5 °C / min to 250 °C, so that the 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane in the vaporization chamber is vaporized. The vaporized 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane is introduced into the passivation chamber to passivate the template. After reacting for 15 minutes, a passivated template is obtained.

[0072] 5. Finally, turn off the heating plate. After natural cooling to room temperature, take out the template. Use a contact angle measuring instrument to characterize the water contact angle of the passivated template. There are 5 test sites (labeled A, B, C, D, and E respectively). The result of test site A in this example is as Figure 2 shown. From Figure 2 the results, it can be seen that first using vaporized F13-TCS and then using vaporized 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane to passivate the template obtains a better passivation effect. The water contact angle is about 117°. The data of the other test sites are shown in Table 1. From Table 1, it can be seen that the contact angle results at different positions of the passivated template in this application are similar, indicating that the passivation process of this application is uniform and dense on the template surface.

[0073] Example 2

[0074] This application example provides a passivation process for a template, including the following steps:

[0075] 1. Plasma-treat the etched template for 5 min. Place the treated template in the passivation chamber of the lower petri dish, and cover the upper petri dish on the lower petri dish so that the upper and lower petri dishes form a sealed atmosphere space, which includes a mutually connected passivation chamber and a vaporization chamber;

[0076] 2. Use a pipette to transfer 25 μL of F13-TCS (trichloro(1H,1H,2H,2H-tridecafluorooctyl)silane) and inject it into the vaporization chamber through the injection hole. Seal the injection hole with a stopper, and F13-TCS drips onto the bottom plate of the vaporization chamber;

[0077] 3. Start the heating plate, which heats the bottom plate of the lower petri dish at a heating rate of 10 °C / min, so that the bottom plate temperatures of both the passivation chamber and the vaporization chamber reach 160 °C. F13-TCS is continuously heated and vaporized in the vaporization chamber, and the vaporized F13-TCS is introduced into the passivation chamber to passivate the template for 20 min;

[0078] 4. Finally, turn off the heating plate. After natural cooling to room temperature, take out the template and use a contact angle measuring instrument to characterize the water contact angle of the passivated template. There are 5 test sites (labeled A, B, C, D, and E respectively). The result of test site A in this example is as Figure 3 shown. From Figure 3 the results, it can be seen that when using vaporized F13-TCS alone to passivate the template, the water contact angle is about 107°. The data of the other test sites are shown in Table 1. From Table 1, it can be seen that the contact angle results at different positions of the passivated template in this application are similar, indicating that the passivation process of this application is uniform and dense on the template surface.

[0079] Example 3

[0080] This application example provides a passivation process for a template, including the following steps:

[0081] 1. Plasma-treat the etched template for 5 min. Place the treated template in the passivation chamber of the lower petri dish, and cover the upper petri dish on the lower petri dish so that the upper and lower petri dishes form a sealed atmosphere space, which includes a mutually connected passivation chamber and a vaporization chamber;

[0082] 2. Use a pipette to transfer 25 μL of 1H,1H,2H,2H-perfluorodecyltrichlorosilane and inject it into the vaporization chamber through the injection hole. Seal the injection hole with a stopper, and 1H,1H,2H,2H-perfluorodecyltrichlorosilane drips onto the bottom plate of the vaporization chamber;

[0083] 3. Start the heat conducting plate. The heat conducting plate heats the bottom plate of the lower surface dish at a heating rate of 10 °C / min, so that the bottom plate temperatures of both the passivation chamber and the vaporization chamber reach 160 °C. 1H,1H,2H,2H-perfluorodecyltrichlorosilane is continuously heated and vaporized in the vaporization chamber. The vaporized 1H,1H,2H,2H-perfluorodecyltrichlorosilane is introduced into the passivation chamber to passivate the template. The passivation time is 20 min, and the passivated template is obtained.

[0084] 4. Finally, turn off the heat conducting plate. After natural cooling to room temperature, take out the template. Use a contact angle measuring instrument to characterize the water contact angle of the passivated template. There are 5 test sites (marked as A, B, C, D, and E respectively). The result of test site A in this example is as Figure 4 shown. From Figure 4 the results, it can be seen that when using vaporized 1H,1H,2H,2H-perfluorodecyltrichlorosilane alone to passivate the template, the water contact angle is about 102°. The data of the remaining test sites are shown in Table 1. From Table 1, it can be seen that the contact angle results at different positions of the passivated template in this application are similar, indicating that the passivation process of this application is uniform and dense on the template surface.

[0085] Example 4

[0086] The present application provides a passivation process for a template, including the following steps:

[0087] 1. Perform plasma treatment on the etched template for 5 min. Place the treated template in the passivation chamber of the lower surface dish. Cover the upper surface dish on the lower surface dish so that the upper surface dish and the lower surface dish form a sealed atmosphere space. The atmosphere space includes a passivation chamber and a vaporization chamber that communicate with each other;

[0088] 2. Use a pipette to transfer 25 μL of 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane and inject it into the vaporization chamber from the injection hole. Seal the injection hole with a plug. The 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane drips onto the bottom plate of the vaporization chamber;

[0089] 3. Start the heat conducting plate. The heat conducting plate heats the bottom plate of the lower surface dish at a heating rate of 10 °C / min, so that the bottom plate temperatures of both the passivation chamber and the vaporization chamber reach 160 °C. 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane is continuously heated and vaporized in the vaporization chamber. The vaporized 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane is introduced into the passivation chamber to passivate the template. The passivation time is 20 min, and the passivated template is obtained.

[0090] 4. Finally, turn off the heat conducting plate. After natural cooling to room temperature, take out the template and use a contact angle measuring instrument to characterize the water contact angle of the passivated template. There are 5 test sites (labeled as A, B, C, D, and E respectively). The result of test site A in this example is as Figure 5 shown. From Figure 5 the results, it can be seen that when using vaporized 1H,1H,2H,2H - perfluorooctyldimethylchlorosilane alone to passivate the template, the water contact angle is about 96°. The data of the remaining test sites are shown in Table 1. From Table 1, it can be seen that the contact angle results at different positions of the passivated template in this application are similar, indicating that the passivation process of this application is uniform and dense on the template surface.

[0091] Comparative Example 1

[0092] The embodiment of this application provides a template passivation process, which specifically includes:

[0093] 1. Perform plasma treatment on the etched template for 5 minutes. Place the treated template in the passivation chamber of the lower surface dish, cover the upper surface dish on the lower surface dish, and align the injection hole of the upper surface dish with the template so that the upper surface dish and the lower surface dish form a sealed atmosphere space. The atmosphere space includes a mutually connected passivation chamber and a vaporization chamber;

[0094] 2. Use a pipette to transfer 25 μL of F13 - TCS and inject it directly from the injection hole onto the surface of the template, and seal the injection hole with a stopper;

[0095] 3. Start the heat conducting plate. The heat conducting plate heats the bottom plate of the lower surface dish at a heating rate of 10 °C / min, so that the temperature of the bottom plate of the passivation chamber reaches 250 °C. F13 - TCS vaporizes on the template and directly passivates the template. The passivation time is 20 minutes to obtain the passivated template.

[0096] 4. Finally, turn off the heat conducting plate. After natural cooling to room temperature, take out the template, detect the appearance of this comparative example, and use a contact angle measuring instrument to characterize the water contact angle of the passivated template. The result of this comparative example is as Figure 6 shown, Figure 6 which is the appearance diagram after template passivation. From Figure 6 the results, it can be seen that when directly dropping F13 - TCS on the template for passivation, excessive F13 - TCS will immediately react on the template surface and undergo a cross - linking reaction to form blocky deposits. Therefore, Figure 6 the white dots in the red circle are formed, indicating that the passivation effect of directly dropping the passivation reagent on the template is poor.

[0097] Comparative Example 2

[0098] The comparative example of this application provides the use of an existing conventional passivation method, which specifically includes:

[0099] The etched template is subjected to plasma treatment for 5 minutes. The treated template is placed on the bottom plate of an incubator at 250 °C. Then, the F13-TCS reagent is dropped onto the bottom plate of the incubator. The F13-TCS reagent does not contact the template. The F13-TCS reagent placed in the incubator vaporizes into a gas and fills the incubator. The F13-TCS gas passivates the template for 2 hours to obtain a passivated template.

[0100] Take out the template and use a contact angle measuring instrument to characterize the water contact angle of the passivated template. There are 5 test sites (labeled A, B, C, D, and E respectively). The results of test site A and test site D in this example are as Figure 7 shown Figure 7 The left figure is the water contact angle result of test site A. Figure 7 The right figure is the water contact angle of test site D. From Figure 7 the results, it can be seen that when using an incubator to passivate the template, the water contact angles of test site A and test site D are approximately 106° and 95° respectively. The data of the remaining test sites are shown in Table 1. It can be seen from Table 1 that the contact angle results at different positions of the passivated template in this application vary greatly, indicating that the passivation of the template surface by the incubator is uneven and not dense. This is because the F13-TCS reagent vaporizes immediately after being dropped into the 250 °C incubator and starts to passivate the template, and its passivation speed is too fast, resulting in non-dense and uneven passivation of the template surface, which in turn affects subsequent demolding.

[0101] Table 1 Contact angle data of test sites A - E in Examples 1 - 4 and Comparative Example 2

[0102] A B C D E Example 1 117° 115° 116° 117° 117° Example 2 107° 106° 105° 106° 105° Example 3 102° 102° 100° 100° 101° Example 4 96° 93° 94° 93° 95° Comparative Example 2 106° 105° 101° 95° 94°

[0103] From the results of the above comparative examples, it can be seen that in the examples of this application, a specific passivation device is used, which can reach the passivation temperature of the template while continuously introducing vaporized fluorochlorosilane, effectively avoiding the violent vaporization and evaporation of fluorochlorosilane at too high a temperature, so that the passivation progresses too fast, resulting in uneven and non-dense passivation of the template surface and affecting demolding.

[0104] The above are only the preferred embodiments of this application. It should be noted that for those of ordinary skill in the art, without departing from the principle of this application, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of this application.

Claims

1. A passivation process for a template, characterized in that, It includes the following steps: Place the template in a passivation device which contains liquid fluorochlorosilane, and then heat the passivation device at a preset heating rate, so that the fluorochlorosilane in the passivation device is continuously vaporized, thereby enabling the template to undergo a passivation reaction; wherein, the liquid fluorochlorosilane does not contact the template; The gas flow rate of the fluorochlorosilane is 1 μL / min to 5 μL / min.

2. The passivation process according to claim 1, characterized in that, That the passivation device contains liquid fluorochlorosilane specifically means: Drop fluorochlorosilane into the passivation device.

3. The passivation process according to claim 1, characterized in that, The passivation device includes a passivation chamber which is used to place the template and conduct the passivation reaction; the passivation reaction specifically includes: Place the template in the passivation chamber and heat the passivation chamber so that the temperature in the passivation chamber reaches a temperature capable of vaporizing fluorochlorosilane.

4. The passivation process according to claim 1, characterized in that, The passivation device further includes a vaporization chamber communicated with the passivation chamber. That the fluorochlorosilane in the passivation device is continuously vaporized, thereby enabling the template to undergo a passivation reaction specifically means: Drop fluorochlorosilane into the vaporization chamber, heat the vaporization chamber, so that the fluorochlorosilane in the vaporization chamber is continuously vaporized and flows into the passivation chamber which has reached a temperature capable of vaporizing the fluorochlorosilane, enabling the template in the passivation chamber to undergo a passivation reaction.

5. The passivation process according to claim 1, characterized in that, The fluorochlorosilane is selected from fluorinated trichlorosilane or / and fluorinated monochlorosilane.

6. The passivation process according to claim 5, characterized in that, The fluorinated trichlorosilane is selected from one or more of trichloro(1H,1H,2H,2H-tridecafluorooctyl)silane, 1H,1H,2H,2H-perfluorodecyltrichlorosilane, 1H,1H,2H,2H-perfluorohexyltrichlorosilane, 1H,1H,2H,2H-perfluorododecyltrichlorosilane, trichloro(12,12,13,13,14,14,15,15,15-nonafluoropentadecyl)silane, trichloro(12,12,13,13,14,14,15,15,16,16,17,18,18,19,19,19-hexadecafluorononadecyl)silane, trichloro(1,1,2,2,3,3-hexafluoropropyl)silane, trichloro(1,1,2,2,3,3,4,4-octafluorobutyl)silane, trichloro(1,3,3,4,4,5,5,6,6,7,8,8-dodecafluorooctyl)silane and trichloro(12,12,13,13,14,14,15,15,16,16,17,17,17-tridecafluoroheptadecyl)silane; the fluorinated monochlorosilane is selected from one or more of 1H,1H,2H,2H-perfluorooctyldimethylchlorosilane, 1H,1H,2H,2H-perfluorodecyldimethylchlorosilane, nonafluorohexyldimethylchlorosilane, chlorodimethyl-3,3,3-fluoropropylsilane, chlorodimethyl-[4,4,4-trifluoro-3,3-bis(trifluoromethyl)butyl]silane, chlorodimethyl-(1,1,3,3,3-pentafluoropropyl)silane and chlorodimethyl-(1,1,2,3,3,3-hexafluoropropyl)silane.

7. The passivation process according to claim 5, characterized in that, The fluorochlorosilane is selected from fluorotrichlorosilane and fluoro monochlorosilane, and the passivation reaction specifically includes: Placing the template in the passivation device, then injecting the fluorotrichlorosilane into the passivation device, and then heating the passivation device at a first heating rate to continuously vaporize the fluorotrichlorosilane, so that the template undergoes the passivation reaction in the first stage; then injecting the fluoro monochlorosilane into the passivation device, and then heating the passivation device at a second heating rate to continuously vaporize the fluoro monochlorosilane, thereby enabling the template to undergo the passivation reaction in the second stage, and obtaining a passivated template.

8. The passivation process according to claim 5, wherein The fluorochlorosilane is selected from fluorotrichlorosilane and fluoro monochlorosilane, the passivation device includes a passivation chamber, and the passivation reaction specifically includes: Placing the template into the passivation chamber, then heating the passivation chamber to a first vaporization temperature, and then continuously introducing the vaporized fluorotrichlorosilane into the passivation chamber to carry out the passivation reaction in the first stage; then heating the passivation chamber to a second vaporization temperature, and then continuously introducing the vaporized fluoro monochlorosilane into the passivation chamber to carry out the passivation reaction in the second stage, and obtaining a passivated template.

9. The passivation process according to claim 2, characterized in that, The passivation device includes: a cavity, a cover body matching with the cavity, a heat conducting plate and an injection hole seal; The interior of the cavity is divided into a template placement area and a fluorochlorosilane dropping area. An injection hole is opened on the cover body, and the projection of the injection hole is located in the fluorochlorosilane dropping area. The injection hole seal is used to seal the injection hole so that the cavity and the cover body covered on the cavity can form a closed space; The heat conducting plate is in contact connection with the bottom of the cavity, and the heat conducting plate is used to heat the cavity so that the fluorochlorosilane in the fluorochlorosilane dropping area of the cavity can be continuously vaporized, thereby enabling the template in the template placement area to undergo a passivation reaction.

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