Preparation method of multifunctional film and optical panel
Patent Information
- Application Number
- CN202311770058.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-20
- Publication Date
- 2026-09-15
- Estimated Expiration
- 2043-12-20
AI Technical Summary
[0003]然而,湿法涂覆的方法存在着涂层与基材结合力不足的问题
[0034] First, in the preparation method provided in this application embodiment, the precursors of titanium dioxide or zinc oxide are bombarded with plasma of corresponding radio frequency power, causing them to decompose and undergo a homogeneous reaction to generate high-purity first oxide particles. Meanwhile, the coating atoms of the organosilicon source precursor, excited by plasma bombardment, are adsorbed onto the surface of the first oxide particles, undergoing a heterogeneous reaction to generate silica particles. Thus, the silica particles form a complete and dense coating layer on the surface of the first oxide particles. When the target particles coated by the coating layer enter the deposition chamber, chemical vapor deposition can occur on the surface of the substrate to be deposited, forming a multifunctional film. In this multifunctional film, the coating layer and the surface to be deposited are connected by chemical bonds within the nanoparticles, thereby effectively improving the adhesion between the coating layer and the substrate.
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Figure CN117778990B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of display technology, and in particular to a method for preparing a multifunctional film and an optical panel. Background Technology
[0002] To improve the clarity of optical windows on devices such as cameras and extend their service life when installed outdoors, the current main method is to prepare SiO2 / TiO2 composite systems using a solution method and then wet-coat them onto the surface of the substrate (i.e., the optical window) to prepare a high-transmittance coating, thereby protecting the optical window.
[0003] However, wet coating methods suffer from insufficient adhesion between the coating and the substrate. Poor adhesion can easily lead to interlayer failure, or even coating blistering or peeling. Although current methods have improved adhesion by adding binders or using hot-pressing processes, the thinness of the coating itself often results in uneven thickness. Therefore, a method for preparing films that effectively improves the adhesion between the film and the substrate is currently lacking. Summary of the Invention
[0004] This application provides a method for preparing a multifunctional film and an optical panel to improve the adhesion between the multifunctional film and the substrate, thereby extending the service life of the multifunctional film.
[0005] Firstly, embodiments of this application provide a method for preparing a multifunctional membrane, comprising:
[0006] Under conditions of temperature greater than or equal to 120°C, atmosphere containing oxygen, and plasma radio frequency power greater than or equal to 580W, the first gas flow of organic titanium source precursor or organic zinc source precursor undergoes a homogeneous reaction under plasma bombardment to generate first oxide particles.
[0007] The second gas flow of the organosilicon source precursor undergoes a heterogeneous reaction with the first oxide particles under the bombardment of the plasma, generating silica particles on the surface of the first oxide particles to obtain target particles; wherein, in the target particles, the coating layer on the surface of the first oxide particles is composed of the silica particles.
[0008] The target particles are deposited on the surface of the target substrate to form the multifunctional film; wherein, the mass fraction of silicon dioxide in the target substrate is greater than or equal to 50%.
[0009] In one possible implementation, the surface to be deposited is pretreated; wherein the pretreatment includes at least one of ozone treatment, plasma cleaning, and ultraviolet grafting.
[0010] In one possible implementation, the flow rate of the first airflow is 6-9 μL / min, and the flow rate of the second airflow is less than the flow rate of the first airflow.
[0011] In one possible implementation, the flow rate of the second airflow is 5-8 μL / min.
[0012] In one possible implementation, the homogeneous reaction is carried out in a reaction channel with a length greater than 50 cm and which is curved along its length.
[0013] One possible implementation includes, before obtaining the oxide particles:
[0014] A third gas flow of the organic doped source precursor is introduced into the reaction channel of the homogeneous reaction, so that the metal corresponding to the organic doped source precursor is doped into the nanoparticles obtained by the homogeneous reaction; wherein the crystal structure of the metal is face-centered cubic.
[0015] The obtained oxide particles include:
[0016] The metal-doped oxide particles are obtained.
[0017] In one possible implementation, the organic doped source precursor includes at least one of an organic silver source precursor, an organic aluminum source precursor, an organic gold source precursor, and an organic copper source precursor.
[0018] In one possible implementation, the flow rate of the third airflow is less than or equal to half the flow rate of the first airflow.
[0019] In one possible implementation, the flow rate of the third airflow is 2-3 μL / min.
[0020] In one possible implementation, the homogeneous reaction and the heterogeneous reaction are carried out in the same reaction channel; then the first gas flow, the second gas flow, and the third gas flow are introduced from the first air inlet, the second air inlet, and the third air inlet of the reaction channel, respectively; wherein,
[0021] The first air inlet and the third air inlet are both on the same side as the first air inlet of the reaction channel, and the second air inlet is on the same side as the outlet located at the tail end of the reaction channel. The first air inlet is used to introduce inert purging gas into the reaction channel.
[0022] In one possible implementation, the organic titanium source precursor includes at least one of tetraisopropoxide titanium, tetradiethylaminotitanium, and tetrabutyl titanate.
[0023] One possible implementation is that the organic zinc source precursor includes at least one of diethyl zinc, zinc gluconate, and zinc acetate dihydrate.
[0024] In one possible implementation, the organosilicon source precursor includes at least one of hexamethyldisiloxane, methyl orthosilicate, and ethyl orthosilicate.
[0025] In one possible implementation, the radio frequency power is less than or equal to 620W.
[0026] In one possible implementation, the temperatures of the homogeneous reaction and the heterogeneous reaction are less than or equal to 150°C.
[0027] Secondly, embodiments of this application provide an optical panel, including:
[0028] The multifunctional membrane obtained by the preparation method described in the first aspect and any possible embodiment.
[0029] Thirdly, embodiments of this application provide a chemical vapor deposition apparatus, comprising:
[0030] A deposition chamber and a reaction channel curved along its length; the reaction channel is longer than 50 cm, and includes a first air inlet, a second air inlet, and a third air inlet; wherein...
[0031] The first air inlet and the third air inlet are both on the same side as the first air inlet of the reaction channel, and the second air inlet is on the same side as the outlet located at the tail end of the reaction channel.
[0032] The first air inlet, the second air inlet, and the third air inlet are all used to introduce precursor gas to generate target particles, which are then introduced into the deposition chamber through the outlet to be deposited on the substrate surface.
[0033] One or more technical solutions provided in the embodiments of the present invention have at least the following technical effects:
[0034] First, in the preparation method provided in this application embodiment, the precursors of titanium dioxide or zinc oxide are bombarded with plasma of corresponding radio frequency power, causing them to decompose and undergo a homogeneous reaction to generate high-purity first oxide particles. Meanwhile, the coating atoms of the organosilicon source precursor, excited by plasma bombardment, are adsorbed onto the surface of the first oxide particles, undergoing a heterogeneous reaction to generate silica particles. Thus, the silica particles form a complete and dense coating layer on the surface of the first oxide particles. When the target particles coated by the coating layer enter the deposition chamber, chemical vapor deposition can occur on the surface of the substrate to be deposited, forming a multifunctional film. In this multifunctional film, the coating layer and the surface to be deposited are connected by chemical bonds within the nanoparticles, thereby effectively improving the adhesion between the coating layer and the substrate.
[0035] Secondly, when an organic doped source precursor is introduced, dopants can be incorporated into the lattice of the first oxide particles, extending the cutoff wavelength of the multifunctional film to the visible light range. This increases the number of photogenerated carriers on the surface of the target particles, resulting in superior hydrophilic self-cleaning functionality. Furthermore, the hydrophilic self-cleaning function of the multifunctional film is no longer limited to sunlight conditions; it remains unaffected under any lighting conditions. Therefore, the hydrophilic self-cleaning function of the multifunctional film provided in this application can be utilized in various scenarios.
[0036] Furthermore, under the aforementioned RF power and temperature conditions, when the first oxide particle is titanium dioxide, the doped atoms enter the lattice of the titanium dioxide particles and can hinder the transformation of the titanium dioxide crystal form by accumulating strain energy, thus ensuring the hydrophilic self-cleaning function of the multifunctional membrane.
[0037] Finally, when the aforementioned homogeneous and heterogeneous reactions are carried out in the reaction channel that is curved along the length direction, the precursor can be frequently collided with the channel wall of the reaction channel. At the same time, since the length of the reaction channel is greater than 50cm, the size and shape of the first oxide particles are guaranteed, thereby enabling the first oxide particles to be uniformly and densely coated by the silicon dioxide particles.
[0038] Other features and advantages of this application will be set forth in the following description and will be apparent in part from the description or may be learned by practicing the application. The purposes and other advantages of this application may be realized and obtained by means of the structures particularly pointed out in the written description, claims, and drawings. It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not intended to limit this disclosure. Attached Figure Description
[0039] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of this application. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.
[0040] Figure 1 A schematic flowchart illustrating a method for preparing a multifunctional film layer according to an embodiment of this application;
[0041] Figure 2 This is a schematic diagram of the shape of a ring-shaped reaction channel that is not connected end to end, as provided in an embodiment of this application. Detailed Implementation
[0042] To address the problem of insufficient adhesion between nano-coatings prepared by current wet coating processes and the substrate, this application provides a method for preparing a multifunctional film. Based on PECVD (Plasma Enhanced Chemical Vapor Deposition), the corresponding precursor undergoes a homogeneous reaction under plasma bombardment to generate oxide particles. An organosilicon source precursor is then introduced, allowing metal ions (silicon ions and / or aluminum ions) in the organic coating source to be completely adsorbed on the surface of the homogeneous reaction product (pure oxide particles), resulting in a heterogeneous reaction and obtaining core-shell structured target particles. These target particles are then chemically deposited on the surface of the substrate to be deposited, forming a dense multifunctional film that is tightly bonded to the substrate surface.
[0043] To better understand the above technical solutions, the technical solutions of this application will be described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the embodiments of this application and the specific features in the embodiments are detailed descriptions of the technical solutions of this application, rather than limitations on the technical solutions of this application. In the absence of conflict, the embodiments of this application and the technical features in the embodiments can be combined with each other.
[0044] The terms "first" and "second" in the specification, claims, and accompanying drawings of this application are used to distinguish different objects, not to describe a specific order. Furthermore, the term "comprising" and any variations thereof are intended to cover non-exclusive protection. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units not listed, or may optionally include other steps or units inherent to these processes, methods, products, or devices. The term "multiple" in this application can mean at least two, for example, two, three, or more, and the embodiments of this application do not impose limitations.
[0045] Please refer to Figure 1 This application proposes a method for preparing a multifunctional membrane, which provides a method for preparing a multifunctional membrane that enables a tight bond between the multifunctional membrane and the substrate, avoiding the problem that current methods of improving adhesion through adhesives lead to a decrease in coating uniformity. The method specifically includes the following steps:
[0046] Step 101: Under conditions of temperature greater than or equal to 120°C, atmosphere containing oxygen, and plasma radio frequency power greater than or equal to 580W, the first gas flow of organic titanium source precursor or organic zinc source precursor undergoes a homogeneous reaction under plasma bombardment to generate first oxide particles.
[0047] The first oxide particles are titanium dioxide particles and / or zinc oxide particles.
[0048] Specifically, the flow rate of the first gas stream is 6-9 μL / min, so that the organo-titanium source precursor or organo-zinc source precursor is decomposed under plasma bombardment and high temperature, generating titanium dioxide particles or zinc oxide particles with an average particle size of 100-150 nm. This average particle size can be obtained through the following method:
[0049] In the SEM test image, the average value is obtained by measuring and calculating N randomly selected particles. N is an integer greater than or equal to 100. The particle size of each particle is the average of the length of the longest line segment in the SEM image whose endpoint is located at the edge of the oxide particle and passes through the geometric center of the oxide particle, and the length of the shortest line segment whose endpoint is located at the edge of the oxide particle and passes through the aforementioned geometric center.
[0050] In some embodiments, the organotitanium source precursor includes at least one selected from titanium isopropoxide, tetradiethylaminotitanium, and tetrabutyl titanate. Preferably, the organotitanium source precursor is one selected from titanium isopropoxide, tetradiethylaminotitanium, and tetrabutyl titanate.
[0051] In some embodiments, the organozinc source precursor includes at least one selected from diethylzinc, zinc gluconate, and zinc acetate dihydrate. Preferably, the organozinc source precursor is one selected from diethylzinc, zinc gluconate, and zinc acetate dihydrate.
[0052] The aforementioned first gas flow can be obtained by high-temperature vaporization of the precursor from the corresponding source.
[0053] To further enhance the cutoff wavelength of the multifunctional film, enabling it to generate a sufficient number of photogenerated carriers under visible light conditions and ensuring its hydrophilic self-cleaning function functions effectively under different light conditions, in some embodiments, during / after the initiation of the aforementioned homogeneous reaction, and before the generation of the first oxide particles, a third gas flow of the organic-doped source precursor is introduced into the reaction chamber of the aforementioned homogeneous reaction, causing the metal corresponding to the organic-doped source precursor to dope into the nanoparticles obtained from the homogeneous reaction. Thus, the resulting oxide particles are metal-doped oxide particles from the organic-doped source precursor.
[0054] The metal in the aforementioned organic doped source precursor is a metal-doped oxide particle.
[0055] In some embodiments, the organic doped source precursor includes at least one of an organosilver source precursor, an organoaluminum source precursor, an organogold source precursor, and an organocopper source precursor.
[0056] The organic silver source precursor can be, for example, one or more of silver diethyldithiocarbamate, silver acetate, and silver diammine hydroxide. Preferably, the organic silver source precursor is one of silver diethyldithiocarbamate, silver acetate, and silver diammine hydroxide.
[0057] The organoaluminum source precursor can be, for example, one or more of triethylaluminum, triisobutylaluminum, and diethylaluminum chloride. Preferably, the organoaluminum source precursor can be one of triethylaluminum, triisobutylaluminum, and diethylaluminum chloride.
[0058] The organometallic precursor can be, for example, ammonium tetrachloroaurate and / or chloro(trialkylphosphine) gold. Preferably, the organometallic precursor can be one of ammonium tetrachloroaurate and chloro(trialkylphosphine) gold.
[0059] The organic copper source precursor can be, for example, copper acetate and / or copper diethyldithiocarbamate. Preferably, the organic copper source precursor is one of copper acetate and copper diethyldithiocarbamate.
[0060] Furthermore, the flow rate of the third airflow is less than or equal to half the flow rate of the first airflow. In some embodiments, the flow rate of the third airflow is 2-3 μL / min.
[0061] The aforementioned radio frequency power can be 580-620W, and the temperature can be 120-140℃, in order to avoid the transformation of the titanium dioxide crystal form from anatase to rutile, which would lead to a decrease in the hydrophilic self-cleaning performance of the multifunctional membrane.
[0062] Furthermore, to promote the generation of pure titanium dioxide particles or pure zinc oxide particles, the above homogeneous reaction is carried out in a reaction channel with a length greater than 50 cm and a curved arrangement along the length direction, so that the organotitanium source precursor or organozinc source precursor can react in a sufficiently long path under plasma bombardment and frequently collide on the channel wall of the reaction channel to generate the first oxide particles.
[0063] The first airflow and the third airflow can enter through the first air inlet and the third air inlet of the reaction channel (i.e., the reaction chamber), respectively. Both the first air inlet and the third air inlet are located near the beginning of the reaction channel.
[0064] Before the first gas flow enters through the inlet at the beginning of the reaction channel, a purge gas is introduced into the reaction channel to ensure that the gas in the reaction channel consists of the purge gas. This purge gas contains oxygen. For example, it can be pure oxygen or a mixture of gases with an oxygen content greater than 60% or higher. The gases in this mixture other than oxygen are inert gases that do not participate in the reaction, such as nitrogen or argon.
[0065] The first distance between the first air inlet and the beginning of the reaction channel and the second distance between the third air inlet and the beginning of the reaction channel may be the same or different.
[0066] In some embodiments, the first distance and the second distance are 3-4 cm.
[0067] In some embodiments, the structure of the reaction channel that is bent along the length direction may include one or more of the following: a ring structure, a spiral structure, and an "S"-shaped structure that are not connected end to end.
[0068] Step 102: The second gas flow of the organosilicon source precursor undergoes a heterogeneous reaction with the first oxide particles under the bombardment of plasma, generating silica particles on the surface of the first oxide particles to obtain the target particles.
[0069] In the target particles, the coating layer on the surface of the first oxide particles is composed of silicon dioxide particles.
[0070] Specifically, the reaction conditions for this heterogeneous reaction are the same as those for the homogeneous reaction in step 101, both being carried out at a temperature greater than or equal to 120°C, in an atmosphere containing oxygen, and with a plasma radio frequency power greater than or equal to 580W.
[0071] The aforementioned organosilicon source precursor can be, for example, at least one of hexamethyldisiloxane, methyl orthosilicate, and ethyl orthosilicate. The second gas stream can be obtained by high-temperature vaporization of the organosilicon source precursor.
[0072] Furthermore, the flow rate of the second airflow is less than that of the first airflow to generate small-sized silica particles, which form a coating on the surface of the first oxide particles. That is, on the surface of the first oxide particles, the silica particles are arranged to form a coating layer, thereby obtaining the target particles with a core-shell structure.
[0073] In some embodiments, the flow rate of the second gas flow is 5-8 μL / min.
[0074] Similar to the aforementioned homogeneous reaction channel, in order to promote heterogeneous reaction, so that the excited silicon ions in the organosilicon source precursor can be completely adsorbed on the surface of the pure first oxide particles (titanium dioxide particles or zinc oxide particles) to generate silica particles, a coating layer composed of silica particles is formed. The heterogeneous reaction can be carried out in a reaction channel with a length greater than 4-6 cm and bends along the length direction.
[0075] The homogeneous and heterogeneous reactions described above can be carried out in different reaction chambers under the same reaction conditions, such as atmosphere, or in the same reaction chamber.
[0076] Preferably, the reaction is carried out in the same reaction chamber. The first and third airflows enter from the first and third air inlets of the reaction channel, respectively, and the second airflow enters from the second air inlet. This second air inlet is on the same side as the outlet of the reaction channel, which is located at the tail end of the reaction channel. Taking a non-connected annular structure of the reaction channel as an example, the relative positions of the air inlets can be found in [reference needed]. Figure 2 .
[0077] Step 103: Deposit the target particles onto the surface of the target substrate to form a multifunctional film.
[0078] In the target substrate, the mass fraction of silicon dioxide is greater than or equal to 50%. Preferably, the mass fraction of silicon dioxide in the target substrate is greater than or equal to 70%.
[0079] This multifunctional membrane possesses at least the functions of hydrophilic self-cleaning and enhanced transparency.
[0080] Specifically, the target substrate can be, for example, glass. In this step, during chemical deposition on the surface of the target substrate, target particles can be introduced into the deposition chamber, where they are deposited under vacuum conditions of 4-6 × 10⁻⁴ Pa on the surface of the target substrate. The silica on the target particle surface then bonds with the silica on the surface to be deposited, allowing the target particles to bond with the surface through Si-O-Si bonds, forming a multifunctional film.
[0081] Furthermore, to ensure the effectiveness of chemical deposition, the surface to be deposited is a pretreated surface. This pretreatment includes at least one of ozone treatment, plasma cleaning, and ultraviolet grafting, thereby grafting hydrophilic hydroxyl groups onto the surface to be deposited to bond with silica, improving the adhesion between the surface to be deposited and the target particles, and thus enhancing the adhesion between the substrate and the multifunctional film.
[0082] Based on the same inventive concept, embodiments of this application provide an optical panel, which includes a multifunctional film prepared by the aforementioned method for preparing a multifunctional film.
[0083] The optical panel also includes a substrate. The substrate contains 50% or more silica, and one side of the surface to which the multifunctional film is attached contains superhydrophilic groups, resulting in a water droplet angle of <5°. The silicon atoms in the nanoparticle coating layer of the chemically deposited multifunctional film bond with silicon atoms on the substrate surface, resulting in a multifunctional film with strong adhesion to the substrate.
[0084] This optical panel can be used as an optical window. Furthermore, the optical panel can be a flat panel or a panel with a curved surface.
[0085] Based on the same inventive concept, embodiments of this application provide a chemical vapor deposition apparatus, which includes a deposition chamber and a reaction channel that is curved along its length.
[0086] The reaction channel is longer than 50cm to allow the precursor to react fully within it, and the curved design of the reaction channel is beneficial for the precursor to frequently impact the channel wall under the bombardment of plasma, further promoting the reaction.
[0087] The reaction channel includes a first air inlet, a second air inlet, and a third air inlet. The first and third air inlets are on the same side as the first air inlet of the reaction channel, and the second air inlet is on the same side as the outlet located at the rear end of the reaction channel.
[0088] The inlet at the front end is used to introduce purge gas and / or plasma, and the outlet at the rear end is used to introduce the target particles into the deposition chamber so that the target particles are deposited onto the substrate surface to be deposited.
[0089] The first, second, and third air inlets are all used to introduce precursor gases to generate target particles. The target particles are then introduced into the deposition chamber through the outlet of the aforementioned reaction channel and deposited on the substrate surface to be deposited.
[0090] Specifically, the first inlet is used to introduce the precursor gas of the inner layer material (i.e., the "core") of the target particle, the second inlet is used to introduce the precursor gas of the coating layer material of the target particle, and the third inlet is used to introduce the doping source gas.
[0091] In some embodiments, the distance between the first air inlet and the third air inlet and the head air inlet is 3-4 cm.
[0092] In some embodiments, the distance between the second air inlet and the outlet is 4-6 cm.
[0093] In some embodiments, the structure of the reaction channel may include one or more of the following: a ring structure, a spiral structure, and an "S"-shaped structure that are not connected end to end.
[0094] The following examples illustrate the preparation method of the multifunctional membrane described in steps 101-103: Example 1
[0095] S1. Select a flat glass substrate as the base material, ultrasonically clean it with deionized water and ethanol for 15 minutes, and after natural drying, place the clean substrate into the plasma cleaning machine for plasma cleaning for 10 minutes.
[0096] S2. Place the pretreated substrate into the chamber, set the radio frequency power to 600W and the reaction chamber temperature to 130℃, and then introduce oxygen to clean the chamber.
[0097] S3. Select a reaction channel with a non-connected shape as the reaction chamber for the precursor. Please refer to [reference needed]. Figure 2 Titanium isopropoxide is vaporized at high temperature and then introduced into the first inlet at a flow rate of 7 μL / min. Silver diethyldithiocarbamate is introduced into the second inlet at a flow rate of 2.3 μL / min.
[0098] S4. After introducing tetraisopropoxide titanium into the first air inlet for 1 minute, hexamethyldisiloxane is vaporized at high temperature and then introduced into the third air inlet at a flow rate of 6 μL / min to generate target particles.
[0099] S5. The target particles enter the vacuum deposition chamber through the outlet of the reaction channel, i.e. the connection between the reaction channel and the deposition chamber, and react on the surface of the glass substrate to form a multifunctional film, resulting in a glass plate with a multifunctional film on its surface.
[0100] Example 2
[0101] The difference from Example 1 is that the flow rate of silver diethyldithiocarbamate in S4 is 4 μL / min. All other steps and parameters are the same as in Example 1.
[0102] Comparative Example 1
[0103] The difference from Example 1 is that the flow rate of hexamethyldisiloxane introduced into the third air inlet in S4 is 7 μL / min.
[0104] Comparative Example 2
[0105] S1. Prepare a sol with a titanium dioxide / silica particle content of 1 mg / mL.
[0106] S2. A sol with a thickness of 120 nm is coated on the surface of a glass substrate and dried at 60°C to form a multifunctional film.
[0107] The following tests were conducted on this multifunctional membrane:
[0108] (1) The bandgap width of the multifunctional film on the glass plate surface was tested using an ultraviolet spectrophotometer. The X-axis was changed to electron volts (eV) and the Y-axis was changed to logF(R). The intercept of the tangent line of the curve with the horizontal axis is the bandgap width of the semiconductor.
[0109] (2) A water droplet angle test was performed on the multifunctional film on the glass plate surface to test the hydrophilic angle of the multifunctional film under visible light conditions. Then, the glass plate containing the multifunctional film was placed in a dark room for 168 hours, and a water droplet angle test was performed in the dark room to test the hydrophilic angle under no visible light conditions.
[0110] (3) Salt spray resistance test of the multifunctional membrane on the glass plate: The multifunctional membrane was placed in a salt spray chamber filled with 5% NaCl for 800 hours. Observe whether the multifunctional membrane peels off and test the hydrophilic angle of the multifunctional membrane.
[0111] (4) After immersing the glass plate connected to the multifunctional film in water for 100 hours, since the glass plate substrate thickness is uniform and the light transmittance is equal everywhere in the aforementioned embodiments and comparative examples, five points can be randomly selected to test the uniformity of light transmittance of the glass plate containing the multifunctional film, in order to characterize the thickness uniformity. The specific test method is as follows:
[0112] First, place the light source emitting the optical band to be measured on one side of the glass plate, and place the receiver of the optical band to be measured on the other side of the glass plate.
[0113] Then, the light passing through a glass plate with a multifunctional film on its surface is collected by a receiver, and the light intensity is determined. Based on this light intensity and the initial light intensity of the optical band emitted by the light source, the transmittance is calculated. With the light source and receiver fixed in place, the fixed support of the glass plate is moved, and the transmittance at different locations (5 collection points) is calculated.
[0114] The transmittance at the above 5 locations is grouped into pairs, and the rate of change of transmittance for each group is calculated. Finally, the average value of the rate of change of transmittance for each group is calculated, and this average value is the thickness change rate of the multifunctional film.
[0115] Table 1
[0116]
[0117] As can be seen, the hydrophilic angle was effectively reduced in the embodiment, thus ensuring its self-cleaning function. Furthermore, it exhibited good performance after salt spray testing, clearly demonstrating its superior density.
[0118] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.
Claims
1. A method for preparing a multifunctional membrane, characterized in that, include: Under conditions of a temperature greater than or equal to 120°C, an atmosphere containing oxygen, and a plasma radio frequency power greater than or equal to 580W, the first gas flow of the organic titanium source precursor or the organic zinc source precursor undergoes a homogeneous reaction under the bombardment of the plasma to generate first oxide particles; the homogeneous reaction is carried out in a reaction channel with a length greater than 50cm and a curved arrangement along the length direction. The second gas flow of the organosilicon source precursor undergoes a heterogeneous reaction with the first oxide particles under the bombardment of the plasma, generating silica particles on the surface of the first oxide particles to obtain target particles; wherein, in the target particles, the coating layer on the surface of the first oxide particles is composed of the silica particles. The target particles are deposited on the surface of the target substrate to form the multifunctional film; wherein, the mass fraction of silicon dioxide in the target substrate is greater than or equal to 50%.
2. The preparation method according to claim 1, characterized in that, The flow rate of the first airflow is 6-9 μL / min, and the flow rate of the second airflow is less than that of the first airflow.
3. The preparation method according to claim 1 or 2, characterized in that, Before obtaining the oxide particles, the process further includes: A third gas flow of the organic doped source precursor is introduced into the reaction channel of the homogeneous reaction, so that the metal corresponding to the organic doped source precursor is doped into the nanoparticles obtained by the homogeneous reaction; wherein the crystal structure of the metal is face-centered cubic. The obtained oxide particles include: The metal-doped oxide particles are obtained.
4. The preparation method according to claim 3, characterized in that, The organic doped source precursor includes at least one of organic silver source precursor, organic aluminum source precursor, organic gold source precursor, and organic copper source precursor.
5. The preparation method according to claim 3, characterized in that, The flow rate of the third airflow is less than or equal to half the flow rate of the first airflow.
6. The preparation method according to any one of claims 1-2, 4-5, characterized in that, The surface to be deposited is a pretreated surface; wherein the pretreatment includes at least one of ozone treatment, plasma cleaning and ultraviolet grafting.
7. The preparation method according to claim 1, characterized in that, The radio frequency power is less than or equal to 620W.
8. The preparation method according to claim 1, characterized in that, The temperatures of the homogeneous reaction and the heterogeneous reaction are less than or equal to 150°C.
9. An optical panel, characterized in that, include: The multifunctional membrane obtained by the preparation method according to any one of claims 1-8.
10. A chemical vapor deposition apparatus for implementing the preparation method according to any one of claims 1-8, characterized in that, include: A deposition chamber and a reaction channel curved along its length; the reaction channel is longer than 50 cm, and includes a first air inlet, a second air inlet, and a third air inlet; wherein... The first air inlet and the third air inlet are both on the same side as the first air inlet of the reaction channel, and the second air inlet is on the same side as the outlet located at the tail end of the reaction channel. The first air inlet, the second air inlet, and the third air inlet are all used to introduce precursor gas to generate target particles, which are then introduced into the deposition chamber through the outlet to be deposited on the substrate surface.
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