Film coating device, film and preparation method of film
By setting up a combination device of a rotating disk and a coating source in a vacuum chamber, and using grazing incidence film formation and ion source bombardment to alternately deposit thin film layers, the problems of poor quality and high cost caused by excessive thickness in the prior art are solved, and good scattering effect and hardness are achieved when the film thickness is less than 20μm.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-06
- Publication Date
- 2026-03-10
AI Technical Summary
In the prior art, excessively thick scattering films result in poor quality and high cost. Furthermore, coating on a transparent substrate increases the complexity of the manufacturing process, making it difficult to achieve good scattering effect and hardness when the film thickness is less than 20 μm.
A coating apparatus is used, in which a first-stage rotating disk and a second-stage rotating disk are set in a vacuum chamber, with the rotating plane of the second-stage rotating disk forming an angle θ with that of the first-stage rotating disk. The first and second film layers are deposited alternately by grazing incidence of the coating source and plasma bombardment by the ion source, and the film thickness is controlled within the range of several micrometers.
It achieves good scattering effect when the film thickness is less than 20μm, improves the hardness and adhesion of the film, reduces the coating cost, and simplifies the process.
Smart Images
Figure CN121629328A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of coating technology, and relates to a scattering thin film, and more particularly to a coating apparatus, a thin film, and a method for preparing the thin film. Background Technology
[0002] Existing filters and reflective films are mostly non-scattering or low-scattering films. Meanwhile, scattering films possess unique visual effects and show promising application prospects in areas such as electronic product decoration. In some cases, a noticeable scattering effect only occurs after coating when the substrate itself has a high roughness. Although a scattering effect can be achieved by coating the back of a transparent substrate and then applying ink to the film surface, this increases the complexity of the manufacturing process and limits its application scenarios. In some cases, a certain scattering effect can be generated through tilted incident deposition, but the film thickness needs to exceed 30μm, which leads to poor film quality and increases coating costs.
[0003] Therefore, there is a need for a coating apparatus, a thin film, and a method for preparing a thin film that has a thin film thickness, good film quality, and scattering effect. Summary of the Invention
[0004] The purpose of this invention is to provide a coating apparatus, a thin film, and a method for preparing a thin film. The coating apparatus and the method for preparing a thin film can achieve good scattering effect when the film thickness is <20μm, and can also make the obtained film have good hardness and adhesion, thus ensuring the quality of the film.
[0005] To achieve this objective, the present invention adopts the following technical solution:
[0006] In a first aspect, the present invention provides a coating apparatus, the coating apparatus comprising a vacuum chamber and a primary rotating disk, a secondary rotating disk and a coating source located within the vacuum chamber;
[0007] The primary rotating disk is disposed at the end of the vacuum chamber, and the axial direction of the rotation axis of the primary rotating disk extends along a first straight line, which passes through the end of the vacuum chamber.
[0008] At least one secondary rotating disk is provided. The secondary rotating disk is connected to the primary rotating disk through a support arm and can rotate around the first straight line with the primary rotating disk.
[0009] The rotation plane of the secondary rotating disk and the rotation plane of the primary rotating disk are at an angle θ, and the angle θ can be adjusted within a range of greater than 0° and less than 90°.
[0010] The secondary rotating disk is used to place the base;
[0011] The coating source is located on the side of the vacuum chamber away from the first-stage rotating disk, that is, the coating source is located on the side of the second-stage rotating disk away from the first-stage rotating disk.
[0012] In the coating apparatus provided by this invention, the secondary rotating disk is tilted towards the coating source, and the rotation plane of the secondary rotating disk forms an angle θ with the rotation plane of the primary rotating disk. The angle θ can be adjusted within a range greater than 0° and less than 90°. As a further preferred technical solution, during the rotation of the primary rotating disk, the value of the angle θ is fixed or periodically oscillates. If the value of the angle θ is fixed, then the angle θ needs to satisfy 65°≤θ<90°. If the angle θ oscillates periodically, then during one rotation of the primary rotating disk, the time when the angle θ ≥ 65° should account for more than 3 / 4 of the total time used for one rotation. Alternatively, during N (N>1) rotations of the primary rotating disk, the total time when the angle θ ≥ 65° should account for more than 3 / 4 of the total time used for N rotations. If the angle θ does not oscillate periodically, during N (N≥1) rotations of the primary rotating disk, the total time when the angle θ ≥ 65° should account for more than 3 / 4 of the total time used for N rotations.
[0013] When using the coating apparatus provided by this invention, the primary rotating disk rotates, driving the secondary rotating disk connected to it to revolve around the central axis, while the secondary rotating disk rotates on its own axis, ensuring the uniformity of the coating thickness. This invention does not further limit the rotation structure of the primary and secondary rotating disks, as long as the revolution and rotation of the secondary rotating disk can be achieved.
[0014] In this invention, the primary rotating disk is disposed at the end of the vacuum chamber, preferably at the top of the vacuum chamber. In this case, the axial direction of the rotation axis of the primary rotating disk extends along a first straight line, which passes through the top of the vacuum chamber.
[0015] As a preferred technical solution, the rotation plane of the primary rotating disk is parallel to the top and bottom of the vacuum chamber. This invention makes the rotation plane of the secondary rotating disk form an angle θ with the rotation plane of the primary rotating disk, so that the film is formed by grazing incidence during coating. This allows the incident angle to change over time during film deposition and exhibits a certain periodicity, increasing the proportion of large angles and thus generating scattering. Furthermore, it ensures that good scattering effect can be achieved with a film thickness of only a few micrometers.
[0016] Preferably, the first straight line coincides with the central axis of the vacuum chamber.
[0017] Furthermore, the present invention can improve the hardness and adhesion of the resulting scattering film by setting the coating source.
[0018] In this invention, there is one primary rotating disk and at least one secondary rotating disk, for example, one, two, three, four, five or six, but not limited to the listed values. Other unlisted values within the range are also applicable.
[0019] Preferably, the maximum distance between the rotation center of the secondary rotating disk and the first straight line is 'a'; it can be understood that the rotation center of the secondary rotating disk refers to the rotation of the secondary rotating disk.
[0020] The maximum distance from the center of the coating source to the first straight line is c;
[0021] Then a and c satisfy a>c.
[0022] In this invention, it is necessary to control the distance between the coating source and the first straight line to be less than the distance between the secondary rotating disk and the first straight line. If a ≤ c, the coating source will be located outside the secondary rotating disk, resulting in unsuccessful coating. However, if the difference between a and c is large, it is not conducive to a sufficiently large change in the incident angle during the coating process. Therefore, as a preferred technical solution, the difference between a and c is less than 50 mm, for example, it can be 50 mm, 45 mm, 40 mm, 35 mm, 30 mm, 25 mm, or 20 mm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0023] Preferably, a ≤ 300 mm, for example, it can be 160 mm, 170 mm, 190 mm, 210 mm, 220 mm, 260 mm, 280 mm or 300 mm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0024] Preferably, c ≤ 278 mm, for example, it can be 150 mm, 160 mm, 180 mm, 200 mm, 240 mm, 250 mm, 270 mm or 278 mm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0025] Preferably, the distance between the center of the secondary rotating disk and the plane where the coating source is located is b.
[0026] When the value of b is too small, it is not conducive to improving the coating quality; while when the value of b is too large, it is not conducive to improving the evaporation efficiency. As a preferred technical solution of the present invention, the value of b satisfies 600mm≤b≤20000mm, for example, it can be 600mm, 800mm, 900mm, 980mm, 1000mm, 3000mm, 5000mm, 8000mm, 10000mm, 15000mm or 20000mm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0027] Preferably, the coating source includes a first coating source and a second coating source.
[0028] Preferably, the distances between the first coating source and the second coating source and the first straight line are equal; more preferably, the first coating source and the second coating source are symmetrically arranged along the first straight line.
[0029] Understandably, the first coating source and the second coating source each have their own a and c values, that is, the a and c values are for the coating source and the secondary rotating disk in the corresponding state; the "corresponding state" here can be the state in which the coating source and the secondary rotating disk are closest to each other.
[0030] Preferably, the coating apparatus includes an ion source, which is located in the vacuum chamber on the side away from the primary rotating disk.
[0031] Preferably, the central axis of the ion source coincides with the first straight line.
[0032] Secondly, the present invention provides a method for preparing a thin film, the method comprising the following steps:
[0033] The coating apparatus described in the first aspect is provided;
[0034] The thin film is obtained by alternately depositing a first film layer and a second film layer on the surface of a substrate.
[0035] The average thickness of the first single film layer is 76.8-85.1 nm;
[0036] The average thickness of a single second film layer is 110.6-123.2 nm;
[0037] The total thickness of the scattering film is <20μm;
[0038] The refractive index of the first film layer alone is greater than the refractive index of the second film layer alone.
[0039] The preparation method provided by the present invention uses the coating apparatus provided in the first aspect to deposit the first film layer and the second film layer. By making the incident angle of the coating source larger, the scattering effect of the obtained film is improved, and the film can be controlled at a thickness of several micrometers, which effectively overcomes the problem of soft film and easy peeling caused by excessive thickness.
[0040] In this invention, the thickness of a single first film layer is 76.8-85.1 nm, for example, it can be 76.8 nm, 78 nm, 80 nm, 81 nm, 82 nm, 84 nm or 85.1 nm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0041] In this invention, the thickness of a single second film layer is 110.6-123.2 nm, for example, it can be 110.6 nm, 112 nm, 115 nm, 118 nm, 120 nm or 123.2 nm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0042] The total thickness of the film is <20μm, for example, it can be 3.78μm, 4μm, 5μm, 6μm, 8μm, 10μm, 12μm, 15μm, 16μm, 18μm or 19μm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0043] The thicker the film, the better the scattering effect. However, excessively thick films are detrimental to improving film adhesion and also increase coating costs; conversely, excessively thin films will reduce the scattering of the resulting film. The film provided by this invention only needs to have a total thickness of less than 20 μm to achieve good scattering effects.
[0044] Preferably, the coating apparatus includes an ion source; the process of coating the first and second films includes a process of plasma bombardment of the substrate.
[0045] Preferably, the coating apparatus includes a first coating source and a second coating source;
[0046] The first coating source is used to deposit the first film layer;
[0047] The second coating source is used to deposit the second film layer.
[0048] Preferably, the composition of the first film layer includes any one or a combination of at least two of Ti3O5, Ta2O5, Nb2O5 or H4. Typical but non-limiting combinations include combinations of Ti3O5 and Ta2O5, combinations of Nb2O5 and H4, combinations of Ti3O5, Ta2O5 and Nb2O5, or combinations of Ti3O5, Ta2O5, Nb2O5 and H4.
[0049] The "H4" refers to an oxide whose main component is lanthanum titanate, which has the characteristics of high refractive index and low absorption rate.
[0050] Preferably, the composition of the second film layer includes SiO2.
[0051] For example, the rotation speed of the primary rotating disk during plating is 8-12 rpm, such as 8 rpm, 9 rpm, 10 rpm, 11 rpm or 12 rpm, but not limited to the listed values. Other unlisted values within the range are also applicable.
[0052] Preferably, the rotation speed of the secondary rotating disk during plating is 28-32 rpm, for example, it can be 28 rpm, 29 rpm, 30 rpm, 31 rpm or 32 rpm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0053] Preferably, the film formation rate of the first film layer is For example, it could be or However, this does not apply to all unlisted values within the range of values.
[0054] This invention does not further limit the film-forming conditions of the first film layer, as long as the film-forming rate is satisfied. That's all.
[0055] Preferably, the film formation rate of the second film layer is For example, it could be or However, this does not apply to all unlisted values within the range of values.
[0056] This invention does not further limit the film-forming conditions of the second film layer, as long as the film-forming rate is satisfied. That's all.
[0057] Preferably, when depositing the first film layer, the parameters of the ion source plasma bombardment are: Beam current of 1150-1250mA, Beam voltage of 1150-1250V, accelerating voltage of 550-650V, E / B (the ratio of neutralizer current to beam current) of 140-160%, first gas flow rate of 55-65sccm, second gas flow rate of 8-12sccm, and third gas flow rate of 6-10sccm.
[0058] When the first film layer is deposited by grazing vapor deposition, the first gas is O2, the second gas is Ar, and the third gas is Ar.
[0059] When depositing the first film layer, the beam current is 1150-1250mA, for example, it can be 1150mA, 1160mA, 1180mA, 1200mA, 1220mA or 1250mA, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0060] When depositing the first film layer, the beam voltage is 1150-1250V, for example, it can be 1150V, 1180V, 1200V, 1220V or 1250V, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0061] When depositing the first film layer, the accelerating voltage is 550-650V, for example, it can be 550V, 560V, 580V, 600V, 630V or 650V, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0062] When depositing the first film layer, the E / B (the ratio of neutralizer current to beam current) is 140-160%, for example, it can be 140%, 145%, 150%, 155% or 160%, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0063] When depositing the first film layer, the first gas flow rate is 55-65 sccm, for example, it can be 55 sccm, 58 sccm, 60 sccm, 63 sccm or 65 sccm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0064] When depositing the first film layer, the second gas flow rate is 8-12 sccm, for example, it can be 8 sccm, 9 sccm, 10 sccm, 11 sccm or 12 sccm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0065] When depositing the first film layer, the third gas flow rate is 6-10 sccm, for example, it can be 6 sccm, 7 sccm, 8 sccm, 9 sccm or 10 sccm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0066] Preferably, when depositing the second film layer, the parameters of the ion source plasma bombardment are: Beam current of 850-950mA, Beam voltage of 850-950V, accelerating voltage of 550-650V, E / B (the ratio of neutralizer current to Beam current) of 140-160%, first gas flow rate of 45-55sccm, and third gas flow rate of 6-10sccm.
[0067] When the second film layer is deposited by grazing vapor deposition, the first gas is O2 and the third gas is Ar.
[0068] When depositing the second film layer, the beam current is 850-950mA, for example, it can be 850mA, 860mA, 880mA, 900mA, 930mA or 950mA, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0069] When depositing the second film layer, the beam voltage is 850-950V, for example, it can be 850V, 860V, 880V, 900V, 920V, 930V or 950V, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0070] When depositing the second film layer, the accelerating voltage is 550-650V, for example, it can be 550V, 560V, 580V, 600V, 630V or 650V, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0071] When depositing the second film layer, the E / B (the ratio of neutralizer current to beam current) is 140-160%, for example, it can be 140%, 145%, 150%, 155% or 160%, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0072] When depositing the second film layer, the first gas flow rate is 45-55 sccm, for example, it can be 45 sccm, 48 sccm, 50 sccm, 52 sccm or 55 sccm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0073] When depositing the second film layer, the third gas flow rate is 6-10 sccm, for example, it can be 6 sccm, 7 sccm, 8 sccm, 9 sccm or 10 sccm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0074] In this invention, the first gas and the second gas are introduced into an ion source, which is used to provide O2. 2+ and Ar + A third gas is introduced into a neutralizer used with the ion source; the neutralizer provides electrons. In this invention, the O2 emitted by the ion source... 2+ and Ar + Electrons emitted from the ion source can combine to form neutral gas molecules with kinetic energy. These high-speed neutral gas molecules can continuously bombard the membrane, making the membrane more compact.
[0075] As a preferred embodiment of the preparation method described in the second aspect of the present invention, the preparation method includes the following steps:
[0076] (1) Load the cleaned substrate onto the secondary rotating disk;
[0077] (2) Evacuate the vacuum chamber and adjust the absolute pressure to ≤0.001Pa; and preheat the substrate to 95-105℃ when evacuating; during the evacuation process, the rotation speed of the first-stage rotating disk is 2-4 rpm and the rotation speed of the second-stage rotating disk is 8-12 rpm.
[0078] (3) When the temperature and absolute pressure in step (2) reach the process requirements, start the ion source to clean the substrate. During cleaning, the rotation speed of the first-stage rotating disk is 8-12 rpm, the rotation speed of the second-stage rotating disk is 28-32 rpm, and the cleaning time is 110-130s. The operating parameters of the ion source during cleaning are: Beam current is 850-950mA, Beam voltage is 850-950V, acceleration voltage is 550-650V, E / B (the ratio of neutralizer current to Beam current) is 140-160%, the first gas flow rate is 45-55sccm, and the third gas flow rate is 6-10sccm. The first gas is O2 and the third gas is Ar.
[0079] (4) After the cleaning described in step (3) is completed, the first coating source and the second coating source are used alternately for vapor deposition to form the first film layer and the second film layer on the surface of the substrate in turn; the vapor deposition is accompanied by plasma bombardment from the ion source.
[0080] The rotation speed of the primary rotating disk during vapor deposition is 8-12 rpm, and the rotation speed of the secondary rotating disk is 28-32 rpm; the film formation rate of the first film layer is... The film formation rate of the second film layer is
[0081] When depositing the first film layer, the parameters of the ion source plasma bombardment are as follows: Beam current is 1150-1250mA, Beam voltage is 1150-1250V, accelerating voltage is 550-650V, E / B (the ratio of neutralizer current to beam current) is 140-160%, first gas flow rate is 55-65sccm, second gas flow rate is 8-12sccm, and third gas flow rate is 6-10sccm; wherein the first gas is O2, the second gas is Ar, and the third gas is Ar.
[0082] When depositing the second film layer, the parameters of the ion source plasma bombardment are as follows: Beam current is 850-950mA, Beam voltage is 850-950V, accelerating voltage is 550-650V, E / B (the ratio of neutralizer current to beam current) is 140-160%, first gas flow rate is 45-55sccm, and third gas flow rate is 6-10sccm; wherein the first gas is O2 and the third gas is Ar.
[0083] (5) After obtaining the required thickness of the film, turn off the first coating source, the second coating source and the ion source, cool down, and reduce the speed of the first rotating disk to 2-4 rpm and the speed of the second rotating disk to 8-12 rpm. After 8-12 minutes, stop the rotation of the first rotating disk and the second rotating disk, fill the vacuum chamber with air to the atmospheric state, and complete the preparation of the film.
[0084] The substrate preheating temperature in step (2) is 95-105℃, for example, it can be 95℃, 96℃, 98℃, 100℃, 103℃ or 105℃, but is not limited to the listed values. Other unlisted values within the range are also applicable. During grazing deposition, the substrate temperature is maintained at the preheating temperature.
[0085] During the vacuuming process described in step (2), the rotation speed of the primary rotating disk is 2-4 rpm, for example, it can be 2 rpm, 2.5 rpm, 3 rpm, 3.5 rpm or 4 rpm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0086] During the vacuuming process described in step (2), the rotation speed of the secondary rotating disk is 8-12 rpm, for example, it can be 8 rpm, 9 rpm, 10 rpm, 11 rpm or 12 rpm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0087] During the cleaning process described in step (3), the rotation speed of the primary rotating disk is 8-12 rpm, for example, it can be 8 rpm, 9 rpm, 10 rpm, 11 rpm or 12 rpm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0088] During the cleaning process described in step (3), the rotation speed of the secondary rotating disk is 28-32 rpm, for example, it can be 28 rpm, 29 rpm, 30 rpm, 31 rpm or 32 rpm, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0089] The cleaning time in step (3) is 110-130s, for example, it can be 110s, 115s, 120s, 125s or 130s, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0090] Thirdly, the present invention provides a thin film comprising alternatingly deposited first and second film layers.
[0091] The average thickness of the first single film layer is 76.8-85.1 nm;
[0092] The average thickness of a single second film layer is 110.6-123.2 nm;
[0093] The total thickness of the film is <20 μm;
[0094] The refractive index of the first film layer alone is greater than the refractive index of the second film layer alone.
[0095] The scattering of the thin film is 50% or more, for example, it can be 50%, 60%, 70%, 80%, 80.4%, 90% or 99%, but is not limited to the listed values. Other unlisted values within the range are also applicable, preferably 80% or more.
[0096] Preferably, the total thickness of the film is <20μm, for example, it can be 3.78μm, 4μm, 5μm, 6μm, 8μm, 10μm, 12μm, 15μm, 16μm, 18μm or 19μm, but is not limited to the listed values, and other unlisted values within the range are also applicable.
[0097] Preferably, the thin film described in the third aspect is prepared by the preparation method described in the second aspect.
[0098] Compared with the prior art, the present invention has the following beneficial effects:
[0099] The coating apparatus provided by the present invention includes a vacuum chamber and a primary rotating disk, a secondary rotating disk, and a coating source located within the vacuum chamber. The present invention achieves grazing incidence during coating by making the rotation plane of the secondary rotating disk form an angle θ with the rotation plane of the primary rotating disk. The film layer has certain periodic characteristics during deposition, thereby producing the desired scattering effect, increasing the proportion of large angles, and thus generating scattering, requiring only a film thickness of a few micrometers. Attached Figure Description
[0100] Figure 1 This is a schematic diagram of the coating apparatus provided in Example 1;
[0101] Figure 2 The image shows the scattering effect of the thin film obtained in Application Example 1 against a white background in an indoor environment.
[0102] Figure 3 The image shows the scattering effect of the thin film obtained in Application Example 1 against a black background in an indoor environment.
[0103] Figure 4 The image shows the scattering effect of the thin film obtained in Application Example 1 against a white background in a sunlight environment.
[0104] Figure 5 The image shows the scattering effect of the thin film obtained in Application Example 1 against a black background in a sunlight environment.
[0105] Among them, 1 is a vacuum chamber; 2 is a first coating source; 3 is a second coating source; 4 is an ion source; 5 is a first-stage rotating disk; and 6 is a second-stage rotating disk. Detailed Implementation
[0106] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.
[0107] To clearly illustrate the technical solution of the present invention, the substrate in the specific embodiment is K9 hemispherical polished glass, and a scattering thin film is deposited on the convex surface of the K9 hemispherical polished glass. The above limitation on the substrate is only for the purpose of clearly illustrating the technical solution of the present invention and is not considered as a further limitation of the present invention.
[0108] In a specific embodiment of the present invention, whether or not the material is demolded is determined by a 100-grid test.
[0109] The definition of scattering degree in the specific embodiments of the present invention is as follows:
[0110] Scattering degree = (Second reflected light scattering degree parameter / First reflected light scattering degree parameter) × 100%;
[0111] The second reflected light scattering parameter and the first reflected light scattering parameter are derived from the second reflected light information and the first reflected light information, respectively. The first reflected light information includes diffuse reflection and specular reflection of the thin film to be detected, and the second reflected light information is the part of the first reflected light information excluding the contribution of specular reflection.
[0112] The method for measuring scattering is as follows:
[0113] (a) The first reflected light information of the thin film was obtained using a Konica Minolta colorimeter, the first reflected light information including diffuse reflection and specular reflection;
[0114] (b) Obtain the second reflected light information of the thin film using a Konica Minolta colorimeter. The second reflected light information includes diffuse reflection, i.e., excluding specular reflection.
[0115] The light source used in the test was D65;
[0116] (c) Extract the first reflected light scattering parameter and the second reflected light scattering parameter from the first reflected light information and the second reflected light information, respectively. The first reflected light scattering parameter and the second reflected light scattering parameter are the brightness (L). * );
[0117] The first reflected light scattering parameter (brightness L) is extracted from the first reflected light information and the second reflected light information, respectively. * ) and second reflected light scattering parameter (brightness L) * The method can refer to the data processing method of the Konica Minolta colorimeter, which involves calculations of reflectance data, light source function and apparent function in the visible light range, which will not be detailed here;
[0118] (d) Calculate the scattering degree, where the scattering degree = second reflected light scattering degree parameter / first reflected light scattering degree parameter.
[0119] Example 1
[0120] This embodiment provides a method such as Figure 1 The coating apparatus shown includes a vacuum chamber 1 and a primary rotating disk 5, a secondary rotating disk 6, a first coating source 2, a second coating source 3, and an ion source 4 located within the vacuum chamber 1.
[0121] The first-stage rotating disk 5 is located at the top of the vacuum chamber 1. The axial direction of the rotation axis of the first-stage rotating disk 5 extends along the first straight line, which passes through the top of the vacuum chamber 1. The rotation plane of the first-stage rotating disk 5 is parallel to the top and bottom of the vacuum chamber 1.
[0122] The primary rotating disk 5 is connected to six secondary rotating disks 6 via a support arm; the secondary rotating disks 6 are tilted toward the ion source 4, and the plane of rotation of the secondary rotating disk 6 is at an angle θ with the plane of rotation of the primary rotating disk 5. The angle θ can be adjusted within a range of greater than 0° and less than 90°.
[0123] Secondary rotating disk 6 is used to place the base;
[0124] The first coating source 2, the second coating source 3, and the ion source 4 are respectively located on the side of the vacuum chamber 1 away from the first-stage rotating disk 5.
[0125] Ion source 4 is located in vacuum chamber 1 on the side away from primary rotating disk 5, and the central axis of ion source 4 coincides with the first straight line;
[0126] The distances between the first coating source 2 and the second coating source 3 and the first straight line are equal; more preferably, the first coating source 2 and the second coating source 3 are symmetrically arranged along the first straight line;
[0127] The maximum distance between the first coating source 2 and the first straight line is c, where c is 278mm.
[0128] The maximum distance between the secondary rotating disk 6 and the first straight line is a, where a is 300mm.
[0129] The distance between the center of the secondary rotating disk 6 and the plane where the coating source is located is b, where b is 980mm.
[0130] Application Example 1
[0131] This application example provides a method for preparing a thin film, which is carried out in the coating apparatus provided in Example 1, and includes the following steps:
[0132] (1) Load a clean substrate (5B in cross-cut test, scattering of 1.5%) onto a secondary rotating disk;
[0133] The material of the first evaporation source is Ti3O5, and the material of the second evaporation source is SiO2;
[0134] (2) Evacuate the vacuum chamber and adjust the absolute pressure to 0.001Pa; and preheat the substrate to 100°C during the evacuation process; the rotation speed of the first-stage rotating disk is 3 rpm and the rotation speed of the second-stage rotating disk is 10 rpm during the evacuation process.
[0135] (3) When the temperature and absolute pressure in step (2) reach the process requirements, start the ion source to clean the substrate. During cleaning, the rotation speed of the first-stage rotating disk is 10 rpm, the rotation speed of the second-stage rotating disk is 30 rpm, and the cleaning time is 120 s. The operating parameters of the ion source during cleaning are: Beam current is 900 mA, Beam voltage is 900 V, acceleration voltage is 600 V, E / B (the ratio of neutralizer current to Beam current) is 150%, the first gas flow rate is 50 sccm, and the third gas flow rate is 8 sccm. The first gas is O2 and the third gas is Ar.
[0136] (4) After cleaning in step (3), the first coating source and the second coating source are used alternately for vapor deposition to form the first film layer and the second film layer on the surface of the substrate in turn; the vapor deposition is accompanied by plasma bombardment from the ion source.
[0137] The angle θ between the rotation plane of the second-stage rotating disk and the rotation plane of the first-stage planetary disk varies with the revolution period of the second-stage planetary disk: during one revolution, θ increases from 80° to 89°, and then decreases from 89° to 80°.
[0138] The rotation speed of the first-stage rotating disk during vapor deposition is 10 rpm, and the rotation speed of the second-stage rotating disk is 30 rpm; the film formation rate of the first film layer is... The film formation rate of the second film layer is
[0139] The average thickness of a single first film layer is 81 nm, and the average thickness of a single second film layer is 119 nm; the total number of layers, including the first and second films, is 38, so the total thickness of the scattering film is 3800 nm.
[0140] During the deposition of the first film layer, the parameters of the ion source plasma bombardment are as follows: Beam current is 1200mA, Beam voltage is 1200V, accelerating voltage is 600V, E / B (the ratio of neutralizer current to beam current) is 150%, first gas flow rate is 60sccm, second gas flow rate is 10sccm, and third gas flow rate is 8sccm; wherein the first gas is O2, the second gas is Ar, and the third gas is Ar.
[0141] When depositing the second film layer, the parameters of the ion source plasma bombardment are as follows: Beam current is 900mA, Beam voltage is 900V, accelerating voltage is 600V, E / B (the ratio of neutralizer current to beam current) is 150%, the first gas flow rate is 50sccm, and the third gas flow rate is 8sccm; wherein the first gas is O2 and the third gas is Ar.
[0142] (5) After obtaining the required thickness of the scattering film, turn off the first coating source, the second coating source and the ion source, cool down, and reduce the speed of the first rotating disk to 3 rpm and the speed of the second rotating disk to 10 rpm. After 10 min, stop the rotation of the first rotating disk and the second rotating disk, fill the vacuum chamber with air to the atmospheric state, and complete the preparation of the film.
[0143] The scattering effect of the thin film obtained in this application example under a white background in an indoor environment is shown in the following figure. Figure 2 As shown in the figure, the left side of the image is the substrate after coating, and the right side is the substrate without coating.
[0144] The scattering effect of the thin film obtained in this application example under a black background in an indoor environment is shown in the following figure. Figure 3 As shown in the figure, the left side of the image is the substrate after coating, and the right side is the substrate without coating.
[0145] The scattering effect of the thin film obtained in this application example under a white background in a sunlight environment is shown in the following figure. Figure 4 As shown in the figure, the left side of the image is the substrate after coating, and the right side is the substrate without coating.
[0146] The scattering effect of the thin film obtained in this application example under a black background in a sunlight environment is shown in the following figure. Figure 5 As shown in the figure, the left side of the image is the substrate after coating, and the right side is the substrate without coating.
[0147] The thin film obtained in this application example has a cross-cut density (CCD) result of 5B and a scattering of 84%.
[0148] In Application Examples 2 to 23, except for the thickness of the single first film layer, the thickness of the single second film layer, the total thickness of the film, the material of the first film layer, the material of the second film layer, and the time proportion of the angle θ between the rotation plane of the second-stage rotating disk and the rotation plane of the first-stage planetary disk, as shown in Table 1, everything else is the same as in Application Example 1.
[0149] Table 1
[0150]
[0151]
[0152] In summary, the coating apparatus provided by this invention includes a vacuum chamber and a primary rotating disk, a secondary rotating disk, a first coating source, a second coating source, and an ion source located within the vacuum chamber. The preparation apparatus system, through the arrangement of the primary and secondary rotating disks, ensures that the deposition of the thin film during evaporation exhibits a certain periodicity while the incident angle changes over time, thereby producing the desired scattering effect. Furthermore, the thickness of the scattering film required to produce the desired scattering is only a few micrometers. In addition, by configuring the coating source, this invention not only obtains thin films with high scattering rates but also improves the hardness and adhesion of the resulting film, thus enhancing the film quality.
[0153] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.
Claims
1. A coating apparatus, characterized by comprising: The coating device comprises a vacuum chamber, a first rotating disc, a second rotating disc and a coating source in the vacuum chamber; The first rotating disc is arranged at the end of the vacuum chamber, and the rotation axis of the first rotating disc extends along a first straight line direction, and the first straight line passes through the end of the vacuum chamber; At least one second rotating disc is arranged, and the second rotating disc is connected to the first rotating disc through a support arm and can rotate around the first straight line with the first rotating disc; The rotation plane of the second rotating disc and the rotation plane of the first rotating disc form an angle θ, and the angle θ can be adjusted in a range greater than 0° and less than 90°; The second rotating disc is used for placing a substrate; The coating source is arranged on the side of the vacuum chamber away from the first rotating disc.
2. The coating apparatus according to claim 1, wherein The maximum distance between the rotation center of the second rotating disc and the first straight line is a; The maximum distance between the center of the coating source and the first straight line is c; Then a and c satisfy a>c; Preferably, the difference between a and c is less than 50 mm.
3. The coating apparatus according to claim 1 or 2, characterized in that, The distance between the center of the second rotating disc and the plane where the coating source is located is b; The value of b satisfies 600 mm≤b≤20000 mm.
4. The coating apparatus of claim 1, wherein The coating source comprises a first coating source and a second coating source; Preferably, the distance between the first coating source and the first straight line is equal to the distance between the second coating source and the first straight line.
5. The coating apparatus of claim 1, wherein The coating device comprises an ion source arranged on the side of the vacuum chamber away from the first rotating disc; Preferably, the central axis of the ion source coincides with the first straight line.
6. A method of producing a film, characterized by, The preparation method comprises the following steps: The coating device of any one of claims 1-5 is arranged; First film layers and second film layers are alternately coated on the surface of the substrate to obtain the thin film; The thickness of a single first film layer is 10-150 nm; The thickness of a single second film layer is 10-250 nm; The total thickness of the thin film is less than 20 μm; The refractive index of a single first film layer is greater than the refractive index of a single second film layer.
7. The production method according to claim 6, wherein The average thickness of a single first film layer is 76.8-85.1 nm, and the average thickness of a single second film layer is 110.6-123.2 nm; Preferably, the coating device comprises an ion source; In the process of coating the first film layers and the second film layers, the process of plasma bombarding the substrate is included; Preferably, the coating device comprises a first coating source and a second coating source; The first coating source is used for coating the first film layers; The second coating source is used for coating the second film layers.
8. The production method according to claim 6 or 7, characterized by, The composition of the first film layers comprises any one or a combination of at least two of Ti3O5, Ta2O5, Nb2O5 or H4; Preferably, the composition of the second film layers comprises SiO2.
9. A film, characterized by, The thin film comprises alternately arranged first film layers and second film layers, and the refractive index of a single first film layer is greater than the refractive index of a single second film layer; The scattering degree of the thin film is more than 50%, preferably more than 80%.
10. The film of claim 9, wherein, The scattering degree of the thin film is more than 80%; Preferably, the composition of the first film layers comprises any one or a combination of at least two of Ti3O5, Ta2O5, Nb2O5 or H4; Preferably, the composition of the second film layer comprises SiO2; Preferably, the total thickness of the thin film is < 20 μm.