CN117947380A - Technological method for improving adhesion of aluminum film and dielectric film layer in magnetron sputtering high-reflectivity aluminum - Google Patents
Technological method for improving adhesion of aluminum film and dielectric film layer in magnetron sputtering high-reflectivity aluminum Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000002310 reflectometry Methods 0.000 title claims abstract description 41
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title abstract description 112
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Abstract
The invention discloses a process method for improving the adhesive force of an aluminum film and a dielectric film layer in magnetron sputtering high-reflectivity aluminum, wherein an AlN film is prepared between the high-reflectivity aluminum Al film and the dielectric film. The preparation method of the AlN film comprises the following steps: an AlN film layer is formed by nitriding the Al film surface of the substrate on which the Al film has been plated or an AlN film is plated on the Al film surface of the substrate on which the Al film has been plated. According to the invention, aluminum nitride is arranged between the high-reflection aluminum metal aluminum film and the dielectric film to form a connecting layer and a buffer layer, so that the adhesive force between the high-reflection aluminum layers is improved, and the optical performance of the high-reflection aluminum is not influenced; during preparation, aluminum nitride can be directly plated on the surface of the metal aluminum film or the surface of the metal aluminum film is nitrided by an ion source to form aluminum nitride, and the required plating equipment can adopt the existing equipment, so that the processing is simple and the cost is low.
Description
Technical Field
The invention belongs to the technical field of film coating, and particularly relates to a process method for improving the adhesive force of an aluminum film and a dielectric film layer in magnetron sputtering high-reflectivity aluminum.
Background
Compared with other film forming modes such as evaporation, the magnetron sputtering metal aluminum film has higher stability, higher film forming efficiency and better repeatability, and is more beneficial to large-scale industrialization and large-size products. The difficulty of independently plating the metal aluminum film is very high when the reflectivity is more than 90, and in order to obtain higher reflectivity, the metal aluminum film is required to be overlapped with a plurality of dielectric films to improve the reflectivity so as to meet the requirement of high reflectivity aluminum, and after a proper dielectric film stack is overlapped, the reflectivity can be up to more than 98. In addition, the single-layer metal aluminum film is easy to oxidize in the use process, the corresponding weather resistance such as salt spray resistance, high temperature and high humidity resistance and the like cannot be exceeded by tests, and after the dielectric film layer is overlapped, the reflectivity is greatly improved, meanwhile, the metal aluminum layer is effectively protected, and the weather resistance such as salt spray resistance, high temperature and high humidity resistance and the like can be improved. The plating of the high-reflection aluminum film can be applied to various substrates, such as PCs, glasses, metals, ceramics and the like. The high-reflection aluminum film is widely applied, such as PC+high-reflection aluminum is applied to head-up display equipment in new energy automobiles, and the large-angle high-reflection film layer can effectively transfer instrument information and the like onto a front windshield, so that the use feeling of a user is greatly improved. For another example, glass+high-reflectivity aluminum is used in smart electrochromic assemblies such as smart rearview mirrors.
However, when the magnetron sputtering metal aluminum film is overlapped with the dielectric film, the magnetron sputtering film is relatively compact, the stress is larger, and the adhesion between the two film layers is poorer due to factors such as larger thermal expansion coefficient deviation of the metal aluminum film and the dielectric film, particularly the higher the reflectivity of the metal aluminum is, the poorer the adhesion between the metal aluminum film and the dielectric film overlapped with the metal aluminum film is.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a process method for improving the adhesive force of an aluminum film and a dielectric film layer in magnetron sputtering high-reflection aluminum, wherein aluminum nitride is arranged between a metal aluminum film and the dielectric film of the high-reflection aluminum to form a connecting layer and a buffer layer, so that the adhesive force among all layers of the high-reflection aluminum is improved without affecting the optical performance of the high-reflection aluminum; during preparation, aluminum nitride can be directly plated on the surface of the metal aluminum film or the surface of the metal aluminum film is nitrided by an ion source to form aluminum nitride, and the required plating equipment can adopt the existing equipment, so that the processing is simple and the cost is low.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The technological process of raising the adhesion between the Al film and the dielectric film in the magnetron sputtered high-reflectivity aluminum layer prepares AlN film between the Al film and the dielectric film.
As a further improvement of the above technical scheme:
The preparation method of the AlN film comprises the following steps: an AlN film layer is formed by nitriding the Al film surface of the substrate on which the Al film has been plated.
Ar and N 2,N2 are introduced into an ion source area to be ionized into ions, the substrate plated with the Al film is fed into the ionization area, and N 3- of the ionization area is used for nitriding the surface of the Al film to generate AlN.
The ion source is an ICP ion source or an anode layer ion source.
When the ICP ion source is used, the RF power source is the power source of the ICP ion source, the RF power source power is 0.5-10 KW, the Ar flow is 20-1000 sccm, the N 2 flow is 10-2000 sccm, and the nitriding treatment time is 10-1800 s.
When the anode layer ion source is used, the voltage is 500-3000V, the Ar flow is 10-1000 sccm, the N 2 flow is 10-2000 sccm, and the nitriding time is 10-1800 s.
The preparation method of the AlN film comprises the following steps: an AlN film is plated on the Al film surface of the substrate on which the Al film has been plated.
The AlN film has a thickness of 1 to 20nm.
AlN is deposited by post-reaction sputtering or by reactive sputtering when an AlN film is plated.
When AlN is deposited by post-reaction sputtering, the power of a target power supply is 1-20 KW, the power of an ion source is 0.5-10 KW, the Ar flow is 20-1000 sccm, and the N 2 flow is 10-2000 sccm; when AlN is deposited by reactive sputtering, the power of a target material is 1-20 KW, the Ar flow is 20-1000 sccm, and the N 2 flow is 10-2000 sccm.
The beneficial effects of the invention are as follows: aluminum nitride is arranged between the metal aluminum film and the dielectric film of the high-reflection aluminum to form a connecting layer and a buffer layer, so that the adhesive force between the layers of the high-reflection aluminum is improved without affecting the optical performance of the high-reflection aluminum; during preparation, aluminum nitride can be directly plated on the surface of the metal aluminum film or the surface of the metal aluminum film is nitrided by an ion source to form aluminum nitride, and the required plating equipment can adopt the existing equipment, so that the processing is simple and the cost is low.
Drawings
FIG. 1 is a reflectance spectrum of a first highly reflective aluminum of the present invention and a reflectance spectrum of a metallic Al film corresponding thereto.
FIG. 2 is a reflectance spectrum of a second highly reflective aluminum of the present invention and a reflectance spectrum of a metallic Al film corresponding thereto.
FIG. 3 is a reflectance spectrum of a third highly reflective aluminum of the present invention and a reflectance spectrum of a metallic Al film corresponding thereto.
FIG. 4 is a graph showing the delamination between the dielectric film and the metal aluminum thin film of the first high-reflection aluminum of the present invention.
FIG. 5 is a graph showing the delamination between the dielectric film and the metal aluminum thin film of the second highly reflective aluminum of the present invention.
FIG. 6 is a graph showing the peeling between a dielectric film of a third highly reflective aluminum and a metal aluminum thin film according to the present invention.
Fig. 7 is a diagram showing the peeling between a dielectric film of high-reflection aluminum and a metal aluminum thin film formed by the present embodiment.
FIG. 8 is a graph showing the peeling between the dielectric film and the metal aluminum film after the high-reflection aluminum formed by the present invention is boiled in water at 100℃for 8 hours.
FIG. 9 is a graph of reflectance for an Al film, high-reflectance aluminum made by method one, and high-reflectance aluminum made by method two.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Spatially relative terms, such as "above … …," "above … …," "upper surface on … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
The technological process of raising the adhesion between the aluminum film and the dielectric film in magnetron sputtering high reflecting aluminum includes preparing aluminum nitride layer between the aluminum film and the dielectric film, i.e. one side of the aluminum nitride layer is connected to the aluminum film and the other side is connected to the dielectric film. Because the adhesive force between the aluminum nitride film layer and the metal aluminum is better, the adhesive force between the aluminum nitride film layer and the dielectric film is also better, so that the adhesive force between the formed high-reflection aluminum film layers is larger, and the optical performance of the high-reflection aluminum film layer is not influenced. For ease of description, aluminum is replaced herein with aluminum of formula Al, aluminum nitride is replaced with aluminum nitride of formula AlN, and nitrogen is replaced with nitrogen of formula N 2.
The preparation of an AlN film layer between an Al film and a dielectric film can be achieved by the following two methods.
The method comprises the following steps: the Al film surface of the substrate on which the Al film has been plated is subjected to nitriding treatment to form an AlN film layer.
Specifically, ar and N 2,N2 are introduced into an ion source region to be ionized into ions, a substrate plated with an Al film is fed into the ionization region, the surface of the Al film is nitrided by N 3- in the ionization region, and a graded AlN layer is formed on the surface of the Al film. The AlN layer formed by the method is thin, and has no influence on the subsequent optical performance. Wherein the ions of the ionization region comprise N 3-、Ar+ and the like. The graded type is that because the method uses an ion source to ionize nitrogen, the generated N 3- reacts with the surface of the Al film, and then a graded nitriding process with the nitriding degree from shallow to deep is necessarily present.
The ion source can ionize N 2, including but not limited to ICP ion sources, anode layer ion sources.
In this embodiment, an ICP ion source and an RF power source, which is a power source of the ICP ion source, are used. The RF power is 0.5-10 KW, ar flow is 20-1000 sccm, N 2 flow is 10-2000 sccm, and nitriding time is 10-1800 s.
When the anode layer ion source is used, the voltage is 500-3000V, the Ar flow is 10-1000 sccm, the N 2 flow is 10-2000 sccm, and the nitriding time is 10-1800 s.
The second method is as follows: an AlN film layer is plated on the Al film surface of the substrate on which the Al film has been plated. The adhesive force between the AlN film layer and the Al film is better, and the adhesive force between the AlN film and the dielectric film is correspondingly better, so that in the high-reflection aluminum film structure formed by overlapping the dielectric films with the Al film, the adhesive force of the whole high-reflection aluminum can be better due to the existence of the linking layer AlN. Preferably, the AlN film layer plated in the second method has a thickness of 1-20 nm.
In the second method, the thickness of the AlN film is not too thick, and the effect on the reflectivity of the entire highly reflective aluminum increases with the superposition of the AlN film thickness. For example, when the thickness of the AlN film layer is 5-10 nm, the reflectivity of the prepared high-reflectivity aluminum is reduced by about 1% compared with that of the high-reflectivity aluminum without the AlN film layer, namely the reflectivity of the high-reflectivity aluminum is lost, but the loss is smaller, and the loss of the reflectivity of the AlN film layer can be counteracted by the film system adjustment of the subsequent dielectric film. The deposition manner of depositing the AlN film on the Al film includes, but is not limited to, post-reaction sputtering deposition AlN process and reaction sputtering deposition AlN process. The film system adjustment can be realized by adjusting the film thickness of a later dielectric film layer or plating an AlN thin layer and the like.
Post-reaction sputtering deposition of AlN refers to sputtering metal Al through a target region, ionizing N 2 and Ar through an ICP ionization region, and nitriding an Al film deposited on the target region into an AlN film by N 3-. Preferably, the AlN is deposited by post-reaction sputtering, wherein the technological parameters are as follows: the power of the target material power is 1-20 KW, the power of the ICP power, namely the RF power, is 0.5-10 KW, the Ar flow is 20-1000 sccm, and the N 2 flow is 10-2000 sccm.
The reactive sputtering deposition AlN process is to generate AlN in a target area through nitriding reaction, and the AlN film is directly deposited on the metal Al film. Preferably, the technological parameters of the reactive sputtering deposition AlN are as follows: the power of the target power supply is 1-20 KW, the Ar flow is 20-1000 sccm, and the N 2 flow is 10-2000 sccm.
The dielectric film material is one or more than one of TiO 2、SiO2 and Nb 2O5 in a superposition combination way.
Table 1 shows a high-reflection aluminum film system structure prepared by the above process, wherein the film layer directly contacting the substrate is a primer layer, and the primer layer material includes but is not limited to Cr, si, al 2O3、ZrO2 and SiO. The Al film is plated on the surface of the priming layer, and the priming layer increases the adhesive force between the Al film and the base material. The Al film layer is an AlN film layer, and the AlN film layer is a dielectric film.
Table 1a membrane system structure suitable for the present solution
| Dielectric film |
| AlN |
| Al |
| And (3) priming: cr, si, al 2O3,ZrO2, siO, etc |
| A base material: glass/(PC, PET, PMMA etc.) organic substrate)/metal/ceramic etc |
Based on the above film system structure, in this embodiment, three kinds of high-reflection aluminum not processed by the above process method are selected, the first high-reflection aluminum film layer structure is shown in table 2, the second high-reflection aluminum structure is shown in table 3, and the third high-reflection aluminum structure is shown in table 4.
TABLE 2 first high-reflection aluminum film layer structure
| Film thickness | |
| SiO2 | 15nm |
| TiO2 | 51.06nm |
| SiO2 | 95.5nm |
| Al | 50nm |
| Cr | 2～10nm |
| PC base material |
TABLE 3 second highly reflective aluminum film structure
| Film thickness | |
| SiO2 | 12.85nm |
| TiO2 | 50.53nm |
| SiO2 | 101.37nm |
| TiO2 | 52.59nm |
| SiO2 | 98.29nm |
| Al | 50nm |
| Cr | 2～10nm |
| PC base material |
TABLE 4 third high-reflection aluminum film layer structure
| Film thickness | |
| SiO2 | 12.60nm |
| Nb2O5 | 47.64nm |
| SiO2 | 90.47nm |
| Nb2O5 | 50.54nm |
| SiO2 | 88.31nm |
| Al | 50nm |
| Si | 2～10nm |
| Glass |
The reflectance spectrum of the first highly reflective aluminum and the reflectance spectrum of the corresponding metal Al film (first highly reflective aluminum removed dielectric film) are shown in fig. 1, and the average reflectance of the first highly reflective aluminum is improved by 6% or more over that of the metal Al film.
The reflectance spectrum of the second highly reflective aluminum and the reflectance spectrum of the corresponding metal Al film (second highly reflective aluminum removed dielectric film) are shown in fig. 2, and the average reflectance of the second highly reflective aluminum is improved by 8% or more over that of the metal Al film.
The reflectance spectrum of the third highly reflective aluminum and the reflectance spectrum of the metal Al film (third highly reflective aluminum removed dielectric film) corresponding thereto are shown in fig. 3, and the average reflectance of the third highly reflective aluminum is improved by 8% or more than that of the metal Al film.
The curves corresponding to the 45 ° angle and the 10 ° angle in fig. 1 to 3 refer to angles when the reflectivity is tested by the reflectivity testing instrument, and the specific testing method thereof is not described herein.
From the above, the reflectivity of highly reflective aluminum is higher than that of metallic aluminum.
The problem of adhesion between the dielectric film and the Al film is easy to occur when the dielectric film is plated on the Al after the plating of the Al is finished, no matter the high-reflection aluminum film of the Al+ dielectric film is plated on the PC substrate or the glass substrate by magnetron sputtering. When the white grid is made, the dielectric film is easy to peel off from the Al film, and as shown in figures 4-6, the peeling phenomenon between the dielectric film and the metal aluminum film is very obvious. The method for manufacturing the white lattice is a method for testing the adhesive force, a hundred small lattices are drawn on a test article by a small knife, then the hundred small lattices are torn by a 3M adhesive tape, and the situation of the aluminum film adhered and pulled by the adhesive tape is observed. The less the aluminum film adhered indicates greater adhesion.
The high-reflection aluminum treated by the scheme is shown in figures 7 and 8, and the peeling condition of the product is shown after the conventional white lattice is made and the white lattice is boiled for 8 hours at 100 ℃. As can be seen from fig. 7 and 8, the adhesion between the layers of the highly reflective aluminum formed by the process of the present embodiment is large, and the less aluminum film is adhered.
As shown in fig. 9, the reflectivity curves of the Al film, the high-reflectivity aluminum obtained by the first method, and the high-reflectivity aluminum obtained by the second method are shown, wherein the base material, the primer layer, and the Al film of the four film system structures are the same, and the dielectric films of the latter three film system structures are the same. The average reflectivity of the Al film is about 89.3% in the wavelength range of 420 nm-680 nm; the average reflectivity of the common high-reflectivity aluminum film (a dielectric film is directly plated on an Al film) is about 94.42 percent; the average reflectivity of the high-reflectivity aluminum film prepared by the method I is about 94.45%; the average reflectivity of the high-reflectivity aluminum film prepared by the second method is about 93.2 percent.
From the above, the high-reflection aluminum prepared by the first method can improve the adhesion between the metal aluminum and the dielectric film without any influence on the optics of the high-reflection aluminum. The reflectivity of the high-reflectivity aluminum prepared by the second method can be slightly influenced, the change of the reflectivity can be matched by correspondingly adjusting the film system of the dielectric film, and the adhesive force of the high-reflectivity aluminum prepared by the second method is improved.
Based on the above process, in this embodiment, a preparation method for preparing high-reflectivity aluminum with an AlN film layer includes:
Step S1: and (5) pretreatment of the base material. Mainly refers to pre-cleaning the substrate.
Step S2: plating a bottom layer. A primer layer Cr or other material is deposited on the substrate.
Step S3: sputtering the Al target to form a metallic Al film.
Step S4: the AlN film layer is prepared by adopting the first method or the second method.
Step S5: plating a dielectric film. In this example, siO 2、TiO2 and SiO 2 were plated sequentially. When SiO 2 is plated, the Si target is subjected to reactive sputtering to generate SiO 2; or plating a Si film, and ionizing O 2,O2- in an ICP region to oxidize the Si film to generate SiO 2. Similarly, when TiO 2 is plated, the Ti target is subjected to reactive sputtering to generate TiO 2; or plating a Ti film, and ionizing O 2,O2- in an ICP region to oxidize the Ti film to generate TiO 2.
The film structure of the obtained high-reflection aluminum film having an AlN film layer is shown in Table 5.
TABLE 5 high-reflection aluminum film system structure with AlN film layer prepared by this scheme
| Film thickness | |
| SiO2 | 15nm |
| TiO2 | 51.06nm |
| SiO2 | 95.5nm |
| AlN | 1～20nm |
| Al | 50nm |
| Cr | 2～10nm |
| PC base material |
The process and preparation methods are performed in a coating apparatus, which in this embodiment comprises three chambers arranged in sequence: a first chamber, a second chamber, and a third chamber. A gate valve is isolated between the first chamber and the second chamber and between the second chamber and the third chamber. The second chamber is a film coating chamber. In the embodiment, the adopted coating equipment is macro-vacuum continuous three-chamber coating equipment HD-SCK1600-ICP.
Steps S1 and S2 above are performed in a first chamber provided with a reactive ion source and a primer layer plating member. The cleaning of the base material and the plating of the priming layer are realized. The coating chamber is internally provided with a target area and an ion source area, the target area is provided with a plurality of targets, the ion source area ionizes gas through ICP, and the ICP is inductively coupled plasma.
The substrate rack is arranged in the film coating chamber and is a barrel-shaped drum, the substrate is fixed on the side surface of the barrel-shaped drum, and the drum rotates around the central shaft of the barrel, namely, the substrate revolves around the central shaft. When the substrate rotates, the substrate sequentially passes through the target area and the ion source area. When the substrate passes through the target area, a plurality of targets are sequentially sputtered and deposited on the substrate, a required Al film or AlN film or dielectric film is formed under the combined action of ionized gases, and the required film layer and film thickness can be obtained by controlling the rotation number of the substrate. I.e. step S3, step S4 and step S5 are all completed in said second chamber.
It should be noted that, the parameter control in the above-mentioned coating process may adopt a scheme in the prior art, and will not be described herein.
Finally, what is necessary here is: the above embodiments are only for further detailed description of the technical solutions of the present invention, and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments made by those skilled in the art from the above description of the present invention are all within the scope of the present invention.
Claims (10)
1. The technological process of raising the adhesion between the high-reflectivity Al film and the dielectric film layer in magnetron sputtering process is characterized by preparing AlN film between the high-reflectivity Al film and the dielectric film.
2. The process according to claim 1, characterized in that: the preparation method of the AlN film comprises the following steps: an AlN film layer is formed by nitriding the Al film surface of the substrate on which the Al film has been plated.
3. A process according to claim 2, characterized in that: ar and N 2,N2 are introduced into an ion source area to be ionized into ions, the substrate plated with the Al film is fed into the ionization area, and N 3- of the ionization area is used for nitriding the surface of the Al film to generate AlN.
4. A process according to claim 3, characterized in that: the ion source is an ICP ion source or an anode layer ion source.
5. The process according to claim 4, wherein: when the ICP ion source is used, the RF power source is the power source of the ICP ion source, the RF power source power is 0.5-10 KW, the Ar flow is 20-1000 sccm, the N 2 flow is 10-2000 sccm, and the nitriding treatment time is 10-1800 s.
6. The process according to claim 4, wherein: when the anode layer ion source is used, the voltage is 500-3000V, the Ar flow is 10-1000 sccm, the N 2 flow is 10-2000 sccm, and the nitriding time is 10-1800 s.
7. The process according to claim 1, characterized in that: the preparation method of the AlN film comprises the following steps: an AlN film is plated on the Al film surface of the substrate on which the Al film has been plated.
8. The process according to claim 7, wherein: the AlN film has a thickness of 1 to 20nm.
9. The process according to claim 8, wherein: alN is deposited by post-reaction sputtering or by reactive sputtering when an AlN film is plated.
10. The process according to claim 9, characterized in that: when AlN is deposited by post-reaction sputtering, the power of a target power supply is 1-20 KW, the power of an ion source is 0.5-10 KW, the Ar flow is 20-1000 sccm, and the N2 flow is 10-2000 sccm; when AlN is deposited by reactive sputtering, the power of a target material is 1-20 KW, the Ar flow is 20-1000 sccm, and the N 2 flow is 10-2000 sccm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211352206.1A CN117947380A (en) | 2022-10-31 | 2022-10-31 | Technological method for improving adhesion of aluminum film and dielectric film layer in magnetron sputtering high-reflectivity aluminum |
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