CN111826614B - Intelligent garage anti-corrosion film layer and preparation method thereof - Google Patents
Intelligent garage anti-corrosion film layer and preparation method thereof Download PDFInfo
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- CN111826614B CN111826614B CN202010529481.0A CN202010529481A CN111826614B CN 111826614 B CN111826614 B CN 111826614B CN 202010529481 A CN202010529481 A CN 202010529481A CN 111826614 B CN111826614 B CN 111826614B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/067—Borides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
Abstract
The invention relates to an intelligent garage anti-corrosion film layer which comprises at least one nitride protection film layer, wherein the nitride protection film layer comprises a bottom layer composed of vanadium carbide, a middle layer composed of a vanadium-aluminum nitride mixed compound and a third layer composed of expanded chromium, and a method for preparing the anti-corrosion film layer. The beneficial effects of the invention are as follows: the multilayer structure material is VN/VAlN/CrB, belongs to metal compounds, and compared with organic coatings, the thermal expansion coefficient of the multilayer structure material is close to that of metal, the performance is more stable, and the corrosion resistance is better.
Description
Technical Field
The invention relates to the field of corrosion prevention of intelligent parking garages, in particular to an intelligent garage corrosion prevention film layer and a preparation process thereof.
Background
The intelligent garage is generally arranged in a basement or outdoors and is corroded by humid air to generate rust, particularly the intelligent garage in coastal areas is corroded by seawater moisture to greatly influence the service life, or the intelligent garage is polluted by rust water in rainy days to stop vehicles.
At present, the steel structure part of the garage is mostly constructed by adopting the fireproof coating, the bottom coating of the fireproof coating of the garage is preferably sprayed by adopting gravity or a spray gun, and the garage is roughly divided into a thin protective coating and a thick protective coating.
The thickness of the thin coating is generally 2 mm-7 mm, the pressure of spraying is about 0.4 MPa, the bottom layer is sprayed for 2-3 times, the thickness of each time is not more than 2.5 mm, after the previous time of drying, the surface decorative coating can be brushed, sprayed or rolled after the previous time of spraying, the surface decorative coating is generally painted for 1-2 times, the surface layer is uniform in color, the connection is smooth, the final time of leveling treatment is carried out, the uniformity and smoothness are ensured, an operator needs to carry a thickness tester to detect the thickness of the coating, and the spraying is ensured to reach the designed thickness.
The thickness of the thick coating is generally 8 mm-15 mm, the thick coating is in a powder surface, the density is low, the heat conductivity is low, and the fire resistance limit can reach 2.5 h-5.0 h. The thick fireproof paint is sprayed by a pressure-feed spraying machine, the air pressure is カ 0.4.4 MPa-0.6 MPa, the diameter of a spray gun opening is 6 mm-10 mm, and the thick fireproof paint is added or diluted strictly according to the mixing ratio during the material preparation, and the thick fireproof paint is mixed while the thickness is proper. The spraying construction should survive by several times, the spraying thickness of each time is preferably 5 mm-7 mm, and the spraying needs to be carried out after the primary drying and curing and the secondary spraying. In the spraying process, an operator needs to adopt a thickness measuring needle to detect the thickness of the sensing coating until the thickness reaches the thickness specified by the design, and the spraying can be stopped.
In conclusion, the garage anticorrosive coating is required to have fireproof performance and anticorrosive performance, and the fireproof coating in the current market basically meets the requirements, but still has the following defects: (1) The coating has aging property, the service life of the coating (usually 20 years) is often far shorter than that of a garage (usually the service life is designed to be more than 40 years), and the coating needs to be repaired regularly; (2) As the fireproof coating is organic matter and the garage structural part is metal, the expansion coefficient difference between the fireproof coating and the garage structural part is too much, and the paint coating can locally bubble under the conditions of high temperature and sunlight within the whole service life of 20 years of the coating, so that the coating layer is damaged, the garage generates rusty spots, rusty water of an outdoor parking garage pollutes and parks vehicles in rainy days, and the mechanical property of a local corrosion position of a serious person is reduced, so that safety accidents are caused.
Disclosure of Invention
In order to solve the technical problem, the invention provides an intelligent garage anti-corrosion film layer which comprises at least one nitride protection film layer, wherein the nitride protection film layer comprises a bottom layer composed of Vanadium Nitride (VN), a middle layer composed of vanadium aluminum nitride (VAIN) and a third layer composed of expanded chromium (CrB).
The preparation method of the anti-corrosion film layer of the intelligent garage comprises the following steps of,
s1: adopting multi-arc vacuum evaporation deposition equipment, respectively installing 1 aluminum target, 1 vanadium target and one chromium boride target on 3 targets, respectively etching and cleaning the 3 heavy targets under negative bias-900V, -1100V and-1200V for 2 min, and eliminating surface oxide films and impurities;
s2: starting a vanadium target (99.95 at.%) in a working state, setting the current to be 60A to 75A, and filling nitrogen into equipment under the process conditions of bias voltage of-50V to-55V, wherein the deposition time is 6-8 min to obtain a Vanadium Nitride (VN) transition layer;
s3: simultaneously starting working states of a vanadium target and an aluminum target, wherein the current is 60A to 75A and 30 to 45A respectively, high-purity nitrogen (99.99%) is introduced, the flow rate is 350 sccm, and a vanadium-aluminum nitride mixed compound (VAIN) layer is obtained after deposition for 5-7 min;
s4: and closing the working state of the vanadium target and the aluminum target, starting the working state of the chromium boride target, setting the current to be 40A-55A, and depositing for 8-10 min under the process conditions that the bias voltage is-50V-55V to obtain the expanded chromium (CrB) layer.
Further, 3 layers or more than 3 layers of a Vanadium Nitride (VN) layer, a vanadium aluminum nitride (VAIN) layer and a puffed chromium (CrB) layer can be deposited alternately and circularly by selecting the circularly alternating S2, S3 and S4 to prepare the nano multilayer structure coating, and the last layer is the puffed chromium (CrB) layer to prevent the surface from obtaining a cover surface layer with high wear-resistant corrosion resistance.
The beneficial effects of the invention are as follows: (1) The multilayer structure material of the invention is VN/VAlN/CrB, belongs to metal compounds, and has a thermal expansion coefficient close to that of metal compared with organic coatings. The performance is more stable; (2) Vanadium, aluminum and chromium metal elements are adopted to react in the deposition process to form VN, VAlN and CrB metal compounds with inert characteristics, and the corrosion resistance is realized.
Drawings
In order that the present invention may be more readily and clearly understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings.
Fig. 1 shows an anti-corrosion film layer of a multilayer structure according to the present invention.
Fig. 2 shows the corrosion-resistant film layer of the multilayer structure after 720 hours of salt spray corrosion.
FIG. 3 is a spectrum scan of the coating after 720 hours salt spray corrosion.
Detailed Description
The intelligent garage anti-corrosion film layer comprises at least one nitride protection film layer, wherein the nitride protection film layer comprises a bottom layer composed of Vanadium Nitride (VN), a middle layer composed of vanadium aluminum nitride mixed compound (VAIN) and a third layer composed of expanded chromium (CrB).
The preparation method of the anti-corrosion film layer of the intelligent garage comprises the following steps,
s1: adopting multi-arc vacuum evaporation deposition equipment, respectively installing 1 aluminum target, 1 vanadium target and one chromium boride target on 3 targets, respectively etching and cleaning the 3 heavy targets under negative bias-900V, -1100V and-1200V for 2 min, and eliminating surface oxide films and impurities;
the 3-target position can be respectively provided with different materials in the 3-target position, which is beneficial to the preparation of a multilayer structure. The 3 target negative bias voltages are set to respectively correspond to the removal voltage positions of the oxide films and the impurities on the surfaces of the three targets.
S2: starting a vanadium target (99.95 at.%) in a working state, setting the current to be 60A, and filling nitrogen into the equipment under the process condition that the bias voltage is-50V, wherein the deposition time is 6 min to obtain a Vanadium Nitride (VN) transition layer;
s3: simultaneously starting the working states of a vanadium target and an aluminum target, wherein the current is respectively 60A and 30A, the flow rate of high-purity nitrogen (99.99%) is 350 sccm, and depositing for 5 min to obtain a vanadium-aluminum nitride mixed compound (VAIN) layer;
s4: and closing the working states of the vanadium target and the aluminum target, starting the working state of the chromium boride target, setting the current to be 40A, and depositing for 8min under the process condition that the bias voltage is-50V to obtain the expanded chromium (CrB) layer.
S5: and repeating the steps of S2, S3 and S4, circularly and alternately depositing a Vanadium Nitride (VN) layer, a vanadium aluminum nitride (VAIN) layer and a puffed chromium (CrB) layer to form 3 composite films or 6 or more films, and preparing the nano multilayer structure coating, wherein the last layer is the puffed chromium (CrB) layer to prevent the surface from obtaining a cover surface layer with high wear-resistant corrosion resistance.
The multilayer structure coating is shown in fig. 1, and the total coating thickness h is 2.257 micrometers.
The first layer deposited VN is because the coating has high bonding strength with an iron matrix, plays a role of a transition layer and has good corrosion resistance; crB is adopted for surface covering because of high inertia, good corrosion resistance and thermal stability. The alternate preparation of 3 coatings, the interface between the coatings is favorable to further hinder the corrosive attack.
And (3) placing the coating in a smoke tester, and carrying out salt spray corrosion performance tests in different test times by adopting artificial seawater corrosive liquid to evaluate the corrosion resistance of the coating. The corrosion time is 240h, 480h and 720h respectively, and the coating still maintains a relatively complete structure after the smoke corrosion of 720h, only the multilayer structure of the coating becomes fuzzy (see figure 2), and the multilayer coating of the invention shows good stability in a marine corrosion environment.
The cross-section element distribution map analysis is carried out on the corrosion coating, and the fact that the 720-hour salt spray corrosion does not cause chlorine ions to diffuse into the coating is found, which shows that the multilayer coating has good corrosion resistance to the chlorine ions in the marine corrosion environment.
The comparison table of the performances of the VN/VAlN/CrB multilayer structure anticorrosive coating and the commercially available steel structure fireproof coating layer is shown in Table 1, and the beneficial effects obtained by the invention are as follows: (1) The multilayer structure material of the invention is VN/VAlN/CrB, belongs to metal compounds, and has a thermal expansion coefficient close to that of metal compared with organic coatings. In the salt spray experiment, the salt spray liquid with 100 ℃ is continuously sprayed for 720 hours, and the phenomena of foaming, falling off and the like do not occur. (2) Vanadium, aluminum and chromium metal elements are adopted to react in the deposition process to form VN, VAlN and CrB metal compounds with inert characteristics, and the compounds have corrosion resistance (rust spots, bubbles and the like do not appear in 720h of a salt spray experiment), and the service life of the compounds is longer than 40 years according to the evaluation of salt service experiment data.
TABLE 1 comparison of anticorrosive and paint coat properties for VN/VAlN/CrB multilayer structures TABLE:
and (3) analyzing the reason of local discoloration in a VN/VAlN/CrB multilayer structure in a 720-hour salt spray experiment, scanning the corroded coating in the direction from the substrate to the surface of the coating by adopting energy spectrum analysis, and scanning energy spectrums at 3 positions in total, wherein the figure is shown in figure 3. The result shows that the coating is not penetrated by chloride ions, and elements of the coating are distributed as shown in figure 3, so that the discoloration of the surface is caused by the fact that the iron matrix is corroded and polluted on the surface of the coating by the solution, and the anti-corrosion film layer prepared by the preparation method is stable and has longer service life.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all equivalent variations made by using the contents of the present specification and the drawings are within the protection scope of the present invention. .
Claims (2)
1. The preparation method of the intelligent garage anti-corrosion film layer is characterized in that the intelligent garage anti-corrosion film layer comprises at least one nitride protection film layer, wherein the nitride protection film layer comprises a bottom layer composed of vanadium nitride, a middle layer composed of a vanadium aluminum nitride mixed compound and a third layer composed of chromium boride;
the preparation method of the anti-corrosion film layer of the intelligent garage comprises the following steps,
s1: adopting multi-arc vacuum evaporation deposition equipment, respectively installing 1 aluminum target, 1 vanadium target and one chromium boride target on 3 targets of the multi-arc vacuum evaporation deposition equipment, and etching and cleaning the 3 heavy targets;
s2: starting the working state of the vanadium target, filling nitrogen into the equipment, and depositing to obtain a vanadium nitride transition layer;
s3: simultaneously starting the working states of the vanadium target and the aluminum target, introducing high-purity nitrogen flow, and depositing to obtain a vanadium-aluminum nitride mixed compound layer, namely an intermediate layer consisting of a vanadium-aluminum nitride mixed compound;
s4: closing the working states of the vanadium target and the aluminum target, starting the working state of the chromium boride target, and depositing to obtain an expanded chromium layer, namely a third layer;
s2, S3 and S4, circularly and alternately depositing a vanadium nitride layer, a vanadium aluminum nitride mixed compound layer and a chromium boride layer to form at least 3 layers, wherein the last layer is the chromium boride layer;
s2, when the working state of the vanadium target is started, the process conditions are set to be 60A to 75A, the bias voltage is-50V to-55V, and the deposition time is 6-8 min;
in S3, when the working states of the vanadium target and the aluminum target are started simultaneously, the currents are 60A to 75A and 30 to 45A respectively, the flow rate of high-purity nitrogen is 350 sccm, and the deposition time is 5-7 min;
and S4, closing the working states of the vanadium target and the aluminum target, and opening the working state of the chromium boride target, wherein the process condition is set to be 40A to 55A, the bias voltage is-50V to-55V, and the deposition time is 8-10 min.
2. The preparation method of the intelligent garage anti-corrosion film layer according to claim 1, wherein the aluminum target, the vanadium target and the chromium boride target are respectively etched and cleaned for 2 min under negative bias of-900V, -1100V and-1200V, and surface oxide films and impurities are eliminated.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CA1004964A (en) * | 1972-05-30 | 1977-02-08 | Union Carbide Corporation | Corrosion resistant coatings and process for making the same |
| DE69527236T2 (en) * | 1994-09-16 | 2003-03-20 | Sumitomo Electric Industries | Multi-layer film made of ultra-fine particles and hard composite material for tools that contain this film |
| CN100419117C (en) * | 2004-02-02 | 2008-09-17 | 株式会社神户制钢所 | Hard laminated film, method of manufacturing the same and film-forming device |
| WO2007136777A2 (en) * | 2006-05-17 | 2007-11-29 | G & H Technologies Llc | Wear resistant coating |
| CN103726012B (en) * | 2012-10-15 | 2015-09-30 | 中国科学院兰州化学物理研究所 | A kind of preparation method of corrosion-resistant hard protection coatings |
| JP6463078B2 (en) * | 2014-10-24 | 2019-01-30 | 日立金属株式会社 | Manufacturing method of coated tool |
| CN106811719B (en) * | 2015-12-02 | 2019-07-19 | 中国科学院宁波材料技术与工程研究所 | Wear Protection coating, preparation method and application |
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