CN114959571A - Nano composite corrosion-resistant coating and preparation method and application thereof - Google Patents

Nano composite corrosion-resistant coating and preparation method and application thereof Download PDF

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CN114959571A
CN114959571A CN202210499888.2A CN202210499888A CN114959571A CN 114959571 A CN114959571 A CN 114959571A CN 202210499888 A CN202210499888 A CN 202210499888A CN 114959571 A CN114959571 A CN 114959571A
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corrosion
layer
resistant
coating
target
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CN114959571B (en
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田灿鑫
赖慧明
简学方
刘秋霖
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Lingnan Normal University
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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
    • C23C14/48—Ion implantation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C23C14/0036—Reactive sputtering
    • 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
    • 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
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • 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
    • C23C14/08—Oxides
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00—Features common to bolt and nut
    • F16B33/008—Corrosion preventing means
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00—Features common to bolt and nut
    • F16B33/06—Surface treatment of parts furnished with screw-thread, e.g. for preventing seizure or fretting
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention belongs to the technical field of anticorrosive coatings, and particularly relates to a nano composite anticorrosive coating and a preparation method and application thereof. The invention adopts a Cr blending layer, a Cr-CrN connecting layer, a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer and an AlCrSiVOx pitting-resistant layer to prepare the nano composite corrosion-resistant coating. Through the mutual synergistic action between the layers, the corrosion resistance of the fastener is improved, the service performance of the fastener is enhanced, and the service life of the fastener is prolonged. The coating is prepared by combining plasma immersion ion implantation with a magnetron sputtering system, so that the prepared coating is uniform and compact, and the corrosion resistance of the coating coated on the surface of the fastener can be further improved.

Description

Nano composite corrosion-resistant coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of anticorrosive coatings. More particularly, relates to a nano composite corrosion-resistant coating, a preparation method and an application thereof.
Background
Offshore equipment is extremely easy to be corroded by high-temperature, high-humidity and high-salt atmospheric environment, and serious corrosion can be caused to the equipment due to spray splashing, tidal water scouring and seawater soaking. The steel member connecting fastener is easy to fretting wear, seawater can contact the base of the fastener through a worn notch to generate chemical corrosion, and the whole equipment facility can be further promoted to corrode in a long-term way.
The current anticorrosion measure of offshore equipment facilities is to coat the surface of the equipment facilities with an anticorrosion coating. For example, the Chinese patent application discloses a marine steel structure long-acting protection multilayer epoxy heavy-duty anticorrosive coating which is formed by compounding three layers of structures, wherein the three layers of structures are sequentially a multi-carboxyl epoxy resin coating, a solvent-free epoxy resin coating, an acrylic epoxy finish paint, a polyurethane epoxy finish paint, an organic silicon epoxy finish paint or a fluorocarbon finish paint from inside to outside. The adopted anticorrosion coating is an organic anticorrosion coating which has good corrosion resistance and protection effect on the offshore steel member, but the organic protection coating has poor adhesion with the steel member, and the coating is easy to fall off in the long-term use process, and generates electrochemical reaction after falling off to cause more serious corrosion; meanwhile, when the structural member bears load, the damage resistance of the organic protective coating is too poor, premature failure occurs, and effective protection cannot be achieved. Particularly for the fasteners with the micro-motion condition, the anti-corrosion coating is easier to wear under the micro-motion condition, so that the requirements on the adhesion capability and the durability of the coating are higher, and the organic anti-corrosion coating is easy to fall off, the adhesion cannot meet the requirements, and the organic anti-corrosion coating is easy to fail prematurely, so that the organic coating is basically not suitable for the fasteners.
For the reasons, it is urgently needed to provide a plurality of marine fastener anticorrosive coatings which have good adhesion to fasteners, are not easy to fall off, have good anticorrosive effect and have long-lasting effect.
Disclosure of Invention
The invention aims to solve the technical problems of poor adhesion, easy falling and premature failure of the anticorrosive coating of the existing offshore fastener and provide a nano composite anticorrosive coating which has good adhesion to the fastener, difficult falling, good anticorrosive effect and lasting effect.
The invention aims to provide a preparation method of a nano composite corrosion-resistant coating.
It is another object of the present invention to provide a use of a nanocomposite corrosion resistant coating in the manufacture of a fastener.
The above object of the present invention is achieved by the following technical solutions:
the nano composite corrosion-resistant coating is characterized by comprising a blending layer, a connecting layer, a corrosion-resistant layer and a pitting-resistant layer from the surface of a fastener substrate to the outside in sequence, wherein the blending layer is formed by mixing Cr and workpiece substrate metal, the connecting layer is Cr-CrN, the corrosion-resistant layer is CrN/(AlCrNbSiTi) Nx/MoN, and the pitting-resistant layer is AlCrSiVOx, wherein x is 0.1-0.5.
The invention creatively adopts the combination of the Cr blending layer, the Cr-CrN gradient structure connecting layer, the corrosion-resistant layer and the pitting-resistant layer to prepare the nano composite corrosion-resistant coating. The Cr blending layer and the Cr-CrN connecting layer can remarkably improve the adhesive force of the nano composite corrosion-resistant coating on a fastener used in a marine environment, the corrosion-resistant layer can remarkably improve the surface hardness of a die-casting die, the corrosion resistance of the fastener is remarkably improved through a three-layer periodic structure formed by CrN, (AlCrNbSiTi) Nx and MoN in sequence, and the pitting corrosion resistance is further improved by the pitting corrosion-resistant layer. The layers are mutually cooperated, so that the hardness and the corrosion resistance of the fastener are further improved, the service performance of the fastener is enhanced, and the service life of the fastener is prolonged.
Preferably, the thickness of the blending layer is 30-50 nm.
Preferably, the thickness of the connecting layer is 100-500 nm.
Preferably, the connecting layer is a composition gradient transition layer from pure metal Cr to pure CrN from the blending layer to the corrosion-resistant layer.
Preferably, the thickness of the corrosion-resistant layer is 3-5 mu m.
More preferably, the corrosion-resistant layer is composed of CrN, (AlCrNbSiTi) Nx and MoN in this order, and from the connection layer to the corrosion-resistant layer, CrN, (AlCrNbSiTi) Nx and MoN in this order.
Preferably, the thickness of the pitting corrosion resistant layer is 2-3 μm.
The invention further provides a preparation method of the nano composite corrosion-resistant coating, which comprises the following steps:
s1, after plasma etching is carried out on a fastener, plasma immersion ion implantation is utilized, a Cr target is opened in combination with a magnetron sputtering system under the inert gas atmosphere, and Cr ions are implanted into the surface of a fastener substrate to form a blending layer;
s2, introducing Ar/N 2 Mixing the gases, starting bias voltage, and depositing a Cr-CrN connecting layer on the blending layer;
s3, opening the AlCrNbSiTi alloy target and the Mo target, and continuously introducing Ar/N 2 And (3) depositing a corrosion-resistant layer CrN/(AlCrNbSiTi) Nx/MoN on the connecting layer by using mixed gas.
S4, introducing O 2 Ar, stopping the introduction of N 2 And opening the AlCrSiV alloy target, closing the Cr target, the Mo target and the AlCrNbSiTi alloy target, and depositing an AlCrSiVOx pitting corrosion resistant layer on the corrosion resistant layer.
The nano composite corrosion-resistant coating is prepared by adopting a plasma immersion ion implantation and magnetron sputtering system, so that a uniform and compact corrosion-resistant layer can be formed, and the corrosion-resistant performance of the nano composite corrosion-resistant coating can be further improved by coating the nano composite corrosion-resistant coating on the surface of a fastener.
Preferably, in step S1, the inert gas is argon.
Preferably, in step S2, the Ar/N 2 The flow of Ar is gradually reduced and N is increased along with the increase of the deposition time of the mixed gas 2 And (4) flow rate.
More preferably, the Ar/N is 2 The flow ratio of the mixed gas is gradually reduced from 3/1 to 1/4.
Preferably, in step S3, the AlCrNbSiTi alloy target has an equal content of each element of 20%.
Preferably, in step S3, the Ar/N 2 The flow ratio of the mixed gas is 1 (0.5-1).
Preferably, in step S4, the AlCrSiV alloy target has an equal content of 25% of each element.
Preferably, in step S4, the flow ratio of the oxygen to the argon is 1 (0.5-1).
Preferably, in steps S2, S3 and S4, the bias voltage is 50-100V or DC bias voltage, and the duty ratio is 60-90%.
Preferably, in step S1, the degree of vacuum of the injection environment is not less than 0.05 Pa.
Preferably, in step S2, the vacuum degree of the deposition environment is 0.5-1 Pa.
Preferably, in step S3, the vacuum degree of the deposition environment is 1-2 Pa.
Preferably, in step S4, the vacuum degree of the deposition environment is 0.1-0.5 Pa.
Preferably, in step S1, the injection is performed at a temperature of 200 to 250 ℃.
Preferably, in the steps S2, S3 and S4, the deposition is carried out at a temperature of 200-250 ℃.
The invention further protects the application of the nano composite corrosion-resistant coating in the preparation of the fastener.
Preferably, the fastener is a bolt, a nut, a stud, a screw.
The invention has the following beneficial effects:
the invention adopts a Cr blending layer, a Cr-CrN connecting layer, a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer and an AlCrSiVOx pitting-resistant layer to prepare the nano composite corrosion-resistant coating. Through the mutual synergistic action between the layers, the corrosion resistance of the fastener is improved, the service performance of the fastener is enhanced, and the service life of the fastener is prolonged. The coating is prepared by combining plasma immersion ion implantation with a magnetron sputtering system, so that the prepared coating is uniform and compact, and the corrosion resistance of the coating coated on the surface of the fastener can be further improved.
Drawings
FIG. 1 is a schematic structural diagram of a nano composite corrosion-resistant coating, wherein 1 is a bolt substrate, 2 is a Cr blend layer, 3 is a Cr-CrN connecting layer, 4 is a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer, which sequentially comprises CrN, (AlCrNbSiTi) Nx and MoN, from the connecting layer to the corrosion-resistant layer, sequentially comprises CrN, (AlCrNbSiTi) Nx and MoN, 5 is a pitting-resistant layer AlCrSiVOx, an inset is a local enlarged view of the corrosion-resistant layer, a is CrN, b is (AlCrNbSiTi) Nx, c is MoN, and x is 0.1-0.5.
FIG. 2 is a corrosion polarization curve for a nanocomposite coated bolt of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1 preparation of a nanocomposite Corrosion resistant coated bolt
S1, deburring, cleaning and drying screw threads of a bolt, placing the bolt into a vacuum coating chamber for plasma etching, utilizing plasma immersion ion implantation and combining with a magnetron sputtering system, opening a Cr target in an argon atmosphere, bombarding the Cr target by using Cr ions, and controlling the temperature to be 200 ℃ and the vacuum degree to be 5 multiplied by 10 under the conditions that the voltage is 20KV, the duty ratio is 2 percent, and the vacuum degree is 5 multiplied by 10 -2 Under the condition of Pa, injecting Cr ions into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness is 50 nm;
s2, after the Cr ion bombardment is finished, introducing Ar and N 2 Mixed gas, Ar/N 2 The flow ratio is gradually reduced from 3/1 to 1/4, the bias voltage is 100V, the duty ratio is 90%, the vacuum degree is 1Pa, the temperature is 200 ℃, and a Cr-CrN layer connecting layer with the thickness of 100nm is deposited on the blending layer;
s3, opening AlCrNbSiTi alloy target and Mo gold target, Ar/N 2 The flow ratio of 1/1, the bias voltage of 100V, the duty ratio of 90%, the temperature of 200 ℃ and the vacuum degree of 2Pa are obtained, and CrN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.45 A corrosion resistant layer of/MoN, 5 μm thick.
S4, introducing O 2 Turn off N 2 Opening the AlCrSiV alloy target, closing the Cr target, Mo target and AlCrNbSiTi alloy target, Ar/O 2 The flow rate ratio of 1/1, the bias voltage of 100V, the duty ratio of 90 percent, the temperature of 200 ℃ and the vacuum degree of 0.5Pa, the AlCrSiVO is deposited on the corrosion-resistant layer 0.4 Self-lubricating pitting corrosion resistant layer with thickness of 3 microns. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating (the coated bolt for short). The structure of the nano composite corrosion-resistant coating is schematically shown in figure 1.
Example 2 preparation of a nanocomposite Corrosion resistant coated bolt
S1, removing burrs of bolt threads, cleaning, drying, placing the bolt threads into a vacuum coating chamber, carrying out plasma etching, utilizing plasma immersion ion implantation and combining with a magnetron sputtering system, opening a Cr target in an argon atmosphere, bombarding the Cr target by using Cr ions, and under the conditions that the voltage is 10KV and the duty ratio is 5%, the temperature is 250 ℃, and the vacuum degree is 5 multiplied by 10 -2 Injecting Cr ions into the bolt substrate by Pa to form a blending layer of metal Cr and the bolt substrate, wherein the thickness is 30 nm;
s2, after the Cr ion bombardment is finished, introducing Ar and N 2 Mixed gas, Ar/N 2 The flow ratio is gradually reduced from 3/1 to 1/4, the bias voltage is 50V, the duty ratio is 60%, the temperature is 250 ℃, the vacuum degree is 0.5Pa, and a Cr-CrN connecting layer with the thickness of 500nm is deposited on the blending layer;
s3, opening AlCrNbSiTi alloy target, Mo gold target, Ar/N 2 The flow ratio of 1/1, the bias voltage of 50V, the duty ratio of 60%, the temperature of 250 ℃ and the vacuum degree of 1Pa, the CrN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.48 A MoN corrosion-resistant layer with a thickness of 3 microns.
S4, introducing O 2 Turn off N 2 Opening the AlCrSiV alloy target, closing the Cr target, Mo target and AlCrNbSiTi alloy target, Ar/O 2 The flow ratio of 1/1, the bias voltage of 50V, the duty ratio of 60%, the temperature of 250 ℃ and the vacuum degree of 0.1Pa, the AlCrSiVO is deposited on the corrosion-resistant layer 0.5 Self-lubricating oil-proofAnd a pitting layer with a thickness of 2 microns. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating.
EXAMPLE 3 preparation of nanocomposite Corrosion resistant coated bolts
S1, removing burrs of bolt threads, cleaning, drying, placing the bolt threads into a vacuum coating chamber, carrying out plasma etching, utilizing plasma immersion ion implantation and combining with a magnetron sputtering system, opening a Cr target in an argon atmosphere, bombarding the Cr target by using Cr ions, and controlling the temperature to be 230 ℃ and the vacuum degree to be 5 multiplied by 10 under the conditions that the voltage is 15KV, the duty ratio is 3 percent, and the vacuum degree is 5 multiplied by 10 -2 Under the condition of Pa, injecting Cr ions into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness is 40 nm;
s2, after the Cr ion bombardment is finished, introducing Ar and N 2 Mixed gas, Ar/N 2 The flow ratio is gradually reduced from 3/1 to 1/4, the bias voltage is 80V, the duty ratio is 70%, the temperature is 230 ℃, the vacuum degree is 0.8Pa, and a Cr-CrN connecting layer with the thickness of 300nm is deposited on the blending layer;
s3, opening AlCrNbSiTi alloy target, Mo gold target, Ar/N 2 The flow ratio of 1/1, the bias voltage of 80V, the duty ratio of 70%, the temperature of 230 ℃ and the vacuum degree of 1.5Pa, the CrN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.4 A corrosion resistant layer of/MoN, 4 microns thick.
S4, introducing O 2 Turn off N 2 Opening the AlCrSiV alloy target, closing the Cr target, Mo target and AlCrNbSiTi alloy target, Ar/O 2 The flow rate ratio 1/1, the bias voltage 50V, the duty ratio 70%, the temperature 230 ℃ and the vacuum degree 0.3Pa, the AlCrSiVO is deposited on the corrosion-resistant layer 0.45 Self-lubricating pitting corrosion resistant layer with thickness of 2.5 microns. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating.
Example 4 preparation of nanocomposite Corrosion resistant coated bolts
S1, removing burrs of bolt threads, cleaning, drying, placing the bolt threads into a vacuum coating chamber, carrying out plasma etching, utilizing plasma immersion ion implantation and combining with a magnetron sputtering system, opening a Cr target in an argon atmosphere, bombarding the Cr target by using Cr ions, and controlling the temperature to be 210 ℃ and the vacuum degree to be 5 multiplied by 10 under the conditions that the voltage is 15KV, the duty ratio is 3 percent, and the vacuum degree is 5 multiplied by 10 -2 Under the condition of Pa, injecting Cr ions into the bolt baseBottom, forming a blending layer of metal Cr and the bolt substrate, wherein the thickness is 40 nm;
s2, after the Cr ion bombardment is finished, introducing Ar and N 2 Mixed gas, Ar/N 2 The flow ratio is gradually reduced from 3/1 to 1/4, the bias voltage is 80V, the duty ratio is 70%, the temperature is 210 ℃, the vacuum degree is 0.8Pa, and a Cr-CrN connecting layer with the thickness of 300nm is deposited on the blending layer;
s3, opening AlCrNbSiTi alloy target, Mo gold target, Ar/N 2 The flow ratio of 1/1, the bias voltage of 80V, the duty ratio of 70%, the temperature of 210 ℃ and the vacuum degree of 1.5Pa, the CrN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.4 A MoN corrosion-resistant layer with a thickness of 4 microns.
S4, introducing O 2 Turn off N 2 Opening the AlCrSiV alloy target, closing the Cr target, Mo target and AlCrNbSiTi alloy target, Ar/O 2 The flow ratio of 1/1, the bias voltage of 50V, the duty ratio of 70%, the temperature of 210 ℃ and the vacuum degree of 0.3Pa, the AlCrSiVO is deposited on the corrosion-resistant layer 0.45 Self-lubricating pitting corrosion resistant layer with thickness of 2.5 microns. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating.
Example 5 preparation of a nanocomposite Corrosion resistant coated bolt
S1, deburring, cleaning and drying screw threads of a bolt, placing the bolt into a vacuum coating chamber for plasma etching, utilizing plasma immersion ion implantation and combining with a magnetron sputtering system, opening a Cr target in an argon atmosphere, bombarding the Cr target by using Cr ions, and controlling the temperature to be 240 ℃ and the vacuum degree to be 5 multiplied by 10 under the conditions that the voltage is 15KV, the duty ratio is 3 percent, and the vacuum degree is 5 multiplied by 10 -2 Under the condition of Pa, injecting Cr ions into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness is 40 nm;
s2, after the Cr ion bombardment is finished, introducing Ar and N 2 Mixed gas, Ar/N 2 The flow ratio is gradually reduced from 3/1 to 1/4, the bias voltage is 80V, the duty ratio is 70%, the temperature is 240 ℃, the vacuum degree is 0.8Pa, and a Cr-CrN connecting layer with the thickness of 300nm is deposited on the blending layer;
s3, opening AlCrNbSiTi alloy target, Mo gold target, Ar/N 2 The flow ratio of 1/1, the bias voltage of 80V, the duty ratio of 70%, the temperature of 240 ℃ and the vacuum degree of 1.5Pa, and CrN/(AlCrNbSiTi) N deposited on the connecting layer 0.4 A corrosion resistant layer of/MoN, 4 microns thick.
S4, introducing O 2 Turn off N 2 Opening the AlCrSiV alloy target, closing the Cr target, Mo target and AlCrNbSiTi alloy target, Ar/O 2 The flow ratio of 1/1, the bias voltage of 50V, the duty ratio of 70%, the temperature of 240 ℃ and the vacuum degree of 0.3Pa, the AlCrSiVO is deposited on the corrosion-resistant layer 0.45 Self-lubricating pitting corrosion resistant layer with thickness of 2.5 microns. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating.
Comparative example 1 preparation of nanocrystalline amorphous composite coating
S1, removing burrs of bolt threads, cleaning, drying, placing in a vacuum chamber, vacuumizing until the vacuum degree is 2Pa, and carrying out plasma cleaning;
s2, opening a Cr target after plasma cleaning is finished, and depositing a Cr bonding layer under the conditions that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
s3, after the deposition of the Cr bonding layer is finished, introducing nitrogen, and depositing a CrN transition layer under the conditions that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
s4, after the deposition of the CrN transition layer is finished, opening an AlCr alloy target, closing a Cr target, and starting to deposit a nanocrystalline amorphous composite layer under the conditions that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
and S5, after the deposition of the nanocrystalline amorphous composite layer is finished, reducing the temperature of the vacuum chamber to be below 100 ℃ to obtain the nanocrystalline amorphous composite layer. Comparative example 2 preparation of a nano superlattice coating
S1, removing burrs of bolt threads, cleaning, drying, placing in a vacuum chamber, vacuumizing until the vacuum degree is 2Pa, and carrying out plasma cleaning;
s2, opening a Cr target after plasma cleaning is finished, and depositing a Cr bonding layer under the conditions that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
s3, after the deposition of the Cr bonding layer is finished, introducing nitrogen, and depositing a CrN transition layer under the conditions that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
s4, after the deposition of the CrN transition layer is finished, opening an AlCr alloy target or a Cr target, and beginning to deposit a nano superlattice layer;
and S5, after the deposition of the nano superlattice layer is finished, reducing the temperature of the vacuum chamber to be below 100 ℃ to obtain the nano superlattice layer.
The nano composite corrosion-resistant coating prepared in the embodiment 1 of the invention and other embodiments has similar structure and performance, so the experiment is only carried out in the embodiment 1 of the invention.
Experimental example 1: research on corrosion resistance of nano composite corrosion-resistant coating
The nano composite corrosion-resistant coating prepared in the embodiment 1 of the invention is subjected to corrosion resistance research and test by a potentiodynamic scanning method, and the nano crystal amorphous composite coating in the comparative example 1 and the nano superlattice coating in the comparative example 2 are used as comparison. The sample to be tested is used as an electric level and is tested under the voltage of-2V, and simultaneously, a potential (V) -current (ampere) curve is recorded. The results are shown in FIG. 2, and the curve of FIG. 2 was fitted to obtain Table 1.
Table 1: corrosion current and corrosion potential of three coatings curve-fitted from FIG. 2
Coating material Corrosion potential/V Corrosion current/10 -7 A
Nanocrystalline amorphous composite coatings -0.33 11.86
Nano superlattice coatings -0.66 1.4
Nano composite corrosion-resistant coating -0.22 1.2
As shown in fig. 2 and table 1: the corrosion potential of the nano composite corrosion-resistant coating prepared by the embodiment of the invention is the largest, which is obviously higher than that of a nano-crystalline amorphous composite coating and a nano superlattice coating, and the corrosion current is the smallest. The larger the corrosion potential is, the less the corrosion is easy to start, and the larger the corrosion current is, the higher the corrosion speed is, so that the corrosion potential of the nano composite corrosion-resistant coating prepared by the method is the largest, the corrosion current is the smallest, and the corrosion resistance is optimal.
Experimental example 2: research on film adhesion of nano composite corrosion-resistant coating bolt
The test method comprises the following steps: the adhesion of the nanocomposite coating was tested using a scratch method (scratch tester). The load is continuously added to a scriber (diamond pressure head) through an automatic loading mechanism, the sample is moved at the same time, the scriber is enabled to cross the surface of the coating, and acoustic emission signals and friction force change signals when the coating falls off are obtained through various sensors, so that the critical load of the binding force of the coating and the substrate is obtained.
And (3) testing results: the nano composite coating prepared in the embodiment 1 of the invention has the adhesive force of more than 60N and good adhesive force.
Experimental example 3: friction coefficient research of nano composite corrosion-resistant coating
The test method comprises the following steps: and testing the friction coefficient by adopting a ball disc type friction and wear instrument. The sample to be tested is placed on a ball-and-disk type friction wear apparatus, a load (positive pressure) is applied to the ball by a weight or continuous loading mechanism, the ball is applied to the surface of the sample while the sample is held on a test platform and rotated at a speed of 300 rpm, causing the ball to rub against the surface of the coating. A friction force signal during friction is obtained through a sensor, and a friction coefficient change curve is obtained through calculation (the friction force is divided by positive pressure).
And (3) testing results: the friction coefficient of the nano composite coating prepared in the embodiment 1 of the invention is lower than 0.3, which proves that the nano composite coating prepared in the embodiment has lower friction coefficient and better antifriction effect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The nano composite corrosion-resistant coating is characterized by comprising a blending layer, a connecting layer, a corrosion-resistant layer and a pitting-resistant layer from the surface of a fastener substrate to the outside in sequence, wherein the blending layer is formed by mixing Cr and a fastener substrate metal, the connecting layer is Cr-CrN, the corrosion-resistant layer is CrN/(AlCrNbSiTi) Nx/MoN, and the pitting-resistant layer is AlCrSiVOx, wherein x is 0.1-0.5.
2. The nanocomposite corrosion-resistant coating according to claim 1, wherein the thickness of the blend layer is 30 to 50 nm.
3. The nanocomposite corrosion-resistant coating according to claim 1, wherein the thickness of the connection layer is 100 to 500 nm.
4. The nanocomposite corrosion-resistant coating according to claim 1, wherein the corrosion-resistant layer has a thickness of 3 to 5 μm.
5. The nanocomposite corrosion-resistant coating according to claim 1, wherein the pitting corrosion-resistant layer has a thickness of 2 to 3 μm.
6. The method for preparing the nano composite corrosion-resistant coating of any one of claims 1 to 5, which is characterized by comprising the following steps:
s1, after plasma etching is carried out on a workpiece, plasma immersion ion implantation is utilized, a Cr target is opened in combination with a magnetron sputtering system under the atmosphere of inert gas, and Cr ions are implanted into the surface of a workpiece substrate to form a blending layer;
s2, introducing Ar/N 2 Mixing the gases, starting bias voltage, and depositing a Cr-CrN connecting layer on the blending layer;
s3, opening the AlCrNbSiTi alloy target and the Mo target, and continuously introducing Ar/N 2 And (3) depositing a corrosion-resistant layer CrN/(AlCrNbSiTi) Nx/MoN on the connecting layer by using mixed gas.
S4, introducing O 2 Ar, stopping the introduction of N 2 And opening the AlCrSiV alloy target, closing the Cr target, the Mo target and the AlCrNbSiTi alloy target, and depositing an AlCrSiVOx pitting corrosion resistant layer on the corrosion resistant layer.
7. The method according to claim 6, wherein in step S3, the AlCrNbSiTi alloy target has an equal content of each element.
8. The method of claim 6, wherein in step S4, the AlCrSiV alloy target has equal contents of each element.
9. The method of claim 6, wherein in step S2, the bias voltage is 50-100V, and the duty ratio is 60-90%.
10. Use of the nanocomposite corrosion resistant coating of any of claims 1 to 5 in the manufacture of a fastener.
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