CN114959571B - 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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CN114959571B
CN114959571B CN202210499888.2A CN202210499888A CN114959571B CN 114959571 B CN114959571 B CN 114959571B CN 202210499888 A CN202210499888 A CN 202210499888A CN 114959571 B CN114959571 B CN 114959571B
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corrosion
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coating
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crn
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CN114959571A (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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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 anti-corrosion coatings, and particularly relates to a nano composite anti-corrosion coating, a preparation method and application thereof. The invention adopts a combination of a Cr blending layer, a Cr-CrN connecting layer, a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer and an AlCrSiVOx pitting corrosion-resistant layer to prepare the nano composite corrosion-resistant coating. Through the mutual synergistic effect between 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 can be further improved when the coating is coated on the surface of a fastener.

Description

Nano composite corrosion-resistant coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of anti-corrosion coatings. More particularly, relates to a nano composite corrosion-resistant coating, a preparation method and application thereof.
Background
Offshore equipment facilities are extremely vulnerable to high temperature, high humidity, high salt atmospheric environmental corrosion, and spray splashing, tidal water flushing and seawater soaking all cause serious corrosion to the equipment facilities. Steel member connection fasteners are subject to fretting wear, seawater can contact the base of the fastener through the worn notch, chemical corrosion occurs, corrosion of the whole equipment is further promoted by the accumulation of the daily life, the safety problems of the whole offshore equipment are related, and corrosion prevention measures for the offshore equipment are needed to be provided.
The current anti-corrosion measure for offshore installations is to apply an anti-corrosion coating to the surface of its installation. The long-acting protective multilayer epoxy heavy-duty anticorrosive coating for the marine steel structure is formed by compounding three layers of structures, and is a multi-carboxyl epoxy resin coating, a solvent-free epoxy resin coating, an acrylic epoxy finish, a polyurethane epoxy finish, an organosilicon epoxy finish or a fluorocarbon finish sequentially from inside to outside. The adopted anti-corrosion coating is an organic anti-corrosion coating, the organic anti-corrosion coating has good anti-corrosion performance and good anti-corrosion protection effect on the offshore steel member, but the organic anti-corrosion coating has poor adhesion with the steel member, the coating is easy to fall off in the long-term use process, electrochemical reaction occurs after falling off, and more serious corrosion is caused; meanwhile, when the structural member bears load, the damage resistance of the organic protective coating is too poor, the condition of premature failure occurs, and effective protection cannot be achieved. Particularly for the fasteners with inching condition, the corrosion-resistant coating is more easily worn under the inching condition, so that the adhesion capability and durability of the corrosion-resistant coating are higher, the organic corrosion-resistant coating is easy to fall off, the adhesion force is not required, and the early failure is easy to occur, therefore, the organic coating is basically not suitable for the fasteners.
For the above reasons, there is an urgent need to provide a variety of marine fastener corrosion protection coatings which have good adhesion to fasteners, are not easy to fall off, have good corrosion protection effect, and have durable action.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of poor adhesive force, easy falling and premature failure of the existing marine fastener anti-corrosion coating, and provides the nano composite anti-corrosion coating which has good adhesive force to the fastener, difficult falling, good anti-corrosion 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 nanocomposite corrosion resistant coating for use in the preparation of fasteners.
The above object of the present invention is achieved by the following technical solutions:
the nano composite corrosion-resistant coating is characterized by sequentially comprising a blending layer, a connecting layer, a corrosion-resistant layer and a pitting corrosion-resistant layer from the surface of a fastener substrate to the outside, wherein the blending layer is a blending layer formed by mixing Cr with workpiece substrate metal, the connecting layer is Cr-CrN, the corrosion-resistant layer is CrN/(AlCrNbSiTi) Nx/MoN, and the pitting corrosion-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 corrosion-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 hardness of the surface of a die casting die, and the corrosion resistance of the fastener is remarkably improved through a three-layer periodic structure formed by CrN, (AlCrNbSiTi) Nx and MoN in sequence, so that the pitting corrosion resistance is further improved. The mutual synergistic effect between the layers further improves the hardness and corrosion resistance of the fastener, enhances the service performance of the fastener and prolongs the service life.
Preferably, the thickness of the blend layer is 30 to 50nm.
Preferably, the thickness of the connection layer is 100-500 nm.
Preferably, the connecting layer is a composition gradient transition layer from pure metal Cr to pure CrN from a blending layer to a corrosion-resistant layer.
Preferably, the thickness of the corrosion-resistant layer is 3 to 5 μm.
More preferably, the corrosion-resistant layer is composed of CrN, (AlCrNbSiTi) Nx and MoN in order, and from the connection layer to the corrosion-resistant layer, crN, (AlCrNbSiTi) Nx and MoN in 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, a Cr target is opened under the inert gas atmosphere by utilizing plasma immersion ion implantation and combining a magnetron sputtering system, and Cr ions are implanted into the surface of a fastener substrate to form a blending layer;
s2, introducing Ar/N 2 The mixed gas is used for starting bias voltage, and a Cr-CrN connecting layer is deposited on the blending layer;
s3, opening an AlCrNbSiTi alloy target and a Mo target, and continuously introducing Ar/N 2 And (3) depositing a corrosion-resistant layer CrN/(AlCrNbSiTi) Nx/MoN on the connecting layer by mixed gas.
S4, introducing O 2 Ar, stopping charging N 2 Opening AlCrSiV alloy targets, closing Cr targets, mo targets and AlCrNbSiTi alloy targets, and depositing AlCrSiVOx pitting corrosion resistant layers on the corrosion resistant layers.
The nano composite corrosion-resistant coating is prepared by adopting a plasma immersion ion implantation and magnetron sputtering system, a uniform and compact corrosion-resistant layer can be formed, and the corrosion resistance of the nano composite corrosion-resistant coating can be further improved when the nano composite corrosion-resistant coating is coated on the surface of a fastener.
Preferably, in step S1, the inert gas is argon.
Preferably, in step S2, the Ar/N ratio 2 The mixed gas gradually reduces Ar flow and increases N along with the increase of deposition time 2 Flow rate.
More preferably, the Ar/N ratio 2 The flow ratio of the mixed gas is gradually reduced from 3/1 to 1/4.
Preferably, in step S3, the content of each element in the AlCrNbSiTi alloy target is equal to 20%.
Preferably, in step S3, the Ar/N ratio 2 The flow ratio of the mixed gas is 1 (0.5-1).
Preferably, in step S4, the content of each element in the AlCrSiV alloy target is equal to 25%.
Preferably, in step S4, the flow ratio of oxygen to argon is 1 (0.5-1).
Preferably, in the steps S2, S3, S4, the bias voltage is 50 to 100V or dc bias, and the duty ratio is 60 to 90%.
Preferably, in step S1, the vacuum degree of the injection environment is not lower than 0.05Pa.
Preferably, in step S2, the vacuum degree of the deposition environment is 0.5 to 1Pa.
Preferably, in step S3, the vacuum degree of the deposition environment is 1 to 2Pa.
Preferably, in step S4, the vacuum degree of the deposition environment is 0.1 to 0.5Pa.
Preferably, in step S1, the implantation is performed at a temperature of 200 to 250 ℃.
Preferably, in steps S2, S3, S4, the deposition is performed at a temperature of 200-250 ℃.
The invention further protects the application of the nano composite corrosion-resistant coating in preparing fasteners.
Preferably, the fastener is a bolt, a nut, a stud, a screw.
The invention has the following beneficial effects:
the invention adopts a combination of a Cr blending layer, a Cr-CrN connecting layer, a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer and an AlCrSiVOx pitting corrosion-resistant layer to prepare the nano composite corrosion-resistant coating. Through the mutual synergistic effect between 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 can be further improved when the coating is coated on the surface of a fastener.
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 blending layer, 3 is a Cr-CrN connecting layer, 4 is a CrN/(AlCrNbSiTi) Nx/MoN corrosion-resistant layer, which sequentially consists of CrN, (AlCrNbSiTi) Nx and MoN, from the connecting layer to the corrosion-resistant layer, crN, (AlCrNbSiTi) Nx and MoN sequentially, 5 is a pitting corrosion-resistant layer AlCrSiVOx, and an illustration is a partial enlarged view of the corrosion-resistant layer, wherein a is CrN, b is (AlCrNbSiTi) Nx, c is MoN, and x is 0.1-0.5.
FIG. 2 is a graph of the corrosion polarization curve of a nanocomposite coated bolt of the present invention.
Detailed Description
The invention is further illustrated in the following drawings and specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
Example 1 preparation of nanocomposite corrosion resistant coated bolts
S1, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum coating chamber, performing plasma etching, opening a Cr target under an argon atmosphere by utilizing a plasma immersion ion implantation combined magnetron sputtering system, bombarding the Cr target by Cr ions, and performing vacuum degree 5 multiplied by 10 at the voltage of 20KV, the duty ratio of 2 percent, the temperature of 200 DEG C -2 Under the condition of Pa, cr ions are implanted into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness of the blending layer is 50nm;
after S2.Cr ion bombardment is finished, ar and N are introduced 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 ℃, a Cr-CrN layer connecting layer is deposited on the blending layer, and the thickness is 100nm;
s3, opening an AlCrNbSiTi alloy target, a Mo gold target and Ar/N 2 The flow ratio is 1/1, the bias voltage is 100V, the duty ratio is 90%, the temperature is 200 ℃, the vacuum degree is 2Pa, crN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.45 and/Mon corrosion resistant layer, 5 microns thick.
S4, introducing O 2 Turn off N 2 Opening AlCrSiV alloy target, closing Cr target, mo target and AlCrNbSiTi alloy target, ar/O 2 The flow ratio is 1/1, the bias voltage is 100V, the duty ratio is 90%, the temperature is 200 ℃, the vacuum degree is 0.5Pa, and AlCrSiVO is deposited on the corrosion-resistant layer 0.4 And a self-lubricating pitting corrosion-resistant layer with the thickness of 3 micrometers. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating (the coating bolt for short). Wherein the schematic structure of the nanocomposite corrosion-resistant coating is shown in fig. 1.
Example 2 preparation of nanocomposite corrosion resistant coated bolts
S1, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum coating chamber, performing plasma etching, opening a Cr target under an argon atmosphere by utilizing a plasma immersion ion implantation combined magnetron sputtering system, bombarding the Cr target by Cr ions, wherein the temperature is 250 ℃ and the vacuum degree is 5 multiplied by 10 under the conditions that the voltage is 10KV and the duty ratio is 5% -2 Pa implants Cr ions into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness of the blending layer is 30nm;
after S2.Cr ion bombardment is finished, ar and N are introduced 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, a Cr-CrN connecting layer is deposited on the blending layer, and the thickness is 500nm;
s3, opening an AlCrNbSiTi alloy target, a Mo gold target and Ar/N 2 The flow ratio is 1/1, the bias voltage is 50V, the duty ratio is 60%, the temperature is 250 ℃, the vacuum degree is 1Pa, crN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.48 and/Mon corrosion resistant layer, thickness 3 microns.
S4, introducing O 2 Turn off N 2 Opening AlCrSiV alloy target, closing Cr target, mo target and AlCrNbSiTi alloy target, ar/O 2 The flow rate is 1/1, the bias voltage is 50V, the duty ratio is 60%, the temperature is 250 ℃, the vacuum degree is 0.1Pa, and the corrosion resistance is realizedDeposition of AlCrSiVO on layer 0.5 And a self-lubricating pitting corrosion-resistant layer with the thickness of 2 micrometers. 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, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum coating chamber, performing plasma etching, opening a Cr target under an argon atmosphere by utilizing a plasma immersion ion implantation combined magnetron sputtering system, bombarding the Cr target by Cr ions, and performing vacuum degree 5 multiplied by 10 at a voltage of 15KV, a duty ratio of 3 percent, a temperature of 230 DEG C -2 Under the condition of Pa, cr ions are implanted into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness of the blending layer is 40nm;
after S2.Cr ion bombardment is finished, ar and N are introduced 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, a Cr-CrN connecting layer is deposited on the blending layer, and the thickness is 300nm;
s3, opening an AlCrNbSiTi alloy target, a Mo gold target and Ar/N 2 The flow ratio is 1/1, the bias voltage is 80V, the duty ratio is 70%, the temperature is 230 ℃, the vacuum degree is 1.5Pa, crN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.4 and/Mon corrosion resistant layer, thickness 4 microns.
S4, introducing O 2 Turn off N 2 Opening AlCrSiV alloy target, closing Cr target, mo target and AlCrNbSiTi alloy target, ar/O 2 The flow ratio is 1/1, the bias voltage is 50V, the duty ratio is 70%, the temperature is 230 ℃, the vacuum degree is 0.3Pa, and AlCrSiVO is deposited on the corrosion-resistant layer 0.45 And a self-lubricating pitting corrosion resistant layer with the thickness of 2.5 micrometers. 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, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum coating chamber, performing plasma etching, opening a Cr target under an argon atmosphere by utilizing a plasma immersion ion implantation combined magnetron sputtering system, bombarding the Cr target by Cr ions, and performing vacuum degree 5 multiplied by 10 at a voltage of 15KV, a duty ratio of 3 percent, a temperature of 210 DEG C -2 Under the condition of Pa, cr ions are implanted into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness of the blending layer is 40nm;
after S2.Cr ion bombardment is finished, ar and N are introduced 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, a Cr-CrN connecting layer is deposited on the blending layer, and the thickness is 300nm;
s3, opening an AlCrNbSiTi alloy target, a Mo gold target and Ar/N 2 The flow ratio is 1/1, the bias voltage is 80V, the duty ratio is 70%, the temperature is 210 ℃, the vacuum degree is 1.5Pa, crN/(AlCrNbSiTi) N is obtained by deposition on the connecting layer 0.4 and/Mon corrosion resistant layer, thickness 4 microns.
S4, introducing O 2 Turn off N 2 Opening AlCrSiV alloy target, closing Cr target, mo target and AlCrNbSiTi alloy target, ar/O 2 The flow ratio is 1/1, the bias voltage is 50V, the duty ratio is 70%, the temperature is 210 ℃, the vacuum degree is 0.3Pa, and AlCrSiVO is deposited on the corrosion-resistant layer 0.45 And a self-lubricating pitting corrosion resistant layer with the thickness of 2.5 micrometers. And naturally cooling after the deposition is finished to obtain the bolt with the nano composite corrosion-resistant coating.
Example 5 preparation of nanocomposite corrosion resistant coated bolts
S1, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum coating chamber, performing plasma etching, opening a Cr target under argon atmosphere by utilizing a plasma immersion ion implantation combined magnetron sputtering system, bombarding the Cr target by Cr ions, and performing vacuum degree 5 multiplied by 10 at the voltage of 15KV, the duty ratio of 3 percent, the temperature of 240 DEG C -2 Under the condition of Pa, cr ions are implanted into the bolt substrate to form a blending layer of metal Cr and the bolt substrate, wherein the thickness of the blending layer is 40nm;
after S2.Cr ion bombardment is finished, ar and N are introduced 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, a Cr-CrN connecting layer is deposited on the blending layer, and the thickness is 300nm;
s3, opening an AlCrNbSiTi alloy target, a Mo gold target and Ar/N 2 A flow rate of 1/1, a bias of 80V, a duty ratio of 70%, a temperature of 240 ℃ and a vacuum of 1.5Pa, and are connectedLayer deposition to obtain CrN/(AlCrNbSiTi) N 0.4 and/Mon corrosion resistant layer, thickness 4 microns.
S4, introducing O 2 Turn off N 2 Opening AlCrSiV alloy target, closing Cr target, mo target and AlCrNbSiTi alloy target, ar/O 2 The flow ratio is 1/1, the bias voltage is 50V, the duty ratio is 70%, the temperature is 240 ℃ and the vacuum degree is 0.3Pa, and AlCrSiVO is deposited on the corrosion-resistant layer 0.45 And a self-lubricating pitting corrosion resistant layer with the thickness of 2.5 micrometers. 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, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum chamber, vacuumizing to a vacuum degree of 2Pa, and cleaning plasma;
s2, opening a Cr target after the 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 the Cr target, and starting to deposit a nanocrystalline amorphous composite layer under the condition that the temperature is 200 ℃ and the vacuum degree is 2 Pa;
s5, after the deposition of the nanocrystalline amorphous composite layer is finished, the temperature of the vacuum chamber is reduced to be below 100 ℃, and the nanocrystalline amorphous composite layer is obtained. Comparative example 2 preparation of a nano superlattice coating
S1, deburring, cleaning and drying screw threads of a bolt, putting the screw threads into a vacuum chamber, vacuumizing to a vacuum degree of 2Pa, and cleaning plasma;
s2, opening a Cr target after the 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 CrN transition layer is deposited, opening an AlCr alloy target or a Cr target, and starting to deposit a nano superlattice layer;
s5, after the deposition of the nano superlattice layer is finished, the temperature of the vacuum chamber is reduced to be below 100 ℃, and the nano superlattice layer is obtained.
The nano composite corrosion-resistant coating prepared in the embodiment 1 of the invention has similar structure and performance as those prepared in other embodiments, so that the experimental example of the invention only adopts the embodiment 1 for experiment.
Experimental example 1: corrosion resistance study of nanocomposite corrosion-resistant coatings
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 amorphous composite coating in the comparative example 1 and the nano superlattice coating in the comparative example 2 are used as controls. The sample to be tested was tested as a level at a voltage of-2V to 2V while recording the potential (V) -current (amp) curve. The results are shown in FIG. 2, and the curve of FIG. 2 is fitted to give Table 1.
Table 1: corrosion current and corrosion potential for three coatings curve fitted by FIG. 2
Coating material Corrosion potential/V Corrosion current/10 -7 A
Nanocrystalline amorphous composite coating -0.33 11.86
Nano superlattice coating -0.66 1.4
Nanocomposite 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 the nanocrystalline amorphous composite coating and the nanocrystalline superlattice coating, and the corrosion current is the smallest. The greater the corrosion potential is, the less easy to start corrosion, the greater the corrosion current is, and the higher the corroded speed is, so that the nano composite corrosion-resistant coating prepared by the method has the advantages of maximum corrosion potential, minimum corrosion current and optimal corrosion resistance.
Experimental example 2: film adhesion study of nano composite corrosion-resistant coating bolt
The testing method comprises the following steps: the adhesion of the nanocomposite coating was tested using a scratch method (scratch meter). And continuously adding load to a scriber (a diamond pressure head) through an automatic loading mechanism, simultaneously moving a sample to enable the scriber to scratch the surface of the coating, and acquiring an acoustic emission signal and a friction change signal when the coating falls off through each sensor to obtain the critical load of the binding force of the coating and the substrate.
Test results: the adhesive force of the nano composite coating prepared by the embodiment 1 of the invention is more than 60N, and the nano composite coating has good adhesive force.
Experimental example 3: friction coefficient research of nano composite corrosion-resistant coating
The testing method comprises the following steps: the coefficient of friction was measured using a ball-and-disc frictional wear meter. The sample to be tested is placed on a ball-and-disc tribometer, a load (positive pressure) is applied to the ball by a weight or continuous loading mechanism, the ball is applied to the sample surface while the sample is fixed to the test platform and rotated at a speed of 300 revolutions per minute, causing the ball to rub against the coated surface. The friction force signal during friction is obtained through a sensor, and a friction coefficient change curve is obtained through calculation (friction force divided by positive pressure).
Test 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 examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (10)

1. The nano composite corrosion-resistant coating is characterized by sequentially comprising a blending layer, a connecting layer, a corrosion-resistant layer and a pitting corrosion-resistant layer from the surface of a fastener substrate to the outside, wherein the blending layer is a blending layer formed by mixing Cr with fastener substrate metal, the connecting layer is Cr-CrN, the corrosion-resistant layer is CrN/(AlCrNbSiTi) Nx/MoN, and the pitting corrosion-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 50nm.
3. The nanocomposite corrosion resistant coating according to claim 1, wherein the tie layer has a thickness of 100 to 500nm.
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 according to 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, a Cr target is opened under the inert gas atmosphere by utilizing plasma immersion ion implantation and combining a magnetron sputtering system, and Cr ions are implanted into the surface of a workpiece substrate to form a blending layer;
s2, introducing Ar/N 2 The mixed gas is used for starting bias voltage, and a Cr-CrN connecting layer is deposited on the blending layer;
s3, opening an AlCrNbSiTi alloy target and a Mo target, and continuously introducing Ar/N 2 Depositing a corrosion-resistant layer CrN/(AlCrNbSiTi) Nx/MoN on the connecting layer by mixed gas;
s4, introducing O 2 Ar, stopping introducing N 2 Opening AlCrSiV alloy targets, closing Cr targets, mo targets and AlCrNbSiTi alloy targets, and depositing AlCrSiVOx pitting corrosion resistant layers on the corrosion resistant layers.
7. The method according to claim 6, wherein in step S3, the content of each element in the AlCrNbSiTi alloy target is equal.
8. The method according to claim 6, wherein in step S4, the content of each element in the AlCrSiV alloy target is equal.
9. The method according to claim 6, wherein in the step S2, the bias voltage is 50 to 100V and the duty ratio is 60 to 90%.
10. Use of a nanocomposite corrosion resistant coating according to any one of claims 1 to 5 in the manufacture of a fastener.
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