CN114959576A - TiCN coating and preparation method and application thereof - Google Patents
TiCN coating and preparation method and application thereof Download PDFInfo
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- CN114959576A CN114959576A CN202210598245.3A CN202210598245A CN114959576A CN 114959576 A CN114959576 A CN 114959576A CN 202210598245 A CN202210598245 A CN 202210598245A CN 114959576 A CN114959576 A CN 114959576A
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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
- C23C14/0664—Carbonitrides
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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
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- 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
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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
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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
- C23C14/24—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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- 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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
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Abstract
The invention discloses a TiCN coating and a preparation method and application thereof, wherein the TiCN coating has the component content Ti/(Ti + C + N) atomic ratio of 35-65% and the C/(C + N) atomic ratio of 20-70%; the wear rate of TiCN coating is 1X 10 ‑16 m 3 /(N·m)‑13×10 ‑16 m 3 V (N.m). The TiCN coating provided by the invention has high hardness and elastic modulus, strong film-substrate combination, small friction coefficient, low wear rate and excellent mechanical property; the preparation method of the TiCN coating can adjust the Ti content by adjusting the power of the co-sputtering Ti target or the current density of the composite deposition metal target, and then realize the controllable adjustment of the C, N content in the TiCN coating, and does not introduce H elementIndustrial production is carried out; the TiCN coating provided by the invention can be widely applied to metal surface treatment or metal processing.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a TiCN coating, and a preparation method and application thereof.
Background
As a large country of manufacturing industry, China needs to consume a large amount of cutting tools every year in the metal cutting and machining industry. Currently, high-efficiency, high-speed and high-precision cutting becomes the main development direction of metal processing, and higher requirements are correspondingly put forward on the performance of cutting tools. The coating treatment of the cutter can improve the mechanical efficiency and the service life of the cutter, and is one of important ways for improving the performance of the cutter, so that the coating technology and the cutter material and the cutter design and manufacture are three key technologies of the cutting cutter. In modern high-speed dry cutting, the coated cutter needs to bear high temperature rise in the high-speed dry cutting process, and the local cutting temperature is up to over 1000 ℃ due to severe friction between the cutter and the surface of a material to be processed, so that the excellent high-temperature stability is the key for realizing the high-speed cutting of the coated cutter. Therefore, the hard tool coating for modern high-speed cutting processing has high thermal stability, high hardness and excellent wear-resisting and friction-reducing performances under a high-temperature service environment.
Currently, hard coatings are being developed towards multi-component, nano-composite, multi-layering. In recent years, TiN is a metal material processing conventional tool coating material. Researches find that the TiN coating has the following problems in a high-temperature service environment: 1) the coating hardness at room temperature is only 24-28 GPa; 2) the oxidation starting temperature is only 450-500 ℃, and the mechanical property of the coating is poor at high temperature; 3) the high-temperature friction coefficient of the coating is large, so that the cutter is easy to generate large cutting force, severe flutter, severe abrasion and the like; 4) in the high-temperature oxidation process of TiN, Ti components are quickly diffused outwards to generate a loose and porous oxide layer with low strength. The TiN coating has insufficient and reduced mechanical properties and large friction coefficient under the service environment, and the service performance of the TiN coating is seriously damaged by micropores and microcracks formed. How to further improve the high temperature oxidation resistance, high temperature mechanics and high temperature friction and wear (wear and friction) resistance of the TiN coating has important theoretical significance and practical application value for promoting the development of coating tools and metal processing industries.
The TiCN coating integrates the advantages of TiN and TiC coatings, compared with the TiN coating, the microhardness is obviously improved, meanwhile, the toughness is better than that of the TiC coating, the TiCN coating has good antifriction performance, and the TiCN coating is widely applied to screw taps, drill bits and milling cutters and is particularly suitable for nonferrous metals such as aluminum alloy and the like and alloysAnd (6) processing. The traditional method for preparing the TiCN nano-structure coating comprises the following steps: magnetron sputtering of Ti 2 CN target material or co-sputtering TiC and TiN target material, but the method is inconvenient for adjusting the C content and is difficult to optimize and adjust the mechanical and tribological properties of the TiCN nano-structure coating; and cathodic arc evaporating the Ti metal target material to N 2 、CH 4 And depositing the TiCN nano-structure coating in the Ar mixed atmosphere, wherein H is easily introduced into the coating by the method, and the coating is low in mechanical property and is brittle. Therefore, it is necessary to develop a preparation method capable of adjusting the C, N content in the TiCN coating.
Disclosure of Invention
In order to overcome the technical problem that the C, N content in the TiCN coating is not easy to adjust in the prior art, one of the purposes of the invention is to provide the TiCN coating; the second purpose of the invention is to provide a preparation method of the TiCN coating; it is a further object of the present invention to provide for the use of such TiCN coatings.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention has the following conception: the TiCN nano-structure coating prepared by adding the C element into the TiN coating can enable the coating to have the characteristics of high hardness, toughness and wear resistance and antifriction, and the condition is that the content of formed coating C, N is controllable and no H is introduced, namely how to realize the controllable adjustment of the coating components and the structure. Preparing a TiCN coating by adopting magnetron sputtering TiC and Ti targets and carrying out co-sputtering deposition based on a composite deposition coating technology; or the TiCN coating is prepared by adopting a magnetron sputtering TiC target material and a cathodic arc evaporation Ti target material simultaneously and performing composite deposition, so that the TiCN coating with strong film-substrate combination, high hardness, wear resistance and friction reduction can be obtained.
The first aspect of the invention provides a TiCN coating, wherein the atomic ratio of the component content Ti/(Ti + C + N) of the TiCN coating is 35% -65%, and the atomic ratio of C/(C + N) is 20% -70%; the TiCN coating has a wear rate of 1 x 10 -16 m 3 /(N·m)-13×10 -16 m 3 /(N·m)。
Preferably, the TiCN coating has a C/(C + N) atomic ratio of 30-70%; more preferably, the TiCN coating layer has a C/(C + N) atomic ratio of 40% to 70%.
Preferably, theThe TiCN coating has a wear rate of 1 x 10 -16 m 3 /(N·m)-10*10 -16 m 3 V (N · m); further preferably, the TiCN coating has a wear rate of 2 x 10 -16 m 3 /(N·m)-5*10 -16 m 3 /(N·m)。
Preferably, the hardness of the TiCN coating is 15GPa-40 GPa; the elastic modulus of the TiCN coating is 250GPa-500 GPa; the TiCN coating has a friction coefficient of 0.2-0.7.
Further preferably, the TiCN coating has a hardness of 20GPa-40 GPa; still more preferably, the TiCN coating has a hardness of 25GPa to 35 GPa.
Further preferably, the elastic modulus of the TiCN coating is 300GPa-500 GPa; still further preferably, the elastic modulus of the TiCN coating is between 350GPa and 450 GPa.
Further preferably, the TiCN coating has a friction coefficient of 0.2 to 0.6; still further preferably, the TiCN coating layer has a friction coefficient of 0.2 to 0.5.
A second aspect of the invention provides a method for preparing a TiCN coating according to the first aspect of the invention, comprising the steps of:
in the nitrogen atmosphere, a TiC target material and a Ti target material are simultaneously subjected to magnetron sputtering, and a TiCN coating is prepared on the surface of the base material through co-sputtering deposition;
or in the nitrogen atmosphere, simultaneously carrying out magnetron sputtering on the TiC target material and carrying out cathodic arc evaporation on the Ti target material, and carrying out composite deposition on the surface of the substrate material to prepare the TiCN coating.
Preferably, the TiC target and the Ti target are simultaneously magnetically sputtered, and the average sputtering power of the TiC target is 1W/cm 2 ～15W/cm 2 (ii) a Preferably, the TiC target and the Ti target are simultaneously magnetically sputtered, and the average sputtering power of the TiC target is 2W/cm 2 ～10W/cm 2 。
Preferably, the TiC target material and the Ti target material are simultaneously magnetically sputtered, and the average sputtering power of the Ti target is 1W/cm 2 ～30W/cm 2 (ii) a Further preferably, the TiC target and the Ti target are simultaneously magnetically sputtered, and the average sputtering power of the Ti target is 2W/cm 2 ～20W/cm 2 。
Preferably, the TiC target material is simultaneously magnetically sputtered by the magnetron sputtering method and the Ti target material is evaporated by the cathode arc method, and the average sputtering power of the TiC target material is 1W/cm 2 ～15W/cm 2 (ii) a Preferably, the TiC target is magnetically sputtered and the Ti target is evaporated by cathode arc at the same time, and the average TiC target sputtering power is 2W/cm 2 ～10W/cm 2 。
Preferably, the TiC target material is magnetically sputtered at the same time, the Ti target material is evaporated by cathode arc, and the average current density of the Ti target material is 0.25A/cm 2 ～5A/cm 2 (ii) a More preferably, the average current density of the Ti target material is 0.5A/cm 2 ～3A/cm 2 。
Preferably, the pressure of the nitrogen gas for the co-sputtering deposition is 0.2 Pa-1.2 Pa; further preferably, the nitrogen pressure of the co-sputtering deposition is 0.3Pa to 1.0 Pa.
Preferably, the pressure of the nitrogen for composite deposition is 0.4 Pa-3.5 Pa; further preferably, the pressure of the nitrogen gas for the composite deposition is 0.5Pa to 3.0 Pa.
Preferably, the temperature of the co-sputtering deposition is 360-440 ℃; further preferably, the temperature of the co-sputtering deposition is 380-420 ℃.
Preferably, the temperature of the composite deposition is 360-440 ℃; further preferably, the temperature of the composite deposition is 380-420 ℃.
Preferably, the time of the co-sputtering deposition or the composite deposition is 0.5h-4 h.
Preferably, the matrix material comprises at least one of iron alloy, alloy steel and hard alloy.
Preferably, the base material further comprises a cleaning step before the co-sputtering deposition or the composite deposition.
Preferably, the cleaning includes at least one of glow cleaning, ion etching, and solvent cleaning.
A third aspect of the invention provides the use of a TiCN coating according to the first aspect of the invention in the treatment of a metal surface or in metal machining.
The invention has the beneficial effects that:
the TiCN coating provided by the invention has high hardness and elastic modulus, strong film-substrate combination, small friction coefficient, low wear rate and excellent mechanical property; the preparation method of the TiCN coating can adjust the Ti content by adjusting the power of the co-sputtering Ti target or the current density of the composite deposition metal target, so that the controllable adjustment of the C, N content in the TiCN coating is realized, H element is not introduced, the preparation method is simple and efficient, and the industrial production can be carried out; the TiCN coating provided by the invention can be widely applied to metal surface treatment or metal processing.
Drawings
FIG. 1 is a diagram of a co-sputtering deposition apparatus and an arc/magnetron composite deposition apparatus according to an embodiment of the present application.
FIG. 2 is a graph showing the TiCN coating element content for examples 1-10 and comparative examples 1-2.
FIG. 3 is a graph of the C/(C + N) atomic ratio of TiCN coatings for examples 1-10 and comparative examples 1-2.
FIG. 4 is a graph of TiCN coating hardness for examples 1-10 and comparative examples 1-2.
FIG. 5 is a graph of the modulus of elasticity of TiCN coatings for examples 1-10 and comparative examples 1-2.
FIG. 6 is a graph of the coefficient of friction of TiCN coatings for examples 1-10 and comparative examples 1-2.
FIG. 7 is a graph of the wear rate of TiCN coatings for examples 1-10 and comparative examples 1-2.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically detailed, are all those that can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available for commercial purchase.
Fig. 1 is a diagram of a co-sputtering deposition apparatus and an arc/magnetron composite deposition apparatus according to an embodiment of the present application, where fig. 1(a) is a diagram of an apparatus for co-sputtering deposition of TiC and Ti targets to prepare a TiCN coating; FIG. 1(b) is a diagram of an apparatus for preparing TiCN coating by composite deposition by simultaneously adopting magnetron sputtering TiC target and cathodic arc evaporation Ti target.
Examples of the base material include iron alloy, alloy steel, hard alloy, etc.
The time of the co-sputtering deposition or the composite deposition of the embodiment is 0.5h-4 h.
Example 1
1. Substrate pretreatment
(1) And carrying out mechanical grinding and polishing treatment on the WC-Co hard alloy matrix.
(2) Solvent cleaning treatment: ultrasonic cleaning with isopropanol for 10min, ultrasonic cleaning with 98% alcohol solution for 10min, and ultrasonic cleaning with ultrapure water for 3 min.
(3) Glow cleaning treatment: cleaning the substrate for 30min by adopting an Ar gas ion source, wherein the environmental pressure is 0.05-0.5 Pa; the bias voltage of the substrate is-500V to-1200V, and the frequency is 80 kHz to 240 kHz.
(4) Ion etching treatment: cleaning the matrix for 30min by using an arc light discharge ion source, wherein the environmental pressure is 0.5-2.0 Pa; the bias voltage of the substrate is-300V to-600V.
2. Simultaneously adopts magnetron sputtering TiC and Ti target materials to prepare the TiCN nano-structure coating by co-sputtering deposition
Meanwhile, the TiCN nano-structure coating is prepared by magnetron sputtering TiC and Ti target materials and co-sputtering deposition, and the average sputtering power of the TiC target is 2W/cm 2 Average sputtering power of Ti target 2W/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, simultaneously starting a TiC and Ti target cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Example 2
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC and Ti target materials to prepare the TiCN nano-structure coating by co-sputtering deposition
Meanwhile, the TiCN nano-structure coating is prepared by magnetron sputtering TiC and Ti target materials and co-sputtering deposition, and the average sputtering power of the TiC target is 2W/cm 2 Average sputtering power of Ti target of 10W/cm 2 . In thatN 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, simultaneously starting a TiC and Ti target cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Example 3
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC and Ti target materials to prepare the TiCN nano-structure coating by co-sputtering deposition
Simultaneously adopting magnetically controlled sputtering TiC and Ti target materials, and preparing the TiCN nano-structure coating by co-sputtering deposition, wherein the average sputtering power of the TiC target is 2W/cm 2 Average sputtering power of Ti target of 20W/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, simultaneously starting a TiC and Ti target cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Example 4
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC and Ti target materials to prepare the TiCN nano-structure coating by co-sputtering deposition
Meanwhile, the TiCN nano-structure coating is prepared by magnetron sputtering TiC and Ti target materials and co-sputtering deposition, and the average sputtering power of the TiC target is 10W/cm 2 Average sputtering power of Ti target 2W/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, simultaneously starting a TiC and Ti target cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Example 5
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC and Ti target materials to prepare the TiCN nano-structure coating by co-sputtering deposition
Meanwhile, the TiCN nano-structure coating is prepared by magnetron sputtering TiC and Ti target materials and co-sputtering deposition, and the average sputtering power of the TiC target is 10W/cm 2 Average sputtering power of Ti target 5W/cm 2 . At N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, simultaneously starting a TiC and Ti target cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Example 6
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC target material and cathode arc evaporation Ti target material, and prepares TiCN nano-structure coating by composite deposition
Meanwhile, a TiCN nano-structure coating is prepared by magnetron sputtering TiC target material and cathode arc evaporation Ti target material through composite deposition, and the average sputtering power of the TiC target is 2W/cm 2 Average current density of Ti target of 0.5A/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And adjusting the pressure of the deposition chamber to 1.5Pa, and simultaneously starting a TiC cathode magnetic control power supply and a Ti target cathode arc evaporation power supply to deposit to obtain the TiCN coating.
Example 7
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Preparing TiCN nano-structure coating by adopting magnetron sputtering TiC target material and cathodic arc evaporation Ti target material and composite deposition
Meanwhile, a TiCN nano-structure coating is prepared by magnetron sputtering TiC target material and cathode arc evaporation Ti target material through composite deposition, and the average sputtering power of the TiC target is 2W/cm 2 Average current density of Ti target 1.5A/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 Gas, regulating deposition chamber pressureAnd (4) applying the force to 1.5Pa, simultaneously starting a TiC cathode magnetic control power supply and a Ti target cathode arc evaporation power supply, and depositing to obtain the TiCN coating.
Example 8
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC target material and cathode arc evaporation Ti target material, and prepares TiCN nano-structure coating by composite deposition
Simultaneously adopting a magnetron sputtering TiC target material and a cathodic arc evaporation Ti target material to prepare the TiCN nano-structure coating by composite deposition, wherein the average sputtering power of the TiC target is 2W/cm 2 Average current density of Ti target 3.0A/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And adjusting the pressure of the deposition chamber to 1.5Pa, and simultaneously starting a TiC cathode magnetic control power supply and a Ti target cathode arc evaporation power supply to deposit to obtain the TiCN coating.
Example 9
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC target material and cathode arc evaporation Ti target material, and prepares TiCN nano-structure coating by composite deposition
Meanwhile, preparing the TiCN nano-structure coating by adopting a magnetron sputtering TiC target material and a cathode arc evaporation Ti target material through composite deposition, wherein the average sputtering power of the TiC target is 10W/cm 2 Average current density of Ti target 1.0A/cm 2 . At N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And adjusting the pressure of the deposition chamber to 1.5Pa, and simultaneously starting a TiC cathode magnetic control power supply and a Ti target cathode arc evaporation power supply to deposit to obtain the TiCN coating.
Example 10
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Simultaneously adopts magnetron sputtering TiC target material and cathode arc evaporation Ti target material, and prepares TiCN nano-structure coating by composite deposition
Meanwhile, preparing the TiCN nano-structure coating by adopting a magnetron sputtering TiC target material and a cathode arc evaporation Ti target material through composite deposition, wherein the average sputtering power of the TiC target is 10W/cm 2 Average current density of Ti target 2.0A/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And adjusting the pressure of the deposition chamber to 1.5Pa, and simultaneously starting a TiC cathode magnetic control power supply and a Ti target cathode arc evaporation power supply to deposit to obtain the TiCN coating.
Comparative example 1
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. TiCN nanostructure coating prepared by magnetron sputtering TiC target material deposition
Preparing TiCN nano-structure coating by adopting magnetron sputtering TiC target material deposition, wherein the average sputtering power of the TiC target is 10W/cm 2 . In N 2 And reacting and depositing the TiCN nano-structure coating in the atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and N is introduced 2 And gas, adjusting the pressure of the deposition chamber to 0.4Pa, starting a TiC cathode magnetic control power supply, and depositing to obtain the TiCN coating.
Comparative example 2
1. Substrate pretreatment
The substrate pretreatment procedure was the same as in example 1.
2. Preparation of TiCN nano-structure coating by cathodic arc evaporation Ti target material deposition
The TiCN nano-structure coating is prepared by adopting cathodic arc evaporation Ti target material deposition, and the average current density of the Ti target is 1.0A/cm 2 . At C 2 H 2 、N 2 And reacting and depositing the TiCN nano-structure coating in the mixed atmosphere. In the coating deposition process, the temperature of the substrate is maintained at 400 ℃, and C is introduced 2 H 2 、N 2 And gas, adjusting the pressure of the deposition chamber to 1.5Pa, starting a Ti target cathode arc evaporation power supply, and depositing to obtain the TiCN coating.
Performance testing
XPS is used to test the content of the coating elements, and FIG. 2 is a graph showing the content of TiCN coating elements in examples 1-10 and comparative examples 1-2. As can be seen from fig. 2, the content of the components of the TiCN coating layer deposited by co-sputtering is: the atomic ratio of Ti/(Ti + C + N) is 40-60%, and the component content of the TiCN coating layer of the magnetic control/electric arc composite deposition is as follows: the atomic ratio of Ti/(Ti + C + N) is 35-65%.
FIG. 3 is a graph of the C/(C + N) atomic ratio of TiCN coatings for examples 1-10 and comparative examples 1-2. As can be seen from FIG. 3, the C/(C + N) atomic ratio of the co-sputter deposited TiCN coating is 40% -70%, and the component content of the TiCN coating compositely deposited by magnetron/arc is 20% -70%.
The coating hardness and the elastic modulus are characterized by adopting a nano-indenter, and the test method and the steps are executed according to the international standard ISO-14577. FIG. 4 is a graph of TiCN coating hardness for examples 1-10 and comparative examples 1-2. As can be seen from FIG. 4, the hardness of the co-sputter deposited TiCN coating is 15GPa-35GPa, and the hardness of the magnetron/arc composite deposited TiCN coating is 15GPa-40 GPa. FIG. 5 is a graph of the modulus of elasticity of TiCN coatings for examples 1-10 and comparative examples 1-2. As can be seen from FIG. 5, the elastic modulus of the co-sputter deposited TiCN coating is 250GPa to 450GPa, and the elastic modulus of the magnetron/arc composite deposited TiCN coating is 300GPa to 500 GPa. Therefore, the TiCN nano-structure coating prepared by adopting co-sputtering deposition or magnetron/arc composite deposition has more excellent mechanical property compared with the TiCN nano-structure coating prepared by a single process (magnetron sputtering or cathodic arc evaporation).
A ball disc type friction and wear testing machine is adopted to represent the friction coefficient and the wear rate of the coating, and FIG. 6 is a graph of the friction coefficient of the TiCN coating of the examples 1-10 and the comparative examples 1-2. As can be seen from FIG. 6, the coefficient of friction of the co-sputter deposited TiCN coating is 0.2-0.55, and the coefficient of friction of the magnetron/arc hybrid deposited TiCN coating is 0.25-0.7. It can be seen that the co-sputtering deposition or the magnetron/arc composite deposition can achieve a lower friction coefficient than the TiCN nanostructure coating prepared by a single process (magnetron sputtering or cathodic arc evaporation).
FIG. 7 is a graph of the wear rate of TiCN coatings for examples 1-10 and comparative examples 1-2. From fig. 7, the wear rate of the co-sputter deposited TiCN coating was 2 x 10 -16 m 3 /(N·m)-13*10 -16 m 3 /(N.m), magnetron/arc hybrid depositionWear rate of TiCN coating 1 x 10 -16 m 3 /(N·m)-11*10 -16 m 3 V (N.m). Therefore, the TiCN nano-structure coating prepared by adopting co-sputtering deposition or magnetron/arc composite deposition has more excellent wear resistance compared with the TiCN nano-structure coating prepared by adopting a single process (magnetron sputtering or cathodic arc evaporation).
The above examples are preferred embodiments of the present invention, but the present invention is not limited to the above examples, 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 they are included in the scope of the present invention.
Claims (10)
1. A TiCN coating characterized by: the TiCN coating has the component content Ti/(Ti + C + N) atomic ratio of 35-65% and C/(C + N) atomic ratio of 20-70%; the TiCN coating has a wear rate of 1 x 10 -16 m 3 /(N·m)-13×10 -16 m 3 /(N·m)。
2. The TiCN coating according to claim 1, characterized in that: the hardness of the TiCN coating is 15GPa-40 GPa; the elastic modulus of the TiCN coating is 250GPa-500 GPa; the TiCN coating has a friction coefficient of 0.2-0.7.
3. A method of preparing a TiCN coating according to claim 1 or 2, characterized in that: the method comprises the following steps:
in the nitrogen atmosphere, magnetically controlling and sputtering a TiC target material and a Ti target material at the same time, and carrying out co-sputtering deposition on the surface of a base material to prepare a TiCN coating;
or in the nitrogen atmosphere, simultaneously carrying out magnetron sputtering on the TiC target material and carrying out cathodic arc evaporation on the Ti target material, and carrying out composite deposition on the surface of the substrate material to prepare the TiCN coating.
4. The production method according to claim 3, characterized in that: the TiC target and the Ti target are simultaneously subjected to magnetron sputtering, wherein the average sputtering power of the TiC target is 1W/cm 2 ～15W/cm 2 (ii) a Flatness of the Ti targetThe average sputtering power is 1W/cm 2 ～30W/cm 2 。
5. The production method according to claim 3, characterized in that: the TiC target material is simultaneously magnetically sputtered and the Ti target material is evaporated by cathodic arc, wherein the average sputtering power of the TiC target material is 1W/cm 2 ～15W/cm 2 (ii) a The average current density of the Ti target material is 0.25A/cm 2 ～5A/cm 2 。
6. The production method according to claim 3, characterized in that: the pressure of the nitrogen gas for the co-sputtering deposition is 0.2 Pa-1.2 Pa; the pressure of the nitrogen for composite deposition is 0.4 Pa-3.5 Pa.
7. The method of claim 6, wherein: the temperature of the co-sputtering deposition is 360-440 ℃; the temperature of the composite deposition is 360-440 ℃.
8. The method of claim 7, wherein: the time of the co-sputtering deposition or the composite deposition is 0.5h-4 h.
9. The method of claim 8, wherein: the base material further comprises a cleaning step before the co-sputtering deposition or the composite deposition.
10. Use of a TiCN coating according to claim 1 or 2 in metal surface treatment or metal working.
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| CN105463372A (en) * | 2015-12-11 | 2016-04-06 | 西北有色金属研究院 | Preparation method of multi-layer composite super-thick self-lubricating hard coating |
| CN110184566A (en) * | 2019-06-05 | 2019-08-30 | 广东省新材料研究所 | A kind of hard coat of Color tunable and preparation method thereof |
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