CN108118299A - A kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method - Google Patents
A kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method Download PDFInfo
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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
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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
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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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- 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
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- 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
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Abstract
The invention discloses a kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method, which is arranged on the matrix of various heterogeneities, and structure is A Mo/Mox1Ay1N1‑x1‑y1/Mox2Aly2CZ2N(1‑x2‑y2‑z2)/Mox3Aly3CZ3Siu3N(1‑x3‑y3‑z3‑u3), wherein, essential elements of the A contained by matrix, 0<x,y,z<1.The present invention is by using more gradients, and the compound means of polynary nanometer improve the comprehensive performance of coating, and compared with prior art, the film prepared has higher hardness, film-substrate cohesion and inoxidizability and low coefficient of friction.
Description
Technical field
The present invention relates to thin-film material and Surface Science technical field more particularly to a kind of nitridation molybdenum base gradients
Polynary nanometer composite coating and preparation method.
Background technology
" made in China 2025 " explicitly points out green manufacturing and intelligence manufacture is the two principal themes of China's manufacturing industry development.Mesh
Before, also there are the problems such as precision is low, energy consumption is big for China's manufacturing industry.Therefore, how to improve material machining accuracy, reduce energy consumption
As urgent problem even as the bottleneck of some industries.Such as cutter, drill bit, mold etc. are in processing difficult-to-machine material
When how to put forward efficiency and precision, how energy exploration improves the service life of drill bit when deep layer detects, deepens investigation depth, with
And how the industries such as Aeronautics and Astronautics reduce friction, improve active time etc..
Process for modifying surface and process for surface coating come into being and of increased attention and attention.Coating knife
The appearance of tool, it is considered to be the revolution in metal cutting tool technograph.Ganoine thin film especially superhard thin film times
Favored.Super-hard film material is plated on metal cutting tool surface with PVD method, has both adapted to modern manufacturing industry to metal cutter
The high-tech requirement of tool, and meet green manufacturing theory.The metal cutting tool that surface is coated with superhard thin film had both maintained its base
The higher intensity of body, and the advantage of its face coat " superhard, tough, wear-resisting, self-lubricating " can be played, so as to substantially increase gold
Belong to durability and adaptability of the cutting tool in modern process.Therefore hard thin film material can be widely applied to machinery
The fields such as manufacture, auto industry, textile industry, geological drilling, mould industry, aerospace.
Common ganoine thin film for titanium-based and chromium base ganoine thin film (TiN, TiC, TiCN, TiAlN, CrN, CrAlN etc.) with
And diamond film and DLC film.Their coefficient of friction is very big, not only influences precision during cutting, but also energy consumption
It is high.Polycrystalline MoNx films are a kind of novel thin films developed in recent years, due to good property (high-melting-point, high electricity
Conductance, high specific surface area, good chemical stability), especially fabulous wearability (wear-resisting rate is approximately 14 times of titanium nitride)
And it gains great popularity.But MoNx coatings there is problems：1) oxidation resistance temperature is low (being less than 350 DEG C)；2) combined with matrix
Force difference；3) technique optimized on a kind of matrix is difficult to copy in other collectives, i.e., universality is poor.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of nitridation molybdenum base graded multicomponent is nano combined
Coating and preparation method, to solve, existing nitridation molybdenum base coating oxidation resistance temperature is low, poor with basal body binding force and universality is poor
Etc. technical problems.
The present invention is achieved by the following technical solutions：
The present invention provides a kind of nitridation molybdenum base graded multicomponent nano-composite coatings, which is arranged on matrix surface, by interior
Outwards successively by A-Mo films, Mox1Ay1N1-x1-y1Film, Mox2Aly2CZ2N(1-x2-y2-z2)Film and Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)
The structure of film composition is A-Mo/Mox1Ay1N1-x1-y1/Mox2Aly2CZ2N(1-x2-y2-z2)/Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)It receives
Rice composite coating, wherein, essential elements of the A contained by matrix, 0<x,y,z<1.
Further, the A-Mo film thicknesses are 5-15nm, Mox1Ay1N1-x1-y1Film thickness is 10-30nm,
Mox3Aly3CZ3N(1-x3-y3-z3)Film thickness is 50-500nm, Mox4Aly4CZ4Siu4N(1-x4-y4-z4-u4)Film thickness is 50-500nm, is applied
Layer overall thickness is 1-5 μm.
It is specific to use the present invention also provides a kind of preparation method of above-mentioned nitridation molybdenum base graded multicomponent nano-composite coating
Prepared by magnetic control sputtering device, comprise the following steps：
(1) surface preparation：Matrix surface is processed by shot blasting, substrate is obtained and is packed into sample stage as sample；
(2) A-Mo layers of preparation：A-Mo targets are mounted on DC cathode, sputter process is carried out under vacuum argon gas state, are made
It is A-Mo layers standby；
(3) A-Mo-N layers of preparation：Nitrogen is passed through, continues sputter process, prepares A-Mo-N layers；
(4)Mox2Aly2CZ2N(1-x2-y2-z2)It is prepared by layer：A-Mo target shielding power supplies are closed, by rotary sample to Mo-Al-C targets
Under, continue sputter process, prepare Mox2Aly2CZ2N(1-x2-y2-z2)Layer；
(5)Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)It is prepared by layer：Mo-Al-C target shielding power supplies are closed, rotary sample is arrived
Under Mo-Al-C-Si composition targets, continue sputter process, prepare Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)Layer.
(6) sputtering is completed, and sample cools down under vacuum, takes out sample, is obtained the nitridation molybdenum base graded multicomponent and is received
Rice laminated coating.
Further, in preparation process, the distance of target-sample surfaces is 40-80mm, and depositing temperature is 400-450 DEG C,
Argon gas nitrogen volume ratio is 4 in gaseous mixture：1-1：4, operating air pressure 0.4Pa-1.0Pa.
Further, the sputter process condition in preparation process meets：
When preparing A-Mo layers, sputtering power 40-60W, sputtering time 5-10min；
When preparing A-Mo-N layers, sputtering power 90-120W, sputtering time 15-30min；
Prepare Mox2Aly2CZ2N(1-x2-y2-z2)During layer, sputtering power 90-120W, sputtering time 10-20min；
Prepare Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)During layer, sputtering power 90-120W, sputtering time 80-
100min。
The present invention has the following advantages compared with prior art：The present invention provides a kind of nitridation molybdenum base graded multicomponent nanometers to answer
Close coating and preparation method, by using more gradients, the compound means of polynary nanometer improve the comprehensive performance of coating, and preparation obtains
The film obtained has higher hardness, film-substrate cohesion and inoxidizability and low coefficient of friction.
Description of the drawings
Fig. 1 is the section SEM pictures of nitridation molybdenum base graded multicomponent nano-composite coating；
Fig. 2 is that the nano-indentation hardness after different coating is deposited on stainless steel (lCrl7Mo) sheet matrix；
Fig. 3 is the bond strength of the coating and matrix on stainless steel (lCrl7Mo) sheet matrix after deposition different coating；
Fig. 4 is the coefficient of friction of the coating after deposition different coating on stainless steel (lCrl7Mo) sheet matrix；
Fig. 5 is the oxidation resistance temperature of the coating after deposition different coating on stainless steel (lCrl7Mo) sheet matrix.
Specific embodiment
Embodiment 1
One kind is present embodiments provided using lCrl7Mo stainless steel substrates as matrix, nitridation molybdenum base is prepared using magnetic control sputtering device
The method of graded multicomponent nano-composite coating, comprises the following steps：
(1) surface preparation：By stainless steel (lCrl7Mo) piece it is polished, cleaning obtain substrate after, be packed into sample stage on；
(2) Cr-Mo layers of preparation：Cr-Mo targets are mounted on DC cathode, the distance for adjusting target and sample is 40-
80mm, start, is evacuated to 8 × 10-4Pa, heated substrate to 400-450 DEG C (depositing temperature) are passed through argon gas, adjust work gas
It is depressed into 0.4-1Pa；Shielding power supply is opened, adjustment sputtering power is 40-60W, controls sputtering time 5-10min, prepares Cr-Mo
Layer；
(3) Mo-Cr-N layers of preparation：Nitrogen is passed through, it is 4 to keep the volume ratio that argon gas nitrogen is passed through：1-1：4, operating air pressure
For 0.4-1Pa, adjustment sputtering power is 90-120W, controls sputtering time 15-30min, prepares Mo-Cr-N layers；
(4)Mox2Aly2CZ2N(1-x2-y2-z2)It is prepared by layer：Cr-Mo target shielding power supplies are closed, rotary sample to Mo-Al-C targets
Under, holding sputtering power is 90-120W, and time control is in 10-20min, preparation Mox2Aly2CZ2N(1-x2-y2-z2)Layer；
(5)Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)It is prepared by layer：Mo-Al-C target shielding power supplies are closed, rotary sample is arrived
Under Mo-Al-C-Si composition targets, holding sputtering power is 90-120W, and time control is in 80-100min, preparation
Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)Layer；
(6) sputtering is completed, and closes sputtering, heating power supply, stops ventilation, and sample cools down under conditions of molecular pump vacuumizes
To less than 100 DEG C, molecular pump is closed, sample after being cooled to room temperature under natural vacuum, is taken out in powered-down source.
Using the direct cutting sample of diamond tool, SEM observations are carried out, obtain SEM sectional views as shown in Figure 1
Piece, it can be seen that coating be by component gradient change nano composite structure, by substrate to surface mainly by：
MoCr, Mo-Cr-N, Mo-Al-N, Mo-Al-C-N, Mo-Al-Si-C-N are formed.
Mo-Cr, Mo-Cr-N, Mo-Al-C-N, Mo- are deposited respectively in stainless steel (lCrl7Mo) on piece using the above method
Al-C-Si-N and nitridation molybdenum base graded multicomponent nano laminated coating of the present invention, the nano impress for comparing different coating are hard
Spend (nano-hardness tester detection) and the bond strength of coating and matrix, the coefficient of friction of coating, oxidation resistance temperature, as a result such as Fig. 2-
Shown in 5：Fig. 2 shows to deposit different coating Mo-Cr, Mo-Cr-N, Mo-Al-N, Mo-Al- on stainless steel (lCrl7Mo) sheet matrix
The hardness of C-N, Mo-Al-C-Si-N film layer is respectively 7,19,23,31,37GPa；These coatings with hardness and ingredient all gradients
Increased form arrangement, prepares graded multicomponent nano-composite coating Mo-Cr/Mo-Cr-N/Mo-Al-C-N/Mo-Al-C-Si-N
Nano-indentation hardness for 39GPa, higher than the hardness of all above coating.Fig. 3 shows to sink on stainless steel (lCrl7Mo) sheet matrix
The film-substrate cohesion of product different coating Mo-Cr, Mo-Cr-N, Mo-Al-N, Mo-Al-C-N, Mo-Al-C-Si-N film layer is respectively
58,35,33,42,48；These coatings in the form of component gradient is increased are arranged, prepare graded multicomponent nano-composite coating
The film-substrate cohesion 74N of Mo-Cr/Mo-Cr-N/Mo-Al-C-N/Mo-Al-C-Si-N, better than the combination power of other coatings.Fig. 4
Show the coefficient of friction of deposition different coating Mo-Cr, Mo-Cr-N, Mo-Al-C-N film layer on stainless steel (lCrl7Mo) sheet matrix
Respectively 0.47,0.40,0.25, these coatings in the form of component gradient is increased are arranged, graded multicomponent nanometer is prepared and answers
The coefficient of friction for closing coating Mo-Cr/Mo-Cr-N/Mo-Al-C-N/Mo-Al-C-Si-N is 0.15, less than the friction of other coatings
Coefficient illustrates that the coating has better greasy property.Fig. 5 shows to deposit different coating on stainless steel (lCrl7Mo) sheet matrix
The oxidation resistance temperature of Mo-Cr-N, Mo-Al-N, Mo-Al-C-N are respectively 510,650,780 DEG C.These coatings with component gradient
Increased form arrangement, prepares graded multicomponent nano-composite coating Mo-Cr/Mo-Cr-N/Mo-Al-C-N/Mo-Al-C-Si-N
Oxidation resistance temperature for 800 DEG C, it is higher than the anti-oxidantization temperature of other coatings.The result of complex chart 1-5, it can be seen that utilize this
Nitridation molybdenum base graded multicomponent nano laminated coating prepared by inventive method, hardness are all significantly increased compared to more other coatings, and
And the combination power of matrix is strong, and inoxidizability is high and coefficient of friction is low.
Be above a kind of detailed embodiment of the invention and specific operating process, be using technical solution of the present invention before
It puts and is implemented, but protection scope of the present invention is not limited to the above embodiments.
Claims (5)
1. a kind of nitridation molybdenum base graded multicomponent nano-composite coating, the coating are arranged on matrix surface, which is characterized in that are by introversion
Outside successively by A-Mo films, Mox1Ay1N1-x1-y1Film, Mox3Aly3CZ3N(1-x3-y3-z3)Film and Mox4Aly4CZ4Siu4N(1-x4-y4-z4-u4)Film
The structure of composition is A-Mo/Mox1Ay1N1-x1-y1/Mox2Aly2CZ2N(1-x2-y2-z2)/Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)Receive
Rice composite coating, wherein, essential elements of the A contained by matrix, 0<x,y,z,u<1.
A kind of 2. nitridation molybdenum base graded multicomponent nano-composite coating according to claim 1, which is characterized in that the A-Mo
Film thickness is 5-15nm, Mox1Ay1N1-x1-y1Film thickness is 10-30nm, Mox3Aly3CZ3N(1-x3-y3-z3)Film and
Mox4Aly4CZ4Siu4N(1-x4-y4-z4-u4)Film thickness is 50-500nm, and total coating thickness is 1-5 μm.
3. a kind of preparation method of nitridation molybdenum base graded multicomponent nano-composite coating as described in claim 1-2, feature exist
In comprising the following steps：
(1) surface preparation：Matrix surface is processed by shot blasting, obtains the sample that substrate is packed into magnetic control sputtering device as sample
On platform；
(2) A-Mo layers of preparation：A-Mo targets are mounted on DC cathode, sputter process is carried out under vacuum argon gas state, prepare A-
Mo layers；
(3) A-Mo-N layers of preparation：Nitrogen is passed through, continues sputter process, prepares A-Mo-N layers；
(4)Mox2Aly2CZ2N(1-x2-y2-z2)It is prepared by layer：A-Mo target shielding power supplies are closed, by under rotary sample to Mo-Al-C targets, after
Continuous sputter process, prepares Mox2Aly2CZ2N(1-x2-y2-z2)Layer；
(5)Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)It is prepared by layer：Mo-Al-C target shielding power supplies are closed, rotary sample to Mo-Al-
Under C-Si composition targets, continue sputter process, prepare Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)Layer.
(6) sputtering is completed, and sample cools down under vacuum, takes out sample, and it is more to obtain the nitridation molybdenum base graded multicomponent nanometer
Layer coating.
4. a kind of preparation method for nitrogenizing molybdenum base graded multicomponent nano-composite coating according to claim 3, feature exist
In in preparation process, the distance of target-sample surfaces is 40-80mm, and depositing temperature is 400-450 DEG C, argon gas nitrogen in gaseous mixture
Air volume ratio is 4：1-1：4, operating air pressure 0.4Pa-1.0Pa.
5. a kind of preparation method for nitrogenizing molybdenum base graded multicomponent nano-composite coating according to claim 3, feature exist
In the sputter process condition in preparation process meets：
When preparing A-Mo layers, sputtering power 40-60W, sputtering time 5-10min；
When preparing A-Mo-N layers, sputtering power 90-120W, sputtering time 15-30min；
Prepare Mox2Aly2CZ2N(1-x2-y2-z2)During layer, sputtering power 90-120W, sputtering time 10-20min；
Prepare Mox3Aly3CZ3Siu3N(1-x3-y3-z3-u3)During layer, sputtering power 90-120W, sputtering time 80-100min.
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