CN106119784A - A kind of Ti Al Mo N multicomponent hard Gradient Film and its preparation method and application - Google Patents
A kind of Ti Al Mo N multicomponent hard Gradient Film and its preparation method and application Download PDFInfo
- Publication number
- CN106119784A CN106119784A CN201610674114.3A CN201610674114A CN106119784A CN 106119784 A CN106119784 A CN 106119784A CN 201610674114 A CN201610674114 A CN 201610674114A CN 106119784 A CN106119784 A CN 106119784A
- Authority
- CN
- China
- Prior art keywords
- ion plating
- arc ion
- gradient film
- coating
- target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of Ti Al Mo N multicomponent hard Gradient Film and its preparation method and application；Belong to special material preparing technical field.Institute of the present invention Ti Al Mo N multicomponent hard Gradient Film includes subordinate's component: Ti 55% 85%, Al 8% 30%, Mo 4% 15%, N 3% 25% by percentage to the quality.Described Gradient Film is prepared as the coating with matrix/TiN/Ti Al Mo N by arc ion plating；This coating can be used for papermaking, print field.Instant component is reasonable in design, and technique is simple, it is simple to apply on a large scale, especially applies on a large scale at print field.
Description
Technical field
The present invention relates to a kind of Ti-Al-Mo-N multicomponent hard Gradient Film and its preparation method and application；Belong to extraordinary material
Material preparing technical field.
Background technology
Arc ion plating is to trigger, at negative electrode and anode, the electric arc that ignites, and arc discharge is only at one or several of target material surface
Carrying out at intensive arc speckle, it is uniform that arc speckle does the whole target of random motion on cathode targets surface with the speed of tens meters per second
Consuming, in cathodic arc deposition, deposition material is to be evaporated by the effect of vacuum arc, source material in electric arc circuit
As negative electrode, the basic process of most of electric arcs all occurs at cathode chamber electric arc point, and the typical sizes of electric arc point is several microns, and
And have the highest electric current density.By the evaporant obtained by arc evaporation by electronics, ion, neutral gas-phase atom and microgranule
Composition.Directly produce plasma can arrange in any direction according to workpiece shapes from negative electrode without molten bath, cathode targets, make folder
Tool is greatly simplified.
Arc ion plating is high because of its deposition, on workpiece cleaning technique simply and on environment without impact before plated film, therefore
To fast development.Under vacuum, utilize gas glow discharge to make gas ionization, produce ion bombardment effects, steam the most at last
Stimulating food and reactant are deposited on matrix.The general film adhesion of product that arc ion plating is deposited is strong, and high energy particle is not
Disconnected bombardment can promote diffusion into the surface and the enhanced primary treatment of film layer；Compared to electric arc for chemical plating, plating, thermal spraying from
Sub-plated product membrane uniformity is preferable, density of film big, and film deposition rate is fast, and being heated evenly property is good.
Arc ion plating TiN product hardness typically can reach about 2000HV, the at any time innovation of technique, rises as far back as TiN
Time the most often bring and Al2O3Relatively.TiAlN product is formed, due to the addition of Al after arc ion plating TiN introduces Al element
Under high temperature, Al diffuses to the surface, and can form one layer of alumina protective layer, wear-resisting for coating of this tunic, and corrosion resisting property helps very
Greatly.
The main research point using arc ion plating (aip) to prepare multicomponent film layer at present is: 1. alloy target material and simple metal
Being applied in combination and content problem of target.2. the adhesion between film base, the adhesion problem between film layer and film layer.3. maximum
Degree strengthens hardness.But up to the present, on matrix prepared by method such as SKD2 ink knife surface arc ion plating
Wear-and corrosion-resistant Ti-Al-Mo-N multicomponent hard Gradient Coating Materials, at home and abroad there is not been reported.
Summary of the invention
The present invention is directed to the defect of prior art, it is provided that a kind of Ti-Al-Mo-N multicomponent hard Gradient Film and preparation side thereof
Method and application.
One Ti-Al-Mo-N multicomponent hard Gradient Film of the present invention；Include following component by percentage to the quality:
Ti 55%-85%, preferably 67%-83%, more preferably 70%-80%；
Al 8%-30%, preferably 10%-21%, more preferably 12%-20%；
Mo 4%-15%, preferably 4%-12%, more preferably 5%-10%；
N 3%-25%, preferably 3%-23%, more preferably 3%-22%.
The preparation method of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, including following proposal: with Ti-Al-
Mo alloys target is raw material, by arc ion plating, prepares Ti-Al-Mo-N multicomponent hard Gradient Film at surface of the work；Electricity
Before arc ion plating, control the vacuum in cvd furnace less than or equal to 0.03Pa；During deposition, in control stove, N air pressure is by force 2.2-
2.66Pa, the electric current controlling Ti-Al-Mo alloys target is 70-80A, control workpiece rotational frequency is 4～6r/min, controls plating temperature
For 450-500 DEG C；
Described Ti-Al-Mo alloys target includes following component by percentage to the quality:
Ti 55%-85%；
Al 10%-30%；
Mo 5%-15%.
The preparation method of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, during arc ion plating, controls deposition
Time is 20-30min.
The preparation method of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, the system of described Ti-Al-Mo alloys target
Preparation Method is:
Take pure titanium, fine aluminium, Ti-Mo intermediate alloy as raw material by design team's distribution, carried out at least 2 to joining the raw material taken
Secondary, preferably 3 vacuum metling, obtains described Ti-Al-Mo alloys target.
Described pure titanium is industrially pure titanium, and its purity is more than or equal to 99.9%；Described fine aluminium is industrial high-purity Al, and its purity is big
In equal to 99.9%；In described Ti-Mo intermediate alloy, the weight/mass percentage composition of impurity is less than 0.1%.
The application of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, including by described Ti-Al-Mo-N multicomponent
Hard Gradient Film making coatings, the structure of described coating is matrix/TiN/Ti-Al-Mo-N.
As preferably, the application of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, the thickness of TiN in described coating
Degree is 0.5-1.2 micron.In described TiN, the weight/mass percentage composition of N is 16-25%, and surplus is Ti.
As preferably, the application of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, Ti-Al-in described coating
The thickness of Mo-N is 1.5-3.0 micron.
As preferably, the application of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, described matrix is selected from SKD1
At least one in ink knife, SKD2 ink knife, ROE ink knife, ABE ink knife, SKH-2 ink knife, preferably
For SKD2 ink knife.
As preferably, the application of the present invention a kind of Ti-Al-Mo-N multicomponent hard Gradient Film, the preparation side of described coating
Method comprises the steps:
Step one
It is that 0.07-0.09um, the preferably base material of 0.08um are placed in arc ions by surface cleaning and surface smoothness Ra
In coating apparatus, the pressure being evacuated in arc ion plating apparatus is 0.03-0.003Pa, then passes to argon to arc ions
When pressure in coating apparatus is 0.16-0.22Pa, opening low energy ion source, the temperature controlled in arc ion plating apparatus is 200
DEG C-250 DEG C, control accelerating potential is 2.3-6.0Kv, is preferably 4.0Kv, and arc stream is 80-100A, it is clear that base material carries out activation
Wash；Obtain activated substrate；
Step 2
With pure Ti for Ti target, Ti target and step one gained activated substrate are placed in arc ion plating apparatus, take out
Vacuum is 0.03-0.003Pa to the pressure in arc ion plating apparatus, control simultaneously the bias of activated matrix for-400～-
450V；Then passing to N gas to the dividing potential drop of the N gas in arc ion plating apparatus is that 1.2-1.4Pa is (owing to reaction film intracavity only has one
Plant reacting gas, so N edema caused by disorder of QI pressure is stagnation pressure.) and to control the electric current of Ti target be 55-60A, carries out arc ion plating,
Rear closing control power supply, is cooled to room temperature with arc ion plating apparatus, obtains the base material with TiN layer；Carry out arc ion plating
Time, the rotating speed controlling activated substrate is 4～6r/min, control plating temperature is 380-400 DEG C；
Step 3
Step 2 gained is placed in arc ion plating apparatus with base material and the Ti-Al-Mo alloys target of TiN layer, takes out true
Empty pressure to arc ion plating apparatus is 0.03-0.003Pa, and the bias simultaneously controlling activated matrix is-400～-450V,
Being passed through N gas to the dividing potential drop of the N gas in arc ion plating apparatus is 2.2-2.66Pa, and the electric current controlling Ti-Al-Mo alloys target is
70-80A, carries out arc ion plating, obtains described coating；When carrying out arc ion plating, control the rotating speed of the base material with TiN layer
Be 4～6r/min, control plating temperature be 450-500 DEG C.
Preferably, in step one, base material is carried out activation and cleans 10-15min.
When industrial applications, surface cleaning and the base material that surface smoothness Ra is 0.07-0.09um are by following side
Prepared by case:
Matrix (such as SKD2 ink knife matrix) is mechanically polished on buffing machine, is polished to about Ra0.08um.
Polishing sample clean water is clean, dries and is placed in platter.Dip acetone wiping plating surface with absorbent cotton, remove surface oil
Dirt, corrosion, oxide layer and impurity.After acetone wiping, clear water rinses, and releases in ultrasonic cleaning 10-in spirituous beaker
15min.Ultrasonic complete, take out deionized water and clean, dry, to be plated.
Preferably, in step 2, the time carrying out arc ion plating is 15-20min.
Preferably, in step 3, the time carrying out arc ion plating is time 20-30min.
Preferably, in step 3, carrying out after arc ion plating terminates, closing control power supply, with arc ion plating
Equipment is cooled to room temperature.
Preferably, described arc ion plating apparatus is Bulat-6 type multi-Arc Ion Plating.Coater is by vacuum
System, coating system and electric control system composition, without additional magnetic filtration system.There are three arc sources in coating chamber, select a left side
Arc source, right both sides starting the arc deposition.
When described arc ion plating apparatus is Bulat-6 type multi-Arc Ion Plating, described Ti target is circular；Institute
Stating a diameter of φ 60mm of circular, thickness is 42mm.
When described arc ion plating apparatus is Bulat-6 type multi-Arc Ion Plating, step 3 carries out arc ion plating
After end, closing Hall and control power supply, workpiece is cooled to room temperature with film chamber and takes out, and seals preservation to be measured.After workpiece takes out, ion
Coater needs evacuation, treats use next time.
Target involved in the present invention such as Ti target, Ti-Al-Mo alloys target can size be processed according to the actual requirements.
Coating designed by the present invention, can be used for the field such as papermaking, printing.
Principal advantage
The present invention passes through arc ion plating (aip), is first bombarded pretreatment by Ar gas at matrix (such as ink blade surface)；Then
It is passed through N gas depositing TiN coating to improve adhesion between multicomponent hard coating；Finally melted self-control alloy target material is sunk
Amass to workpiece, obtain the hard coat that wear and corrosion behavior is excellent.
The present invention uses arc ion plating (aip), is divided by workpiece bias, nitrogen when substrate pretreated process system, plating
The isoparametric synergism of pressure, plating time, arc stream, workpiece rotational frequency, gained coating achieves unexpected effect, the most in fact
Show the matched well of coating mechanical property and serviceability.
Principle and advantage
Meanwhile, present invention is alternatively directed in the defect of domestic scraper properties of product, it is provided that a kind of hard in stable binary system
Plasma membrane TiAlN adds Mo element, obtains the coating with matrix/TiN/Ti-Al-Mo-N structure.When this coating be used for printing,
Serving unexpected effect during papermaking, its possible cause is:
Mo has the self-lubricating property of solid, and it can form MoO3 phase in process of friction and wear and have good wear-resisting
Subtract wiping effect.This system is possible not only to play Al element and forms the anti-corrosion function of alumina protective layer, moreover it is possible to play Mo element
Excellent resistance to wear away wiping property and then be greatly promoted its using effect.
Coating structure of the present invention is matrix/TiN/Ti-Al-Mo-N, and first plating last layer TiN on matrix is in order to preferably
Adhesion between film layer, and in mature T i-Al system, addition Mo element makes the wearability of coating be obviously enhanced.
Compared to methods such as laser melting coating, thermal sprayings, the inventive method can carry out depositing (typically existing at a lower temperature
About 500 DEG C), the Effect on Mechanical Properties that the inhomogeneities that so can keep from heat is caused；Compared to chemical gaseous phase deposition and
The methods such as chemical plating, the mode of production of the inventive method is simple, and ionization level is high, and productivity effect is big, is more beneficial for realizing market and produces
Industry.Arc ion plating Ti-Al-Mo-N has not only widened manufacture of materials field, reduces production cost, improves production effect
Rate, and effectively improve decay resistance and the coating wear resistance of coating.
In a word, the present invention passes through the design of multicomponent hard Gradient Film component, respectively prepares ginseng by constituent element hard Gradient Film
The synergism of number, reaches excellent effect, simultaneously when this multicomponent hard Gradient Film case design structure is applied to coating, and should
Coating show in the field such as papermaking, printing purpose less than advantage,
Detailed description of the invention
For problems such as current ink knife quick abrasion, efficiency are low, the invention provides a kind of wear-and corrosion-resistant hard coat
Preparation method.
Embodiment 1
(1) determination of deposition technique and the preparation of alloy target material:
Using Bulat-6 type multi-Arc Ion Plating deposition coating, coater is by vacuum system, coating system, Yi Ji electricity
Gas control system forms, without additional magnetic filtration system.There are three arc sources in coating chamber, select arc source, left and right sides starting the arc deposition.
The design of target, choose and prepare: during plating TIN coating, selecting the industrially pure titanium target bought, purity 99.9%,
Titanium target shape is processed into a diameter of φ 60mm according to equipment requirements, and thickness is the circular of 42mm.Plating Ti-Al-Mo-N coating
Time, target selects self-control alloys target.Alloys target composition is designed as: the mass percent of Ti is 75%, the mass percent of Al is
20%, the mass percent of Mo is 5%.Alloys target all carries out three vacuum melting, molten alloy by vacuum induction melting furnace
Material is: industrially pure titanium, purity 99.9%；The high-purity Al of industry, purity 99.9%；Ti-Mo intermediate alloy, purity 99.9%.
Line cutting technology is utilized to be processed into the size of needs according to equipment requirements the target prepared.
(2) substrate pretreated:
1. chemistry abatement processes: mechanically polished on buffing machine by ink knife matrix, is polished to Ra0.08um left
Right.Polishing sample clean water is clean, dries and is placed in platter.Dip acetone wiping plating surface with absorbent cotton, remove table
Face greasy dirt, corrosion, oxide layer and impurity.After acetone wiping, clear water rinses, and releases in ultrasonic cleaning in spirituous beaker
15min.Ultrasonic complete, take out deionized water and clean, dry, to be plated.
2. Ar gas pretreating process: before ion film plating, is evacuated to 0.03Pa by film room vacuum background and is passed through Ar gas, to stove
When pressure is increased to 0.16Pa, opening low energy ion source, temperature is maintained between 220 DEG C, accelerating potential is 4.0Kv, arc stream is
80A, sample is carried out activation clean 15min.
(3) electric arc ion-plating deposition coating process:
1. TiN film floor plating technology determines: film room vacuum is evacuated to 0.03Pa, and matrix adds-420V bias, is passed through N gas, by N
Air pressure is maintained at by force 1.25Pa, and titanium target arc current is adjusted to 58A, and workpiece rotational frequency keeps 5r/min, and plating temperature is 400 DEG C, heavy
Long-pending time 15min.
2. Ti-Al-Mo-N film layer plating technology determines: according to coating structure requirement, after matrix plates TiN.Close Hall
Controlling power supply, plated TiN workpiece and be cooled to room temperature with film chamber, calibration vacuum is to 0.03Pa, and matrix adds-450V bias, is passed through N
Air pressure is maintained at by force 2.66Pa, alloys target arc current is adjusted to 73A, workpiece rotational frequency keeps 5r/min, plating temperature to be 470 DEG C,
Sedimentation time 30min.
3. after deposition, closing Hall and control power supply, workpiece is cooled to room temperature with film chamber and takes out, and sealing preserves to be measured.
After taking-up, ion plating equipment needs evacuation, treats use next time.In gained Ti-Al-Mo-N film layer, by percentage to the quality, by under
State component to form:
Ti 71%, Al 18%, Mo 4%, N 7%.
Testing through SEM, the thickness of TiN+Ti-Al-Mo-N is about 3.4um；Recording hardness HIT with nanohardness tester is
3.54GPa, recording coating elastic modulus E IT is 400.6Gpa；Test through electrochemistry experiment, coating corrosion electric current density
3.29uA, contrasts matrix corrosion electric current density 19.3uA, and after plating, corrosion resistance promotes about 6 times.
Embodiment 2
(1) determination of deposition technique and the preparation of alloy target material:
Using Bulat-6 type multi-Arc Ion Plating deposition coating, coater is by vacuum system, coating system, Yi Ji electricity
Gas control system forms, without additional magnetic filtration system.There are three arc sources in coating chamber, select arc source, left and right sides starting the arc deposition.
The design of target, choose and prepare: during plating TIN coating, selecting the industrially pure titanium target bought, purity 99.9%,
Titanium target shape is processed into a diameter of φ 60mm according to equipment requirements, and thickness is the circular of 42mm.Plating Ti-Al-Mo-N coating
Time, target selects self-control alloys target.Alloys target composition is designed as: the mass percent of Ti is 75%, the mass percent of Al is
18%, the mass percent of Mo is 7%.Alloys target all carries out three vacuum melting, molten alloy by vacuum induction melting furnace
Material is: industrially pure titanium, purity 99.9%；The high-purity Al of industry, purity 99.9%；Ti-Mo intermediate alloy, purity 99.9%.
Line cutting technology is utilized to be processed into the size of needs according to equipment requirements the target prepared.
(2) substrate pretreated:
1. chemistry abatement processes: SKD2 ink knife matrix is mechanically polished on buffing machine, is polished to
About Ra0.08um.Polishing sample clean water is clean, dries and is placed in platter.Acetone wiping plating table is dipped with absorbent cotton
Face, removes surface and oil contaminant, corrosion, oxide layer and impurity.After acetone wiping, clear water rinses, and releases in spirituous beaker
Middle ultrasonic cleaning 15min.Ultrasonic complete, take out deionized water and clean, dry, to be plated.
2. Ar gas pretreating process: before ion film plating, is evacuated to 0.03Pa by film room vacuum background and is passed through Ar gas, to stove
When pressure is increased to 0.22Pa, opening low energy ion source, temperature is maintained between 250 DEG C, accelerating potential is 4.0Kv, arc stream is
100A, sample is carried out activation clean 15min.
(3) electric arc ion-plating deposition coating process:
1. TiN film floor plating technology determines: film room vacuum is evacuated to 0.03Pa, and matrix adds-450V bias, is passed through N gas, by N
Air pressure is maintained at by force 1.35Pa, and titanium target arc current is adjusted to 60A, and workpiece rotational frequency keeps 5r/min, and plating temperature is 400 DEG C, heavy
Long-pending time 10min.
2. Ti-Al-Mo-N film layer plating technology determines: according to coating structure requirement, after matrix plates TiN.Close Hall
Controlling power supply, plated TiN workpiece and be cooled to room temperature with film chamber, calibration vacuum is to 0.03Pa, and matrix adds-450V bias, is passed through N
Air pressure is maintained at by force 2.45Pa, alloys target arc current is adjusted to 80A, workpiece rotational frequency keeps 5r/min, plating temperature to be 500 DEG C,
Sedimentation time 20min.
3. after deposition, closing Hall and control power supply, workpiece is cooled to room temperature with film chamber and takes out, and sealing preserves to be measured.
After taking-up, ion plating equipment needs evacuation, treats use next time.In gained Ti-Al-Mo-N film layer, by percentage to the quality, by under
State component to form:
Ti 70%, Al 15%, Mo 6%, N 9%.
Testing through SEM, the thickness of TiN+Ti-Al-Mo-N is about 2.34um；Recording hardness HIT with nanohardness tester is
3.96GPa, recording coating elastic modulus E IT is 344.6Gpa；Test through electrochemistry experiment, coating corrosion electric current density
3.35uA, contrasts matrix corrosion electric current density 19.3uA, and after plating, corrosion resistance promotes about 6 times.
Embodiment 3
(1) determination of deposition technique and the preparation of alloy target material:
Using Bulat-6 type multi-Arc Ion Plating deposition coating, coater is by vacuum system, coating system, Yi Ji electricity
Gas control system forms, without additional magnetic filtration system.There are three arc sources in coating chamber, select arc source, left and right sides starting the arc deposition.
The design of target, choose and prepare: during plating TIN coating, selecting the industrially pure titanium target bought, purity 99.9%,
Titanium target shape is processed into a diameter of φ 60mm according to equipment requirements, and thickness is the circular of 42mm.Plating Ti-Al-Mo-N coating
Time, target selects self-control alloys target.Alloys target composition is designed as: the mass percent of Ti is 70%, the mass percent of Al is
15%, the mass percent of Mo is 15%.Alloys target all carries out three vacuum melting, molten alloy by vacuum induction melting furnace
Material is: industrially pure titanium, purity 99.9%；The high-purity Al of industry, purity 99.9%；Ti-Mo intermediate alloy, purity 99.9%.
Line cutting technology is utilized to be processed into the size of needs according to equipment requirements the target prepared.
(2) substrate pretreated:
1. chemistry abatement processes: mechanically polished on buffing machine by ink knife matrix, is polished to Ra0.08um left
Right.Polishing sample clean water is clean, dries and is placed in platter.Dip acetone wiping plating surface with absorbent cotton, remove table
Face greasy dirt, corrosion, oxide layer and impurity.After acetone wiping, clear water rinses, and releases in ultrasonic cleaning in spirituous beaker
15min.Ultrasonic complete, take out deionized water and clean, dry, to be plated.
2. Ar gas pretreating process: before ion film plating, is evacuated to 0.03Pa by film room vacuum background and is passed through Ar gas, to stove
When pressure is increased to 0.20Pa, opening low energy ion source, temperature is maintained between 240 DEG C, accelerating potential is 4.0Kv, arc stream is
85A, sample is carried out activation clean 15min.
(3) electric arc ion-plating deposition coating process:
1. TiN film floor plating technology determines: film room vacuum is evacuated to 0.03Pa, and matrix adds-400V bias, is passed through N gas, by N
Air pressure is maintained at by force 1.30Pa, and titanium target arc current is adjusted to 55A, and workpiece rotational frequency keeps 5r/min, and plating temperature is 400 DEG C, heavy
Long-pending time 15min.
2. Ti-Al-Mo-N film layer plating technology determines: according to coating structure requirement, after matrix plates TiN.Close Hall
Controlling power supply, plated TiN workpiece and be cooled to room temperature with film chamber, calibration vacuum is to 0.03Pa, and matrix adds-450V bias, is passed through N
Air pressure is maintained at by force 2.50Pa, alloys target arc current is adjusted to 75A, workpiece rotational frequency keeps 5r/min, plating temperature to be 450 DEG C,
Sedimentation time 30min.
3. after deposition, closing Hall and control power supply, workpiece is cooled to room temperature with film chamber and takes out, and sealing preserves to be measured.
After taking-up, ion plating equipment needs evacuation, treats use next time.In gained Ti-Al-Mo-N film layer, by percentage to the quality, by under
State component to form:
Ti 65%, Al 10%, Mo 10%, N 15%.
Testing through SEM, the thickness of TiN+Ti-Al-Mo-N is about 4.13um；Recording hardness HIT with nanohardness tester is
2.97GPa, recording coating elastic modulus E IT is 344.9Gpa；Test through electrochemistry experiment, coating corrosion electric current density
3.82uA, contrasts matrix corrosion electric current density 19.3uA, and after plating, corrosion resistance promotes about 5 times.
Embodiment 4
(1) determination of deposition technique and the preparation of alloy target material:
Using Bulat-6 type multi-Arc Ion Plating deposition coating, coater is by vacuum system, coating system, Yi Ji electricity
Gas control system forms, without additional magnetic filtration system.There are three arc sources in coating chamber, select arc source, left and right sides starting the arc deposition.
The design of target, choose and prepare: during plating TIN coating, selecting the industrially pure titanium target bought, purity 99.9%,
Titanium target shape is processed into a diameter of φ 60mm according to equipment requirements, and thickness is the circular of 42mm.Plating Ti-Al-Mo-N coating
Time, target selects self-control alloys target.Alloys target composition is designed as: the mass percent of Ti is 80%, the mass percent of Al is
15%, the mass percent of Mo is 5%.Alloys target all carries out three vacuum melting, molten alloy by vacuum induction melting furnace
Material is: industrially pure titanium, purity 99.9%；The high-purity Al of industry, purity 99.9%；Ti-Mo intermediate alloy, purity 99.9%.
Line cutting technology is utilized to be processed into the size of needs according to equipment requirements the target prepared.
(2) substrate pretreated:
1. chemistry abatement processes: mechanically polished on buffing machine by ink knife matrix, is polished to Ra0.08um left
Right.Polishing sample clean water is clean, dries and is placed in platter.Dip acetone wiping plating surface with absorbent cotton, remove table
Face greasy dirt, corrosion, oxide layer and impurity.After acetone wiping, clear water rinses, and releases in ultrasonic cleaning in spirituous beaker
15min.Ultrasonic complete, take out deionized water and clean, dry, to be plated.
2. Ar gas pretreating process: before ion film plating, is evacuated to 0.03Pa by film room vacuum background and is passed through Ar gas, to stove
When pressure is increased to 0.22Pa, opening low energy ion source, temperature is maintained between 250 DEG C, accelerating potential is 4.0Kv, arc stream is
100A, sample is carried out activation clean 15min.
(3) electric arc ion-plating deposition coating process:
1. TiN film floor plating technology determines: film room vacuum is evacuated to 0.03Pa, and matrix adds-450V bias, is passed through N gas, by N
Air pressure is maintained at by force 1.40Pa, and titanium target arc current is adjusted to 60A, and workpiece rotational frequency keeps 5r/min, and plating temperature is 400 DEG C, heavy
Long-pending time 20min.
2. Ti-Al-Mo-N film layer plating technology determines: according to coating structure requirement, after matrix plates TiN.Close Hall
Controlling power supply, plated TiN workpiece and be cooled to room temperature with film chamber, calibration vacuum is to 0.03Pa, and matrix adds-450V bias, is passed through N
Air pressure is maintained at by force 2.66Pa, alloys target arc current is adjusted to 80A, workpiece rotational frequency keeps 5r/min, plating temperature to be 500 DEG C,
Sedimentation time 30min.
3. after deposition, closing Hall and control power supply, workpiece is cooled to room temperature with film chamber and takes out, and sealing preserves to be measured.
After taking-up, ion plating equipment needs evacuation, treats use next time.In gained Ti-Al-Mo-N film layer, by percentage to the quality, by under
State component to form:
Ti 72%, Al 10%, Mo 4%, N14%.
Testing through SEM, the thickness of TiN+Ti-Al-Mo-N is about 4.79um；Recording hardness HIT with nanohardness tester is
4.16GPa, recording coating elastic modulus E IT is 375.3Gpa；Test through electrochemistry experiment, coating corrosion electric current density
2.78uA, contrasts matrix corrosion electric current density 19.3uA, and after plating, corrosion resistance promotes about 7 times.
The technical scheme that the embodiment of the present invention provides has the benefit that the Ni-P-Cu-prepared compared to Brush Plating
Optimal hardness value 1200HV of TiN coating, the hardness of the inventive method coating is significantly increased, and depositional coating is uniform, film
Layer density is big, the time significantly shortens.
Claims (10)
1. a Ti-Al-Mo-N multicomponent hard Gradient Film；It is characterized in that including following component by percentage to the quality:
2. the method preparing Ti-Al-Mo-N multicomponent hard Gradient Film as claimed in claim 1, it is characterised in that bag
Include following proposal:
With Ti-Al-Mo alloys target as raw material, by arc ion plating, prepare Ti-Al-Mo-N multicomponent at surface of the work
Hard Gradient Film；Before arc ion plating, control the vacuum in cvd furnace less than or equal to 0.03Pa；During deposition, control N gas in stove
Pressure is 2.2-2.66Pa, and the electric current controlling Ti-Al-Mo alloys target is 70-80A, control workpiece rotational frequency is 4～6r/min, control
Plating temperature processed is 450-500 DEG C；
Described Ti-Al-Mo alloys target includes following component by percentage to the quality:
Ti 55%-85%；
Al 10%-30%；
Mo 5%-15%.
The preparation method of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 2, it is characterised in that:
During arc ion plating, control sedimentation time is 20-30min.
The preparation method of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 2, it is characterised in that；
The preparation method of described Ti-Al-Mo alloys target is:
Take pure titanium, fine aluminium, Ti-Mo intermediate alloy as raw material by design team's distribution, to joined the raw material taken carry out at least 2 times true
Empty smelting, obtains described Ti-Al-Mo alloys target.
5. the application of a Ti-Al-Mo-N multicomponent hard Gradient Film as claimed in claim 1, it is characterised in that: include by
Described Ti-Al-Mo-N multicomponent hard Gradient Film making coatings, the structure of described coating is matrix/TiN/Ti-Al-Mo-N.
The application of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 5, it is characterised in that:
In described coating, the thickness of TiN is 0.5-1.2 micron.In described TiN, the weight/mass percentage composition of N is 16-25%, and surplus is
Ti；
In described coating, the thickness of Ti-Al-Mo-N is 1.5-3.0 micron.
The application of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 5, it is characterised in that:
Described matrix is scraped selected from SKD1 ink knife, SKD2 ink knife, ROE ink knife, ABE ink knife, SKH-2 ink
At least one in cutter.
The application of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 5, it is characterised in that；Described
The preparation method of coating comprises the steps:
Step one
By surface cleaning and surface smoothness Ra be 0.07-0.09um, the base material that is preferably 0.08um is placed in arc ion plating and sets
Standby interior, the pressure being evacuated in arc ion plating apparatus is 0.03-0.003Pa, then passes to argon and sets to arc ion plating
When standby interior pressure is 0.16-0.22Pa, open low energy ion source, control the temperature in arc ion plating apparatus be 200 DEG C-
250 DEG C, control accelerating potential is 2.3-6.0Kv, is preferably 4.0Kv, and arc stream is 80-100A, base material carries out activation cleaning；?
To activated substrate；
Step 2
With pure Ti for Ti target, Ti target and step one gained activated substrate are placed in arc ion plating apparatus, evacuation
Pressure to arc ion plating apparatus is 0.03-0.003Pa, and the bias simultaneously controlling activated matrix is-400～-450V；So
After to be passed through N gas to the dividing potential drop of the N gas in arc ion plating apparatus be 1.2-1.4Pa；And the electric current controlling Ti target is 55-60A,
Carry out arc ion plating, last closing control power supply, be cooled to room temperature with arc ion plating apparatus, obtain the base with TiN layer
Material；When carrying out arc ion plating, the rotating speed controlling activated substrate is 4～6r/min, control plating temperature is 380-400 DEG C；
Step 3
Step 2 gained is placed in arc ion plating apparatus with base material and the Ti-Al-Mo alloys target of TiN layer, is evacuated to
Pressure in arc ion plating apparatus is 0.03-0.003Pa, and the bias simultaneously controlling activated matrix is-400～-450V, is passed through
N gas is 2.2-2.66Pa to the dividing potential drop of the N gas in arc ion plating apparatus, and the electric current controlling Ti-Al-Mo alloys target is 70-
80A, carries out arc ion plating, obtains described coating；When carrying out arc ion plating, controlling the rotating speed with the base material of TiN layer is 4
～6r/min, control plating temperature are 450-500 DEG C.
The application of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 8, it is characterised in that:
In step one, base material is carried out activation and cleans 10-15min；
In step 2, the time carrying out arc ion plating is 15-20min；
In step 3, the time carrying out arc ion plating is time 20-30min.
The application of a kind of Ti-Al-Mo-N multicomponent hard Gradient Film the most according to claim 5, it is characterised in that: institute
The coating of design, can be used for papermaking, print field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610674114.3A CN106119784B (en) | 2016-08-16 | 2016-08-16 | A kind of Ti-Al-Mo-N multicomponent hards Gradient Film and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610674114.3A CN106119784B (en) | 2016-08-16 | 2016-08-16 | A kind of Ti-Al-Mo-N multicomponent hards Gradient Film and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106119784A true CN106119784A (en) | 2016-11-16 |
| CN106119784B CN106119784B (en) | 2018-08-17 |
Family
ID=57259099
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610674114.3A Active CN106119784B (en) | 2016-08-16 | 2016-08-16 | A kind of Ti-Al-Mo-N multicomponent hards Gradient Film and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106119784B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108118299A (en) * | 2017-12-20 | 2018-06-05 | 中国科学院合肥物质科学研究院 | A kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method |
| CN111394705A (en) * | 2020-03-19 | 2020-07-10 | 河北宏靶科技有限公司 | Titanium-aluminum-molybdenum alloy target material and preparation method thereof |
| CN113166919A (en) * | 2018-11-30 | 2021-07-23 | 韩国冶金株式会社 | Hard coating for cutting tool |
| CN115161631A (en) * | 2022-07-05 | 2022-10-11 | 凯诺建设有限公司 | Spatula with composite metal coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597751A (en) * | 2009-04-22 | 2009-12-09 | 江苏科技大学 | Zr-Al-Si-N hard composite coating and preparation method thereof |
| CN101698933A (en) * | 2009-10-30 | 2010-04-28 | 华南理工大学 | Multi-element Ti-Al-N nanometer composite laminated coating and preparation method thereof |
| CN102409308A (en) * | 2011-10-11 | 2012-04-11 | 宁波市瑞通新材料科技有限公司 | Preparation and heat treatment method of Ti-Mo-N multi-element film |
-
2016
- 2016-08-16 CN CN201610674114.3A patent/CN106119784B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597751A (en) * | 2009-04-22 | 2009-12-09 | 江苏科技大学 | Zr-Al-Si-N hard composite coating and preparation method thereof |
| CN101698933A (en) * | 2009-10-30 | 2010-04-28 | 华南理工大学 | Multi-element Ti-Al-N nanometer composite laminated coating and preparation method thereof |
| CN102409308A (en) * | 2011-10-11 | 2012-04-11 | 宁波市瑞通新材料科技有限公司 | Preparation and heat treatment method of Ti-Mo-N multi-element film |
Non-Patent Citations (2)
| Title |
|---|
| C.J.TRAVARES等: "Structure determination on (Ti,Al)N/Mo multilayers", 《THIN SOLID FILMS》 * |
| 崔贯英等: "多弧离子镀（Ti，Al，Zr）N多元超硬梯度膜的制备及力学性能研究", 《真空科学与技术学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108118299A (en) * | 2017-12-20 | 2018-06-05 | 中国科学院合肥物质科学研究院 | A kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method |
| CN108118299B (en) * | 2017-12-20 | 2019-06-28 | 中国科学院合肥物质科学研究院 | A kind of nitridation molybdenum base graded multicomponent nano-composite coating and preparation method |
| CN113166919A (en) * | 2018-11-30 | 2021-07-23 | 韩国冶金株式会社 | Hard coating for cutting tool |
| CN113166919B (en) * | 2018-11-30 | 2023-08-01 | 韩国冶金株式会社 | Hard coating for cutting tool |
| CN111394705A (en) * | 2020-03-19 | 2020-07-10 | 河北宏靶科技有限公司 | Titanium-aluminum-molybdenum alloy target material and preparation method thereof |
| CN115161631A (en) * | 2022-07-05 | 2022-10-11 | 凯诺建设有限公司 | Spatula with composite metal coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106119784B (en) | 2018-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101698362B (en) | Self-lubricating hard nanocomposite laminated coating and preparation method thereof | |
| CN106119784B (en) | A kind of Ti-Al-Mo-N multicomponent hards Gradient Film and its preparation method and application | |
| JP5856148B2 (en) | PVD hybrid method for depositing mixed crystal layers | |
| CN104508171B (en) | Coat system, the matrix of coating and the method with coat system coating matrix surface | |
| CN101230448B (en) | Method for preparing multi-arc ion plating aluminium titanium chrome silicon yttrium nitride multi-component ultra-hard reaction film | |
| CN101092688A (en) | Ion plating modified method for bipolar plate of stainless steel for fuel cell in type of proton exchange membrane | |
| JPS6319590B2 (en) | ||
| CN107058943A (en) | TiCN/CrCN nano-multilayer films and preparation method thereof | |
| WO2008007095A1 (en) | Coating apparatus and method | |
| CN107937873A (en) | Transition metal boride coating, carbon transition metal boride composite coating, preparation method and application and the cutting element of carbon doping | |
| WO2022172954A1 (en) | Coated tool | |
| KR102095344B1 (en) | Coated cutting tool | |
| CN105925946A (en) | Method for preparing TiN or CrN film on surface of aluminum alloy through magnetron sputtering method | |
| CN106929799A (en) | High temperature resistant protective coating and preparation method and application | |
| CN102943240A (en) | Multifunctional plasma enhanced coating system | |
| CN102534514A (en) | Method for plating films of multi-arc ion plating | |
| CN101591766B (en) | Method for preparing titanium-aluminum-zirconium nitride multicomponent hard reaction gradient film | |
| KR20140057253A (en) | Cathodic arc deposition | |
| CN103774092B (en) | It is a kind of to prepare conductive and corrosion-resistant finishes method in Mg alloy surface | |
| Yongqiang et al. | Effects of pulsed bias duty ratio on microstructure and surface properties of TiN films | |
| CN109487214A (en) | A kind of magnesium-alloy surface coating method and Corrosion-resistant magnesia alloy prepared therefrom | |
| Bagcivan et al. | Comparison of (Cr0. 75Al0. 25) N Coatings Deposited by Conventional and High Power Pulsed Magnetron Sputtering | |
| Zhu et al. | Influence of Arc Current on SurfaceProperties and Corrosion Resistance of AlCrN CoatingsDepositedby Multi-arc Ion Plating | |
| CN108251810B (en) | Preparation method of corrosion-resistant sintered neodymium-iron-boron magnet | |
| KR20120129445A (en) | The method of high wear and oxidation resistant multi-layer coating material process. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191016 Address after: No. 1018, xinkaipu Road, Tianxin District, Changsha City, Hunan Province Patentee after: Changsha Kehui Furnace Technology Co., Ltd. Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Patentee before: Central South University |
|
| TR01 | Transfer of patent right |