CN110004415A - High tenacity and the thick Ti/TiAlN laminated coating of high rigidity and preparation method thereof - Google Patents
High tenacity and the thick Ti/TiAlN laminated coating of high rigidity and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—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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Abstract
The present invention relates to hard protection coatings field, specially a kind of high tenacity and the thick Ti/TiAlN laminated coating of high rigidity and preparation method thereof.It is deposited using general arc light ion coating apparatus, selects Ti target and TiAl target as cathode targets, which is deposited on cemented carbide substrate surfaces；The Ti/TiAlN laminated coating is layer structure, including TiN transition zone, multiple TiAlN sublayers and Ti sublayer, the first layer for being deposited on matrix is TiN transition zone, the second layer is TiAlN sublayer, it is later Ti sublayer, TiAlN sublayer and Ti sublayer alternate superposition deposition, and outermost layer is TiAlN sublayer.Ti/TiAlN laminated coating of the present invention has the features such as high thickness, good film substrate bond strength, high rigidity, high tenacity, and has good antioxygenic property.
Description
Technical field:
The present invention relates to hard protection coatings field, the thick Ti/TiAlN multilayer of specially a kind of high tenacity and high rigidity is applied
Layer and preparation method thereof.
Background technique:
Cemented carbide cutting tool is the main force for the modern efficient cutter that China is carrying out, and demand is with average annual 30%
Above speed increases.With the development of modern manufacturing industry, stock-removing machine and Machining Technology for Cutting, which obtain, greatly to be improved, to cutting
Cutting knife tool is put forward higher requirements.Increasingly harsher service condition require cutting tool must have high rigidity, high-wearing feature,
The performances such as high tenacity, enough intensity and good inoxidizability.Applying hard coat on hard alloy cutter can mention
The comprehensive performances such as hardness, toughness and the inoxidizability of high tool surface.
Researcher's discovery, the thickness for increasing coating can significantly improve the cutting ability of cutter, processing efficiency, extend cutter
Service life (referring to document: Surf.Coat.Technol.188-189 (2004) 636-643).But hard ceramic is applied
Layer, with the increase of coating layer thickness, coating internal stress be will increase, in coating higher internal stress and intrinsic brittleness make coating with
The binding performance of substrate is reduced with the increase of thickness.The trend that single layer nitride coatings are peeled off when thickness is more than 6~7 μm is bright
Aobvious to increase, the serious thickness for restricting hard coat limits its industrial application significantly.Metal mistake is introduced in nitride hard coating
Layer is crossed, metal/nitride multi-layer composite coatings are constituted, metal layer can be such that the residual stress in coating obtains as buffer layer
Relaxation, substantially reduces internal stress, obtains the thick metal/nitride coating of the excellent in mechanical performance such as bond strength, toughness, hardness
(10 μm of >).
Chinese patent application (Publication No. CN102676982A) proposes a kind of Al-TiN composite coating, and prepared is compound
Coat inside structure is excellent, good with substrate combinating strength, improves the anti-cracking ability and wearability of coating, extends and uses the longevity
Life, while improving the high temperature oxidation resistance of coating.
Chinese patent application (Publication No. CN107012437A) proposes that a kind of high performance Ti/TiN/ (AlTiCuSi) N is applied
The coating surface quality of layer, alternating deposit preparation is high, coating dense uniform good with basal body binding force, and mechanical property is good.
Chinese patent application (Publication No. CN102161106A) proposes a kind of Ti-TiN&Ti-MoS2/ Ti double-pole finishing coat
Cutter, the comprehensive Ti-TiN high hardness spray coating cutter of the coated cutting tool and Ti-MoS2The advantages of/Ti lubricant coating cutter, both had
Higher hardness, and there is lower coefficient of friction, so that the performance of coated cutting tool is increased significantly.
Summary of the invention:
The problem of for current application practice, it is an object of that present invention to provide a kind of high tenacity and high rigidity
Ti/TiAlN laminated coating and preparation method thereof, the Ti/TiAlN laminated coating have high thickness, good film substrate bond strength,
The features such as high rigidity, high tenacity, and have good antioxygenic property.In addition, the present invention proposes and prepares different Ti sublayers thickness
The Ti/TiAlN laminated coating of degree is regulated and controled under the premise of not changing coating component content using the thickness of Ti sublayer
The hardness and toughness of laminated coating.
The technical scheme is that
A kind of thick Ti/TiAlN laminated coating of high tenacity and high rigidity, is sunk using general arc light ion coating apparatus
Product selects Ti target and TiAl target as cathode targets, which is deposited on cemented carbide substrate surfaces；It is described
Ti/TiAlN laminated coating is layer structure, including TiN transition zone, multiple TiAlN sublayers and Ti sublayer, is deposited on the of matrix
One layer is TiN transition zone, and it is later Ti sublayer, TiAlN sublayer and Ti sublayer alternate superposition that the second layer, which is TiAlN sublayer,
Deposition, outermost layer are TiAlN sublayer.
The thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, TiN transition zone with a thickness of 0.1 μm, each
TiAlN molecular layers thick is 1.5~1.7 μm, and each Ti molecular layers thick is 0.1~0.8 μm, total number of plies of Ti/TiAlN laminated coating
For the even number in 14~24 layers.
The thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, it is preferred that Ti/TiAlN laminated coating it is total
Thickness is adjustable in 14.4~17.1 μ ms.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, the specific steps are as follows:
(1) matrix is pre-processed: the in the mixed solvent that hard alloy substrate is put into dehydrated alcohol and acetone is carried out 5~
15min ultrasonic cleaning, to remove surface and oil contaminant, oxidation film dirt；
(2) icon bombardment cleaning matrix: the matrix pre-processed is loaded on specimen holder, is put into ion plating vacuum chamber
It is interior, room door is closed, being evacuated to vacuum degree is 8.0 × 10-3After Pa or less, it is passed through argon gas, maintains vacuum degree in 0.3~0.5Pa,
It is 800~1200V that matrix, which applies negative bias values, and duty ratio is 50~70%, carries out 5~15min icon bombardment cleaning to matrix；
(3) depositing TiN transition zone: cutting argon gas is passed through nitrogen, maintains vacuum degree air pressure in 1.0~2.0Pa, matrix arteries and veins
Negative bias values control is rushed in 500~700V, Ti target current is opened, is deposited, sedimentation time is 1~10min；
(4) alternating deposit TiAlN sublayer and Ti sublayer: depositing Ti AlN sublayer first closes Ti target current, maintains nitrogen
In 1.5~2.0Pa, substrate negative voltage value is 500~600V for air pressure, and sedimentation time is 18~20min；Subsequent depositing Ti sublayer,
TiAl target current is closed, nitrogen is cut off, is passed through argon gas, operating air pressure is made to maintain 0.3~0.6Pa, substrate negative voltage value is changed to
100~200V, sedimentation time are controlled in 2~9min；TiAlN sublayer and Ti sublayer successively alternating deposit；
(5) outermost layer TiAlN is deposited: after the last layer Ti sublayer deposits, redeposited TiAlN outermost layer, and technique ginseng
Number is identical as step (4).
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, it is in step (1), matrix is pre-
Before processing, matrix first passes through the grinding of SiC sand paper, polishing treatment.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, step (2) is into (5), argon
The bulk purity of gas and nitrogen is 99.99%.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, step (3) is into (5), Ti
Target purity is 99.99wt%, and TiAl target atom ratio is Ti:Al=1:1, the size of Ti target and TiAl target be diameter 80~
120mm, 50~70mm of height, target-substrate distance is from for 180~220mm；In TiN transition zone, atomic ratio Ti:N=1:1；TiAlN sublayer
In, atomic ratio Ti:Al:N=1:1:2.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, step (3) to (5) deposited
Cheng Zhong, target current are controlled in 60~80A, and stable duty ratio is 15~25%.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, step (3) to (5) deposited
Cheng Zhong, specimen holder rotation, revolving speed are controlled in 4~6rpm.
The preparation method of the thick Ti/TiAlN laminated coating of the high tenacity and high rigidity, in whole process, matrix is not
Heating.
Design philosophy of the invention is:
The present invention prepares the thick Ti/TiAlN laminated coating of different sublayer ratios, and the coating and matrix bonding state are good,
The thickness proportion of sublayer determines the hardness and toughness of coating, can achieve by regulation molecular layers thick ratio obtain different hardness and
The laminated coating of toughness value, the coating system are suitable for the application environment of different operating conditions.
Advantages of the present invention and beneficial effect are:
1. the present invention can effectively reduce coating internal stress by control metal layer thickness, prevents cracking and peel off, obtain thickness
The laminated coating excellent more than 10 μm of bond strengths can extend the guard time of coating, increase cutting-tool's used life.
2. the present invention by ion-plating deposition technology can quickly be inhibited crackle generate and extension, high rigidity, high tenacity
Ti/TiAlN laminated coating, technical indicator is as follows: hardness HV=1758~2915, passes through observation coating cross sections impression and generates
Crack length evaluate, crackle is longer, and toughness is poorer, and Ti/TiAlN multilayer coating system of the present invention resists the energy of crack propagation
Power is stronger.Due to TiAlN layers have good inoxidizability, so Ti/TiAlN multilayer coating system of the present invention be likewise supplied with it is good
Good antioxygenic property.
3. sublayer of the invention is easily controllable with total coating thickness, preparation method is simple, and cost is relatively low, can easily realize thickness
The design of hard coat.
Detailed description of the invention:
Fig. 1 is the 1 gained laminated coating surface Ti/TiAlN (a) of embodiment and section (b) scanning electron microscope pattern photo；
Fig. 2 is 1 gained Ti/TiAlN laminated coating section indentation crack pattern photo of embodiment；
Fig. 3 is 4 gained Ti/TiAlN laminated coating Cross Section Morphology of embodiment and section indentation crack pattern photo；
Fig. 4 is TiAlN signal layer coating Cross Section Morphology (a) and section indentation crack pattern (b) photo obtained by comparative example.
Specific embodiment:
In the specific implementation process, the preparation method of the thick Ti/TiAlN laminated coating of high tenacity and high rigidity of the present invention,
Including pretreatment base, icon bombardment cleaning matrix, depositing TiN transition zone, alternating deposit TiAlN sublayer and Ti sublayer, outermost layer
TiAlN deposition.The Ti/TiAlN laminated coating is deposited using general arc light ion coating apparatus, selects Ti target and TiAl target
As cathode targets, which is deposited on cemented carbide substrate surfaces；The Ti/TiAlN laminated coating is
Layer structure, including TiN transition zone, multiple TiAlN sublayers and Ti sublayer, the first layer for being deposited on matrix is TiN transition zone, the
Two layers are TiAlN sublayer, are later Ti sublayer, and TiAlN sublayer and Ti sublayer alternate superposition deposition, outermost layer TiAlN
Sublayer.
The thick Ti/TiAlN laminated coating performance detection of high tenacity and high rigidity of the present invention is as follows:
1. hardness test: using micro Vickers (model: Buehler Micromet 5114), plus load is
25gf, dwell time 10s；
After coating cross sections grinding, polishing treatment, cleans up in dehydrated alcohol, sample is put on the glass sheet later
(selected test is face-up), one piece is put on objective table；Suitable section hardness test position is selected using 500 times of object lens first
It sets, then loads 25gf, after pressure maintaining 10s, demarcate two catercorner lengths of impression, obtain corresponding hardness number, each sample
Test 8 times, is averaged.
2. toughness evaluation: using the toughness of coating cross sections plus load indentation method analysis coating, using the above hardness test
Micro Vickers apply load, plus load 100gf, dwell time 10s；Then scanning electron microscope is utilized
(SEM, model: Philips FEI-Inspect F) observes crack morphology around impression, evaluates the toughness of coating.
Below by specific embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
This.
Embodiment 1
In the present embodiment, hard alloy (WC-6wt.%Co, mass fraction) is ground with SiC sand paper, after polishing treatment,
It is put into the solution of acetone and ethyl alcohol 1:1 mixing by volume, is cleaned by ultrasonic 15min, to remove the dirts such as surface and oil contaminant, oxidation film
The matrix pre-processed is loaded on specimen holder by object, is put into ion plating vacuum chamber, is closed room door, is evacuated to vacuum
Degree is 5.0 × 10-3After Pa, it is passed through argon gas, maintains vacuum degree in 0.4Pa, it is 1000V that matrix, which applies negative bias values, and duty ratio is
60%, 10min icon bombardment cleaning is carried out to matrix.
After cleaning, argon gas is cut off, is passed through nitrogen, maintains vacuum degree air pressure in 1.5Pa, matrix pulsed negative bias value control
System is opened Ti target current, is deposited, sedimentation time 3min in 600V, forms TiN transition zone.Then carry out TiAlN sublayer
With the alternating deposit of Ti sublayer: depositing Ti AlN sublayer first closes Ti target current, maintains nitrogen pressure in 1.5Pa, and matrix is negative
Bias value is 550V, sedimentation time 18.5min；Subsequent depositing Ti sublayer, closes TiAl target current, cuts off nitrogen, is passed through argon
Gas makes operating air pressure maintain 0.3Pa, and substrate negative voltage value is changed to 100V, sedimentation time control in 2min, TiAlN sublayer and
Ti sublayer successively alternating deposit；After the last layer Ti sublayer deposits, redeposited TiAlN outermost layer, technological parameter institute as above
It states.In entire deposition process, specimen holder rotation, revolving speed is controlled in 5rpm；Target current is 70A, duty ratio 20%, and base
Body does not heat.Ti target purity is 99.99wt%, and TiAl target atom ratio is Ti:Al=1:1, and the size of Ti target and TiAl target is
Diameter 100mm, height 60mm, target-substrate distance is from for 200mm.
Wherein, TiN transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick is 1.7 μm, and each Ti molecular layers thick is
0.1 μm, total number of plies is 16 layers.In TiN transition zone, atomic ratio Ti:N=1:1 (i.e. Ti1N1)；In TiAlN sublayer, atomic ratio Ti:
Al:N=1:1:2 (i.e. Ti0.5Al0.5N1)。
As shown in Fig. 1 (a)-(b), surface topography observation is carried out to laminated coating, there are some sizes for discovery coating surface
Different molten drops, cross-section observation discovery TiAlN sublayer and Ti sublayer are evenly distributed dense structure, and Ti/TiAlN laminated coating passes through
Transition zone is well combined with matrix, and white is Ti sublayer, and dark gray is TiAlN sublayer.Detect Ti/TiAlN obtained by the present embodiment
The hardness number of laminated coating is HV 2915, and Fig. 2 is shown in toughness detection, and indentation edge certain length, discontinuous crack occurs, says
The bright extension for preventing crackle, improves the toughness of coating.
Embodiment 2
Difference from Example 1 is:
When TiAlN sublayer deposits, nitrogen pressure 1.6Pa, substrate negative voltage value is 520V, sedimentation time 18min；Ti
When sublayer deposits, for argon gas operating air pressure in 0.35Pa, substrate negative voltage value is 120V, and sedimentation time is controlled in 2.5min；Wherein,
TiN transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.7 μm, each Ti molecular layers thick be 0.2 μm, total number of plies
It is 16 layers.In TiN transition zone, atomic ratio Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
Ti/TiAlN laminated coating TiAlN sublayer and Ti sublayer obtained by the present embodiment are evenly distributed dense structure, Ti/
TiAlN laminated coating is well combined by transition zone and matrix.Detect the hardness of Ti/TiAlN laminated coating obtained by the present embodiment
Value is HV 2852, and toughness detection finds that the discontinuous crack length that indentation edge occurs shortens, prevents the extension of crackle, is improved
The toughness of coating.
Embodiment 3
Difference from Example 1 is:
When TiAlN sublayer deposits, nitrogen pressure 1.7Pa, substrate negative voltage value is 500V, sedimentation time 18min；Ti
When sublayer deposits, for argon gas operating air pressure in 0.4Pa, substrate negative voltage value is 150V, and sedimentation time is controlled in 3.5min；Wherein,
TiN transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.7 μm, each Ti molecular layers thick be 0.3 μm, total number of plies
It is 16 layers.In TiN transition zone, atomic ratio Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
Ti/TiAlN laminated coating TiAlN sublayer and Ti sublayer obtained by the present embodiment are evenly distributed dense structure, Ti/
TiAlN laminated coating is well combined by transition zone and matrix.Detect the hardness of Ti/TiAlN laminated coating obtained by the present embodiment
Value is HV 2611, and toughness detection finds that the discontinuous crack length that indentation edge occurs further shortens, prevents the expansion of crackle
Exhibition, further increases the toughness of coating.
Embodiment 4
Difference from Example 1 is:
When TiAlN sublayer deposits, nitrogen pressure 1.8Pa, substrate negative voltage value is 550V, sedimentation time 18.5min；
When Ti sublayer deposits, for argon gas operating air pressure in 0.45Pa, substrate negative voltage value is 180V, and sedimentation time is controlled in 4.5min；Its
In, TiN transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.7 μm, each Ti molecular layers thick be 0.4 μm, total layer
Number is 16 layers.In TiN transition zone, atomic ratio Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
Ti/TiAlN laminated coating obtained by the present embodiment, TiAlN sublayer and Ti sublayer are evenly distributed dense structure, Ti/
TiAlN laminated coating is well combined by transition zone and matrix.Detect the hardness of Ti/TiAlN laminated coating obtained by the present embodiment
Value is HV 2611, and Fig. 3 is shown in toughness detection, and indentation edge does not find obvious crackle, and the toughness of coating is further enhanced.
Embodiment 5
Difference from Example 1 is:
When TiAlN sublayer deposits, nitrogen pressure 1.9Pa, substrate negative voltage value is 550V, sedimentation time 19min；Ti
When sublayer deposits, for argon gas operating air pressure in 0.5Pa, substrate negative voltage value is 190V, and sedimentation time is controlled in 7min；Wherein, TiN
Transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.6 μm, each Ti molecular layers thick be 0.6 μm, total number of plies be 16
Layer.In TiN transition zone, atomic ratio Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
Ti/TiAlN laminated coating obtained by the present embodiment, TiAlN sublayer and Ti sublayer are evenly distributed dense structure, Ti/
TiAlN laminated coating is well combined by transition zone and matrix.Detect the hardness of Ti/TiAlN laminated coating obtained by the present embodiment
Value is HV 2193, and toughness detection discovery indentation edge does not find crackle, and the toughness of coating is further enhanced.
Embodiment 6
Difference from Example 1 is:
When TiAlN sublayer deposits, nitrogen pressure 2.0Pa, substrate negative voltage value is 600V, sedimentation time 20min；Ti
When sublayer deposits, for argon gas operating air pressure in 0.6Pa, substrate negative voltage value is 200V, and sedimentation time is controlled in 9min；Wherein, TiN
Transition zone with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.5 μm, each Ti molecular layers thick be 0.8 μm, total number of plies be 14
Layer.In TiN transition zone, atomic ratio Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
Ti/TiAlN laminated coating obtained by the present embodiment, TiAlN sublayer and Ti sublayer are evenly distributed dense structure, Ti/
TiAlN laminated coating is well combined by transition zone and matrix.Detect the hardness of Ti/TiAlN laminated coating obtained by the present embodiment
Value is HV 1758, and toughness detection discovery indentation edge does not find crackle, and the toughness of coating is further enhanced.
Comparative example
In this comparative example, thickness TiAlN signal layer coating is prepared, TiN transition zone depositing operation is identical as above embodiments.Deposition
When TiAlN signal layer coating, nitrogen pressure 2.0Pa, substrate negative voltage value is 600V, sedimentation time 135min, other depositions
Parameter is same as described above.
As shown in fig. 4 a, there are fine cracks in TiAlN signal layer coating Cross Section Morphology obtained by this comparative example, coat inside, always
With a thickness of 16.9 μm.Hardness and toughness test are carried out to signal layer coating, detection parameters are same as the previously described embodiments, obtain TiAlN
Hardness number is HV 3035, and toughness detection is shown in Fig. 4 b, 15 μm of long cracks occurs at the impression tip of section, be significantly longer than above-mentioned Ti/
TiAlN laminated coating illustrates that Ti/TiAlN laminated coating toughness is apparently higher than TiAlN signal layer coating.
Embodiment and comparative example the result shows that, Ti/TiAlN laminated coating of the present invention has high thickness, good film base junction
The features such as closing intensity, high rigidity, high tenacity, and have good antioxygenic property.The thick Ti/ prepared using process above
TiAlN laminated coating can be applicable on cemented carbide cutting tool, effectively plays and improves cutter hardness, toughness, extends and uses the longevity
The effect of life.
Claims (10)
1. the thick Ti/TiAlN laminated coating of a kind of high tenacity and high rigidity, which is characterized in that plated using general arc light ion
Equipment is deposited, and selects Ti target and TiAl target as cathode targets, which is deposited on carbide matrix
Body surface face；The Ti/TiAlN laminated coating is layer structure, including TiN transition zone, multiple TiAlN sublayers and Ti sublayer, is sunk
Product is TiN transition zone in the first layer of matrix, and it is later Ti sublayer that the second layer, which is TiAlN sublayer, TiAlN sublayer and Ti sublayer
Superposition deposition is alternateed, outermost layer is TiAlN sublayer.
2. the thick Ti/TiAlN laminated coating of high tenacity according to claim 1 and high rigidity, which is characterized in that TiN mistake
Cross layer with a thickness of 0.1 μm, each TiAlN molecular layers thick be 1.5~1.7 μm, each Ti molecular layers thick be 0.1~0.8 μm,
Total number of plies of Ti/TiAlN laminated coating is the even number in 14~24 layers.
3. the thick Ti/TiAlN laminated coating of high tenacity according to claim 2 and high rigidity, which is characterized in that preferably
, the overall thickness of Ti/TiAlN laminated coating is adjustable in 14.4~17.1 μ ms.
4. according to claim 1 to the preparation method of the thick Ti/TiAlN laminated coating of high tenacity and high rigidity described in one of 3,
It is characterized in that, specific step is as follows:
(1) it pre-processes matrix: 5~15min of in the mixed solvent progress that hard alloy substrate is put into dehydrated alcohol and acetone is surpassed
Sound cleaning, to remove surface and oil contaminant, oxidation film dirt；
(2) icon bombardment cleaning matrix: the matrix pre-processed is loaded on specimen holder, is put into ion plating vacuum chamber,
Room door is closed, being evacuated to vacuum degree is 8.0 × 10-3After Pa or less, it is passed through argon gas, maintains vacuum degree in 0.3~0.5Pa, base
It is 800~1200V that body, which applies negative bias values, and duty ratio is 50~70%, carries out 5~15min icon bombardment cleaning to matrix；
(3) depositing TiN transition zone: cutting argon gas is passed through nitrogen, maintains vacuum degree air pressure in 1.0~2.0Pa, and matrix pulse is negative
Bias value control is opened Ti target current, is deposited in 500~700V, and sedimentation time is 1~10min；
(4) alternating deposit TiAlN sublayer and Ti sublayer: depositing Ti AlN sublayer first closes Ti target current, maintains nitrogen pressure
In 1.5~2.0Pa, substrate negative voltage value is 500~600V, and sedimentation time is 18~20min；Subsequent depositing Ti sublayer, is closed
TiAl target current cuts off nitrogen, is passed through argon gas, and operating air pressure is made to maintain 0.3~0.6Pa, and substrate negative voltage value is changed to 100~
200V, sedimentation time are controlled in 2~9min；TiAlN sublayer and Ti sublayer successively alternating deposit；
(5) outermost layer TiAlN deposit: the last layer Ti sublayer deposit after, redeposited TiAlN outermost layer, technological parameter with
Step (4) is identical.
5. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, in step (1), before substrate pretreated, matrix first passes through the grinding of SiC sand paper, polishing treatment.
6. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, for step (2) into (5), the bulk purity of argon gas and nitrogen is 99.99%.
7. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, for step (3) into (5), Ti target purity is 99.99wt%, and TiAl target atom ratio is Ti:Al=1:1, Ti target and TiAl target
Size be 80~120mm of diameter, 50~70mm of height, target-substrate distance is from for 180~220mm；In TiN transition zone, atomic ratio
Ti:N=1:1；In TiAlN sublayer, atomic ratio Ti:Al:N=1:1:2.
8. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, in step (3) to (5) deposition process, target current is controlled in 60~80A, and stable duty ratio is 15~25%.
9. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, in step (3) to (5) deposition process, specimen holder rotation, revolving speed is controlled in 4~6rpm.
10. the preparation method of the thick Ti/TiAlN laminated coating of high tenacity according to claim 4 and high rigidity, feature
It is, in whole process, matrix is not heated.
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