CN107299330A - A kind of low internal stress coating and preparation method thereof - Google Patents
A kind of low internal stress coating and preparation method thereof Download PDFInfo
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- CN107299330A CN107299330A CN201710222844.4A CN201710222844A CN107299330A CN 107299330 A CN107299330 A CN 107299330A CN 201710222844 A CN201710222844 A CN 201710222844A CN 107299330 A CN107299330 A CN 107299330A
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- voltage
- internal stress
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- plating
- low internal
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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
- C23C14/54—Controlling or regulating the coating process
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a kind of low internal stress coating and preparation method thereof, the preparation method of the low internal stress coating, including cleaning matrix material, plating binder course, plating modulating layer and plating four steps of functional layer, it is characterised in that：Adjustable voltage is used during described plating binder course, voltage is gradually increased to plate to the voltage V1 of modulating layer process from the magnitude of voltage V0 of cleaning matrix material process.Voltage that the present invention is gradually increasing using 40V to 120V in the preparation process of coating so that target molecule is adhered on workpiece, can substantially reduce the internal stress of coating, so as to extend the service life of coating so that target molecule is collided to workpiece.
Description
Technical field
The invention belongs to metal alloy compositions field, and in particular to a kind of low internal stress coating and preparation method thereof.
Background technology
Coating (coating) is that coating once applies resulting solid-state continuous film, is to protect, insulate, decorate
Purpose, is coated on the plastic sheet on the matrixes such as metal, fabric, plastics.Coating can be gaseous state, liquid, solid-state, generally according to
The matrix of spraying is needed to determine the species and state of coating.
At present, a complete PVD coating procedure, typically include cleaning workpiece surface, plating binder course, plating modulating layer,
This four steps of plating functional layer, wherein the process of plating binder course is especially important for whole coating, because binder course and work
The conjugation between compactness and binder course and modulating layer between part, affects the internal stress of whole PVD coatings.If
Internal stress is big, then workpiece can cause the damage of workpiece, have a strong impact on the life-span of workpiece when using to a certain extent.If interior
Stress very little, then workpiece can have a relatively long physical life.At present, the process of binder course is plated, is generally all to use
Fixed voltage, according to fixed voltage, then target is all to impact workpiece according to fixed dynamics, when target particle impacting to workpiece
On quantity when being more than the number of particles for departing from workpiece surface, target particle will stick to workpiece surface, when using fixed electricity
During pressure, dynamics on target particle impacting to workpiece is than more uniform, when target particle is already adhered to workpiece surface, after receiving
During the particle impacting come, it may occur that certain displacement or deformation, that is to say, that first adhere to the particle of workpiece surface, because external force
Effect so that " pulling force " between adjacent particles produces fluctuation, and some places " pulling force " are big, some places " pulling force " are small, this
The stress increase of coat inside is allowed for, when PVD coatings are used to a certain extent, due to the effect of internal stress, whole coating
May moment avalanche, had a strong impact on the service life of workpiece.
The content of the invention
In order to solve problem above, the present invention proposes a kind of low internal stress coating and preparation method thereof, using the present invention's
Preparation method, the coating internal stress prepared is low, can greatly prolong the service life of workpiece.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：A kind of preparation side of low internal stress coating
Method, it is mainly during the plating binder course of PVD coatings, using adjustable voltage, by voltage from the electricity of cleaning process
Pressure value V0 is gradually increased to plate the voltage V1 of modulating layer process.In the process, being continuously increased due to magnitude of voltage, target particle
The dynamics for impacting workpiece can be increasing, and the strength that target particle adheres to workpiece surface is increasing, and the dynamics of adhesion
It is more and more firm.And due to the increase of voltage so that target particle adheres to the particle of workpiece surface even in crashing into originally
When, the relatively small particle impacting of original adhesion dynamics can also be come so that the bigger particle of adhesion dynamics can be more preferable
Combination on the surface of workpiece so that final target particle can be combined firmly in workpiece surface very much, and because impact dynamics
Increase, so as to eliminate the weak target particle of adhesion so that the anisotropic of target particle reduces, so as to reduce coating
Internal stress, greatly add service life.
Further, described adjustable voltage, magnitude of voltage is incrementally increased from the magnitude of voltage V0 of initial cleaning process
To the voltage V1 of plating modulating layer process.The mode of described regulation voltage includes：By the way of increase and decrease reactive power, wattful power
The mode or the mode of change network parameter that rate and reactive power are combined carry out pressure regulation.Specifically, the idle work(of described increase and decrease
The mode of rate includes regulator generator, phase modifier, shunt capacitor and shunt reactor；Described active power and reactive power
Combination includes regulation transformer, changes load tap changer pressure regulation；The mode of described change network parameter includes using
Series capacitor, throwing stop paired running transformer, throw and stop unloaded or underloading high-tension line etc..
Further, described adjustable voltage, magnitude of voltage is incrementally increased from the magnitude of voltage V0 of initial cleaning process
To the voltage V1 of plating modulating layer process, the required time is 10-60min；It is preferred that, the required time is 20-40min；
It is further preferred that the required time is 30min.Using 10-60min time, can cause plating modulating layer during, after
The particle of workpiece surface is already attached to before the effective Ground shock waves of particle in face so that the unstable particle of adhesion is bombarded,
The similar particle of remaining dynamics can stick to workpiece surface, reduce the anisotropic of metallic so that the entirety of coating
Internal stress reduces.
Further, described adjustable voltage, the magnitude of voltage V0 of cleaning process initially size is 30-50V, compared with
To be preferred, V0 size is (40 ± 0.004) V.Initial voltage keeps identical with the voltage of cleaning process, during cleaning,
Using V0 voltage, hydrogen or argon gas can be allowd more easily to bombard workpiece surface, workpiece surface is cleaned
Compare clean, and will not disfiguring workpiece surface.
Further, described adjustable voltage, final magnitude of voltage V1 is the magnitude of voltage of plating modulating layer, V1 size
For 100-150V, more preferred, V1 size is (120 ± 0.012) V.Under this voltage, target particle can be with workpiece knot
Closing must be than stronger.Transition is gentle between binder course and modulating layer, and metallic cohesion is stronger, and anisotropic reduces, coating planted agent
Power reduces.
Further, the material of the functional layer is selected from the amount of Al and Cr material in AlCr, and/or the AlCr materials
Ratio be 70/30.
In addition, the invention also provides low internal stress coating prepared by above-mentioned preparation method, it includes being coated in matrix material
Binder course and the multiple composite beds being covered on binder course on material, described composite bed include modulating layer and are covered in modulating layer
On functional layer, the thickness of the binder course is 0.2-0.7 μm, and/or the thickness of the modulating layer is 0.18 μm, and/or institute
The thickness for stating functional layer is 0.05-0.15 μm, and/or the thickness of the composite bed is 1.15-1.65 μm.
Compared with prior art, advantages of the present invention includes：The invention provides a kind of low internal stress coating and its preparation
Method, by being collided in the preparation process of coating using 40V to the 120V voltages being gradually increasing to target molecule, so that
Target molecule is adhered on workpiece, the internal stress of coating can be substantially reduced, so as to extend the service life of coating.The present invention
It is 70/30 by being used as the ratio of the amount of Al and Cr material in functional layer, and AlCr materials from AlCr materials so that the present invention
The external active force items of functional layer of coating are identical, can effectively improve the action effect of functional layer, play unexpected effect.
Brief description of the drawings
Fig. 1 is the structural representation of low internal stress coating among a typical embodiments of the invention；
Description of reference numerals, 1- matrix materials, 2- binder courses, 31- modulating layers, 32- functional layers 32.
Embodiment
More detailed explanation will hereafter be made to technical scheme.It is understood, however, that in model of the present invention
, can between above-mentioned each technical characteristic of the invention and each technical characteristic specifically described in below (eg embodiment) in enclosing
It is combined with each other, so as to constitute new or preferred technical scheme.As space is limited, no longer tire out one by one herein and state.
With reference to specific embodiment, the present invention is described in detail：
Embodiment 1
A kind of preparation method of low internal stress coating, including cleaning matrix material, plating binder course, plating modulating layer and plating function
Four step of layer, adjustable voltage is used during described plating binder course, by voltage from the electricity of cleaning matrix material process
Pressure value V0 is gradually increased to plate the voltage V1 of modulating layer process.
Further, during voltage is adjusted, adjusted by the way of active power be combined with each other with reactive power
Voltage.
Further, magnitude of voltage incrementally increases the voltage to plating modulating layer process from the magnitude of voltage V0 of initial cleaning process
V1, the required time is 11min；
Further, the magnitude of voltage V0 of initial cleaning matrix material process for 39.996V, plate the electricity of modulating layer process
Pressure V1 is 119.988V.
Further, the material of the functional layer is selected from the ratio of the amount of Al and Cr material in AlCr, the AlCr materials
For 70/30.
In addition, the invention also provides low internal stress coating prepared by above-mentioned preparation method, it includes being coated in matrix material
Binder course and the multiple composite beds being covered on binder course on material, described composite bed include modulating layer and are covered in modulating layer
On functional layer, the thickness of the binder course is 0.2 μm, and the thickness of the modulating layer is 0.18 μm, the thickness of the functional layer
For 0.05 μm, the thickness of the composite bed is 1.15 μm.
Embodiment 2
A kind of preparation method of low internal stress coating, including cleaning matrix material, plating binder course, plating modulating layer and plating function
Four step of layer, adjustable voltage is used during described plating binder course, by voltage from the electricity of cleaning matrix material process
Pressure value V0 is gradually increased to plate the voltage V1 of modulating layer process.
Wherein, during binder course is plated, the mode of regulation voltage is included by the way of increase and decrease reactive power.
Further, magnitude of voltage incrementally increases the voltage to plating modulating layer process from the magnitude of voltage V0 of initial cleaning process
V1, the required time is 59min；
Further, the magnitude of voltage V0 of initial cleaning matrix material process for 40.004V, plate the electricity of modulating layer process
Pressure V1 is 120.012V.
Further, the material of the functional layer is selected from the ratio of the amount of Al and Cr material in AlCr, the AlCr materials
For 70/30.
In addition, the invention also provides low internal stress coating prepared by above-mentioned preparation method, it includes being coated in matrix material
Binder course and the multiple composite beds being covered on binder course on material, described composite bed include modulating layer and are covered in modulating layer
On functional layer, the thickness of the binder course is 0.7 μm, and the thickness of the modulating layer is 0.18 μm, the thickness of the functional layer
For 0.15 μm, the thickness of the composite bed is 1.65 μm.
Embodiment 3
A kind of preparation method of low internal stress coating, including cleaning matrix material, plating binder course, plating modulating layer and plating function
Four step of layer, adjustable voltage is used during described plating binder course, by voltage from the electricity of cleaning matrix material process
Pressure value V0 is gradually increased to plate the voltage V1 of modulating layer process.
Wherein, during binder course is plated, the mode of regulation voltage includes what is be combined with each other using change network parameter
Mode.
More preferred, magnitude of voltage incrementally increases the electricity to plating modulating layer process from the magnitude of voltage V0 of initial cleaning process
V1 is pressed, the required time is 30min.
Further, the magnitude of voltage V0 of initial cleaning matrix material process for 40V, plate the voltage V1 of modulating layer process
For 125V.
Further, the material of the functional layer is selected from the amount of Al and Cr material in AlCr, and/or the AlCr materials
Ratio be 70/30.
In addition, the invention also provides low internal stress coating prepared by above-mentioned preparation method, it includes being coated in matrix material
Binder course and the multiple composite beds being covered on binder course on material, described composite bed include modulating layer and are covered in modulating layer
On functional layer, the thickness of the binder course is 0.45 μm, and the thickness of the modulating layer is 0.18 μm, the thickness of the functional layer
For 0.1 μm, the thickness of the composite bed is 1.4 μm.
The specific preparation method of coating of the present invention comprises the following steps：
S1, choose and clean matrix material 1, matrix material 1 is positioned in vacuum coating equipment first, adjustment equipment is true
Reciprocal of duty cycle is 6 × 10-5Mbar, heats 60min so that temperature is increased to 460-480 DEG C, and described matrix material 1 may be selected from a high speed
Steel, it is standby；
S2, plating binder course 2：It is that 72%, pressure is 2.5 × 10 that AlCr targets are placed in into molecule pump frequency-2Mbar, arc current
To handle 30min in 150A, bias voltage are 40-120V, temperature is 480 DEG C nitrogen environment, i.e., it is made on matrix material 1
The ratio of the amount of Al and Cr material is 70/30 in binder course 2, described AlCr targets；
S3, plating modulating layer 31：By the AlCr targets for being coated with binder course 2 be placed in molecule pump frequency be 72%, pressure be 4 ×
10-2Mbar, arc current are to handle 10min in 180A, the nitrogen environment that bias voltage is 120V, temperature is 480 DEG C, that is, are made and adjust
Preparative layer 31；
S4, plating functional layer 32：It is that 72%, pressure is 4 × 10 that TiSi targets are placed in into molecule pump frequency-2Mbar, arc current
To handle 10min in 200A, bias voltage are 40V, temperature is 480 DEG C nitrogen environment, that is, functional layer 32 is made, it is described
The ratio of the amount of Ti and Si material is 85/15 in TiSi targets；
S5, above steps may be repeated multiple times three prepares the process that modulating layer 31 and step 4 prepare functional layer 32, that is, institute is made
The low internal stress coating stated.
Experimental example
600 close drill bits of quality, outward appearance are chosen, six groups of A, B, C, D, E, F are divided into, in tri- groups of drill bit of A, B, C
It is upper respectively according to embodiment 1, embodiment 2 and embodiment 3 method prepares coating；Also using real on tri- groups of D, E, F drill bit
The method prepares coating of example 1, embodiment 2 and embodiment 3 is applied, but prepares the fixed voltage that 40V is used during binder course.
Experimental result is：Tri- groups of A, B, C drill bit use time average out to 152 days, 150 days, 170 days, tri- groups of D, E, F's
Drill bit use time average out to 68 days, 60 days, 58 days.
It is above-mentioned test result indicates that：Service life can be greatly prolonged using transformation in the preparation process of binder course, its
In it is especially most long with the coating service life prepared by the method for embodiment 3.The technology contents and technical characteristic of the present invention have revealed that
As above, however those skilled in the art are still potentially based on teachings of the present invention and announcement and make a variety of without departing substantially from the present invention
The replacement and modification of spirit, therefore, the scope of the present invention should be not limited to the content disclosed in embodiment, and should include it is various not
Away from the replacement and modification of the present invention, and covered by present patent application claim.
Claims (10)
1. a kind of preparation method of low internal stress coating, including cleaning matrix material, plating binder course, plating modulating layer and plating functional layer
Four steps, it is characterised in that：During described plating binder course use adjustable voltage, by voltage from cleaning matrix material
The magnitude of voltage V0 of process is gradually increased to plate the voltage V1 of modulating layer process.
2. the preparation method of low internal stress coating according to claim 1, it is characterised in that：During binder course is plated,
The mode of regulation voltage includes using increase and decrease reactive power, changes what network parameter, active power and reactive power be combined with each other
Mode.
3. the preparation method of low internal stress coating according to claim 2, it is characterised in that：Described increase and decrease reactive power
Mode includes regulator generator, phase modifier, shunt capacitor and/or shunt reactor.
4. the preparation method of low internal stress coating according to claim 2, it is characterised in that：Described active power with it is idle
The mode that power be combined with each other includes regulation transformer, changes load tap changer pressure regulation.
5. the preparation method of low internal stress coating according to claim 2, it is characterised in that：Described change network parameter
Mode includes stopping paired running transformer using series capacitor, throwing, throws and stop unloaded and/or underloading high-tension line.
6. the preparation method of low internal stress coating according to claim 1, it is characterised in that：Magnitude of voltage is from initial cleaning
The magnitude of voltage V0 of journey incrementally increases the voltage V1 of plating modulating layer process, and the required time is 10-60min.
7. the preparation method of low internal stress coating according to claim 1, it is characterised in that：Magnitude of voltage is from initial cleaning
The magnitude of voltage V0 of journey incrementally increases the voltage V1 of plating modulating layer process, and the required time is 20-40min.
8. the preparation method of low internal stress coating according to claim 1, it is characterised in that：Initial cleaning matrix material mistake
The magnitude of voltage V0 of journey for 30-50V, the voltage V1 of plating modulating layer process is 100-150V.
9. the preparation method of low internal stress coating according to claim 1, it is characterised in that：The material of the functional layer is selected from
The ratio of the amount of Al and Cr material is 70/30 in AlCr, the AlCr materials.
10. low internal stress coating prepared by a kind of preparation method as any one of claim 1-9, it is characterised in that：Bag
The binder course being coated on matrix material and the multiple composite beds being covered on binder course are included, described composite bed includes modulating layer
With the functional layer being covered on modulating layer, the thickness of the binder course is 0.2-0.7 μm, and/or the thickness of the modulating layer is
0.18 μm, and/or the thickness of the functional layer is 0.05-0.15 μm, and/or the thickness of the composite bed is 1.15-1.65 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710222844.4A CN107299330A (en) | 2017-04-07 | 2017-04-07 | A kind of low internal stress coating and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710222844.4A CN107299330A (en) | 2017-04-07 | 2017-04-07 | A kind of low internal stress coating and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111378929A (en) * | 2018-12-29 | 2020-07-07 | 苏州星蓝纳米技术有限公司 | Novel P coating |
| CN112458410A (en) * | 2019-09-09 | 2021-03-09 | 苏州吉恒纳米科技有限公司 | Superhard silicon-based coating |
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| US4842710A (en) * | 1987-03-23 | 1989-06-27 | Siemens Aktiengesellschaft | Method of making mixed nitride films with at least two metals |
| CN1644752A (en) * | 2005-01-15 | 2005-07-27 | 大连理工大学 | Method for substituting yellow brass piece vacuum ion plating for electroplating |
| CN104011256A (en) * | 2011-09-19 | 2014-08-27 | 拉米娜科技 | Coated cutting tool |
| CN104508171A (en) * | 2012-04-16 | 2015-04-08 | 欧瑞康贸易股份公司(特吕巴赫) | High performance tools exhibiting reduced crater wear in particular by dry machining operations |
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2017
- 2017-04-07 CN CN201710222844.4A patent/CN107299330A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4842710A (en) * | 1987-03-23 | 1989-06-27 | Siemens Aktiengesellschaft | Method of making mixed nitride films with at least two metals |
| CN1644752A (en) * | 2005-01-15 | 2005-07-27 | 大连理工大学 | Method for substituting yellow brass piece vacuum ion plating for electroplating |
| CN104011256A (en) * | 2011-09-19 | 2014-08-27 | 拉米娜科技 | Coated cutting tool |
| CN104508171A (en) * | 2012-04-16 | 2015-04-08 | 欧瑞康贸易股份公司(特吕巴赫) | High performance tools exhibiting reduced crater wear in particular by dry machining operations |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111378929A (en) * | 2018-12-29 | 2020-07-07 | 苏州星蓝纳米技术有限公司 | Novel P coating |
| CN112458410A (en) * | 2019-09-09 | 2021-03-09 | 苏州吉恒纳米科技有限公司 | Superhard silicon-based coating |
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