CN107779839A - DLC film plating process based on anode technology - Google Patents
DLC film plating process based on anode technology Download PDFInfo
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- CN107779839A CN107779839A CN201711133112.4A CN201711133112A CN107779839A CN 107779839 A CN107779839 A CN 107779839A CN 201711133112 A CN201711133112 A CN 201711133112A CN 107779839 A CN107779839 A CN 107779839A
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- 238000000034 method Methods 0.000 title claims abstract description 63
- 230000008569 process Effects 0.000 title claims abstract description 20
- 238000005516 engineering process Methods 0.000 title claims abstract description 15
- 238000007747 plating Methods 0.000 title claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 59
- 239000002184 metal Substances 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000010891 electric arc Methods 0.000 claims abstract description 24
- 238000001020 plasma etching Methods 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 16
- 238000010586 diagram Methods 0.000 description 10
- 229910021645 metal ion Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000000992 sputter etching Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 208000028659 discharge Diseases 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000003574 free electron Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
- C23C14/02—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
-
- 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
- C23C14/0635—Carbides
-
- 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
-
- 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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
- C23C16/029—Graded interfaces
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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)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of DLC film plating process based on anode technology, carries out plated film using DLC coating apparatus, comprises at least：Step 1, under an inert atmosphere, it is that negative electrode carries out arc discharge using magnetic control target as anode, electric arc target, produces plasma；It is that anode is biased to base material using base material as negative electrode, magnetic control target, plasma etching cleaning is carried out to base material；Step 2, under an inert atmosphere, it is that anode carries out magnetron sputtering using rotary magnetron target as negative electrode, rotating the arc target；It is that negative electrode is biased using rotating the arc target as anode, workpiece, in deposited on substrates intermediate metal；Step 3, hydrocarbon class unstrpped gas is passed through, is that negative electrode is biased using electric arc target as anode, workpiece, DLC layer is deposited on intermediate metal using PaCVD methods.The present invention is remarkably improved the stability of DLC coating process and the performance of DLC coated products.
Description
Technical field
The invention belongs to technical field of vacuum plating, more particularly to a kind of DLC film plating process based on anode technology.
Background technology
In order to reduce the fuel consumption of automobile, it is desirable to reduce the resistance to sliding for the slide unit being mounted on automobile.It is known to have
Construction for this purpose, i.e., using diamond-like carbon film (DLC, the Diamond Like with low frictional properties and wear resistance
Carbon) slide unit Surface coating is got up.DLC is that the carbon atom with sp3 hydridization accounts for the meta-stable form of very big ratio
Amorphous carbon.DLC typically has high rigidity and smooth surface, also with good wearability, chemical stability, thermal conductivity and
Mechanical performance.
At present, DLC coatings can be prepared on various base materials, to develop new part.The known main side for preparing DLC coatings
Method has PVD method (Physical Vapor Deposition, physical vapor deposition) and PaCVD methods (Plasma assisted
Chemical Vapor Deposition, plasma-assisted chemical vapour deposition method) two kinds.Wherein, PaCVD methods are because film forming speed
Faster, and the workpiece of complicated shape is adapted to, PaCVD methods is turned into the main stream approach for preparing DLC coatings.In PaCVD techniques
Plasma can be excited by DC pulse power source.In DC pulse plasma processing unit, locate in process chamber
It is raw in process chamber by applying DC pulse voltage to base material under the negative pressure state containing hydrocarbon class unstrpped gas environment
Into plasma, so as to which hydrocarbon class unstrpped gas is in plasma, deposit to form DLC coatings in substrate surface.
Directly residual compressive stress very high in DLC coatings, DLC coating phases will be caused in substrate surface deposition DLC coatings
Weak for the adhesive force of base material, for adhesive force of the enhancing DLC layer with respect to base material, a kind of known method is in base material and DLC layer
Between buffering of the evaporation metal transition zone as stress, cross plating process control be one of key technology of DLC coating process.
To adapt to the requirements at the higher level of industrial development, the stability of DLC coating process and the performance of DLC coated products need into
One step improves.
The content of the invention
It is an object of the invention to provide it is a kind of be remarkably improved technology stability and properties of product based on anode technology
DLC film plating process.
A kind of DLC film plating process based on anode technology provided by the invention, plated film is carried out using DLC coating apparatus, extremely
Include less：
Step 1, base material is cleaned using plasma etching method, is specially：
Under an inert atmosphere, it is that negative electrode carries out arc discharge using magnetic control target as anode, electric arc target, produces plasma；With
Base material is negative electrode, magnetic control target is that anode is biased to base material, and plasma etching cleaning is carried out to base material；
Step 2, using magnetron sputtering method in deposited on substrates intermediate metal, it is specially：
Under an inert atmosphere, it is that anode carries out magnetron sputtering using rotary magnetron target as negative electrode, rotating the arc target；With electric rotating
Arc target is anode, workpiece is that negative electrode is biased, in deposited on substrates intermediate metal；
Step 3, DLC layer is deposited on intermediate metal using PaCVD methods, is specially：
Hydrocarbon class unstrpped gas is passed through, is that negative electrode is biased using electric arc target as anode, workpiece, using PaCVD methods in gold
DLC layer is deposited on category transition zone.
Further, it is described in deposited on substrates intermediate metal in step 2, further comprise：
Under an inert atmosphere, in deposited on substrates metal level；
Hydrocarbon class unstrpped gas is passed through, on the metal layer the gradient layer of deposited metal-metal-carbide, metal-carbide one by one
Layer；
Metal level, the gradient layer of metal-carbon metal, metal-carbide layer form intermediate metal.
Further, the DLC coating apparatus include vacuum chamber, rotational workpieces frame, rotating the arc target, rotary magnetron target,
Gas handling system, pumped vacuum systems, heating system and power-supply system, the vacuum chamber ground connection, the power-supply system are splashed including magnetic control
Radio source, arc power, grid bias power supply, first contactor, second contactor, the 3rd contactor and the 4th contactor；Wherein：
Grid bias power supply negative electrode connection rotational workpieces frame on workpiece, by first contactor connect grid bias power supply anode and
Rotating the arc target, the anode and rotary magnetron target of grid bias power supply are connected by second contactor；
The negative electrode connection rotary magnetron target of magnetron sputtering power supply, the anode of magnetron sputtering power supply is connected by the 3rd contactor
With rotating the arc target；
The negative electrode connection rotating the arc target of arc power, the anode and rotary magnetic of arc power are connected by the 4th contactor
Control target.
The film plating process using above-mentioned DLC coating apparatus, comprise at least：
(1) base material is placed on rotational workpieces frame, and vacuum chamber is vacuumized and heated；
(2) second contactor and the 4th contactor are connected, disconnects first contactor and the 3rd contactor, opens arc power
And grid bias power supply, plasma etching cleaning is carried out to base material under an inert atmosphere；
(3) first contactor and the 3rd contactor are connected, disconnects second contactor and the 4th contactor, opens magnetron sputtering
Power supply and grid bias power supply, under an inert atmosphere in deposited on substrates intermediate metal；
(4) first contactor is connected, disconnects second contactor, the 3rd contactor and the 4th contactor, it is former to be passed through hydrocarbon class
Expect gas, open grid bias power supply, DLC layer is deposited on intermediate metal.
Further, in step (1), vacuum chamber is vacuumized and heated, air pressure in vacuum chamber is less than 5.0*10-3Pa,
Temperature reaches 100 degree~300 degree.
Especially it is noted that in the present invention, the DLC layer only refers to carbon-coating, and the DLC coatings include carbon-coating and metal mistake
Layer is crossed, i.e., described DLC coatings include DLC layer and intermediate metal.
At present, a kind of known DLC film plating process that can strengthen DLC layer adhesive force, including at least step：
Step 1, base material is cleaned using plasma etching method；
Step 2, using magnetron sputtering method on base material evaporation metal transition zone；
Step 3, DLC layer is deposited on intermediate metal using PaCVD methods.
Traditional DLC coating process is using vacuum chamber as anode, and using workpiece or target as negative electrode, industry is general, and just more concern is cloudy
Pole process and less focus on anode.The present invention makes full use of anode characteristic based on known DLC film plating process, to lift DLC
The stability of coating process and the performance of DLC coated products.
On step 1, substrate surface oxide can be eliminated by carrying out cleaning to base material, so as in enhancing base materials coating it is attached
Put forth effort.Known base material cleaning can use various ion etching methods, mainly include：1) glow discharge argon ion etching, 2) arc is put
Electric metal ion etching method and 3) ion gun auxiliary etch.
To avoid introducing new pollution in cleaning process, the present invention is carried out using arc auxiliary glow discharge plasma etching method
Substrate surface cleans.The plasma etching method of the present invention has the hardware similar to arc discharge metal ion etching method, by changing
Become pole orientation, plate washer and anode are set, and principle and effect and the conventional arc discharge metal ion of etching are etched with essential distinction.
During arc discharge, cathode surface becomes clear scorching hot cathode protection to outside spatial emission metal ion and free electron, in addition to
The drop not gasified fully.Apply the metal ion in back bias voltage acceleration plasma, metal ion bombardment workpiece table to workpiece
Face.Because the movement locus of cathode protection is by magnetically confined, evaporating surface is made towards workpiece by the magnetic pole of face workpiece, to obtain
Maximum etching effect.Workpiece is equal to base material in the present invention.
It is different from traditional arc discharge metal ion etching method, the arc auxiliary glow discharge plasma etching method of the present invention
In, the pole orientation of electric arc target is back to workpiece, and metal ion and drop are shielded by radome caused by arc discharge, and free electron
Extracted by anode.Free electron produces plasma to ionization Ar atoms during anode movement, on workpiece plus back bias voltage, inhales
Draw Ar ion pair workpiece and perform etching cleaning.
The present invention is had the advantage that using plasma etching cleaning：The pollution of drop in arc discharge can be eliminated, so as to improve DLC
The adhesive force of layer, further, reduces the coefficient of friction of DLC layer, strengthens the decay resistance of DLC layer.
On step 2, conventional magnetron sputtering method as anode and is grounded using sputtering target as negative electrode using vacuum chamber.Due to the moon
Pole and anode spacing are close, are easy to be more readily captured by the anode from electric secondary electron in plasma, and cause plasma from
The shortcomings that rate is not high, coating consistency deficiency.At present, typically asked using closed field unbalanced magnetron sputtering method to solve this
Topic.The core of closed field unbalanced magnetron sputtering method is：Utilize constraint of the magnetic field to free secondary electron and free secondary electron
Along the rule of magnetic line of force screw, increase the free path and collision probability of free secondary electron, improve the ionization of plasma
Rate.
The present invention uses method of the impressed current anode away from negative electrode in magnetron sputtering technique, is prolonged by simpler method
The free path of long free secondary electron, increases electron collision probability, the density of plasma is improved, so as to obtain finer and close painting
Rotating fields.
On step 3, conventional PaCVD methods deposition DLC layer, using workpiece as negative electrode, DLC is formed for receiving CH ions
Layer.Meanwhile byproduct of reaction also can be piled into dielectric film in anode, the insulating barrier of accumulation can influence the plasma of negative and positive electrode systems
Impedance, cause the deviation of technical process.DLC coatings deposition uses batch stove, and processing time is 4 hours~8 hours, plasma resistance
Anti- change can cause the fluctuation of product quality between batch.To ensure that DLC coating products quality is periodically clear in tolerance interval, need
Manage anode.When it is anode to use vacuum chamber, the cleaning work of anode needs the anode that will be exposed in vacuum chamber in plasma
(including interior lining panel, plate washer, heater etc.) dismounting, sandblasting, clean, reinstall, and carrying out precoated shet burin-in process, anode is clear
Manage intricate operation and difficulty.
The present invention is when depositing DLC layer, using impressed current anode, can so conveniently realize the automated cleaning of anode.This
Invention, alternately as negative electrode and anode, when target is anode, is deposited in the dielectric film meeting on its surface using electric arc target and magnetic control target
Peeled off when target makees negative electrode by evaporation.Specifically, in step 3 as anode electric arc target have pass through step 1 plasma etching
Fresh surface after arc discharge is treated.
Summary, the invention has the advantages that and beneficial effect：
(1) using plasma etching method cleaning base material, the pollution of drop produced by arc discharge can be eliminated, so as to improve
The adhesive force of DLC coatings, the coefficient of friction of DLC coatings is reduced, strengthen the decay resistance of DLC coatings.
(2) in the step of magnetron sputtering method evaporation metal transition zone, extended using method of the impressed current anode away from negative electrode
The free path of free secondary electron, increase electron collision probability, the density of plasma is improved, so as to improve the cause of coating structure
Close property.
(3) the automatic clear of anode can so be conveniently realized alternately as negative electrode and anode using electric arc target and magnetic control target
It is clean, so as to avoid the product quality fluctuation caused by anode adheres to insulating barrier, improve technology stability.
Brief description of the drawings
Fig. 1 is the horizontal cross-section schematic diagram of conventional DLC coating apparatus；
Fig. 2 is the horizontal cross-section schematic diagram of DLC coating apparatus of the present invention；
Fig. 3 is the contactor connection schematic diagram of plasma etching stage DLC coating apparatus of the present invention；
Fig. 4 is the contactor connection schematic diagram of magnetron sputtering stage DLC coating apparatus of the present invention；
Fig. 5 is the contactor connection schematic diagram of PaCVD depositional phase DLC coating apparatus in the present invention；
Fig. 6 is the electromicroscopic photograph of DLC coatings prepared by the present invention；
Fig. 7 is the Lip river formula impression photo of DLC coatings prepared by the present invention.
In figure：1- vacuum chambers, 2- rotational workpieces framves, 3- rotating the arc targets, 4- rotary magnetron targets, 5- plate washers, 6- magnetic controls splash
Radio source, 7- arc powers, 8- grid bias power supplies, 9- first contactors, 10- second contactors, the contactors of 11- the 3rd, 12- the 4th
Contactor.
Embodiment
In order to illustrate the embodiments of the present invention more clearly and/or technical scheme of the prior art, accompanying drawing will be compareed below
Illustrate the embodiment of the present invention.It should be evident that drawings in the following description are only embodiments of the invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing, and obtain other embodiments.
Fig. 1 show the horizontal cross-section schematic diagram of conventional DLC coating apparatus, including vacuum chamber 1, rotational workpieces frame 2, rotation
Electric arc target 3, rotary magnetron target 4, plate washer 5, gas handling system, pumped vacuum systems, heating system, evaporation source power-supply system.Rotate work
In vacuum chamber 1, rotating the arc target 3 and the side of rotary magnetron target 4 are provided with for part frame 2, rotating the arc target 3 and rotary magnetron target 4
Plate washer 5；Gas handling system is used for being passed through unstrpped gas into vacuum chamber 1, and pumped vacuum systems is used for vacuumizing vacuum chamber 1, heats
System is used for heating to vacuum chamber.The power-supply system includes magnetron sputtering power supply 6, arc power 7 and grid bias power supply 8, wherein,
Negative pole (i.e. negative electrode) the connection rotary magnetron target 4 of magnetron sputtering power supply 6, the negative pole connection rotating the arc target 3 of arc power 7, partially
Workpiece on the negative pole connection rotary work frame 2 of voltage source 8, magnetron sputtering power supply 6, arc power 7, grid bias power supply 8 positive pole (i.e.
Anode) it is grounded.
Fig. 2 show the horizontal cross-section schematic diagram of DLC coating apparatus of the present invention, its difference with conventional DLC coating apparatus
It is that power-supply system also includes 4 and is used for the contactor that negative electrode and anode switch, grid bias power supply 8 is connected by first contactor 9
Positive pole and rotating the arc target 3, by second contactor 10 connect grid bias power supply 8 positive pole and rotary magnetron target 4, pass through the 3rd
Contactor 11 connects the positive pole and rotating the arc target 3 of magnetron sputtering power supply 6, and arc power 7 is connected by the 4th contactor 12
Positive pole and rotary magnetron target 4.In the present invention, rotating the arc target 3 and rotary magnetron target 4 are preferably Style Columu Talget, but can also be used
Rectangle plane target or circular planar target.
It is anode with vacuum chamber 1, and be grounded in conventional DLC coating apparatus；Also, the magnetic direction of rotating the arc target 3 is just
To workpiece.With rotating the arc target 3 or rotary magnetron target 4 it is then anode in DLC coating apparatus of the present invention, and rotating the arc target 3
Magnetic direction back to workpiece.
Fig. 3 show the connection schematic diagram of contactor in plasma etching stage DLC coating apparatus of the present invention, wherein, the
Two contactors 10 connect with the 4th contactor 12, and the contactor 11 of first contactor 9 and the 3rd disconnects.Fig. 4 show magnetron sputtering
Stage, the contactor connection schematic diagram of DLC coating apparatus of the present invention, wherein, first contactor 9 connects with the 3rd contactor 11,
The contactor 12 of second contactor 10 and the 4th disconnects.Fig. 5 show PaCVD depositional phases, the contact of DLC coating apparatus of the present invention
Device connects schematic diagram, wherein, first contactor 9 connects, and second contactor 10, the 3rd contactor 11, the 4th contactor 12 are disconnected
Open.
The technical process that DLC plated films are carried out using DLC coating apparatus of the present invention is provided below.
Different intermediate metals can be prepared from unstrpped gas using different targets, for example, target can select Ti
Target, Cr targets, WC targets etc., but not limited to this；Unstrpped gas can be in Ar, N2、CH2、H2, CH4Middle selection, but not limited to this, according to
The difference of intermediate metal, DLC can have various structures, for example, Cr/CrC/DLC, Cr/CrN/CrCN/CrC/DLC, Ti/
TiN/TiCN/TiC/DLC, Cr/CrWC/WC-C/DLC.
Below by by taking the DLC coatings of Cr/CrC/DLC structures as an example, illustrate its preparation technology.
1) vacuumize and heat
Workpiece is placed on rotational workpieces frame 3, vacuum chamber 1 is closed, to being vacuumized in vacuum chamber 1 and heating degasification, by vacuum
Temperature is heated to 100 degree~300 degree in chamber 1, and vacuum pressure is less than 5.0*10-3Pa.Close heating system.Here, the temperature of vacuum chamber 1
Degree is preferably 150 degree~250 degree, and vacuum pressure is preferably shorter than 2.0*10-3Pa。
2) plasma etching method cleaning workpiece
Ar gas and H are poured to vacuum chamber 12Vacuum pressure reaches 0.5Pa in the mixed gas of gas to vacuum chamber 1, wherein, Ar
Gas and H2The volume ratio of gas is 4：1.Contactor is connected according to mode shown in Fig. 3, now, rotating the arc target 3 is negative electrode, rotary magnetic
Control target 4 is anode, opens arc power 7, sets target current as 100A~200A, now target voltage is 15V~30V.With workpiece
For negative electrode, rotary magnetron target 4 is biased for anode, sets back bias voltage 100V~200V, frequency 120KHz, dutycycle 80%.
Plasma etching cleaning, cleaning duration 10min~30min are carried out to workpiece.
3) magnetron sputtering method deposited metal transition zone
It is filled with vacuum pressure in Ar gas to vacuum chamber and is maintained 0.3Pa, connects contactor according to mode shown in Fig. 4, now
Rotary magnetron target 4 is negative electrode, and rotating the arc target 3 is anode, opens magnetron sputtering power supply 6, sets power as 10KW.With electric rotating
Arc target 3 is anode, and workpiece is that negative electrode is biased 100V, frequency 120KHz, dutycycle 80%.The deposited metal Cr on workpiece
Layer, about 0.3 μm of sedimentation time 30min, Cr thickness degree.
Then, Cr-CrC gradient layers are deposited on Cr layers in method known to industry.Promote gradually, to be filled with C2H2, and reduce Ar
Flow, it is 0.4Pa to maintain vacuum pressure in vacuum chamber, finally makes Ar and C2H2Volume ratio reach 2：1, and reduce and be biased into
60V.The sedimentation time of Cr-CrC gradient layers is 20min, about 0.2 μm of Cr-CrC Thickness of Gradient Layer.
Finally, maintain the filming parameter of deposition Cr-CrC gradient layers constant, CrC layers are deposited on Cr-CrC gradient layers, are sunk
Product time 30min, about 0.3 μm of CrC thickness degree.
4) PaCVD methods deposition DLC layer
C is filled with to vacuum chamber2H2Vacuum reaches 1.0Pa~1.5Pa in vacuum chamber, connects and connects according to mode shown in Fig. 5
Tentaculum, it is anode with rotating the arc target 3, workpiece is negative electrode, is biased 400V~600V, frequency 120KHz, dutycycle 80%.
Sedimentation time 120min, root Ju load state, gained DLC layer thickness are 2 μm~4 μm.
DLC coating hardness is tested using nanoindenter, using the thickness of ball hole method test DLC coatings, using scanning electricity
The cross section structure of sem observation DLC coatings, is shown in Fig. 6；Using the coating adhesion of Lip river formula indentation method test DLC coatings, Fig. 7 is seen.This
The hardness of DLC coatings prepared by invention is 15GPa~30GPa, and the thickness of DLC coatings is 1.5 μm~3.5 μm.
Fig. 6 is the electromicroscopic photograph of DLC coatings prepared by the present invention, is metal base Cr layers, CrC successively from top to bottom in figure
Gradient layer and DLC layer, Cr layers, which are in the form of a column crystal structure, a clear longitudinal stripe, the CrC extensions columnar crystal structure of Cr layers, and face
The change of the bright composition of color more superficial, DLC layer are glassy states, and surface is smooth, compact structure.Whole membrane system Coating combination is good
It is good.
Fig. 7 is the Lip river formula impression photo of prepared DLC coatings, be can be seen that in figure, there is trickle radial split around impression
Line, uncoated peeling, show that coated film base is well combined.
Present invention difference is anode using vacuum chamber with existing DLC coating process, and magnetic control is used in the plasma etching stage
Target is anode, the use of electric arc target is anode in the magnetron sputtering stage and with the PaCVD depositional phases, is improved by this anode technology
The cleaning performance of plasma etching, the consistency of intermediate metal is improved, and improve the process stabilizing of PaCVD deposition process
Property.
Above-described embodiment is used for illustrating the present invention, rather than limits the invention, the present invention spirit and
In scope of the claims, any modifications and changes are made to the present invention, both fall within protection scope of the present invention.
Claims (3)
1. a kind of DLC film plating process based on anode technology, plated film is carried out using DLC coating apparatus, it is characterized in that, at least wrap
Include：
Step 1, base material is cleaned using plasma etching method, is specially：
Under an inert atmosphere, it is that negative electrode carries out arc discharge using magnetic control target as anode, electric arc target, produces plasma；With base material
It is that anode is biased to base material for negative electrode, magnetic control target, plasma etching cleaning is carried out to base material；
Step 2, using magnetron sputtering method in deposited on substrates intermediate metal, it is specially：
Under an inert atmosphere, it is that anode carries out magnetron sputtering using rotary magnetron target as negative electrode, rotating the arc target；With rotating the arc target
It is that negative electrode is biased for anode, workpiece, in deposited on substrates intermediate metal；
Step 3, DLC layer is deposited on intermediate metal using PaCVD methods, is specially：
Hydrocarbon class unstrpped gas is passed through, is that negative electrode is biased using electric arc target as anode, workpiece, using PaCVD methods in metal mistake
Cross and DLC layer is deposited on layer.
2. the DLC film plating process based on anode technology as claimed in claim 1, it is characterized in that：
It is described in deposited on substrates intermediate metal in step 2, further comprise：
Under an inert atmosphere, in deposited on substrates metal level；
Under an inert atmosphere, be passed through hydrocarbon class unstrpped gas, on the metal layer one by one the gradient layer of deposited metal-metal-carbide,
Metal-carbide layer；
Metal level, the gradient layer of metal-carbon metal, metal-carbide layer form intermediate metal.
3. the DLC film plating process based on anode technology as claimed in claim 1, it is characterized in that：
The DLC coating apparatus include vacuum chamber, rotational workpieces frame, rotating the arc target, rotary magnetron target, gas handling system, take out it is true
Empty set system, heating system and power-supply system, the vacuum chamber ground connection, the power-supply system include magnetron sputtering power supply, electric arc electricity
Source, grid bias power supply, first contactor, second contactor, the 3rd contactor and the 4th contactor；Wherein：The negative electrode of grid bias power supply
Workpiece on rotational workpieces frame is connected, the anode and rotating the arc target of grid bias power supply are connected by first contactor, is connect by second
Tentaculum connects the anode and rotary magnetron target of grid bias power supply；The negative electrode connection rotary magnetron target of magnetron sputtering power supply, passes through the 3rd
Contactor connects the anode and rotating the arc target of magnetron sputtering power supply；The negative electrode connection rotating the arc target of arc power, by the
Four contactors connect the anode and rotary magnetron target of arc power；
When being cleaned in step 1 to base material, second contactor and the 4th contactor are connected, first contactor and the 3rd is disconnected and connects
Tentaculum；In step 2 in deposited on substrates intermediate metal, first contactor and the 3rd contactor are connected, disconnects the second contact
Device and the 4th contactor；In step 3 when depositing DLC layer on intermediate metal, first contactor is connected, disconnects the second contact
Device, the 3rd contactor and the 4th contactor.
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