CN104962914B - Prepare the industrial automation vapor deposition apparatus of DLC film - Google Patents
Prepare the industrial automation vapor deposition apparatus of DLC film Download PDFInfo
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- CN104962914B CN104962914B CN201510383028.2A CN201510383028A CN104962914B CN 104962914 B CN104962914 B CN 104962914B CN 201510383028 A CN201510383028 A CN 201510383028A CN 104962914 B CN104962914 B CN 104962914B
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Abstract
The present invention is to prepare the industrial automation vapor deposition apparatus of DLC film, and the vapor deposition apparatus that solution the sixth of the twelve Earthly Branches has is complicated, and cost is high, the problem of being not easy to operation, can not accurately control.There is physical vapour deposition (PVD) simultaneously in the settling chamber of the equipment（PVD）Unit and physical chemistry vapour deposition（PCVD）Unit, both single unit can have been used individually to carry out the deposition of DLC film, the composite deposition that two units carry out continuous DLC can also be used alternatingly, the equipment is by settling chamber, air supply system, vacuum system, heating system, water-cooling system, magnetic control sputtering system, workpiece high-voltage isulation mounting and clamping system, electric control system, impulse modulation power-supply system etc. forms, it is big with capacity, automaticity is high, precision is high, high safety, scalability is strong, operation and maintenance are simple, products application scope extensively waits many merits, it can be widely applied to machinery, Aero-Space, the numerous areas such as medicine.
Description
Technical field：
The present invention relates to one kind to prepare the full-automatic industrial vapor deposition apparatus of DLC film, belongs to vapour deposition field.
Background technology：
DLC coatings are a kind of new coating materials similar to diamond coatings performance, and it has higher hardness, well
Pyroconductivity, extremely low coefficient of friction, excellent electrical insulation capability, high chemical stability and infrared light transmission performance, so
The every field such as machinery, electronics, optics and medical science are widely applied to, have substantial amounts of document report both at home and abroad using different
Deposition process prepares different type, structure, the DLC coatings of composition.
Coating deposition field is commonly divided into chemical vapour deposition technique（CVD）, physical gas phase deposition technology（PVD）And thing
Physicochemical is vapor-deposited（PCVD）Technology.CVD deposition process is under the conditions of certain temperature, by mixed reaction gas to matrix
Diffusion into the surface, adsorbed, reaction, accumulation and complete, TiN, TiC, TiCN, TiBN, TiB can be achieved2、Al2O3Deng individual layer and more
The deposition of first multi-layer composite coatings, coating is preferable with basal body binding force, and coating layer thickness is up to more than 20 μm at present, although CVD is applied
Layer wearability is preferable, but because its depositing temperature is higher（700—1100℃）, can cause the bending strength of material reduces, for
Many steel part can also because temperature exceed material annealing temperature and caused by material hardness and bond strength reduce, therefore CVD mesh
It is preceding to occupy larger proportion in carbide chip and mould coating, but because the limitation of deposition principle, CVD can not be carried out
The deposition of DLC coatings.
PVD technique is to utilize gas discharge technology, and by evaporation atom partial ionization into ion, the ion for obtaining high-energy can
Effectively to clean workpiece surface, coating itself and the adhesion with workpiece substrate are improved, so as to obtain the coating of high-quality.Adopt
With the coating apparatus of PVD technique, comparative maturity, product have had evolved to the oxide coating in the 7th generation at present, but high-end
Technology is grasped by manufacturers such as Ionbond, Balzers, Platit, Hauzer, Sulzer of foreign countries substantially.PVD technique processing
Temperature is low（Less than 600 DEG C）, substantially without influence, coat inside stress state it is compression on material bending strength, is more suitable for pair
The coating of hard alloy precision complex cutting tool, in addition PVD environment is had no adverse effect, more meet Modern Green manufacture hair
Open up direction.The conventional method of PVD technique has at present：Hollow cathode, hot cathode, cathode arc and magnetic controlled sputtering ion plating etc..
PVD coat types are various, and change is rapid, and having developed has multilayer, compound, nanostructured film layer, and the research of forefront is then oxidation
Thing, carbon containing, boron class film layer, why the present invention, which selects intermediate frequency magnetic control power supply just to allow for such power supply, can deposit Buddha's warrior attendant
Nonconducting coating such as stone, oxide.The DLC coatings deposited using PVD methods are not hydrogeneous, and hardness is high, but deposition speed be present
Rate is slow, self lubricity is relatively poor, poor around plating property, is not suitable for deposit on complex part the shortcomings of, limiting it and applying model
Enclose.
PCVD technologies are the novel surface coating technologies that recent decades grow up, and the technology draws plasma technique
Enter in chemical vapor deposition method, mainly chemical reaction has been activated using the physical action of glow discharge, so as to significantly
Reduce reaction temperature.PCVD depositing temperatures generally can be controlled in less than 600 DEG C, good around plating property, are easy in complex-shaped, big face
Superhard film is obtained on long-pending workpiece, sedimentation rate up to 4~10 μm/h, the coat type that can be deposited at present have TiN, TiCN,
TiSiN, TiAlSiN, TiC, DLC etc..It can be divided into radio frequency, direct current, radio frequency direct current, microwave by mode of excitation PCVD technologies
Plasma, heated filament and pulse direct current technology, but due to the reasons such as preceding four deposition principle, technology maturity and discomfort
Industrial applications are closed, although heated filament technology comparative maturity, general more depositions for being applied to diamond coatings, so very
Positive heavy industrialization application only has pulsed-d.c. PCVD technology at present.Although the country can also prepare industrial pulse direct current
PCVD equipment, but settling chamber is still relatively small, and the PCVD equipment deposition chamber dimension that such as domestic patent CN 1263953A are introduced is only
There are Ф 350mm × 700mm, the Plasma heat teratment stove of domestic patent CN 102011090A introductions, deposition chamber dimension are for another example
Ф 650mm × 1200mm, although the equipment size is relatively large, the equipment compared to external Ф 1500mm × 4500mm
Still there is very big gap, and domestic equipment is not substantially at present automation mechanized operation, is unfavorable for the precision control of technique
System.
With the continuous development of scientific technology, to the adhesion of coating, hardness, thickness, toughness, crystallite dimension, lubricity
Deng performance requirement also more and more higher, especially in fields such as Aero-Space, automobile, optics, acoustics, biomedicine, machinings,
And single CVD, PVD, PCVD coating can not often meet these requirements, so needing the coating of various properties to cooperate
It can complete.By taking the hard alloy cutter with two structural coatings that patent 201010530080 is introduced as an example, in order to reduce coating stress simultaneously
Lower surface roughness is obtained, carries out PVD coatings again after CVD coatings to achieve the goal, but such processing mode phase
To less efficient, because two kinds of coatings can not be carried out in same equipment, so needing coated cutting tool after CVD coatings from anti-
Answer taken out in stove handled after reload coating is carried out in PCVD equipment again, if two kinds of coatings can be in same equipment
Completion will greatly improve operating efficiency.Again using Tool Industry generally use at present for the compound PVD coatings of TiN+TiAlN as
Example, although the current comparative maturity of this kind of coating, when processing cohesive material, its self lubricity is relatively still poor, is easier
Viscous knife, so the space that still has greatly improved, if can on the compound PVD coatings of TiN+TiAlN redeposited one layer of lubricity
Preferable DLC coatings, it will greatly improve the life-span of coated cutting tool.Although also there is the DLC using PVD methods deposition to apply now
Layer, but as saying before, PVD methods are poor around plating property, and the DLC coatings lubricity deposited in this way relative to
The DLC coatings deposited using PCVD methods are much lower, and growth rate is slow many again, so depositing DLC using PCVD methods
More preferably, it is also very necessary while also to illustrate heretofore described equipment to carry out PVD coatings can also carry out PCVD coatings
's.
What is had good grounds at present develops the only South West USA research institute of PVD+PCVD composite coating depositing devices
（US8273222B2）And the Hauzer of Holland（WO2007089216A1）Coatings Corporation, the country yet there are no company and develop class
As industrial equipment.In same type equipment, South West USA research institute using magnetron sputtering PVD+ r. f. PCVDs technology
Combination, due to common magnetron sputtering can not the non-conductive film such as deposition of aluminium oxide, r. f. PCVD ionization level is low in addition, reaction speed
Slowly, its industrial applicability is limited；The technical combinations for the arc filtering PVD+ pulses PCVD that Hauzer companies use, although using
Scope is wide, but due to adding particulate filter arrangement, equipment complex and expensive, and can not possibly be adequately filtered out in deposition process
Bulky grain.
The content of the invention：
The purpose of the present invention is a kind of simple in construction, and low cost, function is strong, easily operated and maintenance, is had a wide range of application, can
To carry out the industrial automation vapor deposition apparatus of the preparation DLC film of the accurate control of technique.
What the present invention was realized in：
Prepare DLC film industrial automation vapor deposition apparatus by settling chamber I, air supply system II, vacuum system III, plus
Hot systems IV, water-cooling system V, medium frequency magnetron sputtering system VI, workpiece high-voltage isulation mounting and clamping system VII, electric control system VIII
And impulse modulation power-supply system Ⅸ forms, air supply system II is made up of multichannel air inlet pipe and flow controller, the air inlet of air inlet pipe
Mouthful the top of settling chamber I is fixed on, can meet the air supply requirement of a variety of coatings, in deposition process, reacting gas leads in the electric field
Cross after a series of processes such as exciting, ionizing, adhering to and deposit on the surface of the workpiece, described vacuum system III and the rear side of settling chamber I
Bleeding point be connected, by diffusion pump 2, mechanical pump 3, lobe pump 4, single-stage sliding vane rotary pump 5, electronic grating valve 6, vent valve 8, high threshold 7,
It is pre- to take out valve 9, maintain valve 10, preceding step valve 11, bypass valve 12, the forevacuum ga(u)ge 14 of high vacuum rule 13, the 1st, 2,3,16,17, thin-film electro
Content regulation 15, reserved vacuum measurement mouth composition, bleeding point through electronic grating valve 6, respectively through high threshold 7, it is pre- take out valve 9, bypass valve 12 with
Diffusion pump 2, lobe pump 4, single-stage sliding vane rotary pump 5 connect, and diffusion pump 2 is respectively through maintaining valve 10, preceding step valve 11 and mechanical pump 3, Roots
Pump 4 connects, in the PCVD deposition process of relatively low vacuum is only needed, it is only necessary to single-stage sliding vane rotary pump 5, lobe pump 4, bypass valve
12nd, it is pre- to take out valve 9 and control pumping speed to meet the needs of vacuum by electronic grating valve 6；Needing the PVD deposition of high vacuum
During, then need to increase diffusion pump 2, lobe pump 4, single-stage sliding vane rotary pump 5, preceding step valve 11 and the collective effect of high threshold 7, again by
Electronic grating valve 6 controls pumping speed；1st, 2,3 forevacuum ga(u)ges 14,16,17, high vacuum rule 13, thin-film electro content regulation 15 is heavy for measuring
The air pressure of product room I；Mechanical pump 3 prevents the diffusion pump oil in diffusion pump 2 from returning oil maintaining the vacuum in diffusion pump 2, described
Heating system IV uses vacuum armouring heater strip 32, and temperature probe 33 is housed, and heater strip is installed on settling chamber I into " U-shaped "
On the heater strip installing plate of inwall, double-deck liner plate is installed between heater strip and vacuum wall, to heating when avoiding coating with this
The pollution of silk, during deposition, heater strip electrified regulation, heat is conducted to workpiece by way of radiation, makes workpiece heat, described
Water-cooling system V be made up of 12 road water rows, water mining makes of stainless steel material, wherein four road water row's connection magnetron sputtering systems
The target of system VI, four road water row's connection deposition chamber walls I, water, which is arranged, all the way connects impulse modulation power-supply system Ⅸ, water row connection all the way
The power supply of medium frequency magnetron sputtering system VI, two path water row's connection diffusion pump 2, cooling water can give each component to cool, prevent each group
Part is burnt because temperature is too high, and the temperature of workpiece in deposition process can also be adjusted by being connected to the cooling water of deposition chamber wall I, so as to
The coating of different performance is obtained, medium frequency magnetron sputtering system VI is the system used during physical vapour deposition (PVD), by band water cooling
Medium frequency magnetron sputtering power supply and sputtering target material composition, sputtering target material can according to coat type carry out unrestricted choice, deposition process
In, settling chamber connects the positive pole of shielding power supply, and target connects the negative pole of shielding power supply, and after switching on power, gas is in the presence of electric field
Ion is ionized into, target atom is sputtered and is deposited on workpiece forms coating, impulse modulation power-supply system Ⅸ is just
Pole is connected in settling chamber I, and negative electrode is connected on the workpiece for needing coating, after switching on power, reacting gas in the electric field by exciting,
Deposited after a series of processes such as ionization, attachment on the surface of the workpiece, form coating, workpiece high-voltage isulation mounting and clamping system VII is by rotating disk
And driving motor is formed, clamping workpiece keeps apart workpiece and settling chamber I on rotating disk, by insulating materials, electrical control
System VIII is made up of host computer 26 and programmable controller PLC 28, and programmable controller PLC 28 passes through input/output port I/O
With vacuum meter 29, impulse modulation power supply 30, intermediate frequency magnetic control power supply 31, mass flowmenter stop valve 34, mass flowmenter 35, diffusion
Pump 2, mechanical pump 3, lobe pump 4, single-stage sliding vane rotary pump 5, electronic grating valve 6, vent valve 8, high threshold 7, pre- valve 9 is taken out, valve 10 is maintained, is preceding
Step valve 11, bypass valve 12, heater strip 32 are connected, and temperature probe 32 is connected with temperature controller 27, temperature controller 27 is connected with host computer 26,
Vacuum meter 29 is connected with settling chamber I, the multichannel air inlet pipe of mass flowmenter stop valve 34, mass flowmenter 35 and air supply system II
Connection, programmable controller PLC 28 are connected by network with host computer 26.
Mass flowmenter 35 is connected by Process FieldbusROFIBUS with programmable controller PLC 28, can be with coating procedure
The setup parameter of control flowmeter 35 obtains the deposition that required gas flow carries out coating manually, or in advance in host computer 26
Input flow rate parameter automatic running in operation interface, during automatic running, by real-time detection flows numerical value, if there is flow to be discontented with
Foot requires that equipment will carry out automatic alarm prompting and determine that " wait " shape is closed or entered to equipment automatically according to actual conditions
State, when entering " wait " state, equipment other systems after problem exclusion, continue to apply still in normal operating conditions
The deposition of layer.
Host computer 26 is connected by modbus agreements with temperature controller 27 and temperature probe 33, can be with hand in coating procedure
Dynamic design temperature carries out the deposition of coating, design temperature can also be inputted in the operation interface of host computer 26 in advance and transported automatically
OK, during automatic running, the temperature that persistently detection is set of temperature controller 27, if prompting automatic alarm beyond certain deviation.
Settling chamber I is by 304 stainless steel material processing and fabricatings, using the double door 18 of angle at a right angle, complete machine overall dimensions
1500mm × 1500mm × 2800mm, internal effectively working region size 1000mm × 1000mm × 1000mm, side wall are provided with
Observation window 19 and expanded function spare interface 20.
There is physical vapour deposition (PVD) simultaneously in the settling chamber of the present invention（PVD）Unit and physical chemistry vapour deposition（PCVD）
Unit, it can both use single unit individually to carry out the deposition of DLC film, two units can also be used alternatingly and carry out continuously
DLC composite deposition.Can on instrument, mould, cutter depositing diamond-like DLC film coating, meet industry-by-industry to DLC film apply
The demand of layer.Compared to the same type equipment of foreign countries, invention is using magnetron sputtering PVD+ pulses PCVD technical combinations, structure letter
Single, low cost, function is strong, has a wide range of application.With capacity is big, automaticity is high, precision is high, high safety, expansible
Property strong, operation and safeguard many merits such as simple, products application scope is wide, can be widely applied to machinery, Aero-Space, medicine etc.
Numerous areas.
Both single PVD coatings or PCVD coatings can have been carried out, continuous PVD and PCVD coatings can also have been carried out, together
When can carry out TiN, TiAlN, ZrN, TiSiN, TiSiAlN, TiCN, oxide, diamond, DLC etc. it is a variety of single or
The deposition of person's composite coating, economic and reliable, can meet that the needs of multiple fields, especially oil, automobile, Aero-Space etc. need
Large complicated parts are carried out with the field of coating.The present invention is automation equipment, can carry out the accurate control of technique, production
Quality is stable, and production efficiency is high.
Brief description of the drawings：
Fig. 1 is structure chart of the present invention.
Fig. 2 is Fig. 1 top view.
Fig. 3 is vacuum system schematic diagram
Fig. 4 is high-voltage isulation mounting and clamping system figure
Fig. 5 is Fig. 4 left view
Fig. 6 power-supply system control block diagrams
Fig. 7 pump valve system control block diagrams
Fig. 8 air supply system control block diagrams
Fig. 9 temperature control system block diagrams
Figure 10 power-supply system automatic running flow charts
Figure 11 vacuum systems evacuate flow chart automatically
Figure 12 mass flowmenters are supplied gas flow chart automatically
Figure 13 temperature automatic control flow charts
Figure 14 automatic film coating flow charts
The Raman spectrum of Figure 15 embodiments
Embodiment：
Below by the realization means that the present invention is described with reference to the drawings
Prepare DLC film industrial automation vapor deposition apparatus by settling chamber I, air supply system II, vacuum system III, plus
Hot systems IV, water-cooling system V, medium frequency magnetron sputtering system VI, workpiece high-voltage isulation mounting and clamping system VII, electric control system VIII
And impulse modulation power-supply system Ⅸ forms, air supply system II is made up of multichannel air inlet pipe and flow controller, the air inlet of air inlet pipe
Mouthful the top of settling chamber I is fixed on, can meet the air supply requirement of a variety of coatings, in deposition process, reacting gas leads in the electric field
Cross after a series of processes such as exciting, ionizing, adhering to and deposit on the surface of the workpiece, described vacuum system III and the rear side of settling chamber I
Bleeding point be connected, by diffusion pump 2, mechanical pump 3, lobe pump 4, single-stage sliding vane rotary pump 5, electronic grating valve 6, vent valve 8, high threshold 7,
It is pre- to take out valve 9, maintain valve 10, preceding step valve 11, bypass valve 12, the forevacuum ga(u)ge 14 of high vacuum rule 13, the 1st, 2,3,16,17, thin-film electro
Content regulation 15, reserved vacuum measurement mouth composition, bleeding point through electronic grating valve 6, respectively through high threshold 7, it is pre- take out valve 9, bypass valve 12 with
Diffusion pump 2, lobe pump 4, single-stage sliding vane rotary pump 5 connect, and diffusion pump 2 is respectively through maintaining valve 10, preceding step valve 11 and mechanical pump 3, Roots
Pump 4 connects, in the PCVD deposition process of relatively low vacuum is only needed, it is only necessary to single-stage sliding vane rotary pump 5, lobe pump 4, bypass valve
12nd, it is pre- to take out valve 9 and control pumping speed to meet the needs of vacuum by electronic grating valve 6；Needing the PVD deposition of high vacuum
During, then need to increase diffusion pump 2, lobe pump 4, single-stage sliding vane rotary pump 5, preceding step valve 11 and the collective effect of high threshold 7, again by
Electronic grating valve 6 controls pumping speed；1st, 2,3 forevacuum ga(u)ges 14,16,17, high vacuum rule 13, thin-film electro content regulation 15 is heavy for measuring
The air pressure of product room I；Mechanical pump 3 prevents the diffusion pump oil in diffusion pump 2 from returning oil maintaining the vacuum in diffusion pump 2, described
Heating system IV uses vacuum armouring heater strip 32, and temperature probe 33 is housed, and heater strip is installed on settling chamber I into " U-shaped "
On the heater strip installing plate of inwall, double-deck liner plate is installed between heater strip and vacuum wall, to heating when avoiding coating with this
The pollution of silk, during deposition, heater strip electrified regulation, heat is conducted to workpiece by way of radiation, makes workpiece heat, described
Water-cooling system V be made up of 12 road water rows, water mining makes of stainless steel material, wherein four road water row's connection magnetron sputtering systems
The target of system VI, four road water row's connection deposition chamber walls I, water, which is arranged, all the way connects impulse modulation power-supply system Ⅸ, water row connection all the way
The power supply of medium frequency magnetron sputtering system VI, two path water row's connection diffusion pump 2, cooling water can give each component to cool, prevent each group
Part is burnt because temperature is too high, and the temperature of workpiece in deposition process can also be adjusted by being connected to the cooling water of deposition chamber wall I, so as to
The coating of different performance is obtained, medium frequency magnetron sputtering system VI is the system used during physical vapour deposition (PVD), by band water cooling
Medium frequency magnetron sputtering power supply and sputtering target material composition, sputtering target material can according to coat type carry out unrestricted choice, deposition process
In, settling chamber connects the positive pole of shielding power supply, and target connects the negative pole of shielding power supply, and after switching on power, gas is in the presence of electric field
Ion is ionized into, target atom is sputtered and is deposited on workpiece forms coating, impulse modulation power-supply system Ⅸ is just
Pole is connected in settling chamber I, and negative electrode is connected on the workpiece for needing coating, after switching on power, reacting gas in the electric field by exciting,
Deposited after a series of processes such as ionization, attachment on the surface of the workpiece, form coating, workpiece high-voltage isulation mounting and clamping system VII is by rotating disk
And driving motor is formed, clamping workpiece keeps apart workpiece and settling chamber I on rotating disk, by insulating materials, electrical control
System VIII is made up of host computer 26 and programmable controller PLC 28, and programmable controller PLC 28 passes through input/output port I/O
With vacuum meter 29, impulse modulation power supply 30, intermediate frequency magnetic control power supply 31, mass flowmenter stop valve 34, mass flowmenter 35, diffusion
Pump 2, mechanical pump 3, lobe pump 4, single-stage sliding vane rotary pump 5, electronic grating valve 6, vent valve 8, high threshold 7, pre- valve 9 is taken out, valve 10 is maintained, is preceding
Step valve 11, bypass valve 12, heater strip 32 are connected, and temperature probe 32 is connected with temperature controller 27, temperature controller 27 is connected with host computer 26,
Vacuum meter 29 is connected with settling chamber I, the multichannel air inlet pipe of mass flowmenter stop valve 34, mass flowmenter 35 and air supply system II
Connection, programmable controller PLC 28 are connected by network with host computer 26.
Mass flowmenter 35 is connected by Process FieldbusROFIBUS with programmable controller PLC 28, and host computer 26 passes through
Modbus agreements are connected with temperature controller 27 and temperature probe 33.
Settling chamber I is by 304 stainless steel material processing and fabricatings, using the double door 18 of angle at a right angle, complete machine overall dimensions
1500mm × 1500mm × 2800mm, internal effectively working region size 1000mm × 1000mm × 1000mm, side wall are provided with
Observation window 19 and expanded function spare interface 20.
1st, equipment settling chamber I is made by 304 stainless steel materials, air supply system II, vacuum system III, heating system IV, water
Cooling system V, magnetic control sputtering system VI, workpiece high-voltage isulation mounting and clamping system VII, electric control system VIII and impulse modulation power supply system
System Ⅸ is connected to the corresponding site of settling chamber I by special purpose interface.
2nd, before deposition starts, workpiece to be deposited is cleaned into drying, settling chamber's door 18 is opened, workpiece is put in the system of being loaded
Upper VII.The tray being loaded in system can be selected according to the shape of workpiece, the negative electrode of impulse modulation power supply Ⅸ and the storage
Disk is connected, and anode is connected with deposition chamber wall.To carry out PVD coatings, choose corresponding sputtering target material and be installed on magnetron sputtering system
The relevant position of system VI.
3rd, after workpiece has been placed, close settling chamber's door 18, open air supply system II in the gas bomb in need used
Cylinder valve, check steel cylinder pressure；Open water-cooling system V, check cooling water temperature and flow, inspection be connected to deposition chamber wall I,
Whether the cooling water on impulse modulation power-supply system Ⅸ, the power supply of magnetic control sputtering system VI and diffusion pump 2 has leakage.
4th, program editing is carried out from the host computer 26 in electric control system VIII, various reaction gases is set according to coat type
Flow, sedimentation time, the temperature of heating system IV, the vacuum values of vacuum system III, the magnitude of voltage of magnetic control sputtering system VI and the pulse of body
The parameters such as the voltage of modulation power source Ⅸ and dutycycle.The program and starting device are preserved after program editing, deposition starts.
If the program editted can directly invoke the program and be deposited.
5th, after program starts, settling chamber I is heated and vacuumized first.There are two kinds of mode of operations when vacuumizing.First
Kind, the relatively low PCVD depositions of vacuum requirement are carried out, bypass valve 12 is first turned on and single-stage sliding vane rotary pump 5 is evacuated down to several pas, then
Bypass valve 12 is closed, is opened and is taken out valve 9 and lobe pump 4 in advance and pumping speed is controlled by electronic grating valve 6.Second, utilize PVD deposition
Method, due to needing high vacuum, so after vacuum is extracted into position using first way, step valve 11 and high threshold 7 before opening, close
Close it is pre- take out valve 9, by diffusion pump 2, lobe pump 4 and the pumping high vacuum of single-stage sliding vane rotary pump 5, taken out again by the control of electronic grating valve 6
Speed.If PVD deposition finishes is returned to PCVD depositions again, due to not needing high vacuum now, it is possible to step valve 11 before closing
With high threshold 7, bypass valve 9 is opened, is only vacuumized by lobe pump 4 and single-stage sliding vane rotary pump 5, i.e. first way, meanwhile, in order to prevent
Diffusion pump oil in diffusion pump 2 returns oil, should also open and maintain valve 10 and mechanical pump 3 to maintain the vacuum in diffusion pump 2.
After temperature and vacuum in settling chamber I reach requirement, the operation of next step can be carried out.
6th, either PVD deposition or PCVD deposit, and will carry out Ion Cleaning to workpiece before coating is carried out to go
Except the partial impurities that workpiece surface does not remove, after vacuum and temperature reach requirement, corresponding working gas is by air supply system II
Interface loaded on the top of settling chamber I enters settling chamber, passes through the intermediate frequency power supply or impulse modulation power supply of magnetic control sputtering system VI
Ⅸ applies a suitable voltage, makes working gas ionization and accelerates to rush at workpiece and bang workpiece in the presence of electric field
Hit, the Ion Cleaning to workpiece is realized by this process, but voltage now must be appropriate, and voltage crosses conference and causes workpiece to damage
Wound, it is too small, do not have the effect of Ion Cleaning.
7th, coating is carried out after carrying out Ion Cleaning.If carrying out PCVD coatings, air supply system II is filled with not according to coat type
Congener working gas, after impulse modulation power supply Ⅸ provides suitable voltage, gas is ionized simultaneously in whole settling chamber I
Chemical reaction is participated in, coating uniform is deposited on whole workpiece.If carrying out PVD coatings, air supply system II is according to coating kind
Class is filled with different types of working gas, and the intermediate frequency power supply of magnetic control sputtering system VI applies a suitable voltage, gas by
Region near the nearly target of magnetic control sputtering system VI, which forms gas ionization zone and participates in reaction, forms coating, so workpiece is in order to obtain
Uniform coating is obtained, work, which transfers from one department to another system VII, should set a rational rotating speed.
8th, gas ionization situation and the color of coating can be checked in settling chamber I in deposition process by observation window 19 to sentence
Whether each deposition parameter that breaks has deviation, so as to be adjusted correspondingly.
9th, after depositing, settling chamber I is made to naturally cool to room temperature.
10th, vent valve 8 is opened in room I to be deposited after being cooled to room temperature, settling chamber I is recovered to normal pressure.
11st, sample is taken out.
If the 12, need to carry out Function Extension to whole equipment later, phase can be connected by expanded function spare interface 20
The functional module answered.
DLC deposition is carried out on monocrystalline silicon piece using the PCVD units in this equipment.
1）Silicon chip is positioned in cleaning fluid and is cleaned by ultrasonic 5min, is positioned over again after being washed with deionized water only ultrasonic in acetone
5min is cleaned, is positioned in equipment and is loaded on the tray in system after drying.
2）Settling chamber's door is closed, opens the valve of all water-cooling systems and air supply system, checks water-carrying capacity, temperature, gas
The indexs such as pressure.
3）Vacuumize.The pressure in settling chamber is evacuated within 10Pa in advance by sliding vane rotary pump and lobe pump first, then opened
Diffusion pump and corresponding valve are opened, the pressure in settling chamber is reached 5.0 × 10-3Pa。
4）Heating.Treat that pressure value reaches 5.0 × 10-3During Pa, heating system is opened, settling chamber and workpiece are heated,
It is set to be slowly heated to 400 DEG C.
5）Because PCVD need not be carried out under a high vacuum, so corresponding flapper valve is closed before gas is passed through, only
Deposition house vacuum is maintained by sliding vane rotary pump and lobe pump.
6）DLC is deposited.Deposition parameter is as follows：
Voltage：3000V
Frequency：2000Hz
Pulsewidth：5us
Air pressure：14Pa
Temperature：400℃
H2：1000sccm
Ar：50sccm
C2H2：150sccm
CH4：300sccm
Sedimentation time：1.5h
1）Cooling.After end to be coated, gas system, power-supply system and heating system are closed, makes settling chamber's natural cooling
To room temperature.
2）Analysis.Raman spectrum is present analysis DLC most intuitively analysis methods, by observing position and the intensity at peak,
Whether the coating that can determine whether to prepare is DLC, and substantially judges SP in coating2Key and SP3The ratio of key.By to Raman spectrogram
Analysis, it is determined that deposition coating be DLC coatings.
Claims (4)
1. prepare the industrial automation vapor deposition apparatus of DLC film, it is characterised in that by settling chamber（Ⅰ）, air supply system（Ⅱ）、
Vacuum system（Ⅲ）, heating system（Ⅳ）, water-cooling system（Ⅴ）, medium frequency magnetron sputtering system（Ⅵ）, workpiece high-voltage isulation clamping
System（Ⅶ）, electric control system（Ⅷ）And impulse modulation power-supply system（Ⅸ）Composition, air supply system（Ⅱ）By multichannel air inlet pipe
And flow controller composition, the air inlet of air inlet pipe are fixed on settling chamber（Ⅰ）Top, in deposition process, reacting gas is in electric field
In by exciting, ionizing, depositing on the surface of the workpiece, described vacuum system（Ⅲ）With settling chamber（Ⅰ）The bleeding point phase of rear side
Even, by diffusion pump（2）, mechanical pump（3）, lobe pump（4）, single-stage sliding vane rotary pump（5）, electronic grating valve（6）, vent valve（8）, high threshold
（7）, take out valve in advance（9）, maintain valve（10）, preceding step valve（11）, bypass valve（12）, high vacuum rule（13）, the 1st, 2,3 forevacuum ga(u)ges
（14）、（16）、（17）, thin-film electro content regulation（15）, reserved vacuum measurement mouth composition, bleeding point is through electronic grating valve（6）, respectively pass through
High threshold（7）, take out valve in advance（9）, bypass valve（12）With diffusion pump（2）, lobe pump（4）, single-stage sliding vane rotary pump（5）Connection, diffusion pump（2）
Respectively through maintaining valve（10）, preceding step valve（11）With mechanical pump（3）, lobe pump（4）Connection, is only needing the PCVD of relatively low vacuum
In deposition process, it is only necessary to single-stage sliding vane rotary pump（5）, lobe pump（4）, bypass valve（12）, take out valve in advance（9）, and pass through electronic grating
Valve（6）Control pumping speed can meet the needs of vacuum；During the PVD deposition of high vacuum is needed, then increase is needed to spread
Pump（2）, lobe pump（4）, single-stage sliding vane rotary pump（5）, preceding step valve（11）And high threshold（7）Collective effect, again by electronic grating valve
（6）Control pumping speed；1st, 2,3 forevacuum ga(u)ges（14）、（16）、（17）, high vacuum rule（13）, thin-film electro content regulation（15）For measuring
Settling chamber（Ⅰ）Air pressure；Mechanical pump（3）To maintain diffusion pump（2）In vacuum, prevent diffusion pump（2）In diffusion pump oil
Return oil, described heating system（Ⅳ）Using vacuum armouring heater strip（32）, and temperature probe is housed（33）, heater strip is into " U
Shape " is installed on settling chamber（Ⅰ）On the heater strip installing plate of inwall, double-deck liner plate is installed between heater strip and vacuum wall, with
Pollution when this is avoided coating to heater strip, during deposition, heater strip electrified regulation, heat is conducted by way of radiation to workpiece
On, make workpiece heat, described water-cooling system（Ⅴ）It is made up of 12 road water rows, water mining makes of stainless steel material, wherein four
Road water row's connection magnetic control sputtering system（Ⅵ）Target, four road water row's connection deposition chamber walls（Ⅰ）, water row connection impulse modulation all the way
Power-supply system（Ⅸ）, water, which is arranged, all the way connects medium frequency magnetron sputtering system（Ⅵ）Power supply, two path water row connection diffusion pump（2）, it is cold
But water can give each component to cool, and prevent each component from being burnt because temperature is too high, be connected to deposition chamber wall（Ⅰ）Cooling water may be used also
To adjust the temperature of workpiece in deposition process, so as to obtain the coating of different performance, medium frequency magnetron sputtering system（Ⅵ）It is to carry out
The system used during physical vapour deposition (PVD), it is made up of the medium frequency magnetron sputtering power supply with water cooling and sputtering target material, sputtering target material can
Unrestricted choice is carried out according to coat type, in deposition process, settling chamber connects the positive pole of shielding power supply, and target connects the negative of shielding power supply
Pole, after switching on power, gas is ionized into ion in the presence of electric field, and target atom is sputtered and is deposited on workpiece
Form coating, impulse modulation power-supply system（Ⅸ）Positive pole be connected to settling chamber（Ⅰ）On, negative electrode is connected on the workpiece for needing coating,
After switching on power, reacting gas by exciting, ionizing, depositing on the surface of the workpiece, forms coating, workpiece high pressure is exhausted in the electric field
Edge mounting and clamping system（Ⅶ）It is made up of rotating disk and driving motor, clamping workpiece is on rotating disk, by insulating materials by workpiece with depositing
Room（Ⅰ）Keep apart, electric control system（Ⅷ）By host computer（26）And programmable controller PLC（28）Composition, programmable control
Device PLC processed（28）Pass through input/output port（I/O）With vacuum meter（29）, impulse modulation power supply（30）, intermediate frequency magnetic control power supply
（31）, mass flowmenter stop valve（34）, mass flowmenter（35）, diffusion pump（2）, mechanical pump（3）, lobe pump（4）, single-stage rotation
Piece pump（5）, electronic grating valve（6）, vent valve（8）, high threshold（7）, take out valve in advance（9）, maintain valve（10）, preceding step valve（11）, bypass
Valve（12）, heater strip（32）Connection, temperature probe（32）With temperature controller（27）Connection, temperature controller（27）With host computer（26）Even
Connect, vacuum meter（29）With settling chamber（Ⅰ）Connection, mass flowmenter stop valve（34）, mass flowmenter（35）With air supply system
（Ⅱ）Multichannel air inlet pipe connection, programmable controller PLC（28）Pass through network and host computer（26）It is connected.
2. the industrial automation vapor deposition apparatus according to claim 1 for preparing DLC film, it is characterised in that quality stream
Gauge（35）Pass through Process FieldbusROFIBUS and programmable controller PLC（28）Connection, can manual controlling stream in coating procedure
Gauge（35）Setup parameter obtain needed for gas flow carry out the deposition of coating, or in advance in host computer（26）Operation circle
Input flow rate parameter automatic running on face,, will if there is flow to be unsatisfactory for by real-time detection flows numerical value during automatic running
To ask, equipment will carry out automatic alarm prompting and determine that " wait " state is closed or entered to equipment automatically according to actual conditions,
During into " wait " state, equipment other systems after problem exclusion, continue the heavy of coating still in normal operating conditions
Product.
3. the industrial automation vapor deposition apparatus according to claim 1 for preparing DLC film, it is characterised in that host computer
（26）Pass through modbus agreements and temperature controller（27）And temperature probe（33）It is connected, in coating procedure, temperature can be manually set
Degree carries out the deposition of coating, can also be in advance in host computer（26）Operation interface on input design temperature automatic running, automatically
In running, temperature controller（27）The temperature of lasting detection setting, if prompting automatic alarm beyond certain deviation.
4. the industrial automation vapor deposition apparatus according to claim 1 for preparing DLC film, it is characterised in that settling chamber
（Ⅰ）By 304 stainless steel material processing and fabricatings, using the double door of angle at a right angle（18）, complete machine overall dimensions 1500mm ×
1500mm × 2800mm, internal effectively working region size 1000mm × 1000mm × 1000mm, side wall are provided with observation window
（19）And expanded function spare interface（20）.
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| CN105441888A (en) * | 2015-12-08 | 2016-03-30 | 深圳市三鑫精美特玻璃有限公司 | Automatic control system for multifunctional continuous magnetron sputtering vacuum coating line |
| CN107142463B (en) * | 2017-04-27 | 2019-03-05 | 湖州金象科技股份有限公司 | A kind of coating method that plasma activated chemical vapour deposition is compound with magnetron sputtering or ion plating |
| EP3658702A1 (en) | 2017-07-26 | 2020-06-03 | Saint-Gobain Glass France | Temperable coatings comprising diamond-like carbon |
| WO2019020481A1 (en) | 2017-07-26 | 2019-01-31 | Saint-Gobain Glass France | Coating with diamond-like carbon by means of a pecvd magnetron method |
| CN110288867B (en) * | 2019-06-28 | 2022-03-04 | 徐州工业职业技术学院 | Simulation experiment device for detection and control of chemical production line |
| CN111676463B (en) * | 2020-06-11 | 2022-06-17 | 河北省激光研究所有限公司 | Method for depositing diamond coating on inner wall of annular workpiece |
| FR3124805B1 (en) | 2021-06-30 | 2024-03-22 | Saint Gobain | Substrate coated with at least one layer of diamond-like carbon protected by a temporary layer based on germanium or based on germanium oxide |
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