CN106929806A - High-barrier nano inorganic non-metallic film, its preparation method and vacuum winding filming equipment - Google Patents
High-barrier nano inorganic non-metallic film, its preparation method and vacuum winding filming equipment Download PDFInfo
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- CN106929806A CN106929806A CN201610938315.XA CN201610938315A CN106929806A CN 106929806 A CN106929806 A CN 106929806A CN 201610938315 A CN201610938315 A CN 201610938315A CN 106929806 A CN106929806 A CN 106929806A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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Abstract
The invention discloses a kind of high-barrier nano inorganic non-metallic film, its preparation method and vacuum winding filming equipment, including：Material to be deposited is positioned in the electron gun annular crucible of e type electron gun group evaporation coating devices；Flexible parent metal is arranged at the unwinding device of driving system for winding, and film path is walked according to winding and complete to wear film；Vacuum regulation and control to coating chamber, open driving system for winding and e type electron gun group evaporation coating devices, treat deposition material high temperature deposition, and evaporated film is formed with flexible parent metal surface, and e type electron gun groups are combined by least two e type electron guns and formed；The power of e type electron guns is 1~10kW.The arrangement mode launching electronics beam stood using the linear a line of e type electron guns or to dislocation in evaporation process of the invention, accelerate evaporation rate, improve the throughput rate of winding film plating, reduce production cost, it is often more important that obtain the nano inorganic nonmetal oxide high-isolation film of function admirable.
Description
Technical field
The present invention relates to technical field of vacuum plating, in particular to a kind of high-barrier nano inorganic non-metallic film,
Its preparation method and vacuum winding filming equipment.
Background technology
Inorganic non-metallic oxide such as silica (SiO2), aluminum oxide (Al2O3), titanium oxide (TiO2) etc., it is high as a class
Barrier material, with good barrier property, especially has excellent barrier to oxygen and vapor.It is above-mentioned that these are inorganic
Non pinetallic nano barrier material has more advantage, and such as it uses wider range, goes for refrigerating or directly heats, and
The microwave transparent of this kind of material preferably, can be directly used for heating using microwave；Inorganic non-metallic barrier layer has outstanding resistance toization
Medicine is learned, can be used for the packaging of the chemicals such as soda acid；Inorganic non-metallic high-isolation film material has the good transparency,
Content is high-visible, product introduction of being more convenient for；And high-barrier inorganic nano material can substitute conventional metallic aluminium barrier layer
Packing film material, reduces the use of metal material, with environment friendly and pollution-free.
The preparation method of the vacuum winding plated film of inorganic non-metallic oxide generally includes following several：Plasma chemistry
Vapour deposition winding film plating, magnetron sputtering coil film coating, high temperature evaporation winding film plating and ald winding film plating etc. wind
Plated film.Plasma activated chemical vapour deposition technique be by organosilane monomers (for example：HMDO HMDSO) and oxygen
Gas plasmaassisted effect under, in Plastic film surface cvd silicon oxide barrier layer, and in course of reaction produce by-product
Thing is discharged by vavuum pump.The advantage of the technique is the method for employing chemical vapor deposition, so silica barrier layer has
Preferable barrier property, and it is strong with the adhesive force of base material.And intermediate frequency or radio-frequency power supply, produced thermal effect are used in the technique
Should be relatively low, it is to avoid influence of the high temperature to plastic substrate film.But the technique there is also some defects, such as investment is higher, raw
Product is less efficient, and the speed of winding film plating is about 200m/min, is controlled in technical process in addition particularly critical, it is desirable to higher.
Magnetron sputtering coil film coating is mainly using under magnetic fields, and Ar Ions Bombardment inorganic non-metallics target material surface is generated
Inorganic Non-metallic Materials is deposited in Plastic film surface, and the major defect of this technique is relatively low sputter rate, winding film plating speed
Target material surface is easily enriched with electronics during degree is about 5m/min, and technical process, causes target material surface to be poisoned, and reduces sputtering strong
Degree, production efficiency is relatively low.
High temperature evaporation winding film plating, with aluminum oxide (Al2O3) as a example by, fed intake by the difference of metal aluminum filament and evaporate aluminium steam,
Reactive deposition process is in metallic aluminium evaporation process, oxygen gas transmission nozzle to be positioned over into evaporation region, and by plasma
Body assistant depositing, finally in plastic film substrate surface deposition of aluminium oxide barrier layer.Plating is wound in the reactive evaporation coating process
The speed of film is up to 500m/min, and aluminum oxide is generated using metal aluminum filament thermal evaporation and oxygen reaction, cost of raw material input compared with
Low, barrier film surface will not be presented pale yellow colored appearance, and operating efficiency suitable industrialized production higher, other techniques that compare set
Standby overall input is relatively low.But thermal evaporation reaction process process is difficult to control to, aluminum oxide barrier layer is intercepted due to its fragility, film layer
Performance is more sensitive to the dilatation of base film, and the barrier property of product is in medium level.
Above-mentioned winding film plating mode has barrier property when the inorganic non-metallic sull of high-barrier is prepared
Difference, the uneven defect such as not fine and close of film.Therefore, at present in the urgent need to there is a kind of new winding film plating mode, it can make
It is standby go out the preferable inorganic non-metallic oxide nano-film of barrier property.
The content of the invention
The present invention is intended to provide a kind of high-barrier nano inorganic non-metallic film, its preparation method and vacuum winding plated film
Equipment, it is only that the electron beam vacuum winding obtained using many e types electron gun combinations is deposited with, it is possible to prepared with excellent
The inorganic non-metallic oxidate nano high-isolation film of good barrier property, and the throughput rate of winding film plating is also improved, increase
Add economic benefit, reduce the input of production equipment cost.
To achieve these goals, the invention provides a kind of preparation method of high-barrier nano inorganic non-metallic film,
Comprise the following steps：Material to be deposited is positioned in the electron gun annular crucible of e type electron gun group evaporation coating devices；By flexible base
Material is arranged at the unwinding device of driving system for winding, and completes to wear film preparation according to winding film path；To coating chamber
Vacuum regulated and controled, and open driving system for winding and e type electron gun group evaporation coating devices, treating deposition material carries out high temperature
Evaporation, so that it forms evaporated film on flexible parent metal surface；Wherein, e types electron gun group is by least two e type electron guns
Combination is formed；The power of e type electron guns is 1~10kW；Preferably 4kW.
Further, e types electron gun group is applied in combination by 3~5 e type electron guns；It is preferred that being combined by 4 e type electron guns
Use, horizontal positioned when 4 e types electron guns are combined, linear a line arrangement；Or mutually contradictory Heterogeneous Permutation is in parallel four side
Shape is arranged.
Further, the step of vacuum to coating chamber regulates and controls includes：Using vacuum pump group, by the true of coating chamber
Reciprocal of duty cycle is evacuated to the required scope of technique evaporation；It is preferred that it is 3.0 × 10 to be evacuated to Vacuum Deposition-3Pa；Afterwards in the upper end of electron gun crucible
Input port is input into auxiliary discharge gas, and it is 3.5~6.5 × 10 to adjust the operating air pressure in coating chamber-2Pa；Preferably 5.0 ×
10-2Pa；The auxiliary discharge gas preferably oxygen that the electron gun is passed through when being deposited with；Temperature during evaporation is 1600~2100
℃；When material to be deposited is silica, it is 1600 DEG C to be preferably deposited with temperature；It is preferably to be deposited when material to be deposited is aluminum oxide
Temperature is 2100 DEG C.
Further, the electronic beam current of e types electron gun is 300~700mA, and voltage is -6.0~-9.0kV；Preferably 400
~600mA, voltage is -7.0~-8.0kV；More preferably electronic beam current is 500mA, and voltage is -7.8kV.
Further, after electron beam evaporation plating film, also including use ion gun to bombard the film after evaporation with
The step of improving evaporated film barrier property；The quantity of ion gun is identical with the quantity of e type electron guns；The auxiliary discharge of ion gun
Gas is argon gas；Preferably, operating voltage when ion gun bombards is 80~120V, and operating current is 3~6A；Further preferably
Operating voltage is 100V, and operating current is 5A.
Further, the winding speed of the driving system for winding is 10~200m/ minutes；Preferably 50~200m/ points
Clock；More preferably 100m/ minutes；Preferably, flexible parent metal is PET, PEN or PA plastic sheeting；The thickness of the flexible parent metal
It is 12 μm~125 μm；Preferably 50~90 μm.
According to another aspect of the present invention, a kind of high-barrier nano inorganic non-metallic film is additionally provided, it is using upper
Any one method is stated to be prepared from.
According to another aspect of the invention, a kind of vacuum winding filming equipment is additionally provided, for preparing high-barrier nano
Inorganic non-metallic film, it is characterised in that including：
Winding transmission device, it includes unwinding device and wrap-up, for by flexible parent metal since on unwinding device
Unreel, and be wound on wrap-up so that its surface at one with refrigeration axle is stretched out, exposed to the evaporating area of evaporation source
Domain；Cooling device, is arranged on region to be evaporated, and it has refrigeration axle, for being cooled down to the film after evaporation；E type electronics
Rifle group evaporation coating device, as evaporation source, the region to be evaporated lower section that it is arranged on evaporated film transmission route, for holding and adding
Heat material to be evaporated makes it be evaporated in evaporation region, and forms evaporated film on flexible parent metal surface；Ion source assisted
Device, is arranged on the rear of cooling device, for being bombarded the evaporated film after cooling to improve its barrier property；It is described
E type electron gun groups evaporation coating device is that multiple electron gun crucibles combine to be formed.
Further, e types electron gun group evaporation coating device is made up of 3-5 platform e type electron gun crucibles；More preferably by 4 e types electricity
Sub- rifle crucible composition；4 e type electron gun crucibles are horizontally arranged, and are arranged on the underface of evaporation region；Electron gun crucible is in line
Property a line or mutually contradictory dislocation parallelogram arrangement；The θ of deposition angles scope 2 of each e type electron gun be 30~
45 °, preferably 35 DEG C；The distance between adjacent e types electron gun is 350mm
Further, the upper end of electron gun crucible is provided with auxiliary discharge gas input port.
Beneficial effects of the present invention：
The electron beam evaporation winding evaporation process that the present invention is applied in combination using many e type electron guns, by many e type electronics
Such as 4 e type electron guns of rifle are placed horizontally at the underface of cooling device, to reach the maximum amount of evaporation, and are in by e type electron guns
Linear a line or parallelogram arrangement are deposited with, by the distance between adjacent e types electron gun, e types electron gun and flexibility
The angular range of vertical range and evaporation between base material is controlled in certain scope, and controls driving system for winding simultaneously
So that flexible parent metal to be deposited is limited within the specific limits Parameter Conditions when being deposited with certain speed rates, so that
Optimal evaporation is reached, the nano inorganic nonmetal oxide high-isolation film with good barrier properties energy is obtained.The evaporation side
E types electron gun launching electronics beam in the way of linear array is combined is used in method, the steaming of Inorganic Non-metallic Materials is not only accelerated
Plating speed, improves the throughput rate of winding film plating, also reduces the input of production equipment cost, increased economic benefit.
Brief description of the drawings
Fig. 1 is coil film coating apparatus schematic diagram according to an exemplary embodiment of the present invention；
Fig. 2 is the structural representation of evaporated film when 4 electron guns are horizontally arranged in the embodiment of the present invention；
Fig. 3 is evaporation in electron gun crucible when inorganic non-metal composite material film is deposited with embodiments of the invention 3
The structural representation of material arrangement.
Specific embodiment
Technical scheme is described in detail below by way of exemplary specific embodiment.But should not be by these
Embodiment is construed to limiting the scope of the invention.All technologies realized based on the above of the present invention are encompassed by this
Invention is intended in the range of protection.
Unless otherwise indicated, raw material described in embodiment and reagent are commercially available prod.
Electron gun use magnetic biasing it is rotatable (e shapes rifle), due to electron beam flexing path proximity e fonts, can be divided into 180 DEG C and
270 DEG C two kinds, its basic structure is divided into filament cathode, anode, focusing electrode, permanent magnet, field coil and crucible etc. six
Point, thermoelectron is disengaged by the negative electrode tungsten filament of hyperpyrexia, and the high voltage electric field using negative electrode and front anode accelerates, and line focus extremely gathers
Bunchy pass through centre bore, the magnetic field that field coil is formed then can flexing electron beam the direction of motion, be allowed to bend to material to be plated
Material surface.Due to there is an externally-applied magnetic field, crucible receives this magnetic fields to this structure with the secondary electron produced by evaporation source material,
Can deflect and be absorbed by diversion, can so reduce the influence caused by secondary electron, the deflection of electron beam is main by magnetic
The electric current of field coil is manipulated, and the size for changing magnetic field is the position that movable electronic beam bombards material surface X-direction, if add
Y-direction magnetic field then can simultaneously make the planar graph scanning in the directions of XY two, it is to avoid material borehole phenomenon, and can uniform construction store
Material.
As Figure 1-3, the invention provides a kind of winding film plating equipment, it is used to prepare the inorganic non-gold of high-barrier nano
Category film.The winding film plating equipment include driving system for winding, e type electron gun groups evaporation coating device 40, cooling device 50 and from
Component assistant depositing device 60.Wherein, winding transmission device includes unwinding device 10, wrap-up 20 and the biography for controlling
Dynamic device, by transmission device so that flexible parent metal 30 is unreeled and wound.One end of flexible parent metal 30 is arranged on and unreels dress
To put start on 10 and unreel, be transmitted by the deflector roll 70 of transmission device, come in the refrigeration axle surface extension of cooling device 50,
Exposed to the evaporation region of evaporation source, that is, enter into the evaporation region positioned at the top of e type electron gun groups evaporation coating device 40.It has been deposited with
Wound into wrap-up 20 into the rear deflector roll 70 by transmission device.
E type electron gun groups evaporation coating device 40 is arranged on the lower section of the cooling device 50 of film transmission route, for holding and
Heating material to be evaporated makes it be evaporated in evaporation region, and evaporated film layer is formed on the surface of flexible parent metal 30.E type electron guns
Group evaporation coating device 40 can be combined to be formed by multiple electron gun crucibles.Electron gun crucible horizontal positioned, it can be linear group
The mode of conjunction is evaporated, for example, arrange in a row；Can also be placed in the way of mutually contradictory dislocation, such as be in parallel four side
The mode of shape is deposited with.
The scope of deposition angles can be entered according to the height of the vertical range between electron gun and the refrigeration axle of cooling device
Row regulation.Angle when representing evaporation with θ between edge electronic beam and vertical curve, then when electron gun crucible is with linear combination,
The θ of deposition angles scope 2 of each e type electron gun is 30~45 °, preferably 35 DEG C；And the distance between adjacent electron gun is
350mm.It is preferred that vaporising device 40 is 3-5 platform e type electron gun crucibles；More preferably 4 e type electron gun crucibles.
The present invention using four e type electron gun horizontal positioneds and arrangement in a row, and by the spacing between adjacent electronics rifle,
The θ of deposition angles scope 2 of electron gun is limited within the specific limits, so as to possess evaporation wide cut greatly, the advantage such as process stabilizing.It is whole
Individual technical process is simple, easy and safe to operate, volume when can be deposited with by the transmission power and then control that regulate and control e type electron guns
Around speed, and then regulate and control thickness of the nano inorganic Nonmetal barrier layer on the surface of flexible parent metal 30, obtain to oxygen and vapor
Barrier layer with preferable barrier, while also achieving serialization evaporation production, opens e types electron gun in winding
The coating process field of plated film and inorganic non-metallic oxide.
Present invention also offers a kind of preparation method of high-barrier nano inorganic non-metallic film, it is using above-mentioned volume
It is deposited with around filming equipment.Electron beam evaporation winding film plating of the invention is using solid oxygen SiClx or aluminum oxide as evaporation material
Material, is heated by e type electron guns and flashes to gaseous state, after evaporating afterwards in the presence of cooling device, in the table of flexible parent metal
Face deposits, generation transparent inorganic nanometer barrier layer.The raw material and organic monomer material phase being deposited with using electron gun evaporation process
Compare more cheap, plated film efficiency high, barrier layer has preferable barrier property.
Specifically, winding evaporation process is realized in：The cooling device of film route is walked in driving system for winding first
50 lower section, places the e type electron guns of linear a line arrangement or mutually contradictory Heterogeneous Permutation as needed, is put in plated film rear end
Put same amount of ion gun.Complete after winding wears the preparation of film, to add to be deposited inorganic non-in electron gun crucible
The addition of metal material, such as silica or aluminum oxide, or both interval, closes vacuum chamber, and vacuum equipment is vacuumized.
After reaching setting technique vacuum, start winding film plating transmission system, after the winding speed of flexible parent metal reaches setting speed,
E type electron gun power supplys are opened, after stabilization to be deposited, the baffle plate above e type electron guns, the flexible base being wound through to top is opened
Material carries out the evaporation of nano inorganic nonmetal oxide thin-film material.Open the ion gun of film path rear end simultaneously, to being steamed
The film of plating is bombarded.Vacuum to coating chamber regulates and controls, and opens driving system for winding and electron gun emission system,
Treating deposition material carries out high temperature plating, so that it forms evaporated film layer on flexible parent metal surface.
E types electron gun group of the present invention can be combined by least two e type electron guns.Wherein, e types electron gun
Power be 1~10kW, preferably 4kW.According to the present invention, e types electron gun can be combined by 3~5 e type electron guns
Use.More preferably it is applied in combination by 4 e type electron guns.Horizontal positioned when 4 e types electron guns are combined, linear a line or
Mutually contradictory dislocation parallelogram arrangement, such as 4 e types electron guns form parallelogram arrangement.
According to the present invention, the electronic beam current of e type electron guns is 300~700mA, and voltage is -6.0~-9.0kV.It is preferred that e types
The electronic beam current of electron gun is 400~550mA, and voltage is -7.0~-8.0kV.More preferably electronic beam current be 500mA, voltage for-
7.8kV.The present invention is by accurately controlling the electronic beam current and voltage of electron gun, so that regulate and control the evaporation rate of deposition material,
To avoid the evaporation rate of material to be deposited too fast, if evaporation rate is too fast, the particle of evaporated film can be caused larger,
There is more crackle in evaporated film, so as to the barrier property of nano inorganic nonmetal film can be reduced.By regulating and controlling electron beam
Stream and voltage so that evaporation power and speed are maintained in certain scope, so as to obtain, particle is smaller and arrangement is fine and close, table
The less evaporated film of surface roughness, improves the barrier property of nano inorganic nonmetal film.
Include according to the present invention, the step of the vacuum to coating chamber regulates and controls：Using vacuum pump group, by coating chamber
Vacuum is evacuated to the required scope of technique evaporation；It is preferred that it is 3.0 × 10 to be evacuated to Vacuum Deposition-3Pa.Afterwards in the upper of electron gun crucible
End input port input auxiliary discharge gas, and it is 3.5~6.5 × 10 to adjust the operating air pressure in coating chamber-2Pa；Preferably 5.0
×10-2Pa.Wherein, the auxiliary discharge gas preferably oxygen being passed through when electron gun is deposited with.It is such as straight because beam energy is higher
Silica anoxic can be caused when connecing evaporation silica, oxygen is passed through and is enabled to deposition material to aoxidize, it is ensured that in flexible parent metal
Surface deposition is silicon oxide film.Temperature during evaporation is 1600~2100 DEG C.When material to be deposited is silica, preferably
Evaporation temperature is 1600 DEG C；When material to be deposited is aluminum oxide, temperature preferably to be deposited is 2100 DEG C.
The evaporation radiation scope of every e type electron guns of the invention in 300-350mm or so, using many e type electron guns
It is applied in combination the need for disclosure satisfy that big wide cut plated film.Evaporation particle when the present invention is applied in combination using e type electron guns is abundant
Ionization, the nano film material better quality for being deposited, film layer is finer and close, with more preferable barriering effect.
In a preferred embodiment of the invention, the winding speed of driving system for winding is 10~200m/ minutes；Preferably 50
~200m/ minutes；More preferably 100m/ minutes.Flexible parent metal of the present invention can be thin for PET, PEN or PA plastics
Film.The thickness of general flexible parent metal is 12 μm~125 μm；Preferably 50~90 μm.
According to the present invention, after evaporated film, the step of also bombardment the film after evaporation including use ion gun.
The quantity in preferred ion source is identical with the quantity of e type electron guns.The auxiliary discharge gas of ion gun is argon gas.The present invention is by adopting
The sull after evaporation is bombarded with ion gun, the purpose is to pass through energetic ion source bombardment film layer, can be by film
The loose structure compacting of layer surface is fine and close, and can refine bulky grain, the roughness on evaporated film surface is reduced, so as to carry
Evaporated film surface soundness high, plays the effect for improving barrier property.
According to the present invention, operating voltage when ion gun bombards is preferably 80~120V, and operating current is preferably 3~6A.
Further preferred operating voltage is 100V, and operating current is 5A.
Embodiment 1
During aluminum oxide deposition particle uniformly made an addition into electron gun annular crucible, and adjust electron gun adjacent during evaporation
The distance between be 350mm.The PET coiled materials of 12 μ m-thicks are positioned at the unreeling shaft of unwinding device, and according to winding Zou Mo roads
Footpath completes to wear film preparation.Plated film vacuum chamber is closed, prepares to vacuumize.
When the vacuum in plated film vacuum chamber reaches 5.0 × 10-3During Pa base vacuums, by electron gun crucible upper end oxygen
Input port is input into oxygen, regulation plated film operating air pressure to 5.0 × 10-2Pa.The work of e types electron gun is opened, electronic beam current is
550mA, voltage is -8.0kV, and about 2100 DEG C of evaporations of high temperature are carried out to aluminum oxide deposition particle.Open driving system for winding, setting
When the winding speed of driving system for winding is 100m/min, e type electron gun upper guard-plates are opened after evaporation stabilization so that e types electricity
The θ of deposition angles scope 2 of sub- rifle is 35 DEG C, carries out the evaporation of nano aluminium oxide Inorganic Non-metallic Materials.
After the completion of evaporation, in film transmission path rear end, ion gun setting operating current 5A, voltage 100V, after evaporation
Membranous layer of silicon oxide bombarded, to improve film quality.The nano oxygen of 12 μ m-thick PET films is carried out according to above-mentioned technological parameter
Change aluminium inorganic non-metallic Oxide Electron beam evaporation.
Embodiment 2
During silica deposition particle uniformly made an addition into electron gun annular crucible, and adjust e types electricity adjacent during evaporation
The dislocation of sub- rifle interval is placed, and the distance between adjacent electronics rifle is 350mm.The PET coiled materials of 12 μ m-thicks are positioned over and unreel dress
At the unreeling shaft put, and complete to wear film preparation according to winding film path.Vacuum chamber is closed, prepares to vacuumize.
Vacuum reaches 5.0 × 10-3During Pa base vacuums, oxygen is input into by electron gun crucible upper end oxygen input port,
Adjust plated film operating air pressure to 5.0 × 10-2Pa.The work of e types electron gun is opened, electronic beam current is 500mA, and voltage is -7.8kV,
1600 DEG C of high temperature deposition is carried out to silica deposition particle.Driving system for winding is opened, the winding of driving system for winding is set
When speed is 100m/min, e type electron gun upper guard-plates are opened after evaporation stabilization so that the deposition angles scope 2 of e type electron guns
θ is 35 DEG C, carries out the evaporation of nano silicon oxide inorganic non-metallic high-isolation film.
After the completion of evaporation, in film transmission path rear end, ion gun setting operating current 5A, after voltage 100V is to evaporation
Membranous layer of silicon oxide is bombarded, and improves film quality.The nano silicon oxide of 12 μ m-thick PET films is carried out according to above-mentioned technological parameter
Inorganic non-metallic Oxide Electron beam is deposited with.
Embodiment 3
The placement as shown in figure 3, the electron gun crucible group that will be placed with particle silica to be deposited and aluminum oxide is in line,
And the distance between electron gun adjacent during evaporation is adjusted for 350mm.The PET coiled materials of 12 μ m-thicks are positioned over and unreel place, and
Film path is walked according to winding to complete to wear film preparation.Vacuum chamber is closed, prepares to vacuumize.
When the vacuum in plated film vacuum chamber reaches 5.0 × 10-3During Pa base vacuums, by electron gun crucible upper end oxygen
Input port is input into oxygen, regulation plated film operating air pressure to 5.0 × 10-2Pa.The work of e types electron gun is opened, the e types of aluminum oxide are deposited with
The electronic beam current of electron gun is 550mA, and voltage is -8.0kV, and the electronic beam current for being deposited with the e type electron guns of silica is 500mA,
Voltage is -7.8kV.1600 DEG C of high temperature deposition is carried out to silica deposition particle, 2100 DEG C are carried out to aluminum oxide deposition particle
High temperature deposition.
Driving system for winding is opened, when setting the winding speed of driving system for winding as 100m/min, is beaten after evaporation stabilization
Open e type electron gun upper guard-plates so that the θ of deposition angles scope 2 of e type electron guns is 35 DEG C, carries out nano silicon oxide/aluminum oxide
The evaporation of material.
After the completion of evaporation, in film transmission path rear end, ion gun setting operating current 5A, voltage 100V, after evaporation
Silica/alumina composite film layer bombarded, to improve film quality.12 μ m-thicks are carried out according to above-mentioned technological parameter
The nano silicon oxide inorganic non-metallic Oxide Electron beam evaporation of PET film.
Embodiment 4
Its preparation method is same as Example 3, and difference is in the embodiment 4 after the completion of evaporation, not thin
The rear end of film transmission path uses ion gun to be bombarded silica/alumina composite film layer to improve film quality.
Table 1
Note：The PET original film OTR oxygen transmission rates of 12 μ m thicks are 130cc/m2.day, moisture-vapor transmission is 40g/m2.day；
Test condition：OTR：25 DEG C, RH 0%, WVTR：38 DEG C, RH90%.
From the result of embodiments of the invention 1-3, evaporated device is wound by multigroup e types electron beam of the invention and is steamed
Plating silica or aluminum oxide or silica/alumina as nano inorganic Nonmetal barrier thin-film material, obtain with compared with
The evaporated film of good barrier property, its product meets conventional packaging barrier.Can be substantially from the data in table 1
Go out, either the single silica material in embodiment 1 in single alumina material or embodiment 2, obtained after its evaporation
Not as the composite alumina/silicon oxide film in embodiment 3, illustrate to be prepared using this method is had barrier layer properties
The composite film layer of more preferable oxygen and vapor water barriers performance.
Compared with comparative example 1, the laminated film after evaporation is bombarded as a result of ion gun in embodiment 4, led to
Cross ion gun bombardment can silica/alumina evaporation on further ionization evaporation particle, bombardment evaporated film layer, ram
Real evaporated film layer, thinning film layer particle so that the film compactness of deposition more preferably, further increases barrier property.
The above, is only several embodiments of the application, any type of limitation is not done to the application, although this Shen
Please disclosed as above with preferred embodiment, but and be not used to limit the application, any those skilled in the art are not taking off
In the range of technical scheme, make a little variation using the technology contents of the disclosure above or modification is equal to
Effect case study on implementation, belongs in the range of technical scheme.
Claims (10)
1. a kind of preparation method of high-barrier nano inorganic non-metallic film, it is characterised in that comprise the following steps：
Material to be deposited is positioned in the electron gun annular crucible of e types electron gun group evaporation coating device (40)；
Flexible parent metal (30) is arranged at unwinding device (10) place of driving system for winding, and film path is walked according to winding and complete to wear
Film preparation；
Vacuum to coating chamber regulates and controls, and opens driving system for winding and e types electron gun group evaporation coating device (40), treats
Deposition material carries out high temperature deposition, so that it forms evaporated film on the flexible parent metal (30) surface；
Wherein, e types electron gun group is to be combined to be formed by least two e type electron guns；The power of the e types electron gun be 1~
10kW；Preferably 4kW.
2. preparation method according to claim 1, it is characterised in that e type electron gun groups are combined by 3~5 e type electron guns
Use；It is preferred that being applied in combination by 4 e type electron guns, horizontal positioned when 4 e types electron guns are combined, linear a line arrangement
Or mutually contradictory dislocation parallelogram arrangement.
3. preparation method according to claim 1, it is characterised in that the step of vacuum to coating chamber regulates and controls wraps
Include：
Using vacuum pump group, the scope needed for the vacuum of coating chamber is evacuated into technique evaporation；It is preferred that be evacuated to Vacuum Deposition for 3.0 ×
10-3Pa；
Auxiliary discharge gas is input into the upper end input port of electron gun crucible afterwards, and adjusts the operating air pressure in coating chamber and be
3.5~6.5 × 10-2Pa；Preferably 5.0 × 10-2Pa；The auxiliary discharge gas preferably oxygen that the electron gun is passed through when being deposited with
Gas；
The temperature during evaporation is 1600~2100 DEG C；When material to be deposited is silica, it is 1600 DEG C to be preferably deposited with temperature；
When material to be deposited is aluminum oxide, temperature preferably to be deposited is 2100 DEG C.
4. preparation method according to claim 1, it is characterised in that the electronic beam current of the e types electron gun is 300~
700mA, voltage is -6.0~-9.0kV；Preferably 400~600mA, voltage is -7.0~-8.0kV；More preferably electronic beam current is
500mA, voltage is -7.8kV.
5. preparation method according to claim 1, it is characterised in that after electron beam evaporation plating film, also including using from
The step of component is bombarded the film after evaporation to improve evaporated film barrier property；The quantity of the ion gun with it is described
The quantity of e type electron guns is identical；The auxiliary discharge gas of the ion gun is argon gas；When preferably, the ion gun bombards
Operating voltage is 80~120V, and operating current is 3~6A；Further preferred operating voltage is 100V, and operating current is 5A.
6. preparation method according to claim 1, it is characterised in that
The winding speed of the driving system for winding is 10~200m/ minutes；Preferably 50~200m/ minutes；More preferably
100m/ minutes；
Preferably, the flexible parent metal (30) is PET, PEN or PA plastic sheeting；The thickness of the flexible parent metal (30) is 12 μ
M~125 μm；Preferably 50~90 μm.
7. a kind of high-barrier nano inorganic non-metallic film, it is characterised in that it is the side using any one of claim 1-6
Method is prepared from.
8. a kind of vacuum winding filming equipment, for preparing high-barrier nano inorganic non-metallic film, it is characterised in that including：
Winding transmission device, it includes unwinding device (10) and wrap-up (20), for by flexible parent metal (30) from unreeling dress
To put start on (10) and unreel, and be wound on wrap-up (20) so that its surface at one with refrigeration axle is stretched out, and is exposed
In the evaporation region of evaporation source；
Cooling device (50), is arranged on region to be evaporated, and it has refrigeration axle, for being cooled down to the film after evaporation；
E types electron gun group evaporation coating device (40), used as evaporation source, it is arranged under the region to be evaporated of evaporated film transmission route
Side, makes it be evaporated in evaporation region, and evaporation is formed on flexible parent metal (30) surface for holding and heating material to be evaporated
Film；
Ion source assisted device (60), is arranged on the rear of the cooling device (50), for thin to the evaporation after cooling
Film is bombarded to improve its barrier property；
E types electron gun group evaporation coating device (40) to be formed for multiple electron gun crucibles are combined.
9. vacuum winding filming equipment according to claim 8, it is characterised in that the e types electron gun group evaporation coating device
(40) it is made up of 3-5 platform e type electron gun crucibles；More preferably it is made up of 4 e type electron gun crucibles；4 e types electron gun earthenwares
Crucible is horizontally arranged, and is arranged on the underface of evaporation region；
Described linear a line of electron gun crucible or mutually contradictory dislocation parallelogram are arranged；Each e type electron gun
The θ of deposition angles scope 2 is 30~45 °, preferably 35 DEG C；The distance between adjacent e types electron gun is 350mm.
10. vacuum winding filming equipment according to claim 8, it is characterised in that the upper end of the electron gun crucible sets
It is equipped with auxiliary discharge gas input port.
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| CN109817732A (en) * | 2018-12-19 | 2019-05-28 | 北京铂阳顶荣光伏科技有限公司 | A method and device for preparing copper indium gallium selenide thin film battery |
| CN112247153A (en) * | 2020-10-12 | 2021-01-22 | 内蒙古碳谷科技有限公司 | Preparation method of metal-fullerene composite nano powder |
| CN114657516A (en) * | 2020-12-23 | 2022-06-24 | 山东浪潮华光光电子股份有限公司 | Method for evaporating thick chromium metal layer by using single crucible |
| CN115198245A (en) * | 2022-07-18 | 2022-10-18 | 浙江弘康半导体技术股份有限公司 | Oxide high-barrier film, preparation method and vacuum winding coating equipment |
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| CN115584473A (en) * | 2022-11-02 | 2023-01-10 | 广东振华科技股份有限公司 | A double-sided electron beam evaporation roll-to-roll coating device and its application method |
| CN116043173A (en) * | 2023-03-31 | 2023-05-02 | 山东永聚医药科技有限公司 | Preparation method and application of vacuum silicon oxide plated ultrathin polyester film material |
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